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Additive Manufacturing for the

Aerospace Industry
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Additive Manufacturing
for the Aerospace
Industry

Edited by

Francis Froes
Light Metals Industry, Tacoma, WA,
United States
Advanced Materials Industries, Tacoma,
WA, United States

Rodney Boyer
RBTi Consulting, Bellevue, WA, United States
School of Materials Science and Engineering,
University of Shanghai for Science and
Technology, Shanghai, P.R. China
Elsevier
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Contents

List of Contributors xiii

1 Introduction to aerospace materials requirements and the role


of additive manufacturing 1
Francis Froes, Rodney Boyer and B. Dutta
1.1 Aerospace materials and their requirements 1
1.2 Additive manufacturing 1
1.3 Additive manufacturing fabrication of various types of materials 3
1.4 Contents of this book 6
References 6

2 Review of additive manufacturing technologies and applications


in the aerospace industry 7
Joel C. Najmon, Sajjad Raeisi and Andres Tovar
2.1 Aerospace requirements and opportunities for additive
manufacturing 7
2.1.1 Design requirements 8
2.1.2 Manufacturing capabilities and benefits 10
2.2 Additive manufacturing technologies 12
2.2.1 Additive metal technologies 12
2.2.2 Additive nonmetal technologies 14
2.3 Additive manufacturing applications 17
2.3.1 Direct digital manufacturing 18
2.3.2 Rapid tooling 19
2.3.3 Rapid prototyping 19
2.3.4 Repair 20
2.4 Challenges and potential future applications 22
2.4.1 Challenges 22
2.4.2 Potential future applications 23
References 24

3 Qualification and certification of metal additive manufactured


hardware for aerospace applications 33
Richard Russell, Douglas Wells, Jess Waller, Behrang Poorganji,
Eric Ott, Tsuyoshi Nakagawa, Hector Sandoval, Nima Shamsaei
and Mohsen Seifi
3.1 Introduction 33
vi Contents

3.2 Special considerations for fracture-critical hardware 37


3.3 Current qualification and certification state-of-the-art and gap
analysis 39
3.3.1 Standardization gaps related to qualification and
certification 39
3.3.2 Recent directions in qualification, certification,
and quality control for additive manufacturing 40
3.4 Industry qualification and certification approaches 43
3.4.1 General Electric qualification and certification approach 43
3.4.2 Lockheed Martin qualification and certification approach 49
3.5 Government agency approaches 51
3.5.1 National aeronautics and space administration
qualification and certification approach 51
3.5.2 Federal Aviation Administration qualification and
certification approach 60
3.6 Summary and recommendations 61
Acknowledgments 62
References 62

4 Design for metal additive manufacturing for aerospace applications 67


Manish Kamal and Gregory Rizza
4.1 Introduction 67
4.2 Methods and approaches 68
4.2.1 Topological optimization 68
4.2.2 Part consolidation 71
4.2.3 Part integration and repair 72
4.2.4 Other techniques 73
4.3 Process aspects of design 74
4.3.1 Part performance 74
4.3.2 Part quality 78
4.3.3 Part evaluation: in-situ and after process nondestructive
evaluation (NDE) 79
4.3.4 Post processing 80
4.4 Cost considerations 81
4.5 Product and process design tools 82
4.5.1 Additive manufacturing design software 83
4.5.2 Additive manufacturing process software 83
4.6 Conclusions 84
Acknowledgments 84
References 85

5 Structure formation in A.M. processes of Titanium


and Ni-base alloys 87
I.S. Polkin, S.V. Skvortsova, G.A. Turichin and M.B. Novikova
5.1 Evaluation of the structure of powder particles of different sizes 89
Contents vii

5.2 A dependence of the microstructure of powder particles


in the initial state on their size 92
5.3 Determination of changes in the structure using samples
produced by different additive technologies 93
5.4 Testing of mechanical properties of samples of parts produced
by direct metal deposition and selective laser melting 95
5.5 Conclusions 97
Acknowledgement 97
Reference 97
Further reading 98

6 Measurement of powder characteristics and quality for additive


manufacturing in aerospace alloys 99
Thomas F. Murphy and Christopher T. Schade
6.1 Introduction 99
6.2 Quality control measurements 99
6.2.1 Particle size and distribution 99
6.2.2 Apparent density and flow 101
6.2.3 Tap density 105
6.2.4 Moisture analysis 106
6.2.5 Inclusion analysis 108
6.2.6 Shape factor 110
6.2.7 Porosity 111
6.3 Advanced metallographic techniques 113
6.3.1 Background 114
6.3.2 Metallographic sample preparation 117
6.3.3 Light optical microscopy—automated image analysis 122
6.3.4 Shape and texture analysis 124
6.3.5 Microstructural analysis 135
6.3.6 Chemical analysis 136
References 140

7 The processing and heat treatment of selective laser melted


Al-7Si-0.6Mg alloy 143
Jeremy H. Rao, Paul Rometsch, Xinhua Wu and Chris H.J. Davies
7.1 Selective laser melted Al alloy A357 143
7.1.1 Process control 143
7.1.2 Density optimization 145
7.2 Post selective laser melting heat treatment 150
7.2.1 Tensile properties 150
7.2.2 Fractography 151
7.3 Refinement of laser melting and postprocessing parameters 153
7.3.1 The selection of optimized heat treatment parameters 153
7.3.2 The selection of optimized laser parameters 153
7.3.3 Tensile properties 155
7.3.4 Fractography 156
viii Contents

7.4 Conclusions 157


Acknowledgments 158
References 158

8 Superalloys, powders, process monitoring in additive


manufacturing 163
Kevin Minet, Ankit Saharan, Anja Loesser and Niko Raitanen
8.1 Applications: materials in gas turbines 164
8.2 Material and processing challenges in additive manufacturing
of superalloys and different approaches for solutions 169
8.2.1 Challenges with additive manufacturing—theory
on weldability issues 169
8.2.2 Solidification cracking 170
8.2.3 Liquation cracking (HAZ) 171
8.2.4 Strain-age cracking 172
8.2.5 Ductility dip cracking 173
8.3 Powder material properties 174
8.4 Process monitoring 177
8.4.1 Quality assurance in AM 177
8.4.2 Challenges with tradition postprocess inspection
techniques 179
8.4.3 Novel QA approaches 179
8.5 Sensor types for in situ process monitoring 179
8.5.1 Optical in situ process monitoring systems for AM 179
8.6 Quality assurance tie-in 181
8.7 Defect data correlation automated, future closed-loop control
possibilities 182
References 185

9 Fusion and/or solid state additive manufacturing for aerospace


applications 187
James C. Withers
9.1 Introduction 187
9.2 Experimental examples 198
References 210
Further reading 211

10 Profile electron beam 3D metal printing 213


Dmytro Kovalchuk and Orest Ivasishin
Summary 231
References 232

11 Additive manufacturing of titanium aluminides 235


Wei Chen and Zhiqiang Li
11.1 Applications of TiAl 235
11.2 Fundamentals of TiAl 236
Contents ix

11.3 Processings of TiAl 237


11.3.1 Casting 237
11.3.2 Wrought processing 238
11.3.3 Powder metallurgy 239
11.3.4 Additive manufacturing 240
11.4 Laser metal deposition of TiAl 240
11.5 Selective laser melting of TiAl 245
11.6 Electron beam melting of TiAl 248
11.7 Summary and prospects 256
References 258
Further reading 263

12 Aerospace applications of the SLM process of functional


and functional graded metal matrix composites based
on NiCr superalloys 265
Shishkovsky Igor
12.1 Introduction 265
12.2 Metal matrix composites fabrication via additive technologies 266
12.3 Metal matrix composites on the nickel alloy based 268
12.4 Methods and materials 269
12.5 Results and discussion 270
12.6 Conclusions 276
Acknowledgments 276
References 276
Further reading 281

13 Surface roughness and fatigue properties of selective laser


melted Ti6Al4V alloy 283
Zhuoer Chen, Sheng Cao, Xinhua Wu and Chris H.J. Davies
13.1 Introduction 283
13.1.1 Surface roughness of selective laser melted metallic
components 283
13.1.2 Post-selective laser melting surface treatment 285
13.1.3 Fatigue performance of selective laser melted
Ti6AL4V 286
13.2 Experimental procedure 286
13.2.1 Material 286
13.2.2 Selective laser melting of Ti6Al4V specimens 286
13.2.3 Surface roughness measurements 288
13.2.4 Postselective laser melting heat treatment of fatigue
samples 288
13.2.5 Fatigue testing 288
13.3 Results and discussion 289
13.3.1 Surface roughness 289
13.3.2 Fatigue properties 293
x Contents

13.4 Conclusions 297


References 298

14 Aluminum alloys for selective laser melting  towards improved


performance 301
Paul Rometsch, Qingbo Jia, Kun V. Yang and Xinhua Wu
14.1 Introduction 301
14.2 Processingmicrostructureproperty considerations
for current alloys in selective laser melting 302
14.3 Alloy and process design for improved performance 310
14.3.1 Design of new alloys for selective laser melting 311
14.3.2 Adaptation of existing high strength alloys
for selective laser melting 316
14.3.3 Development of composite materials for selective
laser melting 319
14.4 Summary and outlook 321
Acknowledgments 322
References 322

15 Additive aerospace considered as a business 327


Lawrence Gasman
15.1 3D printing technologies for tooling and prototyping 328
15.2 Factors driving additive manufacturing in the aerospace
industry 328
15.2.1 Weight reduction 328
15.2.2 Additive manufacturing and improved aircraft design 329
15.2.3 Software as a limiting factor on additive manufacturing
aerospace 329
15.3 How additive manufacturing is improving the supply chain
the aerospace industry 330
15.3.1 Service providers 330
15.3.2 Siemens 330
15.3.3 SAP 331
15.4 Materials for additive manufacturing aerospace 331
15.4.1 Metals 331
15.4.2 Directed energy deposition 333
15.4.3 Polymers 334
15.4.4 Polymer bed fusion 336
15.4.5 Composites 337
15.5 Regulatory factors in additive manufacturing aerospace 338
15.5.1 Europe 339
15.5.2 United States 339
15.6 The geography of additive manufacturing aerospace 339
15.7 Competitive implications of additive manufacturing aerospace 340
Contents xi

16 Surface texture characterization and optimization of metal


additive manufacturing-produced components for aerospace
applications 341
Agustin Diaz
16.1 Introduction 341
16.1.1 The basics of additive manufacturing surface texture 341
16.1.2 Surface anatomy of additive manufacturing components 342
16.2 Best practices for surface texture characterization of additive
manufacturing components 345
16.2.1 Introduction 345
16.2.2 Brief surface texture review 345
16.2.3 Surface texture characterization of additive
manufacturing components 349
16.3 Surface finishing of additive manufacturing components 355
16.3.1 Introduction 355
16.3.2 Basics of surface finishing to take into account
before printing 356
16.3.3 Surface finishing of additive manufacturing components 358
16.4 Additive manufacturing-built components surface-finished
by the Extreme ISF Process 361
16.4.1 Introduction 361
16.4.2 Examples of surface treated by the Extreme ISF Process 362
16.4.3 Improvement of the mechanical properties of additive
manufacturing-built components by Extreme
ISF Process 364
16.4.4 Further analysis of surface texture parameters
associated with mechanical performance 365
16.5 Conclusions 367
16.6 Corollary 367
Acknowledgments 371
References 371

17 Developing and applying ICME 1 modeling tools to predict


performance of additively manufactured aerospace parts 375
Brain W. Martin, Thomas K. Ales, Matthew R. Rolchigo
and Peter C. Collins
17.1 Introduction 375
17.2 Part 1: Process modeling 379
17.3 Part 2: Predicting chemistry 384
17.3.1 Solute loss (vaporization) or pickup (gettering) 385
17.3.2 Solidification partitioning 386
17.4 Part 3: Predicting microstructure 387
17.5 Part 4: Predicting properties and performance 391
17.6 Limitations 393
17.7 Summary 395
References 396
xii Contents

18 Nondestructive evaluation of additively manufactured metallic


parts: in situ and post deposition 401
Lucas W. Koester, Leonard J. Bond, Hossein Taheri
and Peter C. Collins
18.1 Introduction 401
18.1.1 Additive manufacturing components in service 401
18.1.2 Regulatory actions and standardization 402
18.1.3 Material properties and defects in additive
manufacturing 404
18.2 State of the art 406
18.2.1 Optical and thermal monitoring 406
18.2.2 Post-production inspection 409
18.2.3 Emerging methods 409
18.3 Practical considerations 413
Acknowledgments 414
References 414

19 Combining additive manufacturing with conventional casting


and reduced density materials to greatly reduce the weight
of airplane components such as passenger seat frames 419
Francis Froes
Conclusions 425
References 425

20 Synergetic technologies of direct layer deposition in aerospace


additive manufacturing 427
Petr A. Vityaz, Mikhail L. Kheifetz and Sergei A. Chizhik
20.1 Introduction 427
20.2 System analysis of the processing methods using
the concentrated energy fluxes 428
20.3 Additive synergetic technologies of layer by layer synthesis 432
20.4 Ion implantation and ion deposition of coatings 434
20.5 Electron-beam heating of a coated surface 438
20.6 Conclusion 445
Acknowledgments 446
References 446

Index 449
List of Contributors

Thomas K. Ales Department of Materials Science and Engineering, Iowa State


University, Ames, IA, United States

Leonard J. Bond Center for Nondestructive Evaluation, Applied Sciences


Complex II, Iowa State University, Ames, IA, United States; Department of
Mechanical Engineering, Iowa State University, Ames, IA, United
States; Department of Aerospace Engineering, Iowa State University, Ames, IA,
United States

Rodney Boyer School of Materials Science and Engineering, University of


Shanghai for Science and Technology, Shanghai, P.R. China; RBTi Consulting,
Bellevue, WA, United States

Sheng Cao Monash Centre for Additive Manufacturing (MCAM), Monash


University, Notting Hill, VIC, Australia; School of Materials Science and
Engineering, University of Shanghai for Science and Technology, Shanghai, P.R.
China

Wei Chen AVIC Manufacturing Technology Institute, Beijing, P.R. China

Zhuoer Chen Department of Mechanical and Aerospace Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia

Sergei A. Chizhik Presidium of the National Academy of Sciences of Belarus,


Minsk, Republic of Belarus; A.V. Lykov Heat and Mass Transfer Institute of the
National Academy of Sciences of Belarus, Minsk, Republic of Belarus

Peter C. Collins Department of Materials Science and Engineering, Iowa State


University, Ames, IA, United States

Chris H.J. Davies Department of Mechanical and Aerospace Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia

Agustin Diaz REM Surface Engineering, Brenham, TX, United States


xiv List of Contributors

B. Dutta DM3D Technology, Auburn Hills, MI, United States

Francis Froes Light Metals Industry, Tacoma, WA, United States; Advanced
Materials Industries, Tacoma, WA, United States

Lawrence Gasman SmarTech Markets Publishing Crozet, Virginia, United States

Shishkovsky Igor Center for Design, Manufacturing and Materials, Skolkovo


Institute of Science and Technology, Moscow, Russia

Orest Ivasishin G.V. Kurdyumov Institute for Metal Physics, Kyiv, Ukraine

Qingbo Jia Department of Materials Science and Engineering, Monash University,


Clayton, VIC, Australia; Monash Centre for Additive Manufacturing (MCAM),
Monash University, Notting Hill, VIC, Australia

Manish Kamal Arconic Inc., Arconic Fastening Systems, Carson, CA, United
States

Mikhail L. Kheifetz Presidium of the National Academy of Sciences of Belarus,


Minsk, Republic of Belarus; State Scientific and Production Association hhCenterii
of the National Academy of Sciences of Belarus, Minsk, Republic of Belarus

Lucas W. Koester Center for Nondestructive Evaluation, Applied Sciences


Complex II, Iowa State University, Ames, IA, United States

Dmytro Kovalchuk JSC NVO Chervona Hvilya, Kyiv, Ukraine

Anja Loesser EOS North America Inc

Zhiqiang Li AVIC Manufacturing Technology Institute, Beijing, P.R. China

Brain W. Martin Department of Materials Science and Engineering, Iowa State


University, Ames, IA, United States

Kevin Minet EOS Finland Oy

Thomas F. Murphy Hoeganaes Specialty Metal Powders LLC, Cinnaminson, NJ,


United States

Joel C. Najmon Department of Mechanical and Energy Engineering, Indiana


UniversityPurdue University Indianapolis, Indianapolis, IN, United States

Tsuyoshi Nakagawa JAXA Safety and Mission Assurance, Tokyo, Japan


List of Contributors xv

M.B. Novikova All-Russia Institute of Light Alloys, JSC, Moscow, Russia

Eric Ott General Electric Additive, West Chester, OH, United States

I.S. Polkin All-Russia Institute of Light Alloys, JSC, Moscow, Russia

Behrang Poorganji General Electric Additive, West Chester, OH, United States

Sajjad Raeisi Department of Mechanical and Energy Engineering, Indiana


UniversityPurdue University Indianapolis, Indianapolis, IN, United States

Niko Raitanen EOS Finland Oy

Jeremy H. Rao Department of Materials Science and Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia

Gregory Rizza Arconic Inc., Arconic Fastening Systems, Carson, CA, United
States

Matthew R. Rolchigo Department of Materials Science and Engineering, Iowa


State University, Ames, IA, United States

Paul Rometsch Department of Materials Science and Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia; Rio Tinto Arvida
Research and Development Centre, Jonquière, QC, Canada

Richard Russell NASA Engineering and Safety Center, Kennedy Space Center,
FL, United States

Ankit Saharan EOS North America Inc

Hector Sandoval Lockheed Martin Missiles and Fire Control, Grand Prairie, TX,
United States

Christopher T. Schade Hoeganaes Specialty Metal Powders LLC, Cinnaminson,


NJ, United States

Mohsen Seifi ASTM International, Washington, DC, United States

Nima Shamsaei National Center for Additive Manufacturing Excellence, Auburn


University, Auburn, AL, United States
xvi List of Contributors

S.V. Skvortsova Moscow Aviation Institute (National Research University),


Moscow, Russia

Hossein Taheri Center for Nondestructive Evaluation, Applied Sciences Complex


II, Iowa State University, Ames, IA, United States; Department of Mechanical
Engineering, Iowa State University, Ames, IA, United States

Andres Tovar Department of Mechanical and Energy Engineering, Indiana


UniversityPurdue University Indianapolis, Indianapolis, IN, United States

G.A. Turichin St. Petersburg State Maritime Technical University, St. Petersburg,
Russia

Petr A. Vityaz Presidium of the National Academy of Sciences of Belarus, Minsk,


Republic of Belarus; Joint Institute of Mechanical Engineering of the National
Academy of Sciences of Belarus, Minsk, Republic of Belarus

Jess Waller NASA-Johnson Space Center White Sands Test Facility, Las Cruces,
NM, United States

Douglas Wells NASA Marshall Space Flight Center, Huntsville, AL, United States

James C. Withers ATS-MER, LLC, Tucson, AZ, United States

Xinhua Wu Department of Materials Science and Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia

Kun V. Yang Department of Materials Science and Engineering, Monash


University, Clayton, VIC, Australia; Monash Centre for Additive Manufacturing
(MCAM), Monash University, Notting Hill, VIC, Australia; CSIRO
Manufacturing, Clayton, VIC, Australia
Introduction to aerospace
materials requirements and the 1
role of additive manufacturing
Francis Froes1, Rodney Boyer2,3 and B. Dutta4
1
Advanced Materials Industries, Tacoma, WA, United States, 2School of Materials
Science and Engineering, University of Shanghai for Science and Technology, Shanghai,
P.R. China, 3RBTi Consulting, Bellevue, WA, United States, 4DM3D Technology, Auburn
Hills, MI, United States

1.1 Aerospace materials and their requirements


Aerospace materials are frequently metal alloys, although they also include poly-
meric based materials, that have either been developed for, or have come to promi-
nence through, their use for aerospace purposes. Aerospace uses often require
exceptional performance, strength or heat resistance, even at the cost of consider-
able expense in their fabrication or conventional machining. Others are chosen for
their long-term reliability in this safety-conscious field, particularly for their resis-
tance to fatigue loading. The field of materials engineering is an important one
within aerospace engineering. Its practice is defined by the international standards
bodies that maintain standards for the materials and processes involved, such as
ASTM, AMS or company specifications (Table 1.1 shows specifications for addi-
tive manufacturing [AM]). Generally, not a lot of information is contained in
company specs, but with the controls required, a company spec will be mandatory
due to the complexity of the process, where the customer will want to know a lot
more details than will ever get into a public spec due to protection of proprietary
information. A further requirement is observer observation of fabrication of
acceptable quality, including microstructures (Fig. 1.1).

1.2 Additive manufacturing


In publications over the past few years [15], the cost of fabricating various titanium
precursors and mill products has been discussed (very recently the price of TiO2 has
risen to $2.00 per pound and TiCl4 to $0.55 per pound) and it has been pointed out
that the cost of extraction is a small fraction of the total cost of a component fabri-
cated by the cast and wrought (ingot metallurgy) approach. To reach a final compo-
nent, the mill products must be machined, often with very high buy-to-fly ratios

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00001-7


© 2019 Elsevier Inc. All rights reserved.
2 Additive Manufacturing for the Aerospace Industry

Table 1.1 Specifications released and in-work for additive manufacturing (AM)
components

Specification no. Specification title Status


AMS 4998 Titanium alloy powder, Ti6Al4V Released—1977
AMS 4999 Titanium alloy laser deposited products, Released—2002
Ti6Al4V, annealed
AMS 7000 Additive manufacture of aerospace parts In work
from Ni-base superalloy 625 via laser
powder bed process
AMS 7001 Ni base 625 superalloy powder for use in In work
laser powder bed manufacturing of
aerospace parts
AMS 7002 Process requirements for production of In work
powder feedstock for use in laser powder
bed additive manufacturing of aerospace
parts
AMS 7003 Laser powder bed fusion process In work
AMS 7004 Titanium alloy preforms from high In work
deposition rate additive manufacturing
on substrate Ti6Al4V stress relieved
AS9100 Quality management systems— Issued 1997,
requirements for aviation, space, and Current Rev. D,
defense organizations 2016
The AS (Aerospace Standards) are utilized for details with regard to quality management systems. They do not cover
specific material requirements such as properties, inspection, etc.

(which can reach as high as 40:1). The generally accepted cost of machining a com-
ponent is that it doubles the cost of the component. The feedstock for AM can be a
wire or a powder. Using powder, there are two basic approaches to AM: powder bed
fusion (PBF) and direct energy deposition (DED), Figs. 1.1 and 1.2. The PBF

Figure 1.1 Schematic showing powder bed fusion technology.


Introduction to aerospace materials requirements and the role of additive manufacturing 3

Laser beam Final focus optics

Nozzle shielding
gas
To powder feeder

Feedback
Feedback sensor 2
sensor 1

Solid free form


Workholding shape by direct
fixture deposition

Substract or die
preform

Figure 1.2 Schematic showing DMD technology. DMD, Direct metal deposition.

technique allows the fabrication of complex features, hollow cooling passages, high
precision parts, and single metal builds. The DED approach allows large build envel-
opes, high deposition rates, multiple materials, and addition of material to existing
components. Mechanical properties are at least at ingot metallurgy levels (including
fracture toughness). Examples of AM manufactured parts and parts which could be
AM fabricated in an advanced engine are shown in Fig. 1.3.

1.3 Additive manufacturing fabrication of various types


of materials
The AM technique has been applied to metals, ceramics, and polymeric materials
(Figs. 1.31.5)
After the AM build, ceramic parts are porous and, if desired, can be infiltrated
or fired in a postprocess step. This method is used for fine art ceramics. The pri-
mary advantages for 3-D printing, especially binder jetting (binder jetting is an AM
process in which a liquid binding agent is selectively deposited to join powder
particles. Layers of material are then bonded to form an object, for example by hot
isostatic pressing) are low cost, high speed, scalability, ease of building parts in
4 Additive Manufacturing for the Aerospace Industry

Figure 1.3 (A) Examples of metallic parts fabricated by additive manufacturing. (B) The
propulsion system for the F-35 lightening, which contains a substantial number of
components that can be fabricated by additive manufacturing.

multiple materials, and versatility for use with ceramic materials. Originally
evolved from systems that used thermoplastics, the binder jetting method has been
modified to accept ceramic slurries or ceramic powders in wax or liquid binder car-
riers. Material jetting has significant challenges, including getting materials to flow
through nozzles at reasonable speeds without clogging. Work is ongoing to improve
the rheology of material systems for ceramic materials, such as alumina and zirco-
nia. This method promises good surface finishes and high tolerances for parts that
can be printed and then fired to high density. PBF originated with selective laser
Introduction to aerospace materials requirements and the role of additive manufacturing 5

Figure 1.4 Examples of ceramic parts fabricated by the additive manufacturing technique.

Figure 1.5 Examples of polymeric materials fabricated by additive manufacturing.

sintering (SLS). SLS uses a powder bed layer in a build box, similar to the binder
jet method, but it is placed in a system that brings the powder to an elevated tem-
perature and then exposes select areas to a laser beam. This causes localized sinter-
ing of the ceramic powder. The part has sufficient strength for handling, but
requires a conventional postprocess firing to achieve full density. All PBF methods
share certain characteristics, including one or more thermal sources for inducing
6 Additive Manufacturing for the Aerospace Industry

fusion or sintering between particles, a method for prescribing fusion in a region of


each layer, and mechanisms for adding and smoothing powder layers. Electron
beam melting has become a popular approach to PBF as it is fast, efficient, and can
provide fully dense parts. The downside for ceramics is that the powder bed needs
to be electrically conductive. Directed energy deposition is also a technique that is
better suited to metals. Polymerization is used for polymers that can be loaded with
ceramic powders.
Polymeric parts range from epoxy-based, ABS (acrylonitrile butadene styrene a
lightweight thermoplastic polymer resin of the polyester family), wax, polystyrene,
ceramic, and nylon. All the systems follow the principles of building layer by layer,
but vary in how the materials are applied (e.g., as a fine powder, liquid polymer, or
molten plastic) and how they are cured (e.g., by melting with a laser or activating
UV resin with a laser). The material most commonly used in nonimplantable medical
applications is nylon 12.

1.4 Contents of this book


In this book an attempt was made to contact all the major AM fabricators and aero-
space user (airframes, engines, and missile) world-wide to fully cover all the signif-
icant activity in the AM in aerospace field. Not all the organizations contacted
expressed an interest in participating in this book. However it is considered that
enough information has been gathered to give the reader a comprehensive view of
the field. One rumor which was dispelled is that the USAF is very negative on AM,
they are not. Read the 40 articles which follow this introduction to get a broad view
of the use of AM in aerospace applications.

References
[1] B. Dutta, F.H.(Sam) Froes, Additive manufacturing of titanium alloys, Adv. Mater. Proc.
(2014) 1823.
[2] B. Dutta, F.H.(Sam) Froes, Chapter 24: the additive manufacturing of titanium alloys,
in: M. Qian, F.H. (Sam) Froes (Eds.), Titanium Powder Metallurgy, Butterworth-
Heinemann, 2015.
[3] F.H.(Sam) Froes, B. Dutta, The additive manufacturing of titanium alloys, in:
Proceedings of the World Conference on Titanium, San Diego, CA, 2015.
[4] B. Dutta, F.H. Froes, Additive manufacturer of titanium alloys, in: A. Badiru (Ed.),
Additive Manufacturing Handbook: Product Development for the Defense Industry,
2016.
[5] B. Dutta, F.H. Froes, Book Additive Manufacturing of Titanium Alloys, Elsevier
Publishing, Amsterdam, 2016.
Review of additive manufacturing
technologies and applications in 2
the aerospace industry
Joel C. Najmon, Sajjad Raeisi and Andres Tovar
Department of Mechanical and Energy Engineering, Indiana UniversityPurdue
University Indianapolis, Indianapolis, IN, United States

2.1 Aerospace requirements and opportunities for


additive manufacturing
Additive manufacturing (AM) is being established as a fabrication technology that
brings revenue to the aerospace industry throughout its supply chain and repair
operations [1]. For the last 10 years, the aerospace industry has been one of the top
sectors leading the AM market (Figs. 2.1 and 2.2). Today, 18.2% of the revenue in
the AM industry is received from the aerospace industry. The aerospace sector is
also the fastest growing sector, showing an annual increase of 1.6% in 2016, fol-
lowed by motor vehicles with a growth of 1.0%. The revenues from the AM are
estimated at $2.7 billion in 2016 (growth of 12.9% with respect to 2015) and
are expected to surpass $100 billion within the next two decades, mostly in the
aerospace industry [3].
The market for AM parts in aerospace can be divided into metallic and nonme-
tallic (mostly polymer) components, which are generally related to critical and non-
critical aircraft parts, respectively. Boeing and Bell Helicopter started using
polymer AM parts for nonstructural components in the mid-1990s. In March 2015,
Boeing fabricated more than 200 unique parts for 10 different aircraft using AM
technologies. By that time, more than 20,000 nonmetallic AM parts were installed
in airplanes [1]. Today, Boeing has installed tens of thousands of AM parts on 16
commercial and military aircraft [4]. In 2017, Boeing started using at least four AM
titanium-alloy parts to produce its 787 Dreamliner aircraft with near-future plans to
manufacture almost 1000 parts via AM to save $23 million per airplane [5].
Airbus is also a main player in AM. It has installed AM metal brackets and bleed
pipes on the Airbus A320neo and the A350 XWB test aircraft [6]. It also has a
multiyear cooperative research agreement with Arconic to produce large-scale AM
airframe components (1 m in length) [7]. NASA, the European Space Agency, and
SpaceX are exploring the use of AM igniters, injectors, and combustion chambers
on their rocket engines. Honeywell Aerospace, Lockheed Martin, and Northrop
Grumman are also important users of AM. The unique design requirements from

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00002-9


© 2019 Elsevier Inc. All rights reserved.
8 Additive Manufacturing for the Aerospace Industry

Figure 2.1 Additive manufacturing market share by industry in 2016.


Source: Wohlers, A., Wohlers Report 2016. 3D Printing and Additive Manufacturing State of
the Industry. Annual Worldwide Progress Report. 2016: Associates Wohlers. Wohlers Report
2016. Wohlers Associates, Inc. [2].

Figure 2.2 Additive manufacturing market share by industry in 2017.


Source: Wohlers, A., Wohlers Report 2017. 3D Printing and Additive Manufacturing State of
the Industry. Annual Worldwide Progress Report. 2017: Associates Wohlers. Wohlers Report
2017. Wohlers Associates, Inc. [4].

the aerospace industry and capabilities of AM technologies are discussed in this


section.

2.1.1 Design requirements


The aerospace industry is constantly demanding lightweight aircraft components
with a high strength-to-weight ratio to improve fuel efficiency, reduce emissions,
and respond to safety and reliability requirements [8]. To this end, aerospace
designers strive to minimize the amount of material used in every component,
Review of additive manufacturing technologies and applications in the aerospace industry 9

which results in increased design complexity with respect to the structure, function,
and property [9]. AM allows the fabrication of parts with virtually any shape (free-
form fabrication).

2.1.1.1 Structural design


Structurally complex designs are characterized by nontraditional (freeform, organic-
like) external shapes that provide high mechanical performance with minimum
mass. AM allows the fabrication of parts with complex designs with some con-
straints, depending on the specific AM technology [10]. Frame designs are exam-
ples where topology optimization is used. Complex aircraft structures can be also
designed to maximize internal space (packing ratio) [11]. When compared with tra-
ditional manufacturing processes, like injection molding or milling, AM is signifi-
cantly more versatile due to its layer-by-layer fabrication process [12]. This allows
for the optimization and manufacturing of lightweight, strong, and robust parts [13].
Structural complexity also describes the multiscale internal hierarchical architec-
tures of lattice/cellular arrays (mechanical metamaterials) [1416]. Such complex
structures can be obtained with use of topology optimization algorithms [1723].
Commercial software that can provide lattice materials to optimize designs includes
Netfabb, Within, Materialise, and Simpleware, as well as topology optimization
tools such as OptiStruct, Genesis, and Meshify. The solution of topology optimiza-
tion problems involves multiphysics simulations and multiscale design methods to
find the best compromised solution among multiple objectives [24]. With the use of
these software tools, aerospace designers have the ability to reduce material and
weight while making the design suitable for AM. These tools also allow the ability
to retain or increase the part’s mechanical performance and reduce manufacturing
cost. Lightweight parts can deliver substantial cost savings from the fabrication pro-
cedure to the end of the airplane’s life [25].

2.1.1.2 Functional complexity


Functional complexity refers to the ability of parts to integrate multiple functions
(multifunctional parts), including functions that are traditionally not assigned to the
part, for example, heat dissipation, electrical circuitry, flexibility, capillarity to a
load-bearing component. Examples in aerospace include structural components that
also act as conduits, such as airfoils and turbine blades with embedded cooling
channels [26,27].
Functional complexity also defines functions that are difficult to achieve by a
single component. An example is the design of the swirler inside a jet engine that
forces combustion products to recirculate inside the chamber, generating a highly
turbulent flow. Since increasing the turbulence can reduce the chamber pressure,
the swirler geometry must be designed precisely to deliver the desired turbulence
suitably to mix the injected fuel and the airflow [28]. Such a complex function is
difficult to achieve without the freeform fabrication capabilities of AM.
10 Additive Manufacturing for the Aerospace Industry

2.1.1.3 Property requirements


Finally, behavioral complexity describes changes in the material properties across
the component. This includes multimaterial designs and functionally graded materi-
als (FGMs). FGMs can be fabricated by local microstructure modifications from
thermally-induced transformations [2933] or by changes in the architecture of the
cellular/lattice structure [3436].
The ability to tailor mechanical properties is particularly relevant to additive
metal technologies (AMTs), like directed energy deposition (DED) and powder bed
fusion (PBF) [37]. In PBF, the powder grain size and distribution can be varied to
change the density and corresponding properties [38,39]. The processing parameters
can be varied to tailor the quality of the part’s hardness, fatigue strength, surface
microstructure, and surface finish [39,40]. This allows for the manufacturing of
metal parts with local control of residual stress concentrations [41].

2.1.2 Manufacturing capabilities and benefits


The increased complexity of the structure, function, and property of an aerospace
component entails fabrication challenges and higher costs [42]. Traditionally, the
design is simplified for manufacturing and assembly operations at the expense of
part performance. AM, however, allows freeform fabrication and reduces assembly
through part consolidation. It also reduces material waste and allows the use of pre-
mium materials that are difficult to process with other manufacturing techniques.
Unlike conventional manufacturing, AM reduces or even eliminates the need for
tooling, which allows the production of small production runs and parts that require
quick turnaround time. The benefits of AM for the aerospace industry are discussed
in this section.

2.1.2.1 Part consolidation


Traditionally, complex aerospace components contain multiple simple parts that are
joined together using different types of fasteners (welds, bolts, and brazes).
However, such assemblies offer lower reliability and require greater inspection,
tooling, and sustainment costs when compared to a single part [43]. In addition,
geometric errors and undesired misalignments or deformations may exceed allow-
able tolerances in aerospace components [44].
Part consolidation can be attained using AM. This enables feature integration as
well as increased reliability and performance [45]. When a complex part is fabri-
cated on a single AM machine, the part inventory is reduced and the economies of
scale associated with large centralized factories are also reduced [1]. Decreasing the
number of parts in an assembly reduces (1) the number of tools held in inventory,
(2) the costs associated with documentation, inspection, and production, (3) the
assembly line footprint, and (4) the overall manufacturing costs.
GE Aviation has reported a reduction from 855 parts produced using conven-
tional manufacturing into a dozen parts using AM technologies. The simplified
Review of additive manufacturing technologies and applications in the aerospace industry 11

design reduced weight, improved fuel efficiency up to 20%, and achieved 10%
more power. A bearing support and sump were redesigned to consolidate 80 parts
into one. Also, a 20-part nozzle was consolidated into a single AM unit and the
weight was reduced by 25% [46]. Similarly, Airbus reduced a 126-part hydraulic
housing tank to a single AM part [47] (Fig. 2.3).

2.1.2.2 Material economy


A significant contributor to the high fabrication cost of aerospace components is the
buy-to-fly ratio, which is defined as the weight ratio between the raw material and
the weight of the final component. Aerospace components with large volume
envelope-to-volume ratios (e.g., thin-walled structures and turbine blades) have
buy-to-fly ratios as high as 2040:1 [48], which makes CNC tool planning time
consuming and impractical due to the massive amount of waste material. In these
cases, the material use and the manufacturing cost can be significantly improved
with AM freeform fabrication capabilities and reduce the buy-to-fly ratio closer to
1:1. For PBF processes, the amount of waste produced is around 5% compared to
that of traditional milling, which can produce up to 95% waste [12,49]. Reducing
the material waste and the part weight also has a significant positive effect on the
environment [50,51].
The aerospace industry constantly demands premium metals, such as titanium
alloys, aluminum alloys, nickel-based super alloys, and special steels. Titanium
alloys, for example, provide outstanding characteristics, like high strength-to-
weight ratio, a wide range of operating temperatures, high corrosion resistance, and
composite compatibility. However, titanium alloys are highly limited by their rela-
tively high cost compared to other materials [52] and their poor machinability [53].
A growing number of premium materials are available in AM technologies, includ-
ing titanium. For instance, GE Avio Aero is producing low-pressure turbine blades
in titanium aluminide (TiAl) using AM [54]. Today, Norsk Titanium owns the
world’s largest titanium AM facility and supplies aerospace-grade AM structural
titanium components, approved by the Federal Aviation Administration (FAA) of
the United States, to companies like Boeing.

Figure 2.3 (A) AM hydraulic reservoir rack from Airbus consolidating 126 parts. (B)
Consolidated design into one part. AM, Additive manufacturing.
Source: Photo copyright Airbus  Hermann Jansen.
12 Additive Manufacturing for the Aerospace Industry

2.1.2.3 Small production runs and turnaround time


In comparison to conventional manufacturing processes, AM tend to be more
expensive for large production runs; however, the relatively high investment costs
of fixtures and tools are avoided or considerably reduced in AM [12]. Therefore,
AM is more cost effective for customized parts and small production runs, which
are common in the aerospace industry.
Since aircraft have lifespans of over 30 years, maintaining and replacing legacy
parts and tooling may involve high inventory costs [55]. AM enables the production
of test and replacement parts on demand for rapid shipment and installation [56].
This minimizes downtime and associated costs. According to Airbus, the turn-
around for test or replacement parts was as low as 2 weeks in 2014. Finally, AM
allows parts to be manufactured at decentralized locations. This lowers transporta-
tion and storage costs. This simplification in supply chains also leads to a reduction
in maintenance-based downtime and turnaround time [57].

2.2 Additive manufacturing technologies


The American Society for Testing and Materials International Committee F42 clas-
sifies AM technologies into seven categories: binder jetting, DED, material extru-
sion, material jetting, PBF, sheet lamination, and vat photopolymerization [58].
According to the material, AM technologies in aerospace can be classified into
AMTs and additive nonmetal technologies. These technologies are described in this
section.

2.2.1 Additive metal technologies


The two most common AMTs for aerospace applications are DED and PBF.
Widespread DED technologies in the aerospace industry include laser metal deposi-
tion (LMD), laser engineering net-shaping (LENS), electron beam welding (EBW),
electron beam free-form fabrication (EBF3), and wire arc AM (WAAM).
PBF technologies include direct metal laser sintering (DMLS), selective laser
melting (SLM), and electron beam melting (EBM). Other relevant AMTs for aero-
space applications include binder jetting and supersonic particle deposition (SPD),
also known as cold spray (Table 2.1). This section describes the most relevant
AMTs to the aerospace industry.

2.2.1.1 Directed energy deposition


DED technology works by melting material that is fed to a local site on the build
layer, usually occurring within an inert gas atmosphere [1,59]. While this can be
used for nonmetal materials, it is predominately used with metals and metal alloys
[1,6062]. Feedstock usually comes in the form of powder or wire and is melted
with a focused energy source, such as laser beams, electron beams, and arcs [1,48].
Review of additive manufacturing technologies and applications in the aerospace industry 13

Table 2.1 Additive metal technologies in the aerospace industry

AMTs

Directed energy deposition Powder bed fusion Other


G
LMD/LENS G
DMLS G
Binder jetting
G
EBW/EBF3 G
SLM G
SPD/cold spray
G
WAAM G
EBM
LMD, Laser metal deposition; LENS, laser engineering net-shaping; EBF3, electron beam free-form fabrication;
EBW, electron beam welding; WAAM, wire arc AM; DMLS, direct metal laser sintering; SLM, selective laser
melting; EBM, electron beam melting; SPD, supersonic particle deposition; AMTs, additive metal technologies.

DED processes build up the 3D part, layer by layer; however, the technology
can be implemented in a multiaxial machine and provide 3D positioning [1]. This
allows manufacturing of complex parts without the need of support structures. Due
to increased versatility in orientation, DED technologies are ideal for component
repair of turbine blades, engine combustion chambers, compressors, airfoils, and
blisks [1,62,63]. Turbine airfoils have been repaired to within 0.030 mm accuracy
of the original blade and shown that for a repair volume of 10%, there is a at least a
45% improvement in the carbon footprint and a 36% total energy savings [64]. The
mechanical properties of an AM part produced by wire-fed laser and arc beam
deposition processes rely heavily on process parameters, load direction, and post
build-up heat treatment; however, both processes produced parts with comparable
properties and are suitable for aerospace applications [60].

2.2.1.2 Powder bed fusion


PBF technologies work by locally melting metal powder on a substrate to form
layers. After a new layer is formed, a leveling roller distributes a new layer of pow-
der. Un-melted powder is reusable and becomes the support for successive layers,
reducing the need for support structures [1,59]. To avoid powder oxidation, SLM
and DMLS occur in an inert gas atmosphere, while EBM occurs in a vacuum
[65,66]. Consequently, the requirement of a vacuum makes EBM attractive for
outer space manufacturing [59,67]. Compared to DED processes, PBF processes
have the ability to create internal passages and, typically, produce higher-fidelity
build features [68]. Titanium alloy (Ti6Al4V) has been typically used in the
fabrication of AM parts via EBM technology [6974]. Topology optimized
Ti6Al4V brackets were manufactured with an Arcam Q10 Plus EBM system,
demonstrating that geometry and microstructure are dependent on the build time or
cross-sectional area of each layer [74].

2.2.1.3 Other relevant additive metal technologies


Binder jetting is used for quick and reliable rapid prototyping of metal AM parts,
such as impellers and turbine blades [75,76]. It is also used for rapid tooling in the
14 Additive Manufacturing for the Aerospace Industry

fabrication of AM sand cores and molds to produce large metal parts. Typical metals
used are aluminum and copper alloys, gray and ductile iron, and magnesium. Binder
jetting AM of sand cores and molds allows the removal of patterns used in indirect
rapid tooling and simplifies the steps involved in the creation of low volume produc-
tion parts [77]. Applications of direct rapid tooling through metal binder jetting
include complex gear cases and covers, fuel tanks, transmission housings, compo-
nents requiring draft free walls, lightweight engine parts, and structural hinges [78].
SPD, or cold spray, works through the consolidation of supersonic, microsized,
metal particles onto a suitable substrate upon impact (ballistic impingement). This
technology is also suitable for ceramic and polymer powders [79]. The particles are
accelerated with a spray gun fitted with a convergent-divergent rocket nozzle using a
heated high-pressure gas (helium or nitrogen). Since the metal powder is not signifi-
cantly heated during this process, with consolidation occurring in the solid form, the
risks of oxidation, residual stress accumulation, and changes in the powder’s micro-
structure are avoided [79]. SPD has been utilized for repairing and enhancing the air-
worthiness and integrity of aging aircraft structures [8082]. Nitrogen-based SPD
has been shown limited particle deformation resulting in high degrees of porosity,
while helium-based SPD had substantially more microstructural deformation with
very little porosity [83]. Aircraft that are often exposed to salt spray, like navy res-
cue/patrol helicopters, should be repaired and treated with helium-based SPD [55].

2.2.2 Additive nonmetal technologies


Additive nonmetal technologies most relevant to the aerospace industry include:
selective laser sintering (SLS), stereolithography (SLA), fused deposition modeling
(FDM), and PolyJet [84] (Table 2.2). This section presents the main characteristics
of these technologies and their relevance to the aerospace industry.

2.2.2.1 Selective laser sintering


SLS is a PBF process that typically uses a laser energy source to melt polymer
powders [59]. It has the ability to produce large parts with good mechanical
strength at a relatively low cost [91]. For aerospace applications, SLS is primarily
used for rapid prototyping of nonfunctional parts and direct digital manufacturing
(DDM) of noncritical components [92]. Glass-filled nylon is used in SLS fabrica-
tion of engine compartments that require heat resistance, for example, tarmac noz-
zle bezel [85]. Nylon 12 is used in SLS produced parts that require flexibility, such
as ducts and bellow directors for airflow [86] (Fig. 2.4). It has been shown that the
percent crystallinity of SLS nylon-12 parts is dependent on the degree of the parti-
cle melt, to the extent that sufficiently different percent crystallinity part volumes
can be treated as different materials [93]. This opens up the possibility of producing
FGM parts with SLS. SLS parts produced with acrylic styrene and polyamide
(nylon) show nearly the same mechanical properties as plastic injected counterparts
[94,95]. In most applications, SLS is known to be cost effective for the production
of small volume parts for aircraft [59].
Review of additive manufacturing technologies and applications in the aerospace industry 15

Table 2.2 Additive nonmetal technologies in the aerospace industry

Additive nonmetal technologies

Application Example part Requirements Recommended Recommended


process material

Engine Tarmac nozzle Heat resistant SLS Glass-filled


compartment bezel [85] functional nylon
parts
Air ducts Airflow ducting Flexible ducts SLS Nylon 12
[86] and bellow
directors
Full size panels Seat backs and Large parts with SLA Standard resin
entry doors smooth
[84] surface finish
Casted metal Brackets and Cast metal parts SLA and Castable resin or
parts door handles using 3D- PolyJet wax
[87] printed
patterns
Lights Headlight Fully transparent, SLA and Clear resin
prototypes high-detail PolyJet
[84] models
Bezels Dashboard End-use custom PolyJet Digital ABS
interface [84] screen bezels
UAV Wings and High strength, FDM ULTEM
fuselage [88] lightweight,
durability
Prototypes and Camera case Rigidity, FDM ULTEM
tools prototype and dimensional
tool to install stability
wiring [89]
Cabin Door handle Customizable FDM ULTEM
accessories covers [90] and robust
handles

SLS, Selective laser sintering; SLA, stereolithography; FDM, fused deposition modeling.
Source: Adapted from B. Artley, Aerospace 3D Printing Applications, in: D. Hubs (Ed.). ,https://www.3dhubs.com/knowledge-base/
aerospace-3d-printing-applications. [84].

2.2.2.2 Stereolithography
SLA, also known as vat photopolymerization, is a method of creating 3D objects
using a light-emitting device (laser or digital light processing) that illuminates and
cures a liquid photopolymer resin (thermosetting plastic) layer by layer [96]. SLA
has the ability to produce fine features and provide good surface finish with mini-
mum stair stepping effect [91]. Several photopolymer resins can be utilized with
SLA: standard (rigid, opaque), castable, and clear, as well as flexible, high tempera-
ture, and dental, among others [97]. High-fidelity rapid prototypes for testing, veri-
fication, and design of aeroelastic airfoils have been produced with low-stiffness
resins, where model similarity between prototypes was highly desired [98]. Cabin
accessories such as console control parts with functional knobs as well as full size
16 Additive Manufacturing for the Aerospace Industry

Figure 2.4 Air ducts for laminar flow made with polyamide 12 (PA 2200) from EOS [86].

panels, seat backs, and entry doors have been produced with SLA standard resin
[84]. Castable and high-temperature SLA resins are used to fabricate mold patterns
(indirect rapid tooling) and injection molds (direct rapid tooling), respectively.
Prototypes of highly-detailed, fully transparent aircraft headlights are produced with
SLA clear resins [84].

2.2.2.3 PolyJet
PolyJet, also known as material jetting, uses inkjet printing technology to jet liquid
photopolymer droplets onto a build substrate and then cure it with UV light. It has
the ability to fabricate parts with fine features and good surface finish, while exhi-
biting little stair stepping effect [91]. Some PolyJet systems also boast the ability to
produce multimaterial parts through FGM, allowing a wide range of material prop-
erties selection [99]. The role of PolyJet in the aerospace industry includes rapid
prototyping, indirect rapid tooling (mold pattern fabrication), and DDM. Material
jetting occurs through two processes: drop on demand (DOD) and continuous inkjet
(CIJ). The DOD process offers high part resolution at the expense of build time,
making it favorable for applications requiring a fine surface finish, such as proto-
type light fittings and intricate wing design prototypes (bat-like ornithopter, lattice
structure wing struts) [100,101]. The CIJ process offer faster build times at lower
part resolutions and is better suited for noncritical, nonmetallic part fabrication, like
interface bezels [102].

2.2.2.4 Fused deposition modeling


FDM, also known as material extrusion, is currently the most popular AM technol-
ogy on the market [103]. It allows the fabrication of durable components made of
Review of additive manufacturing technologies and applications in the aerospace industry 17

high-strength thermoplastics such as ULTEM, polycarbonate, polyphenylsulfone,


polylactic acid, and acrylonitrile butadiene styrene (ABS) [104]. FDM systems are
widely versatile in applications, ranging from quick and inexpensive rapid prototyp-
ing to tough and rigid parts suitable for end-use. The aerospace industry has been
substituting traditionally metal parts with sufficiently strong FDM-produced parts to
reduce weight and turnaround time for part repairs [105]. Approximately 70
production-grade thermoplastic parts, are being implemented in NASA’s Mars rover
because they are lightweight, yet durable enough to withstand the rigors of space
[106]. For prototype applications that do not require high resolution and surface fin-
ish, FDM technology is ideal because it is economical and does not require chemi-
cal postprocessing [107]. Stratasys and Aurora Flight Sciences fabricated the largest
and fastest AM unmanned aerial vehicle (UAV) using FDM. Low weight and high
strength are achieved using ULTEM 9085 as the build material in addition to add-
ing an internal honeycomb structure to the internal wing design.

2.3 Additive manufacturing applications


AM technologies for aerospace applications usually fall under one of the following
categories: DDM, rapid tooling, rapid prototyping, and repair. Table 2.3 shows a
breakdown of AM technologies into metal and nonmetal application categories. DDM
refers to the production of parts to be utilized in the aircraft. Such parts can be critical
components required for the operation (e.g., nozzles, combustion chambers) and

Table 2.3 Metal and nonmetal additive manufacturing technologies with select aerospace
examples

Application AM Aerospace examples


technology
Metal G
DDM (direct G
DED G
Helicopter engine combustion
metal part G
PBF chamber fabrication (DED) [108]
fabrication) G
Cold G
Blisk airfoil repair (DED) [109]
G
Rapid tooling spray G
Satellite antenna bracket (PBF)
G
Repair G
Binder [110]
jetting G
Lap joint reinforcement (SPD) [81]
Nonmetal G
DDM (fixtures G
SLS G
Ratchet wrench printed by NASA
and G
SLA on International Space Station
accessories) G
PolyJet (SLS) [111]
G
Rapid G
FDM G
UAV wing design (PolyJet) [91]
prototyping G
Boeing 777-300ER door handle
G
Rapid tooling (FDM) [90]
G
Camera case prototyping (FDM)
[89]
DDM, Direct digital manufacturing; DED, directed energy deposition; PBF, powder bed fusion; SLS, selective laser
sintering; SLA, stereolithography; FDM, fused deposition modeling; UAV, unmanned aerial vehicle.
18 Additive Manufacturing for the Aerospace Industry

noncritical parts (e.g., brackets, fixtures, and accessories). Rapid tooling refers to the
fabrication of tools and patterns required for the fabrication of the final part. It can be
classified into direct rapid tooling (e.g., molds and dies) and indirect rapid tooling
(e.g., mold patterns). Rapid prototyping refers to the fabrication of nonfunctional parts,
usually using nonmetal technologies. Finally, repair entails the repair and reinforce-
ment of metallic parts and joints usually through DED and cold spray processes.

2.3.1 Direct digital manufacturing


2.3.1.1 Direct metal part fabrication
DED systems from companies like TWI (The Welding Institute) and EOS GmbH
(Electro-Optical Systems) are being used to fabricate complex and overhanging
metal structures as the multiaxis orientation systems can orient the part so that jut-
ting structures are built off of existing layers. TWI’s five-axis LMD system has
been used in the production of an IN718 helicopter engine combustion chamber,
featuring an overhanging flange [108] (Fig. 2.5). RUAG Switzerland has used AM
with topology optimization to reduce the weight of the Sentinel satellites’ antenna
bracket by 40% [110]. The optimized bracket is made of aluminum alloy,
AlSi10Mg, manufactured with the EOS M 400, an SLM AM system. Boeing’s 787
Dreamliner is now using four additive manufactured titanium parts that will eventu-
ally reduce its production costs by up to $3 million [5].
Multipart assemblies have been consolidated into a single complex part using
EOS’s M 290 DMLS system. The ArianeGroup was able to reduce a 248-part upper
stage propulsion module to a single part through DMLS [112]. Vectoflow used
DMLS to fabricate a compact, one-piece, flow measurement device, designed to
withstand the severe stresses of aircraft in the subsonic and supersonic range [113].
GE has used Arcam’s EBM Q20plus to produce Ti6Al4V turbine blades and
structural airframe components [114]. A liquid oxygen flange has been additively
manufactured, in lieu of traditional manufacturing means, for use on the upper stage
of United Launch Alliance Launch Vehicles [42].

Figure 2.5 TWI’s five-axis LMD printer manufacturing an IN718 helicopter engine
combustion chamber. LMD, Laser metal deposition.
Source: C. Hauser, Case Study: Laser Powder Metal Deposition Manufacturing of Complex
Real Parts. 2014, TWI. Image Courtesy of TWI Ltd.
Review of additive manufacturing technologies and applications in the aerospace industry 19

Postprocessing necessities can be addressed through hybrid manufacturing [115].


Hybrid manufacturing is the combination of additive and subtractive manufacturing
into a single system [116]. AM builds up the metal part, while traditional subtrac-
tive manufacturing (CNC milling) is used for spot milling and surface finishing.
This combined process simplifies part fabrication by reducing the number of pro-
duction steps. Several companies are introducing hybrid manufacturing systems
(Hybrid Manufacturing Technologies’ Ambit Series 7 and ELB-Schliff’s millGrind)
to the aerospace industry for part fabrication and repair. ELB-Schliff’s millGrind is
the world’s first hybrid manufacturing featuring grinding for in-process repair of
aerospace components [117].

2.3.1.2 Fixtures and accessories


While, most mechanical and structural components of aircraft are made of metal, fix-
ture and interior accessories are often made from nonmetals to save weight and cost.
China Eastern Airlines used FDM to manufacture misprinted seat signs on its Boeing
777 aircraft, an expensive and time-consuming fix [118]. Northrop Grumman utilize
SLA to fabricate repair kits for specific aircraft repairs simplifying teardown proce-
dures and reducing maintenance-related downtime [119]. Similarly, Moog Aircraft
Group has adopted FDM to manufacture component maintenance manual fixtures for
internal inspection [120]. AM of these parts have other benefits, like assembly part
consolidation. Advanced Aerials uses 3D systems’ SLS technology to fabricate tough
parts for its unmanned vehicle systems [121]. Honeywell also used SLS for the
manufacturing of control pod casings on its RQ-16 T-Hawk UAV [122].

2.3.2 Rapid tooling


Rapid tooling describes any mold-making process that can create tools quickly and
with minimum direct labor [123]. Generally, AM rapid tooling processes fall under
indirect or direct rapid tooling. Indirect rapid tooling is the use of AM methods to
produce a temporary part model. A reverse ceramic or sand mold is created from
this model for metal part casting. One subprocess of indirect rapid tooling is recon-
figurable tooling [124]. Reconfigurable tooling allows the reuse of molds through
the use of state-changing materials for mold creation. This subprocess has been
used to produce splashes and tools of wing shapes for aircraft in the field without
the need for disassembly [124]. Airbus used indirect rapid tooling to create struc-
tural door hinges for the Airbus A320 [1]. With direct rapid tooling, molds and
inserts are made directly with AM processes. Thus, direct rapid tooling does not
require as many steps as indirect rapid tooling and has the potential to preserve
overall part density more effectively [124].

2.3.3 Rapid prototyping


Rapid prototyping allows for realization and verification of computer simulation
models of aerospace parts and aircraft. Prototypes are useful for identifying
20 Additive Manufacturing for the Aerospace Industry

design drawbacks and opportunities that only become apparent through a phy-
sical model. In addition, prototypes are beneficial for wind tunnel testing and
model verification of streamlines. Fig. 2.6 shows the complete model of an air-
craft made for wind tunnel testing. Depending on the use case, most prototypes
do not need to be manufactured with the actual part material, however proto-
types should possess sufficient rigidity and fidelity to achieve accurate results
in testing [125]. Generally, polymer-based AM processes, like SLA or FDM,
produce models with sufficient rigidity and fidelity for prototype testing. Thus
relatively expensive metal-based AM processes can be avoided, making rapid
prototyping a quick and inexpensive way to validate physical features and
computational fluid dynamic models.
PolyJet has been used to prototype rapidly and test various wing designs for
UAV applications. NASA carried out a study to evaluate design approaches for a
next-generation commercial aircraft with AM rapid prototyping. The preparation of
a wind tunnel model is a crucial stage of this project, as it is used to assess the aero-
dynamics, propulsion, operation, and structure of the proposed design. FDM AM
technology shorten design cycles and lead times [126]. Furthermore, Airbus has
used rapid prototyping to test and develop a small-sized unmanned aircraft proto-
type, the structure of which is 90% manufactured from plastic polyamide powder.
The time-saving measures of rapid prototyping allowed the aircraft to be manufac-
tured in only 8 weeks [127].

2.3.4 Repair
Using AMTs for repair has several profitable outcomes. First, AMTs allow for
expensive, damaged parts to be repaired instead of scrapping and replacing them.
This has been shown to have significant cost savings [68]. Studies have also shown
that repair through AM has a significantly smaller environmental footprint when
compared to repair through conventional processes [128]. This section provides
applications of AMTs for part repair under two categories: geometry restoration
and structural integrity restoration.

Figure 2.6 (A) Complete aircraft model for wind tunnel testing [125]. (B) Flapping-wing
UAV [91]. UAV, Unmanned aerial vehicle.
Review of additive manufacturing technologies and applications in the aerospace industry 21

2.3.4.1 Geometry restoration


Geometry restoration focuses on restoring missing and worn geometry of the part.
This is relatively easy to achieve given current DED processes, and provides direct
and immediate cost savings [3]. In the commercial sector, the company Optomec
has created the LENS Blisk Repair Solution system, which uses DED processes to
repair blisks and other complex aircraft parts. Optomec did a case study on a T700
blisk, which had suffered erosion damage on the leading edge of the airfoils [109].
Fig. 2.7 shows the results of this study. RPM International Inc demonstrated a low-
wattage repair of titanium components [129]. This type of low-wattage repair
exhibited minimal distortion, making this application suitable for structural compo-
nents of aircraft [129].
Researchers at Pennsylvania State University have successfully repaired compres-
sor blade tips of the F402 engine in an AV-8B, resulting in increased engine perfor-
mance [130]. LMD has been used to repair a CFM56 HPT Turbine Shroud SX [131].
The repair steps taken include scanning the damaged surface, planning the deposition
path, and depositing melted powder to form the renewed SX structure [131].

2.3.4.2 Structural integrity restoration


Structural integrity restoration looks at restoring or enhancing the structural integ-
rity of a part. This typically involves repairing cracks and corrosive damage and is
usually done through SPD [55,81,82]. RUAG Australia used an aluminum alloy
SPD to prevent the corrosion of the magnesium alloy main transmission of a Royal
Australian Navy Seahawk [55]. The United States military used titanium SPD to
repair chafing damage on an aircraft hydraulic line [132].
SPD can also be applied to overlapping joints to increase structural integrity of
the joint and prevent further corrosive damage. Hence, SPD can be used to repair
holes and avoids the structural integrity compromises of traditional patch and
strap repairs [55,81]. Furthermore, the application of an SPD doubler on a fuselage
lap joint has shown significant reduction in peak stress compared to the fuselage
lap joint without the SPD doubler [81].

Figure 2.7 (A) Airfoil repair using a LENS additive manufacturing system. (B) T700 blisk
after edge repair. (C) T700 blisk after finishing. LENS, Laser engineering net-shaping.
Source: Optomec, LENS Blisk Repair Solution.
22 Additive Manufacturing for the Aerospace Industry

2.4 Challenges and potential future applications


2.4.1 Challenges
2.4.1.1 Manufacturing limitations
All AM technologies have limitations in terms of resolution, build quality and con-
sistency, and warping, among other defects [9]. Of particular interest in the aero-
space industry are the limitations associated with AMT. For metal sintering
processes, the part resolution is limited to approximately 90% of the powder’s size
[43]. For melting processes, the part resolution is limited by large powder particles,
which increase the size of the melt pool [43]. Additional resolution limitations and
uncertainties source from minimum incremental length of servo motors and transla-
tion quality of the CAD model to nozzle path planning [43].
Similarly, DED processes have shown that build quality can be inconsistent
from build to build [133]. This can lead to uncertainty when measuring material
performance at different regions of a part. Furthermore, there is significantly high
cost associated with qualifying materials in the aerospace industry through tradi-
tional methods [133]. While a system’s build quality can be predicted and
accounted for, this quality can change with the manufacturing of new parts or sub-
sequent use the AM system.
For AMTs, the spot size (area of energy source on powder) can be subjected to
large variations across different combinations of energy sources and metallic pow-
ders. Depending on the emissivity and reflectivity of the powder, the powder can
strongly reflect incoming energy sources, resulting in the powder not melting
completely [43]. Additionally, resulting residual stresses and distortions, from sin-
tering and melting processes, cannot always be predicted. Specifically, due to their
nature, buckling distortions can be difficult to predict [133]. This limitation is espe-
cially relevant to large topology optimized designs containing thin trusses [133].
Furthermore, large build volumes may be expensive or unrealistic for AMTs that
require an inert atmosphere or vacuum.

2.4.1.2 Postprocessing realities


For aerospace applications, most DED and PBF processes will require some type of
postprocessing [43]. Processes that use powder as the feedstock often produce
parts with substantial porosity. This can be addressed with a hot isostatic pressing,
which reduces porosity and increases part strength and reliability [43,134,135].
Occasionally an annealing postprocess is applied to consolidate the grain structure
and obtain desired properties [43].
Surface finishing is often required for AM parts in aerospace applications. While
traditional machining tools can finish the surface of most parts, complex parts often
require unconventional methods, such as shot peening, chemical etching, and vibra-
honing [43]. This need can limit the complexity of topology optimized parts, as the
need and feasibility of surface finishing must be considered [133]. This can delay
the lead time for parts and reduces the buy-to-fly ratio of the part, however these
Review of additive manufacturing technologies and applications in the aerospace industry 23

are still relatively small compared to traditional manufacturing methods and can be
improved with further innovation of hybrid manufacturing systems.

2.4.1.3 Specification and standard development


While there have recently been several new standards on AM for aerospace applica-
tions [136], there remains a large amount of research to qualify AM components.
Furthermore this research is open ended and often lacks consensus [133]. Although
the use of AM for aerospace components is not a novel application, the process of
standard development for this application is in its infancy and is gradual [137].
Current standards have been developed specifying feedstock details, defect types,
and inspection methods for additively manufactured parts; however, surface finish
improvement techniques and damage tolerance refinements are potential areas for
development [136,138].

2.4.2 Potential future applications


Through the vast geometric freedom offered by AM technologies, multifunctional
structures are more easily obtainable and have many potential advantages for the
aerospace industry. Multifunctional structures are structures that can perform sev-
eral engineering functions at once. This can be seen through part consolidation or
part redesign and innovation. Several examples include embedded electronics
within structures or surfaces (composite layers), structures with rigid and soft mate-
rial gradients, integrated acoustic and thermal insulation, and 4D printing [43]. 4D
printing refers to AM of parts with geometries that change with respect to time
through environmental parameters, such as humidity, heat, and radiation [43,139].
PolyJet has started gaining a presence in AM for its ability to manufacture function-
ally complex parts, like multistage responsive 4D and shape-recovering structures
[140,141]. The response of a polymer part to external environments, like tempera-
ture, can be used for the consolidation and removal of assemblies and servo motors,
such as a passive air temperature regulator [141].
Multimaterial DED processes allow designers the ability to tailor a component’s
response and behavior under mechanical loading and thermal environments [1,102]
and help consolidate parts, simplifying the assembly procedure [11]. While topol-
ogy optimization methods have been used for weight reduction, aeroelastic wing
design, and optimum stiffener layout [11,110,142,143], multimaterial DED pro-
cesses allow designers to apply multimaterial topology optimization to aerospace
component design [1].
As AM technologies further develop, the foreseeable increase in system build
volumes will eventually lead to larger and larger part fabrication, with the prospects
of fabricating large components like an airplane wing [1]. AM also has the flexibil-
ity and convenience to establish an on demand, short lead time, supply chain for
aircraft component replacement [1]. Such establishments are currently being studied
for space use by Made in Space, Lunar Buildings, and NASA, investigating the
potential of AM tools and parts in zero gravity environments [1].
24 Additive Manufacturing for the Aerospace Industry

Similarly, AM can be used for quick, cost-effective repair of high-value compo-


nents [1,62,109,132,144]. A majority of the time and cost of AM repair is spent pre-
paring the damaged part for AM repair. Automation of these preparation measures
would allow for an automated repair process, which would have significantly lower
cost and turnaround time when compared to fabricating a new part [1]. Recently,
the European project, RepAIR, has researched a new high-batch repair system for
the aerospace industry [145]. The system automatically determines geometrical
deviations between the damaged part and original part and uses this data to recon-
struct the geometry. Further development includes further automation of surface
preparation and support for large-scale components. These automated repair sys-
tems can be incorporated into short turnaround supply chains that analyze a dam-
aged component and decide if it is eligible for repair or needs an on demand
replacement part fabricated.

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Qualification and certification of
metal additive manufactured 3
hardware for aerospace
applications
Richard Russell1, Douglas Wells2, Jess Waller3, Behrang Poorganji4,
Eric Ott4, Tsuyoshi Nakagawa5, Hector Sandoval6, Nima Shamsaei7 and
Mohsen Seifi8
1
NASA Engineering and Safety Center, Kennedy Space Center, FL, United States, 2NASA
Marshall Space Flight Center, Huntsville, AL, United States, 3NASA-Johnson Space Center
White Sands Test Facility, Las Cruces, NM, United States, 4General Electric Additive, West
Chester, OH, United States, 5JAXA Safety and Mission Assurance, Tokyo, Japan,
6
Lockheed Martin Missiles and Fire Control, Grand Prairie, TX, United States, 7National
Center for Additive Manufacturing Excellence, Auburn University, Auburn, AL, United
States, 8ASTM International, Washington, DC, United States

3.1 Introduction
Additive manufacturing is revolutionizing the traditional aerospace part design and
manufacturing paradigm. For existing designs, additive manufacturing offers the
ability to reduce cost, especially for one-of-a-kind or limited production run quanti-
ties. For new designs, high cost and long lead times associated with the production
of complex hardware by conventional manufacturing routes have convinced manu-
facturers to rely on meticulous analyses to mitigate or eliminate the chance of fail-
ure. With the advent of additive manufacturing, prototype hardware designs can be
iterated early in the design cycle with minimal cost and impact to schedule, restor-
ing the role of incremental testing and iterative redesign.
It is anticipated that by using metal additive manufacturing processes, aerospace
companies will be able to produce essential, but otherwise unavailable, on-demand
parts of simple design in days rather than months once process and part qualifica-
tions have been performed. Significant reductions are also anticipated for the
design, development, test, and evaluation (DDT&E) time for more complex aero-
space components and systems such as commercial aviation gas turbine engines [1]


Disclaimer: The views presented in this paper are those of the authors and should not be construed as
representing official rules interpretation or policy of ASTM International, General Electric (GE),
Lockheed Martin Corporation (LMCO), National Aeronautics and Space Agency (NASA), Japanese
Space and Exploration Agency (JAXA), or the Federal Aviation Administration (FAA).
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00003-0
© 2019 Elsevier Inc. All rights reserved.
34 Additive Manufacturing for the Aerospace Industry

or spaceflight rocket engines [2]. For example, in National Aeronautics and Space
Administration (NASA) rocket engines, which can contain a variety of metal addi-
tive manufactured (AM) components including turbopumps, injectors, combustion
chambers, and nozzles, reductions are anticipated in the DDT&E time (710 years
to 24 years), hardware lead time (36 years to 6 months), and costs (order-of-
magnitude reductions possible) [2]. Other benefits are also anticipated, namely
reduced weight, lower subassembly part counts, smaller inventories, high levels of
geometric complexity, and better performing topology of optimized parts [3].
However, to realize these gains and exploit the full potential of additive
manufacturing, robust quality control and qualification procedures along with clear
interpretation of certification requirements are needed, especially for fracture criti-
cal metal AM hardware. Because the concepts of qualification, certification, and
quality control are related to one another and are frequently not easily separable in
the literature on this subject, this chapter will use the terminology Q&C (qualifica-
tion and certification) when the three concepts are being considered as a group, but
will occasionally refer to the individual terms when differentiation is needed.
Despite the lack of publicly available Q&C procedures for AM hardware, some
aerospace companies and organizations have begun, or are planning, to install AM
hardware in aircraft and spacecraft. To enable this advancement, internal proprie-
tary processes for qualification and quality control have been developed by some
organizations. On the commercial aviation side, General Electric (GE) has received
Federal Aviation Administration (FAA) approval to fly a metal AM compressor
inlet temperature sensor housing in its GE90 jet engines [4], has dual certified with
the FAA and the European Aviation Safety Agency metal AM fuel nozzles for its
Leading Edge Aviation Propulsion (LEAP) engine and has subsequently ramped up
component production and engine shipment [5]. On the noncivilian side, NASA is
actively considering the use of metal AM components in its rocket engines [6,7]. In
these types of applications, it is essential to manage risk with appropriate Q&C pro-
cedures. Some examples of AM metal hardware used or slated for use in civilian
and noncivilian aerospace applications are shown in Figs. 3.1 and 3.2, respectively.
While additive manufacturing is increasingly being used in the development of
new products in the aerospace sector, a universal understanding of the contributions
and control methodologies for dimensional tolerances, anomalies such as pores and
voids, microstructural variations, higher than desired surface roughness, and resid-
ual stress along with their potential effect on part acceptability and mechanical
properties are still developing. If not fully understood for the material and part
being implemented by the component and system owner, efforts to manage perfor-
mance risks can limit a part’s use especially in high-value or mission-critical appli-
cations. In some cases, engineering inexperience in the technology area, by itself,
may also contribute to a system owner’s conservatism in design and application.
Like many other conventional manufacturing processes, variation in part quality
and mechanical properties exists but can be minimized by implementing appropri-
ate process controls. These process controls are preemptive measures that mitigate
or eliminate factors known to influence part quality and the finished part’s proper-
ties. Process control methodologies are known and widespread in the production of
Qualification and certification of metal 35

Figure 3.1 FAA-approved T25 compressor inlet temperature sensor (left), and fuel nozzle
for the CFM International (partnership between GE Aviation and Safran Aircraft Engines)
LEAP jet engine (right), both employing GE additive manufacturing processes. GE, General
electric; LEAP, leading edge aviation propulsion.
Source: Adopted from T. Kellner, The FAA cleared the first 3D printed part to fly in a
commercial jet engine from GE, in: GE Reports, ,https://www.ge.com/reports/post/
116402870270/the-faa-cleared-the-first-3d-printed-part-to-fly-2/., 2015; T. Kellner, Mind
meld: how GE and a 3D-printing visionary joined forces, in: GE Reports, ,https://www.ge.
com/reports/mind-meld-ge-3d-printing-visionary-joined-forces/., 2017.

Figure 3.2 Additive manufactured injectors (left) and combustion chambers (right)
fabricated and tested by the NASA Marshall Space Flight Center.
Source: Adopted from P.R. Gradl, S.E. Greene, C. Protz, J. Buzzell, C. Garcia, J. Wood,
et al., Additive manufacturing of liquid rocket engine combustion devices: a summary of
process developments and hot-fire testing results, in: 2018 Joint Propulsion Conference,
AIAA Propulsion and Energy Forum (AIAA 2018-4625). ,https://arc.aiaa.org/doi/abs/
10.2514/6.2018-4625..
36 Additive Manufacturing for the Aerospace Industry

high-quality parts and it comes as no surprise that these are key to manufacturing
processes such as additive manufacturing. Because of the intimate link between
process conditions and the development of material structure and quality during the
additive deposition operation, the necessity of defining appropriate levels and types
of process control becomes important for many additive parts. The factors (and
metrics) most commonly implicated for variation of quality and properties in addi-
tive manufacturing are:
G
Feedstock attributes (purity, powder particle shape and size distribution, and chemistry).
G
Processing conditions and controls (laser or electron beam power, hatch width, and scan
rate).
G
Thermal conditions during build (layer thickness and platform preheating).
G
Build atmosphere and purity (shield gas or high vacuum).
G
Post-processing [Hot Isostatic Pressing (HIP), heat treatment, and machining].
G
Finished part properties (microstructure, discontinuities, roughness, and nondestructive
and destructive test methods).
G
Equipment (machine to machine variation, calibration, and maintenance).
G
Personnel (training and certification).
G
Facilities (certification).
While a robust Q&C program will address the above factors, it must be pointed
out that several technology areas are being actively developed that hold the promise
of more effective control of the processingstructureproperty envelope for a
given AM process. These areas are: (1) integrated design approaches for materials,
processes, and parts; (2) physics-based models relating to process, microstructure,
and properties; and (3) closed-loop, in-process monitoring methods and improved
process analytics for detecting real-time material and process anomalies [8,9].
While these areas are highly desirable for the qualification path and in an ongoing
quality control plan, additional research is needed before being fully incorporated
into future metal AM Q&C methods. At the core of this future Q&C push, lies the
premise that the source(s) of process-induced discontinuities and microstructural
heterogeneity must first be understood, thresholds of acceptability determined, and
then mitigated by control of the AM process(es). Also, since location-dependent
properties in as—built AM parts are affected by complex interactions between dis-
continuity—dominated and microstructure-dominated failure mechanisms, the inter-
action between discontinuities and microstructure needs to be better understood
[10,11]. This highlights the need for a comprehensive examination of various fac-
tors (e.g., discontinuities, microstructure, and residual stress, etc.) controlling the
mechanical behavior of AM materials, while also integrating modeling and experi-
mentation efforts to produce AM parts with the desired location-specific properties
[1214].
In the past five years, road mapping activities by the National Institute of
Standards and Technology (NIST) [15] and NASA [16] have echoed and expanded
on the above Q&C needs and challenges related to metal AM materials, processes,
and parts. For example, the 2013 NIST metals-based AM roadmap identified four
key Q&C needs impeding largescale deployment of AM; namely, closed-loop
Qualification and certification of metal 37

process control, standardized Q&C guidelines, shared databases, and established


protocols for making reproducible parts. The 2014 NASA roadmap identified needs
specific to nondestructive evaluation (NDE), such as developing standardized NDE
methods tailored specifically to metal AM parts, obtaining a better understanding of
effect-of-defect on finished part properties, and adopting quantitative NDE accept/
reject criteria. Although significant progress has been made in each of these areas
since 2014, NDE-based Q&C of metal AM hardware is still evolving. Existing
NASA quality documentation [17,18] calls out NDE for Q&C of spaceflight hard-
ware made by laser-powder bed fusion (L-PBF) as part of the general part produc-
tion quality control requirements. However, procedural details of the actual NDE
methods used on the shop floor are not given. This is despite the fact that NDE is a
means to accept/reject a L-PBF part and can determine whether a part is approved
for service or returned to an internal material review board for final disposition
(which will be addressed in Section 3.6). Fortunately, the state-of-the-art of cur-
rently available NDE methods that have application to AM hardware is rapidly
evolving. Some of the more established methods are computed tomography (CT),
eddy current (ET), metrology (MET), process compensated resonance testing
(PCRT), penetrant testing (PT), radiographic testing (RT), and ultrasonic testing
(UT). These methods have been captured in a soon-to-be-completed draft of the
American Society of Testing and Materials (ASTM) standard [19].
While production of an AM part can be conducted within one company (from
initial product design through to processing and post-processing, and finally to the
finished product), qualification of such a part for use in civilian and noncivilian
applications can require the collection of a large amount of labor-intensive proces-
sing, microstructure, and property-based information. In many cases, data must be
collected by the Original Equipment Manufacturer (OEM) from many different
companies, who must then make the information available to pave the path for
eventual Q&C. However, there are many potential intellectual property hurdles in
both the generation and analysis of such data [10]. One approach that can provide
the necessary infrastructure to accelerate Q&C involves the use of an Integrated
Computational Materials Engineering (ICME)-based platform (MiCloud.AM) to
develop an understanding of the microstructure, potential defects, and source(s) of
defect generation [20]. These are all influenced by process control while linkages
between those variables and melt pool geometry are required to eliminate/minimize
such defects and produce the desired properties. While ICME is not covered in this
chapter, it does warrant mention.

3.2 Special considerations for fracture-critical hardware


The level of criticality of AM aerospace parts is expected to increase as this tech-
nology matures and gains widespread acceptance [21]. As the use of metal AM
parts in fracture-critical applications becomes more accepted, the need for Q&C
38 Additive Manufacturing for the Aerospace Industry

standards covering all aspects of the part lifecycle becomes more prevalent.
Fracture-critical properties are affected by a variety of factors and two of the domi-
nant factors are discontinuity density and microstructural variation.
While the goal of producing defect-free parts in as-deposited materials remains
an area of extreme interest, inspection procedures (e.g., CT, MET, PCRT, and UT,
etc.) and various post-processing techniques (e.g., HIP and heat treatment, etc.)
may continue to be needed in fracture-critical applications. However, noncritical
locations with no structural demand (i.e., low stress or strain) in fracture-critical
parts may not require the same damage tolerance or properties as required in highly
stressed areas.
The type and rigor of Q&C procedures will be driven by the relevant industrial
sector and end-use application (aerospace, defense, medical, energy, or automotive).
For example, the Q&C requirements for high-value, limited quantity production run
aerospace parts will be more stringent than for high quantity production run com-
modity parts. These requirements will, in large part, be attributable to the unique
safety concerns associated with human space flight and with military and commer-
cial aviation which impose added rigor and stringency than is justified in other
sectors.
As is noted elsewhere [3], perhaps the key challenge confronting NASA
[17,18], the FAA, Department of Defense (DoD), and the commercial aerospace
sector [21] is the qualification of fracture-critical AM parts using either inspection
(NDE) or testing, especially in applications where structural margins are low and
the consequence of failure is high. Such parts use a damage-tolerant rationale and
require careful attention. Currently, it is not clear that defect sizes from NASA-
STD-5009 [22], which were derived from conventionally made metal hardware,
are applicable to AM hardware, particularly when the as-built AM part surface is
still present and surface-sensitive NDE techniques such as ET and PT are used.
To quantify the risks associated with these parts, it is incumbent upon the struc-
tural assessment community, such as the ASTM Committee E08 on Fracture and
Fatigue, to define critical initial flaw sizes (CIFS) for the part in order to establish
the objectives of the NDE. Specifically, more effort needs to be focused on the
characterization and understanding of fatigue and fracture properties of AM mate-
rials and the corresponding testing methodologies. In addition to “conventional”
crystallographic fatigue crack initiation mechanisms in homogeneous substrate
materials, crack initiation due to the presence of inherent AM material anomalies
such as porosity, lack of fusion defects, or inclusions also needs to be considered
[2329].
It should be noted that the characterization of flaws in fracture-critical AM parts
needs to be based on realistic variation in material properties, microstructure, and
material defect characteristics representative of the full-scale production environ-
ment. Failure to do so may result in “lessons learned” similar to those experienced
during the early days of powder metallurgy (PM) when an undetected nonmetallic
inclusion in a PM turbine disk was found responsible for the failure of a fracture-
critical component that caused the crash of an F-18 aircraft [21].
Qualification and certification of metal 39

3.3 Current qualification and certification state-of-the-


art and gap analysis
Broader Q&C standardization needs for AM have been recently addressed in a vol-
untary consensus standards (VSC) gap analysis performed by the America Makes-
American National Standards Institute (ANSI) Additive Manufacturing
Standardization Collaborative (AMSC) [30]. Federal agencies, including NIST,
NASA, the DoD, FAA, and others, as well as several standards development orga-
nizations (SDOs) were instrumental in the formation of this collaborative. SDOs
whose scope of work directly or indirectly relates to aerospace AM standardization
include the American Society of Mechanical Engineers (ASME), ASTM
International, American Welding Society (AWS), International Organization for
Standardization (ISO), Metal Powder Industries Federation (MPIF), and the Society
for Automotive Engineers (SAE) International. This collaborative recognized the
need for AM standards and conformance procedures to advance the adoption of
AM technologies in the United States which, to date, has been largely dependent on
proprietary OEM specifications. Unfortunately, AM does not have the benefit of
years of incremental refinement by third-party practitioners and OEMs. To counter
some of the inefficiencies and shortcomings associated with a reliance on OEMs
and to develop technologies having a broader national impact, America Makes and
the Penn State Center for Innovative Materials and Processing-3D (CIMP-3D)
cosponsored a technical exchange meeting in October 2015 to coordinate United
States’ standards development activities for AM [31]. This meeting and initiative
led to the formation of America Makes-ANSI AMSC, culminating in a recently
released standardization roadmap [30]. The AMSC roadmap can be viewed as a
tool to help focus and combine resources where possible, by bringing together sta-
keholders in the planning and development of industrywide standards and related
research and development (R&D) activities to the extent R&D is needed. The stan-
dards identified by the AMSC are deemed important for use by industry during
qualification of AM materials, processes, and systems, as well as use by regulatory
bodies during certification of AM parts.
To develop the roadmap, the AMSC took the approach of conducting a lifecycle
assessment of an AM part, from initial design, through production, and ending with
post-production testing, qualification, and maintenance. Thus, the AMSC initially
organized itself around five primary working groups covering Design, Process and
Materials, Q&C, NDE, and Maintenance. The Process and Materials group was fur-
ther divided into four subgroups covering Precursor Materials, Process Control,
Post-Processing, and Finished Materials Properties. This approach allowed Q&C
and Q&C-related standardization gaps to be identified.

3.3.1 Standardization gaps related to qualification and


certification
Whereas metal AM parts are tested for performance much the same as traditionally
manufactured cast, wrought, and forged items, there are aspects unique to AM that
40 Additive Manufacturing for the Aerospace Industry

must be addressed before such parts are deployed for service. This is especially true
for mission- and safety-critical parts and applications. For example, a critical part
may be required to be built from qualified materials, using qualified processes, etc.
There are many types of qualifications that can be discussed within the scope of
AM. As such, Q&C is a major focus area for AM parts [15]. In the most recently
released roadmap [30], 95 standards are identified that are either in progress or
identified for development. Of those standards, 11 are listed in Table 3.1 according
to priority that deal specifically with Q&C of aerospace AM parts. While this list is
noninclusive, it is representative of the standardization needs of the aerospace sec-
tor. Standardization needs for the medical sector [30] which may have some appli-
cation to the aerospace sector such as protocols for image accuracy (QC7),
personnel training for image data set (QC9), and verification of the 3D model
(QC10) have not been included in Table 3.1.

3.3.2 Recent directions in qualification, certification, and quality


control for additive manufacturing
Input was invited from AMSC participants on relevant qualification procedures
[30], allowing current Q&C guidance documentation to be identified. For example,
aviation, space, and defense organizations must provide, and continually improve,
safe and reliable products and services that meet or exceed customer and applicable
statutory and regulatory requirements. To accomplish this goal and to help improve
and sustain its overall quality performance with respect to the products and services
provided, an organization can adopt a quality management system (QMS). A QMS
commonly used by the aerospace industry is SAE AS9100 [33] (or an approved
equivalent). A QMS is required to ensure necessary process controls and to mitigate
risks associated with noncompliance, especially in cases where there is significant
reliance on process controls for the reliability of the product.
In addition to a QMS, another key resource that aerospace companies use to con-
trol their vendor supply chains is the National Aerospace and Defense Contractors
Accreditation Program (NADCAP) [34]. NADCAP is an industry-managed program
administered by the Performance Review Institute (PRI) devoted to improving qual-
ity and reducing costs of special process accreditations throughout the aerospace
and defense industries. Prior to NADCAP, aerospace companies audited vendors in
their supply chain using their process requirements to verify compliance. Since the
processes used by vendors were often similar or identical, this led to duplicate
audits that added to the workload without adding value. In October 2013, the
Welding Task Group was assigned the responsibility to assess AM industry needs
and develop audit criteria specifically for AM vendors, focusing on L-PBF and EB-
PBF processes [30]. Draft checklists were developed, culminating in the approval
of the checklist AC7110/14 [35] in early 2017. Since then, audits have been per-
formed and suppliers accredited to the AC7110/14 checklist. Based on early com-
ments, future revisions are planned. In addition to the AC7110/14 checklist, a core
checklist relevant to AM, AC7110, is also available [36]. The NADCAP checklists
Qualification and certification of metal 41

Table 3.1 Prioritized list of standardization gaps related to quality control, qualification,
and certification of aerospace partsa

Gapb Recommendation Priorityc Organization(s)


Harmonization of Adopt uniform terminology High ASTM F42/ISO
AM Q&C for the terms qualification, TC 261,
Terminology certification, verification, ASME, SAE
(QC1) and validation captured in
ISO/ASTM 52900 [32]
AM Part Develop a part classification High NASA, AWS
Classification system to describe the level
System (QC2) of risk associated with a
part and may be used as a
metric to gauge appropriate
qualification requirements
Material properties Develop standards identifying High ASTM F42/ISO
(FMP1) the means to establish TC 261, SAE,
statically validated AWS,
minimum mechanical MMPDS,
properties for metals made NIST
using a given set of AM
parameters for a given
design
Harmonizing Q&C Develop standardized Medium ASTM F42/ISO
terminology for terminology for process TC 261, AWS,
process parameters for use across all SAE
parameters (QC3) AM equipment,
incorporated into ISO/
ASTM 52900 [32]
Post-processing Issue guidelines that require Medium AWS, ASTM 42/
qualification and consistent post-processing ISO TC 261,
production builds for the various AM SAE
(P1) processes to be applied for
qualification and production
builds
Process approval for Starting with the most mature Medium ASME, ASTM
DoD-procured technologies, such as F42/ISO TC
parts (QC4) L-PBF, develop standards 261, DoD,
that assess required checks Industry, SAE
for levels of criticality and
safety as part of the DoD
procurement process. DoD
should participate in the
development of such
standards and specify the
certification requirements
needed
(Continued)
42 Additive Manufacturing for the Aerospace Industry

Table 3.1 (Continued)

Gapb Recommendation Priorityc Organization(s)


Machine Develop guidelines for control Medium NIST, AWS,
qualification of machine-to-machine SAE, ASTM
(PC4) variability using broader F42, DoD,
part-specific, process- NASA
specific, material-specific,
and application-specific
practices beyond fit and fit
Data fusion (NDE5) Develop industry standards to Medium ASTM
allow combination of
additional or
complementary NDE data to
provide a simple, unified
interpretation of results
Phantoms (QC8) Develop materials- and Medium ASTM, ISO
process-specific guidelines
for creating and using
phantoms used to check the
accuracy of a given process,
based on what is being
imaged and the modality in
use (for example, CT or
UT)
Machine operator Develop AM operator training Low NASA, SAE,
training and and qualification standards AWS, OEMs,
qualification or guidelines. Training ASTM F42/
(QC5) should cover the various ISO TC 261
AM materials and processes
available in the market and
be performance based to
ensure consistent AM part
quality
Neutral build file Develop a standard AM file Low ASTM F42 and
dormat (D20) format building on STL and ISO/TC 261
AMF that can represent all
applicable slice files, build
path, materials, density,
orientation, etc., into a
single file format
a
AM, Additive manufacturing; ANSI, American National Standards Institute; ASME, American Society of
Mechanical Engineers; ASTM, American Society for testing and Materials; AWS, American Welding Society; CT,
computed tomography; DoD, Department of Defense; ISO, International Organization for Standardization; NASA,
National Aeronautics and Space Administration; NDE, nondestructive evaluation, NIST, National Institute of
Standards and Technology; OEM, Original Equipment Manufacturer; Q&C, qualification and certification; SAE,
society for automotive engineers; STL, stereolithography; TC, technical committee; UT, ultrasonic testing.
b
Analogous gaps in Ref. [27] given in parentheses.
c
Rankings based on four criteria: (1) criticality, (2) achievability, (3) scope, and (4) effect [30].
Qualification and certification of metal 43

are used by some aerospace prime vendors. Basic elements of the Q&C approach
used by aerospace primes GE and Lockheed Martin are discussed in Sections 3.4.1
and 3.4.2, respectively.
The Metallic Materials Properties Development and Standardization (MMPDS)
Handbook [37], which was formerly published as MIL-HDBK-5 (obs.), is an
accepted source for metallic material and fastener system “A” and “B” basis design
allowables recognized by the FAA, DoD, and NASA. The MMPDS has had limited
exposure to a few AM materials, beginning with AMS 4999 [38]. However, at pres-
ent, no metal AM alloys are included in the Handbook. Inclusion of an alloy and
material form in the MMPDS is predicated on two major factors: (1) the existence
of public industry specifications; and (2) the expectation that a single set of defined
property limits representative of common process knowledge can be reliably estab-
lished. In the case of AM, public industry material and processing specifications
have not generally been available, and datasets submitted to Battelle have been
judged inadequate for deriving publishable design allowables. Specifications for
materials and processes are now beginning to emerge from ASTM, SAE, and ISO,
for example. Common process knowledge sufficient to enable universally accepted
(nonproprietary) capability minimums for AM processes have not yet been forth-
coming. Currently, the MMPDS organization is assessing whether AM materials
could be published in a separate volume or document with special guidance more
suited to AM materials.
Lastly, the objectives and schedules of programs has created a significant pull on
engineering organizations in industry and government to establish AM requirements
as the process understanding evolves. While it is clear that industry standards from
SDOs will eventually play a key role in governing the AM process for NASA
spaceflight hardware, for example, none have yet become sufficiently mature to
adopt independently. Given the significant need to frame the AM requirements in
the context of NASA’s overarching standards for materials, structures, and fracture
control, NASA Marshall Space Flight Center (MSFC) has developed two quality
documents to meet existing materials, structures, and fracture control requirements
for AM parts produced with the L-PBF [17,18]. Some of the more salient features
of the MSFC quality documents will be addressed in more detail in Section 3.5.1.

3.4 Industry qualification and certification approaches


3.4.1 General Electric qualification and certification approach
As part of the industrialization of manufacturing processes, materials and ultimately
components in most fields of use, the qualification of the material, process, and part
are necessary steps in defining, validating, and establishing a production product.
Qualification processes are typically formal validation and approval processes that
follow process and material development stages. The ongoing verification of
continued acceptability with time relies on the closely connected quality control
plan. In some fields of use such as aviation, defense, medical, healthcare, power
44 Additive Manufacturing for the Aerospace Industry

Figure 3.3 Qualification and certification processes relating to materials, processes, and
parts in the manufacturing environment.

generation, and others, an additional certification process may also be required. The
qualification process and subsequent quality control processes typically extend
across organizational/functional boundaries within a producer and between a sup-
plier and customer/part integrator. Certification is more often between a product
producer and a regulatory body. A schematic of Q&C processes is shown in
Fig. 3.3. The attributes of an ongoing quality control regimen for a given AM part
are made up of the QMS required by the system OEM, definition of critical process
control variables, definition of product control measures, agreement on quantifiable
and meaningful process, and product attribute control levels which differentiate
between acceptable and unacceptable products, and measurement/monitoring
frequencies.

3.4.1.1 Qualification of additive materials


In new technologies such as additive manufacturing, it is essential to validate and
demonstrate process maturity and controls that would be the basis of generating spe-
cifications and process documents. This will facilitate and accelerate the development
of analysis methods and associated design allowables that can be constructed using
statistical analysis techniques common in the industry (e.g., the MMPDS Handbook
[37]) or by company-specific property data representation rules. In the additive
manufacturing field, similar Q&C processes are being used to define requirements
and to establish that attributes meet internal, customer, and regulatory requirements.
The procedures used are similar to those for other manufacturing processes like
Qualification and certification of metal 45

casting, forging, and machining, etc., and just like in these conventional manufactur-
ing approaches, each has particular product and process requirements, methodologies,
and sensitivities that must be considered in assuring that high quality and
repeatable products are produced. As additive processing has begun penetrating main-
stream production, particularly in high-technology products, the industry has begun to
develop a more complete understanding of the scope of qualifications and certifica-
tions that are needed. In additive manufacturing, the feedstock (powder or wire mate-
rial) transforms as the build progresses. Therefore, material qualification should
involve the feedstock, melting-solidification transformation processes, and post-
processing (heat treatment, HIP, etc.) requirements.
Recently, the FAA released a draft advisory circular [39] for public comment
relating to certification approaches for additive-produced aviation engine compo-
nents. This document highlights a potential path (but not the only path) to certifica-
tion of flight hardware. Since the certification process is essentially the endpoint of
a series of subtler qualification processes, the content offers insight into the qualifi-
cation steps that are anticipated for AM processes and materials. A summary of typ-
ical qualification steps that a part needs to include from this document are:
G
Feedstock attributes, chemistry, morphology versus acceptability windows and specific
vendor qualifications.
G
Powder handling, use, reprocessing, and reuse limits and controls.
G
AM process parameters, controls, and windows for each material and machine type.
G
Deposition environment controls and windows for each facility and machine type.
G
Validation of material sample performance versus design allowables and specification
requirements.
G
Surface modification process evaluation.
G
Support structures and support and powder removal process qualification.
G
Post-processing controls including heat treatment.
G
Component and witness part inspection using NDE.
G
Component acceptance tests.
G
Component cut-up assessment.

The strong linkage of AM processing to the structure and properties of the mate-
rial and part has driven the need for more careful consideration of raw materials,
processes, and equipment controls. An example is shown in Fig. 3.4 of the varia-
tions in structure of nickel alloy UNS N07718 produced by an L-PBF process, fol-
lowed by differing post-processing treatments helps to demonstrate the range of
behaviors that may result (and variability if processes are not controlled) [40,41].
These effects may be perpetuated through heat treatment. Overall, these effects
reflect layer-by-layer processes creating structure and performance capability, not
merely part shape.
A necessary, but insufficient, condition for the production, qualification, and cer-
tification process is the establishment of specifications that control methods and
acceptability standards for materials, processes, and parts are key to the definition
and control for production additive manufacturing. Frequently these specifications
46 Additive Manufacturing for the Aerospace Industry

Figure 3.4 Examples of microstructural variation observed in laser powder bed nickel alloy
UNS N07718 depending on deposition and post-processing treatment showing: (A) an
as-deposited structure; (B) a mixed directional and equiaxed structure; and (C) an equiaxed
structure produced by variations in thermal post-processing [40,41].

are proprietary to a company, but are shared with a company’s supply base. In the
additive field, SDOs have initiated significant activities described in Ref. [30] to
identify needed publicly available specifications for materials, processes, and parts.
Some examples of these include efforts by the SAE-AMS Additive Manufacturing
Committee, ASTM International Committee F42, ISO Technical Committee 261,
and others. The establishment of these types of accessible, consensus-driven
requirements documents are beneficial for the more widespread implementation of
new processes and for setting baseline expectations on level of capability and reli-
ability to bolster technology adoption and prevalence.
An outline of typical qualification steps for an aviation-type, high-quality com-
ponent is:
1. Completion of development of material (alloy) and process leading to a review and
approval of technology and method maturity and fitness for production using a gated
review process, such as a tollgate or readiness level review. An example may be the
“technology readiness level” and “manufacturing readiness level” type ratings similar to
those defined by NASA and other organizations [42,43]. This is typically a predecessor to
a qualification process, but is necessary to provide the technical understanding to define
specifications, requirements, and essential controls to assure repeatability. The develop-
ment process is also key to providing mechanical performance data and representations of
the variation in data contributed by raw materials, processes, structure, size, and
Qualification and certification of metal 47

geometry, etc., suitable for part design and analysis for service. This portion of the devel-
opment and initial qualification process may involve thousands of hours of technical
effort, tens to hundreds of process trials, hundreds to thousands of test specimens, and
demonstration parts to complete. Timelines may be a few months to several years depend-
ing on intensity of effort, historical experience, complexity, and field of application.
2. Qualification of the raw material (powder, wire, etc.), process, and specific production
vendor to validate both the long-term capability to meet any raw material specification
requirements, but also to demonstrate the fitness of the raw material for use by the addi-
tive process and to establish sufficiency of a vendor’s fixed/controlled process limits in
meeting the overall engineering/manufacturing intent.
3. Qualification of a manufacturing source’s compliance in terms of quality system, controls,
procedures, and facilities for production of certain types of components to industry norms,
such as through ISO, SAE AS9100 [33], and NADCAP [44].
4. Qualification of individual machines and procedures/process limits by trained process
experts to assure that specific equipment is capable of being used for production
manufacturing. The criteria may extend the gamut from spatial precision of optics, set-
tings, and tolerance/control limits to demonstration material specimens for evaluation.
5. Qualification of critical process steps and related machines and procedures for steps that
are considered significant in terms of helping to define the part acceptability, perfor-
mance, and quality. For AM, this includes qualification of specific additive manufacturing
machines, operating procedures, deposition parameter settings and ranges, and even main-
tenance and calibration requirements.
6. Qualification of the final component or subcomponent attributes versus engineering and
quality requirements, drawings, and specifications. This also includes the definition and
approval of fixed or frozen processes which assures that processes, once qualified and
approved, are not changed without consideration of potential partial or full requalification.
Frequently, this qualification step involves nondestructive and destructive evaluations of
initial production parts that have been produced to meet all the relevant requirements.
Attributes may also be evaluated and monitored over time to assure ongoing quality and
reproducibility as part of the qualification process. Regardless, key evaluations are also
then applied to the ongoing quality control plan to assure acceptability of parts over time.
7. Once fully qualified, any changes to the above qualification steps require review and
potentially may need requalification.

Although more extensive than may be necessary in some application fields out-
side of aviation, elements of the above qualification process for additive (and other
nonadditive) parts are equally applicable in other fields.

3.4.1.2 Certification of additive materials


Downstream certification steps may make use of some or all of the qualification steps’
results to demonstrate acceptability to certifying organization or agency requirements.
Some example regulatory requirements for certification of aviation airframe materials
and structures include 14 Code of Federal Regulations (CFR) Part 33 [45] for aircraft
engines, 14 CFR Part 23 [46] for general aviation airplanes, and 14 CFR Part 25 [47]
for commercial transport airplanes, Boiler and Pressure Vessel Code [48] for power gen-
eration and pressure vessel type components, and US Food and Drug Administration
Federal Food, Drug, and Cosmetic Act [49] for medical devices. In general, the
48 Additive Manufacturing for the Aerospace Industry

certification requirements of a regulator pertain to the final product attributes and perfor-
mance and are less often related to the details of the processes by which products are
made. As a result, the continual evolution and advancement of manufacturing process
technology does not necessarily result in a change or addition to regulatory requirements.
The potential for significant disparities in the understanding, application, and level of
control of new processes can create a need for an increasing level of awareness and tech-
nical engagement by regulatory bodies and may also lead to the development of regula-
tory body minimum expectations on the level of disclosure by the part owner to allow
validation of meeting the regulatory requirements.

3.4.1.3 Quality control in additive materials


Primary objectives of quality control are to assure that the process and part meet the
acceptance requirements and that the capability level of the process and part are con-
trolled and represent those verified in the qualification process and do so repeatably
over time. Additional process control guidance from GE for AM is shown in Figs. 3.5
and 3.6 [50]. The process controls shown in Fig. 3.5 parallel analogous controls exer-
cised by NASA MSFC’s quality documents for equipment, materials, and processes
discussed in Section 3.5.1.1. Similarly, the use of nondestructive and destructive tests
by GE in its Q&C activities, as shown in Fig. 3.6, mirrors NASA MSFC’s combination
of inspection and test to develop an integrated rationale for structural integrity of a
part, also discussed later. Measurement and monitoring of process and part quality
occurs at a frequency determined by the sensitivity of the process and material, initial
process/part repeatability, and the application type, criticality, and risk management
needs. Transition to a more integral use of process monitoring, analytics, in situ

Qualify Explicit controls on machine, material and process


(Examples shown, not an all inclusive list)

Powder specification Laser parameters


• Spot size
STRESS CAPABILITY

• Powder source
• Powder size • Laser power
• Powder composition • Laser travel speed
• Powder reuse procedures • Laser dwell time
GE
’s m
Calibration & maintenance Hatch strategy ate
ria
• Preventive maintenance Ind l
• Contour pass
• Pre-build calibration us
• Sky writing try
• Factory environ controls • Line spacing or boundary overlap

Post processing Recoat parameters


• Layer thickness CYCLES TO FAILURE
• Mechanical finishing
• Thermal exposure • Recoater arm material
Contour
• Recoater arm design

Thermal processing Build chamber Hatch


• HIP cycle parameters • Build atmosphere
• Heat treat/solution atmosphere • Purge gas
• Braze HT parameters • Airflow
• Solution temperature • Preheat temp
• Interpass temp
Laser parameters

Figure 3.5 Explicit Q&C controls for equipment, materials, and processes [50]. Q&C,
Qualification and certification.
Qualification and certification of metal 49

Validate Inspection and quality touch points

Qualification Inspection

Machine Material Process Part Non-destructive Destructive

CT/VCT/CMM Functional Part Specimen


checks

Prof Grain size


Defect Fuel flow On-going
pressure porosity
Dimensional recognition airflow Cut-ups material
ultimate surface
other testing
test finish

Validate
In-situ inspection, modeling and analytics

Computational Meltpool
materials process
engineering monitoring

Faster
• Material development
• Process qualification PREDIX Analytics
• Part certification

Figure 3.6 Summaries of GE Q&C activities for additive manufactured parts, including
qualification, inspection, and testing (top) and computational modeling, in-process
monitoring, and analytics approaches (bottom) [50]. Q&C, Qualification and certification;
GE, General Electric.

inspection, and material modeling are being pursued and the technologies are advanc-
ing rapidly to support future integration with Q&C methodologies.

3.4.2 Lockheed Martin qualification and certification approach


Lockheed Marin Corporation (LMCO) was an early adopter of additive manufactur-
ing. Uses today range in technical complexity from trade-show models or rapid pro-
totyping, tooling and test fittings, to production applications. The pace for
implementing additive manufacturing has been driven by the program requirements,
50 Additive Manufacturing for the Aerospace Industry

Figure 3.7 A Lockheed Martin engineer inspects a 3D printed 1.16 m-wide dome prototype
made by an Electron Beam Additive Manufacturing process [51].

cost target, and customer needs. In several cases, use of AM technology has reduced
risk, cut costs, and helped LMCO get new products into the market more quickly.
LMCO’s accomplishments in additive manufacturing are notable. Most recently,
LMCO fabricated 1.16 m-wide titanium domes (Fig. 3.7) to cap off satellite fuel
tanks and in so doing reducing waste, cost, and time of production [51]. The domes,
which were made by an Electron Beam Additive Manufacturing [EBAM (EBAM is a
registered trademark of Sciaky, Inc., Chicago, IL 60638)] process, are some of the
largest AM parts made to date and completed final rounds of quality testing in July
2018. Since a small leak or flaw could be catastrophic for a satellite’s operations,
LMCO engineers and technicians rigorously evaluated the structure, conducting a full
suite of tests to demonstrate high tolerances and repeatability [51].
Qualification and certification of metal 51

Details describing the basic elements of LMCO’s Q&C approach are given else-
where and are driven by part functionality (primary or secondary structure, or non-
structural), criticality (fracture critical or nonfracture critical), and customer
requirements (variable) [52,53]. For example, a part used in a critical structural
application would require more stringent part acceptance testing than a part used in
a nonstructural application or a prototype part with no adverse consequence of fail-
ure [53]. This is similar to NASA’s approach, which will be discussed in
Section 3.5.1, which requires a comprehensive volumetric and surface NDE for all
metal L-PBF parts regardless of the consequence of failure or structural demand
[17]. In NASA’s case, only for parts with a low consequence of failure that could
fit into a “do no harm” category designated as Class C would NDE be waived. This
NASA “do-no-harm” Class C part category or, similarly, the Japanese Space
Exploration Agency (JAXA) nonflight, nonstructural Class C and D part categories,
may be intrinsically similar to LMCO’s nonstructural, noncritical, or prototype part
categories where only a basic quality of workmanship and/or visual inspection is
performed [53].
Similar to industry peers such as GE, LMCO relies on internal and industry stan-
dards along with certifications to SAE AS9100 [33] and NADCAP [34] to deter-
mine compliance of suppliers’ quality systems, controls, procedures, and facilities
for production of AM parts relative to industry norms.
Within LMCO there are various checklists covering applicable part category
classes similar to the checklists developed by NADCAP for metal L-PBF and EB-
PBF parts used in critical structural applications [53]. However, since LMCO is
using a wider variety of AM processes for a diverse range of applications, a need
arose to develop additional checklists suitable for its manufacturing operations.

3.5 Government agency approaches


3.5.1 National aeronautics and space administration
qualification and certification approach
While additive manufacturing offers the ability to manufacture complex part
designs rapidly at a reduced cost, the extreme pace of implementation introduces
risks to the safe adoption of this developing technology. The development of aero-
space quality standards and specifications is required to balance the benefits of
additive manufacturing technologies properly with the inherent risks. Many compa-
nies have developed or are developing in-house standards and specifications for
additive manufacturing. However, as a certifying authority, NASA’s design and
construction standards do not yet include specific requirements for controlling the
unique aspects of the additive manufacturing process and the resulting hardware. A
significant national effort is now focused on developing standards for additive
manufacturing [30]. However, the content and scheduled release of many of the
consensus standards needed to ensure proper Q&C of AM hardware do not support
the near-term programmatic needs of NASA.
52 Additive Manufacturing for the Aerospace Industry

NASA and its commercial partners in manned spaceflight (i.e., the Commercial
Crew, Space Launch System, and Orion Multi-Purpose Crew Vehicle programs) are
actively developing AM parts for flight as early as 2018. To bridge this gap, NASA
MSFC personnel authored a Center-level standard (MSFC-STD-3716 [17]) to estab-
lish standard practices for the L-PBF process. The MSFC standard has been used as
a basis for L-PBF process implementation for each of the manned spaceflight pro-
grams. This standard and its companion specification [18] will provide a consistent
framework for the development, production, and evaluation of additively manufac-
tured parts for spaceflight applications.
Based on the principles of MSFC-STD-3716 [17], the development of agency-
level standards to meet NASA AM-related program needs is underway. A team
with representatives from nine NASA centers with consultants from other govern-
ment agencies has been formed. The goal of this team is to develop standards that
will apply to AM processes being used by NASA and be readily adaptable to all
NASA centers, programs, and projects. Three standards are currently under devel-
opment for manned spaceflight, noncrewed spaceflight, and aeronautics. As part of
this effort, several additional specifications may be required to address raw materi-
als, parts procurement, and processes to supplement these three standards if the
determination is made that no existing VCS standards exist or if existing VSC stan-
dards do not serve the public interest or are incompatible with NASA’s missions,
authorities, priorities, and budget resources [54]. The standards under development
will introduce requirements with guidance that can then be used to develop
manufacturing plans and provide product specifications for both general and spe-
cific applications. The standards will not specifically dictate how to manufacture or
certify a component, but the requirements will identify factors that must be
addressed for all phases of design, manufacture, and qualification.
The NASA standards under development will be applicable to mature technolo-
gies. Specific technologies will be discussed in the documents, but to allow for
expansion, the documents will not be limited to only these technologies. The stan-
dards will concentrate specifically on metals (powder fed PBF, and wire and pow-
der fed Directed Energy Deposition [DED]) and polymers (wire fed FDM/DED).
Materials determined to be out of scope include ceramics, composites, regolith, and
printed circuits.

3.5.1.1 General qualification requirements


The MSFC Technical Standard [17] and Specification [18] provides the framework,
and establishes general requirements, for the development and production of space-
flight hardware produced using the L-PBF AM processes. While structural design
criteria are not dictated, these documents accommodate requirements from NASA’s
governing design and safety standards [5558], thus, providing the necessary con-
trols to ensure safe implementation of AM technology. Fig. 3.8 illustrates the key
products and processes controlled by MSFC-STD-3716 and, figuratively, how each
product or process is related. The general requirements of an Additive
Manufacturing Control Plan (AMCP) that governs foundational process controls
Qualification and certification of metal 53

AMCP General requirements


QMS
MSFC-SPEC-3717
=Requirements levied by MSFC-STD-3716
Feedstock
Foundational process controls specification
Definition of ECP Qualification
Fusion
metallurgical maintenance
process
process calibration
Thermal
process
Qual. Training Training
of met. plan
Machine 1 process
Master
QMP/R
Machine 2 Machine 3 Machine 4 Machine “n”
QMP/R QMP/R QMP/R QMP/R

PCRD SPC criteria


data
MPS
data Design
properties

Part
Part production controls

Design Classify PPP


process part

Pre-prod article Pre-prod article Pre-prod article


plan evaluation report

AMRR
MRB
QPP

Witness
Production SPC, NDE,
Production
engineering acceptance
controls tests

Service

Controlling document, requiring NASA approval.

Controlling document(s), not requiring NASA approval, but available for review.

Active database, not requiring NASA approval, but available for review.

Action or process.

Decisional action or process, with result available for review.

Part Representation of part entering process.

Requirements with procedural details contained in MSFC-SPEC-3717.

Service Representation of part entering service.

Identifies key points of QMS involvement.


Identifies PBF requirements levied by MSFC-STD-3716 with procedures in MSFC-SPEC-3717
Negative outcome of decisional action

Figure 3.8 Key products and processes in MSFC-STD-3716 (top), and symbol legend
(bottom) [17].
54 Additive Manufacturing for the Aerospace Industry

and part production controls is also shown. These controls provide the basis for reli-
able part design and production. Foundational controls include a Qualified
Metallurgical Process (QMP) for each machine, an Equipment Control Plan (ECP),
personnel training, and material property development via a Material Property Suite
(MPS). The MPS is a collection of L-PBF material property data specific to a mate-
rial and process that includes all test data, design values, and criteria needed to
implement and maintain Statistical Process Control (SPC) for the L-PBF process.
Part production controls are typical of aerospace operations and include part cat-
egories, a Part Production Plan (PPP), a Qualified Production Plan, and other mis-
cellaneous production controls. The symbols in Fig. 3.8 (bottom) indicate the type
of product or action, such as internal documents, documents requiring approval,
databases, or decisional actions. Fig. 3.8 further illustrates the flow of the products
and processes through the general, foundational, and part production controls.
While showing the figurative relationships of the key products and processes,
Fig. 3.8 cannot be read as a serial flow chart, particularly in the prerequisite founda-
tional controls. The AMCP also defines how active QMS is integrated throughout
the process. Key points of QMS integration are illustrated with a green triangle
symbol in Fig. 3.8. The AMCP and the QMS govern the engineering and quality
assurance disciplines, respectively, from start to finish.
An essential element for all AM parts manufactured for the aerospace industry is
the creation of an AMCP. The three NASA standards will be based on the princi-
ples put forth in MSFC-STD-3716. This can only be accomplished through tailor-
ing; therefore, an AMCP is needed to document the requirements that are based on
the appropriate NASA standard. The AMCP will also include the means by which
subcontractor and vendor engineering compliance will be managed.
In addition to an AMCP, a QMS that conforms to SAE AS9100 [33] or an
approved equivalent is also required. The QMS will ensure that QA controls are
properly implemented and noncompliance is properly managed.

3.5.1.2 Additive manufacturing part categories


To allow requirements to be tailored for a particular NASA application, a classifica-
tion system has been established to define and communicate the risk associated
with a given AM part and to levy appropriate levels of process control, qualifica-
tion, and inspection. The current NASA MFSC classification system [17], shown in
Fig. 3.9, is based on three key decisions: consequence of failure, structural demand,
and AM risk. Additive manufacturing risk is calculated based on five ratings crite-
ria: (1) Can all surfaces and volumes be reliably inspected, or does the design per-
mit adequate proof testing based on stress state? (2) Can as-built surface be fully
removed on all fatigue-critical surfaces? (3) Are surfaces interfacing with sacrificial
supports fully accessible and improved? (4) Are structural walls or protrusions
$ 1 mm in cross-section? (5) Critical regions of the AM part do not require sacrifi-
cial supports. This decision tree leads to eight distinct classifications.
To aid in tailoring the three proposed NASA standards for manned spaceflight,
noncrewed spaceflight, and aeronautics a slightly different approach was developed,
Qualification and certification of metal 55

Figure 3.9 MSFC-STD-3716 additive manufactured part classification system [17].

Figure 3.10 Proposed classification system for new NASA standards.

as shown in Fig. 3.10. The new classification system has three levels of primary
classification (A, B, and C) and allows for a secondary classification for certain
cases for Class A and B parts. The primary classification drives the tailoring of
requirements for each part and the secondary classification acts as a communication
tool to allow for effective risk management when necessary.
56 Additive Manufacturing for the Aerospace Industry

The first decision gate is the same as given in [17], but the criteria are modified
to address all NASA applications. Initially, a part will be designated as Class A
(high consequence of failure) if one or more of the following criteria are met:
G
Fracture-critical as per NASA-STD-5019A [22].
G
Failure would lead to a catastrophic hazard (i.e., loss of life, disabling injury, or loss of a
major national asset).
G
Failure would lead to the loss of one or more primary/minimum mission objectives.

Note that in the event of part redundancy, Class A may still be applicable if the
project decides that the risk of a common mode failure is credible.
Unlike the classification scheme used in [17], the new classification shown in
Fig. 3.9 will allow parts with a low consequence for failure that could fit into a “do
no harm” category to be designated as Class C. Parts that do not meet this criterion
will be assigned as Class B. The exact definition of which attributes would allow
for a Class C designation is under development.
QA activities requiring inspection (NDE) are only required for parts used in
spacecraft and in applications where there is a structural demand. For spaceflight
hardware subjected to structural loads, but for which NDE cannot be used or is dif-
ficult to perform, a new category A0 is introduced. For spaceflight hardware not
subjected to structural loads, a category C1 is introduced analogous to the proposed
NASA “do no harm” Class C designation. For category C1 parts, no NDE is cur-
rently required by JAXA. Lastly, for hardware not used in spaceflight application, a
category D1 is introduced. These parts are only used during the development phase
or in ground applications. Like category C1 parts, no NDE is currently required by
JAXA for category D1 parts. Analogously, no NDE is required by LMCO for Class
II nonstructural parts and Class I noncritical, prototype, or model parts [53].
Considering the overall similarities and differences between the NASA, JAXA, and
LMCO part classification systems, perhaps the greatest strength of the NASA sys-
tem is the premium placed on assigning and communicating the risk associated
with a given AM part (safety constraint). Similarly, perhaps the greatest strength of
the JAXA system is the premium placed on part design, complexity, and application
as primary drivers of the type and requisite accuracy of any post-process NDE per-
formed (NDE capability constraint).

3.5.1.3 Integrated structural integrity rationale


The largest latent risk associated with AM parts used in critical spaceflight applica-
tions lies in the limitations to verify individual part integrity (see Appendix B in
[17]). Currently, process control methods implemented during build are not suffi-
ciently mature or qualified to verify part integrity independently. In these cases,
structural integrity must be verified through inspection (NDE) or test (proof and
functional acceptance testing) performed in finished parts (or witness coupons) after
build. For parts classified with high AM risk, a combination of inspection and tests
may be needed to achieve full coverage of the part, thus, ensuring its structural
integrity. However, given the extreme diversity of AM parts slated for NASA
Qualification and certification of metal 57

applications, it is not practical to levy specific QA requirements stipulating the


degree of inspection or tests needed for a given part.
Despite the vagaries associated with the manner in which QA activities such as
process control methods, and post-process inspection and tests are imposed, some
simplifying rules do exist. For example, AM parts in NASA Classes A1 through to
B2, as shown in Fig. 3.9, must be subjected to a qualification test program that
demonstrates part performance and functionality meet the design mission require-
ments, life factors, and lifecycle capability [17]. This program also includes com-
prehensive surface and volumetric NDE within the limitations of the NDE method
used and part complexity. Stated differently, the rigor of the inspection and test-
based QA activities used shall be commensurate with the part’s classification. For
example, Class A fracture-critical parts typically require a quantitative rationale
involving, in the case of NDE, the detection of flaws with a known probability of
detection as stipulated in NASA-STD-5009 [22]. The rationale also identifies areas
or volumes of the part relying solely on process controls, that is, not verifiable by
post-build NDE as risk areas for further consideration.

3.5.1.4 Influence of mission classification


For NASA science missions and payloads, a risk-based mission classification is
assigned as per NASA Procedural Requirement (NPR) 8705.4 [59]. Fig. 3.11

Figure 3.11 Mission classes.


Source: Appendix Bin NASA Procedural Requirement, Risk classification for NASA
payloads, in: NPR 8705.4, 2012.
58 Additive Manufacturing for the Aerospace Industry

provides a description of the mission classes. To capture all the missions that would
be covered by the three NASA standards, a total of six mission classes should be
considered:
1. Manned Spaceflight
2. Class A (per NPR 8705.0004)
3. Class B (per NPR 8705.0004)
4. Class C (per NPR 8705.0004)
5. Class D (per NPR 8705.0004)
6. Associated ground support equipment and test hardware
The NASA team considered three possible approaches to how part classification
and mission classification could interact. These three cases are:
1. Part class determines the requirement set independent of mission class (similar to the
JAXA approach).
2. Mission class influences part class through consequence of failure or other criteria.
3. Part class and mission class requirements are combined into a common risk matrix.

The team consensus and recommended approach was that the part classification
and the mission classification should be considered independently. This decision
led to the recommendation to develop three separate NASA standards.

3.5.1.5 Tailoring approach


For each NASA standard, the requirements summary given in Appendix F,
Table VIII, in [17] will be used as the basis for tailoring. Table VIII contains
Additive Manufacturing Requirements (AMRs). For each NASA standard, a unique
requirements matrix will be developed that modifies each AMR to make it applica-
ble for its application. Fig. 3.12 shows an example of a requirements matrix.
The matrix will designate each requirement based on part classification to be used

Requirement
Requirement MSFC-STD-3716 NASA-STD (proposed language)
description A B C Notes
[AMR-3] The CEO responsible for the [AMR-3] The CEO responsible for the
Additive
design and manufacture of L-PBF design and manufacture of AM hardware
AMR-3 Manufacturing
hardware shall provide an AMCP that shall provide an AMCP that
Control Plan
accomplishes each of the following: accomplishes each of the following:
a.Documents the implementation of each a. Documents the implementation of each
of the requirements of this MSFC of the requirements of this NASA
Technical Standard. Technical Standard.
b. Documents and provides rationale for b. Documents and provides rationale for
any tailoring of the requirements of this any tailoring of the requirements of this
MSFC Technical Standard. NASA Technical Standard. See
c. Documents the methods used to Appendix
c. Documents the methods used to control AW T O
control compliance with these for Tailoring
compliance with these requirements by
requirements by subcontractors and Guildlines
subcontractors and vendors.
vendors.

d. Provides for complete governance for


d. Provides for complete governance for
the implementation of L-PBF such that,
the implementation of AM such that, once
once approved by the procuring
approved by the procuring authority, the
authority, the AMCP becomes the
AMCP becomes the document used for
document used for verification of L-PBF
verification of AM requirements.
requirements.

Figure 3.12 Requirements matrix example.


Qualification and certification of metal 59

as-written, optional, or tailorable. Tailoring guidelines will be written and provided


in either the body of the specification or an appendix.

3.5.1.6 Industry standards


The NASA standards will be written to the utilized industry-developed AM stan-
dard when appropriate. Because industry standards are being developed and are rap-
idly changing, a separate NASA specification will be created to list these standards
and provide revision-level configuration controls. This will allow the NASA AM
community to make adjustments without revising the actual standards.

3.5.1.7 Process specifications


The use of process specifications will be defined in the requirements matrix. In
cases where no industry standard exists or the standard is considerably substandard,
NASA may decide to author a unique specification. For areas covered by MSFC-
SPEC-3717 [18]; namely, the procedural requirements for foundational process
control in L-PBF (Fig. 3.8), including, for example, virgin powder and reuse
requirements, process parameters, restart procedures, post-processing, QMPs, equip-
ment calibration and maintenance, facilities qualification, and personnel training,
tailoring guidance will be provided either in the body of the text or in an appendix.

3.5.1.8 Procurement specifications


Guidance will be provided on how to write a procurement specification. Certain
procurement specifications may be written to make it as easy as possible to buy a
“good” part from a “proven” manufacturer. These may not be appropriate for Class
A1 parts on Class A missions. Industry standards will be leveraged as much as
possible. These procurements will focus primarily on raw material requirements,
vendor quality/process controls, historical material property trends, and limited
part-specific requirements. When appropriate, procurement specifications will inten-
tionally be written in a nonspecific manner to allow a vendor to control proprietary
processes.

3.5.1.9 Additional guidance


In addition to tailoring and procurement specification guidelines, additional appen-
dices may be required to cover topics such as:
G
Guidance in writing an AMCP.
G
Guidance in writing a PPP.
G
Guidance on what should be in a process qualification or feedstock specification.

3.5.1.10 Warnings
There is growing concern in the NASA Durability and Damage Tolerance (D&DT)
community [59] that technology gaps exist that may lead to the use of D&DT tools
60 Additive Manufacturing for the Aerospace Industry

beyond their capability. These shortfalls could be accelerated with the use of AM
parts where complex designs and unknown local material properties exist. Several
research studies and development or testing programs have been proposed or are
already underway to close these gaps.

3.5.2 Federal Aviation Administration qualification and


certification approach
Q&C requirements for commercial aircraft parts have been traditionally linked to
the level of part criticality, defined with various degrees of specificity [3,21]. For
instance, the FAA rule for materials (14 CFR 25.603) defines its applicability as
“parts, the failure of which could adversely affect safety” [47]. The FAA Advisory
Circular 25.571-1D defines principal structural elements (PSEs) as elements “whose
integrity is essential in maintaining the overall structural integrity of the airplane,”
including “structures susceptible to fatigue cracking, which could contribute to a
catastrophic failure.” [60] The FAA rule 14 CFR 37.70 for Engine Life-Limited
Parts (LLPs) [61], defines LLPs as parts “whose primary failure is likely to result
in a hazardous engine effect.”
Throughout the FAA rules and guidance materials for various product types, a
common denominator emerges in that an appropriate damage tolerance assessment
needs to be performed on parts of high criticality such as PSEs or LLPs. Two ele-
ments of such assessment are crack growth analysis using fatigue testing and
inspections using NDE. These two elements are also evident in NASA’s [17,18]
quality processes and documents. Due to the random nature of material anomalies
(not specific to AM materials), the FAA Advisory Circular 33.70-1 defining dam-
age tolerance requirements for engine LLPs states that “the probabilistic approach
to damage tolerance assessment is one of two elements necessary to appropriately
assess damage tolerance” [62]. To support such an assessment, the appropriate char-
acterization of material anomalies is needed, in addition to conventional fatigue and
fracture properties of substrate materials. Such characterization should focus on
developing the size distribution and frequency of occurrence of material anomalies.
As discussed in [21], this information can be used to define an exceedance curve
for a given class of material defects which is the key input into probabilistic frac-
ture mechanics-based assessment, such as the one defined in the FAA Advisory
Circulars 33.14-1 [63] and 33.70-2 [64] for specific types of material or
manufacturing defects.
The FAA Part 25 rule for “Fabrication Methods” (14 CFR 25.605) [47] states
that “the process must be performed under an approved process specification” and
that “each new aircraft fabrication method must be substantiated by a test pro-
gram.” However, the rule-level certification requirements often do not define the
specific acceptable testing or inspection procedures. This level of detail has been
left open for the OEM to define as a part of the means to determine compliance
with the rules (i.e., means of compliance or MoC), as reviewed and approved by
Qualification and certification of metal 61

certification authority. Developing effective MoC for new technologies such as


AM is especially challenging. For this reason, standardization of the methods for
testing and inspections can be viewed as enablers for efficient and robust (i.e.,
consistent) Q&C processes across the aviation industry. For AM, being a rela-
tively new technology, the specific testing and inspection procedures are still
under development or are proprietary, and must reflect the unique materials, pro-
cessing constraints, and design attributes of metal AM parts such as anisotropy,
inherent material and microstructural anomalies, residual stresses, and location-
specific properties, etc. [3,21].
Due to the broad range of potential AM applications in civil aviation that include
design and production of new parts, replacement parts, and repairs, the FAA has
recently issued several documents. These include an internal memorandum provid-
ing guidance to the regional aircraft certification offices and Manufacturing
Inspection District Offices regarding the engineering and manufacturing considera-
tions for certification of AM parts, as well as the Notice for the Flight Standards
District Offices inspectors [65], to provide an introduction and awareness regarding
the use of AM technology in maintenance, alterations, and repairs of aircraft and
engine components. The latter notice [65] also cites the “lack of industrywide stan-
dards for AM” as one of the current challenges, certain aspects of which were sum-
marized in Section 3.3.1.

3.6 Summary and recommendations


State-of-the-discipline Q&C approaches used by industry and government to control
AM materials, processes, and parts have been summarized in this chapter. As noted,
the slow pace of adopting much-needed voluntary consensus Q&C standards is
forcing companies and government agencies with procuring authority for AM parts
to establish internal Q&C requirement documentation suited to their needs, pro-
grams, and resources. Aspects of current best Q&C practices adopted by the indus-
try (GE and LMCO) and governments (NASA, JAXA, and the FAA) have been
summarized. Similarities among these best practices have emerged, such as the
need to establish AM part categories to define and communicate the risk associated
with a given AM part and the need to adopt specific testing and inspection proce-
dures suited to the procuring authority’s requirements and OEM’s capabilities. In
addition to levying Q&C requirements for testing and inspection, requirements
must be imposed to control the design, input materials, fabrication processes, equip-
ment, personnel training, and post-processing. All of these requirements issued by
the various procuring authorities are likely to evolve as more information and field
experience become available in the near future.
To facilitate the adoption of future Q&C standards and to further the advance-
ment of Q&C protocols tailored to AM, it is proposed that companies and agencies
62 Additive Manufacturing for the Aerospace Industry

adopt a model of multi-organizational collaboration with peers toward addressing


some of the more complex and labor-intensive Q&C challenges. Possible areas of
collaboration include:
G
Establishment of consensus understanding of the terms qualification, certification, and
quality control and their differences and interrelationships.
G
Develop and adopt Q&C-related industry standards summarized in Table 3.1, especially
those deemed to be high priority.
G
Produce and test new NDE capability standards with intentional features and defects to
mature current NDE detection capabilities for technologically important AM defects,
including improved metrological capability for intricate internal features.
G
Produce and test sacrificial defect standards with known loadings of specific defect types,
sizes, and distributions to determine effect-of-defect and facilitate determination of quanti-
tative accept/reject criteria.
G
Advance current in-process monitoring state-of-the art, focusing on commercially avail-
able monitoring and sensing technologies.
G
Increase industry/government collaboration to advance process analytics, modeling, and
simulation tools.

Acknowledgments
The authors wish to acknowledge Jim McCabe and Sarah Bloomquist of ANSI and members
of the ANSI-America Makes AMSC Qualification and Certification Working Group for their
efforts to identify and prioritize Q&C standardization gaps. The authors also wish to
acknowledge Deborah Whitis of GE Additive for her contributions to the GE section.

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[58] NASA-STD-6016, Standard Materials and Processes Requirements for Spacecraft,
available from the NASA Technical Standards System at the NASA website www.stan-
dards.nasa.gov, 2016.
[59] NASA Procedural Requirement, Risk classification for NASA payloads, in: NPR
8705.4, 2012.
[60] FAA, Damage Tolerance and Fatigue Evaluation of Structure, Advisory Circular
25.571-1D, January 13, 2011, https://www.faa.gov/regulations_policies/advisory_circu-
lars/index.cfm/go/document.information/documentID/865446.
[61] FAA, Code of Federal Regulations Part 14, Airworthiness Standards: Engine Life-
Limited Parts,” Part 37.70, January 1, 2018.
[62] FAA, Guidance Material for Aircraft Engine Life-Limited Parts Requirements,
Advisory Circular 33.70-1, February 24, 2017, https://www.faa.gov/documentLibrary/
media/Advisory_Circular/AC_33_70-1_Chg_1.pdf.
[63] FAA, Damage Tolerance for High Energy Turbine Engine Rotors - Including Change
1, Advisory Circular AC 33.14-1, January 8, 2001, https://www.faa.gov/regulations_po-
licies/advisory_circulars/index.cfm/go/document.information/documentID/22920.
[64] FAA, Damage Tolerance of Hole Features in High-Energy Turbine Engine Rotors,
Advisory Circular 33.70-2, August 28, 2009, https://www.faa.gov/documentLibrary/
media/Advisory_Circular/AC.33.70-2.pdf.
[65] U.S. Department of Transportation-Federal Aviation Administration Notice N 8900.
391, Additive Manufacturing in Maintenance, Preventive Maintenance, and Alteration
of Aircraft, Aircraft Engines, Propellers, and Appliances, Washington, DC, 2016.
Design for metal additive
manufacturing for aerospace 4
applications
Manish Kamal and Gregory Rizza
Arconic Inc., Arconic Fastening Systems, Carson, CA, United States

4.1 Introduction
Additive manufacturing (AM), is a manufacturing process the use of which has
been largely driven by its ability to create relatively unhindered design customiza-
tion while containing fewer process constraints when compared to traditional
manufacturing processes. In traditional design for manufacturing, most steps to part
design assume for simplicity an isotropic material, and the production of part
definitions using any variety of conventional methods, such as forging, casting, or
subtractive machining. AM as a process separates itself from these traditional
methods in that it adds an increased amount of design flexibility when choosing the
shape and geometry of a desired part. As well, the additive capabilities of the
process, involving the fusing of material layer-by-layer, allow for the application of
AM features to a wrought substrate with a differing microstructure. This permits
the creation of custom functionally graded materials through AM, and introduces
the possibility of materials with tailored microstructures designed for specified
applications and performance.
When describing design for AM (DFAM), the authors apply a holistic approach
to the design process, where the method in developing a part that utilizes AM
comprises equally the process of designing the part, as well as the method of its
fabrication. In this view, this chapter will focus on both design and process consid-
erations for AM, and their interrelationship for producing metal components for
aerospace applications. The topics discussed in detail are:
G
Methods and approaches to AM design, identifying the different design techniques
currently in use for AM part design,
G
Process aspects of AM design, illustrating the relevance of material properties, part
performance, and post processing operations (part evaluation and inspection will also be
discussed in some detail),
G
Current design tools available for AM,
G
Economic considerations when evaluating AM as a production process.

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00005-4


© 2019 Elsevier Inc. All rights reserved.
68 Additive Manufacturing for the Aerospace Industry

The objective of this chapter is to give the reader a thorough summary of the
key considerations when deciding whether to manufacture an aerospace product
using AM, and the importance of the interrelationship between part and process.
When selecting AM as a manufacturing method, there are several types of
AM processes that can be used to produce metallic parts. Of these processes, the
two most common AM fabrication systems currently in use are the laser
powder bed systems and directed energy deposition systems [1,2]. Both methods
are currently used today to produce AM parts in aerospace, with the percentage of
AM parts on both aircraft and spacecraft increasing each year [3]. To limit the
scope of this chapter, these two methods for producing AM parts will be the only
methods touched upon in detail.

4.2 Methods and approaches


There is a strong coupling that exists between process and design when evaluating
AM as a method of production. The design freedoms allotted from the various
processes that currently exist for producing AM parts allow for new flexibility
when selecting the geometric design of a part. For this reason, it is difficult to
design a part that utilizes fully the capability of AM without understanding the
flexibility and limitations the process provides. The following section will describe
various methods that are currently being used in the design and development of
AM parts.

4.2.1 Topological optimization


One of the major focal points of AM design is the capability of the process to create
geometry and features that cannot be produced easily or economically using
conventional manufacturing techniques. The AM process lends itself very naturally
to a type of “free-form” design in which complex geometries and features can be
fabricated without inflicting additional process costs outside of the standard costs
associated with the metal AM process. For this reason, many of the AM parts
reported in literature usually have very intricate geometries and shapes related to
the operational performance of the part [14]. To reflect this, Fig. 4.1 shows an

Figure 4.1 Topologically optimized hinge for AM. (A) Initial hinge design, (B) new hinge
designed using topological optimization, (C) additive manufactured hinge. AM, additive
manufacturing.
Design for metal additive manufacturing for aerospace applications 69

example of how an aerospace hinge product has been redesigned to function by


altering the part’s topology, and then fabricated using an AM laser powder bed
process. The topology of the hinge has been modified to meet existing structural
performance requirements, and optimized to reduce the overall weight of the part.
Both performance and cost are key parameters when deciding if AM is appropri-
ate for part fabrication and large-scale production of a specific part. Cost will be
discussed in greater detail later in the chapter, but in terms of design, factors that
directly affect the cost of producing a metal AM part are:
G
Overall part volume and weight,
G
The AM system selected for the printing process,
G
The required secondary operations needed to transition an “as printed” part to a finalized
form that meets geometric, surface and performance specifications.
All these parameters should be considered when deciding to design a part to be
produced using AM.
Focusing on the first design parameters mentioned, part weight and volume, a
major advantage of AM is the ability of the process to allow existing components
within an aircraft or spacecraft to be redesigned resulting in a new, operationally
comparable AM part with some degree of weight reduction over its predecessor
[5,6]. Since weight is always a critical factor for applications related to flight,
weight reduction is a common practice when it comes to AM design methodologies.
However, just reducing part weight through material reduction and expecting com-
parable performance is not a straightforward process. When redesigning an existing
part or designing a brand-new part to be fabricated using AM, the utilization of
some form of topological optimization is usually applied as a guide in the design
process.
Topological optimization is a process that focuses on the modification of the
topology or surface of a structure by altering that surface using a predefined objec-
tive along with applied design constraints. Typically, with metal AM part design,
the objective of a topological optimization is to reduce part weight/volume with the
constraint that the part not yield or fail under the part’s prescribed operational
requirements. In performing a topological optimization of a part, there are several
software tools that can be used to aid in the design process (some of these tools
will be briefly discussed later in the chapter).
Topological optimization through simulation is usually conducted in collabora-
tion with a finite element (FE) software package in which the optimization algo-
rithm uses outputs from a FE model such as stress, strain, contact force, and
displacement. Through an iterative process, the optimization algorithm modifies the
topology of a part until the desired objective is completed within the constraints of
the application [4]. Fig. 4.2 shows an optimization example of an aero-structure
bracket. The optimized part in this case was 2 3 stiffer than the originally designed
part under the same load conditions, and was also 15% lighter in weight. This was
achieved from the bracket being redesigned to meet function rather than to meet an
existing manufacturing process, while striving to reduce as much weight as possible
in the part.
70 Additive Manufacturing for the Aerospace Industry

Figure 4.2 FE topological optimization of a bracket. (A) Initial bracket design, (B) bracket
design after FE topological optimization, (C) additive manufactured bracket. FE, Finite element.

The numerical algorithms used in the topological optimization processes usually


act upon an element’s mass or stiffness, such that through each optimization
iteration, individual element stiffness or mass is altered and adjusted to achieve the
desired optimization objective. To generalize the process briefly, for a structural
component undergoing topological optimization, noncrucial areas outside the load
path will see a reduction in element’s stiffness or mass, while elements in the load
path will be unaffected, since reduction in stiffness could result in not meeting
the desired objective and problem constraints. The ideal scenario for utilizing
topological optimization as a design tool for AM would be using an iterative
optimization process in which many design iterations are generated, eventually
leading toward an optimized final design, which can be numerically validated and
then fabricated using an AM process. In practice, this method is usually more
complicated than this simplified description, and the process of topological optimi-
zation has several attributes that are difficult to generalize for all cases.
There are several challenges that exist when applying topological optimization
as a design tool for AM. Some key challenges that should be considered in the
optimization process are:
G
Topological optimization software, when it is applied in conjunction with a FE software
package, is highly dependent on the boundary conditions and problem setup within the FE
environment. For this reason, if a FE model is not sufficiently representative of the
application of interest, the resulting topological optimized design may not be useful or
adequately meet the desired application requirements.
G
Features or geometries created from a topological optimization may not be easily
fabricated using existing AM processes. Examples of such features could be thin walls,
overhangs, or features that require complex support structures that cannot be easily
removed using secondary operations.
G
Features or geometries created from a topological optimization may have structural
limitations due to the creation of stress concentration sites, and may be more susceptible
to cyclic load failure conditions such as fatigue cracking or partial structural damage
when loaded beyond the material’s yield strength [7]. An example of these types of
features are internal lattice structures used as a replacement for a solid body.
G
Features or geometries created from a topological optimization process may be prone to a
greater collection of defects and material anomalies. This can be due to the specific AM
build process being used, the part’s susceptibility to environmental contamination during
a build, the specific fabrication material, location of the feature within the part, or some
combination of the before mentioned.
Design for metal additive manufacturing for aerospace applications 71

Even though challenges do exist, and the method of topological optimization


applied to AM is not yet a fully streamlined design process, it is still an effective
tool when being applied to AM design. The limitations of the topological optimiza-
tion process, the inputs necessary for the process, and the relevance of generated
outputs based on input assumptions must all be understood to ensure the effective-
ness of the tool. In the end, topological optimization is only one tool of many that
can be applied to AM design, and is best used as a guide when being utilized for
the design or redesign of parts and structures for AM.

4.2.2 Part consolidation


Part consolidation in the framework of AM is a process applied specifically to mul-
tiple part assemblies and structures. It is the method of using the competencies of
the AM fabrication process to reduce a multiple part assembly made up of many
components into a redesigned part that has the same operational functionality, but
designed to include fewer overall components. The benefits of part consolidation in
AM is part simplification, potential performance improvement, and reduction in
necessary tooling and fabrication time. From a manufacturer’s standpoint, fewer
components can be a substantial cost driver in reducing overhead cost associated
with labor, tooling, part traceability, and inventory needed for that assembly.
From an operator or user standpoint, it usually means easier use and maintenance
of the product. For these reasons, part consolidation and simplification directly cor-
relate to cost reduction for both suppliers and customers.
The method of part consolidation in AM is straightforward in that an existing
part or structure made up of multiple components is redesigned to minimize
the number of components needed for functional operation of the part. Fig. 4.3
shows an example of part consolidation in an aero-engine cowl latch, where the
components encompassing the handle assembly (Fig. 4.3A) have been consolidated
into a single component (Fig. 4.3B). The difficulties with this method are not
usually in the execution of the consolidation process, but in the selection of parts
for the process that are appropriate. Typically, cost is the primary driver of part
applicability for this process.

Figure 4.3 AM component consolidation of a jet engine cowl latch (A) initial latch handle
assembly made up of 5 components, (B) AM redesigned handle with components
consolidated into a single component, (C) additive manufactured jet engine cowl latch. AM,
additive manufacturing.
72 Additive Manufacturing for the Aerospace Industry

Part consolidation through AM can be categorized, as can many applications


of AM, as a disruptive process looking to displace an incumbent process for pro-
ducing a part. For example, assume a part is currently made of 3 components, and
the manufacturer of that part has a known order volume and cost of the part and
its associated components. To displace the current manufacturing process using
part consolidation through AM, the goal would be to consolidate the 3 compo-
nents into a single new component with the same/comparable functionality. Still,
for this to be an effective process for the manufacturer of this part, the new AM
part made up of a single component must be at the minimum comparable in cost
and time needed for fabrication to the incumbent process and product. Applying
this general requirement has a limiting effect when evaluating possible parts and
structures for AM redesign. As AM technology improves, and cost drivers to pro-
duce AM parts decrease, the family of parts to which this process can be applied
should grow.

4.2.3 Part integration and repair


The concept of part integration is not new to structure fabrication, but in the
context of AM, it involves the process of combining components or subassemblies
together using AM material as a medium. The benefits of part integration are
application dependent, but a general benefit is utilizing this process to integrate
separate parts using AM to reduce assembly issues or labor. A proposed example of
this application is shown in Fig. 4.4 for aero-engine casing. The existing process for
fabricating a turbine engine case includes complex machining steps whereby
boss and pad features are machined out, holes are drilled and tapped, and specialty
fasteners called inserts or studs are then threaded into these tapped holes. Drilling
and tapping a hole on a large curved surface of a casing with accuracy is inherently
challenging. Additionally, since superalloys are commonly used, this further
increases the difficulty of machining such features. Machinists often invest signifi-
cant time and resources machining a case only to reject the casing in the final
stages of machining due to a faulty hole drilling/tapping or a faulty fastener

Figure 4.4 An aero-engine casing (A) a typical boss feature in a casing, (B) a typical issue
during installation of inserts into boss hole, (C) a hybrid casing with an AM boss feature
encapsulating a machined receptacle added onto a wrought base casing using AM. AM,
additive manufacturing.
Design for metal additive manufacturing for aerospace applications 73

installation because of improper drilling/tapping. In this case, a specially designed


receptacle would be manufactured and prepared to accept an insert or stud. The
receptacles would be placed on the base casing and the boss or pad would be built
around the receptacles using AM, tying the receptacles in place and making them
an integral feature of the boss. This would likely need to be finish machined to
meet the specified surface finish requirements, and inserts/studs would be added
to the receptacle after machining. Since the receptacle has already been prepared to
accept the inserts/studs, installation would be much easier and would reduce the
risk associated with preparing a tapped hole to accept an insert or stud. It should be
recognized that the process is not inherently limited to studs and inserts, but, in
fact, can be used to add other types of hardware, such as bearings, bearing journals,
bushings, inspections ports, or sensors.
Another benefit of the process is its application in maintenance and repair
operations, where a structure or part is repaired using AM when it has incurred
some sort of damage to one of its components that is not easily repaired and
replaced using conventional methods. Rather than scrapping the entire part or
structure, AM material can be added to the damage site as replacement material
reattaching a new component to the structure, and then performing any necessary
secondary operations needed to return the overall part or structure to operation [8].
As stated initially, the use of part integration utilizing AM is application
dependent, and should not be used for all applications involving the combination or
repair of components. Characteristics of AM part integration that affect its
application are material properties and microstructures seen along the interfaces
between the AM material and substrate material. The microstructure of the interface
is highly dependent on the AM process and parameters used for fabrication, and
usually the AM material microstructure will typically not have the fine grain size
seen in wrought materials. So, when applying this method to wrought parts, there
will usually be some transition in microstructure and grain size at the interface,
which may affect the mechanical performance of the structure or part depending on
the specifics of the application (Fig. 4.5). In most applications, though, it is
typically possible to manage AM process parameters to achieve performance
characteristics of the assembly [9].

4.2.4 Other techniques


One application of AM worth briefly mentioning is the use of the process as a
means of increasing the bearing strength of a part or structure. Specifically using
AM as a plating or cladding process to increase the wear resistance of a part, or

Figure 4.5 Inconel 718 alloy material interface between AM material printed atop a wrought
substrate. AM, additive manufacturing.
74 Additive Manufacturing for the Aerospace Industry

using it to create a sacrificial layer along the bearing surface of a part, which is in
contact with a secondary part or structure. This usually involves adding material
onto a substrate of different base material utilizing an AM process. Challenges is
this method usually stem from the quality of the additive and base material inter-
face. Depending on the material choices and AM process used, such issues can arise
from varying residual stresses during printing or the presence of anomalies and
voids at the interface.

4.3 Process aspects of design


Design opportunities with AM, as discussed in the previous section, continue to be
one of the key propellants for interest in AM. Regardless of the manufacturing
techniques used for fabrication, all parts need to perform some function, and this is
where the process aspects of design become critical. Is it possible to print a
part successfully? What kind of performance can be expected from the parts? Is it
economically feasible? The following section touches on these concerns focusing
on the process aspect of AM part design.

4.3.1 Part performance


With any part design, it is important to understand the underlying behavior of
the material being used to simulate part performance. Traditionally, most
designs assume for simplicity an isotropic material, and part sizing is then done
accordingly. Compared with traditional manufacturing processes, AM does not just
provide a great deal of flexibility with design, but it also creates new challenges.
With the possibility of tailored microstructure, functionally graded material, and the
ability to add features to a wrought substrate with a different microstructure, the
traditional realms of design would need to be updated to include design based on
location specific properties in the same part. Also, like most other manufacturing
processes, the microstructure and resultant mechanical properties in AM parts are
process route dependent. Here laser power, scanning strategy, or build orientation
can significantly impact the properties of the part, or the occurrence and magnitude
of defects. Fig. 4.6 illustrates this point. Ti6Al4V properties are shown here as
reported in literature [1013]. Such variation in properties of the material is not
observed with typical manufacturing techniques. The pedigree of the material data
used for part design needs to be fully understood to ensure its similarity to the
intended AM process in order to be confident in the simulation predictions of the
optimized part.

4.3.1.1 Microstructure
There are several public and private entities engaged in AM. Process parameters
and their effects on mechanical properties or distribution of defects tend to be
Design for metal additive manufacturing for aerospace applications 75

Figure 4.6 Boxplots of Ti-64 static mechanical properties at room temperature as reported
in literature [1013].

Figure 4.7 Typical 15-5PH microstructure, with no heat treatment, using a typical laser
powder bed AM system. AM, additive manufacturing.

proprietary company information, and little is reported in published literature.


However, some key points are listed over here.
Since AM deposition is a layer-by-layer process, the microstructure of the
material reflects this effect. Fig. 4.7 shows a typical microstructure observed with
76 Additive Manufacturing for the Aerospace Industry

Figure 4.8 EBAM Ti-64 macrostructure, as-deposited, section normal to X direction.


EBAM, Electron beam additive manufacturing.

laser powder bed printed 15-5PH material. The process involved is the melting of
multiple layers of powder as the laser passes through. In the image, layer height
can be clearly differentiated. Fig. 4.8 shows a similar effect in electron beam AM
(EBAM) printed Ti6Al4V material. This behavior typically has limited effects
on tensile behavior but, depending on material type, may significantly affect fatigue
performance.
Microstructural features are usually much finer with AM processes when
compared to cast parts. This is due to the smaller melt pool and resultant rapid
solidification [1416]. The solidification rate is much higher than what is possible
by traditional casting techniques with up to 104 K/s possible reported with Laser
Engineered Net Shaping (LENS) technique [14]. This provides higher strength to
material via Hall-Petch effect due to smaller grain size. However, there is a range
of AM techniques possible with widely varying deposition rates (0.05 kg/h for
powder bed systems to 7 kg/h for some EBAM techniques), leading to resultant
changes in microstructure. This does provide opportunities to modulate the
microstructure per performance needs; for example, finer grain sizes at an interface
to improve tensile/fatigue properties with larger grains at other areas that are not
critical, lowering the associated deposition costs.
Orientation effects are also observable with the AM microstructure.
Microstructural features may be refined in one orientation and elongated in another.
Fig. 4.9 shows this effect for Ti6Al4V deposited via EBAM. Since the
deposition substrates (build plates) are typically much cooler than the build media,
a preferential heat transfer direction is setup during cooling of the molten metal.
This establishes elongated grains in plane normal to the deposition substrate.
Careful control of deposition parameters may alleviate this effect.
Design for metal additive manufacturing for aerospace applications 77

Figure 4.9 EBAM Ti6Al4V macrostructure, as-deposited at 200 3 magnification. (A)


Section normal to X direction and (B) section normal to Z direction.

If the goal is to use AM as a near-net-shape technique for producing parts, there


is very limited thermo-mechanical work that can be done in the material to refine
the structure further. There are some techniques, like AmpliFORGE, which are
using a hybrid approach by starting with an AM preform to reduce multiple forging
costs, and then refining the structure using a one-step forging operation [17].

4.3.1.2 Defects
Defects may be possible in AM parts. Lack-of-fusion defects and gas porosity or
voids are some of the more commonly observed defects [14,18]. The occurrence
and magnitude of these are dependent on the AM technique applied, and the
corresponding process parameters. With appropriate part/process design and process
controls, these can be significantly minimized or eliminated. A discussion on this is
beyond the scope of this chapter. Additional details on defects may be found
elsewhere in the book.

4.3.1.3 Mechanical properties


Static mechanical properties of AM parts (tensile strength) are typically very close
or slightly lower than their wrought counterparts. Elongation values may be
lower depending on the occurrence of defects. Mechanical properties also show an
orientation dependence, as expected, due to the microstructure changes. X/Y
(directions parallel to the build surface) tensile values are typically higher than Z
(direction perpendicular to the build surface) tensile values, and the degree
depends on the AM technique applied and process parameters. Some specifica-
tions like AMS 4999 for Ti6Al4V show the typical directionality associated
with AM process.
Fatigue values are significantly affected by the AM process and tend to be lower
than wrought counterparts. Fractography shows that fatigue cracks initiate faster in
AM parts due to presence of voids/porosity near surface (see Fig. 4.10).
Process parameters that reduce the occurrence of such porosity/voids are critical in
improving fatigue life. Another way to address the issue is with the use of hot
78 Additive Manufacturing for the Aerospace Industry

Figure 4.10 Example of two 15-5PH H1025 fatigue samples tested at different stress levels
showing the origin of fatigue cracks near surface.

isostatic pressing (HIP). This reduces the size of the pores, lowering the stress con-
centration factor, and improving fatigue life, but at the expense of adding cost to
the final part. Lack-of-fusion defects, which typically have high aspect ratios, are
not desired as they may lower fatigue life more so than spherical pores.
Since AM technology is still at its early stages, other properties like fracture
toughness and creep have not been evaluated as extensively. It is worth noting that
AM part performance is tied directly to process parameters, which can be tuned per
requirements.

4.3.2 Part quality


Any AM parts producer would need to manufacture parts that meet their customers’
quality requirements. These requirements may be dimensional, surface finish,
microstructure, or mechanical property requirements. The following are
some aspects of the AM process that should be investigated when trying to ensure a
specified level of part quality:
G
Resolution: Feature resolution is dependent on the AM technique applied and on the depo-
sition rate. Typically, with a higher deposition rate, the feature resolution goes down. For
example, the feature resolution with a powder bed technique is in the range of 0.1 mm
whereas with higher deposition techniques like EBAM this goes down to 3 mm.
Therefore, selection of an AM technique to be applied is also dependent on what kind of
feature resolution is desired, along with the post processing needs of the part.
G
Surface finish: AM surfaces are typically rougher than casting counterparts and the degree
depends on the process conditions used. Fig. 4.11 shows the typical surface roughness in
a 15-5PH part produced using a laser powder bed process. Most customers have a surface
finish requirement in their parts that the AM process would need to meet.
G
Residual stress and build failure: Since molten metal is being deposited and solidified
onto a substrate, there is potential for significant residual stresses in the AM build.
Residual stresses can influence part performance, part geometry, and, specific to AM, can
also affect the likelihood of a build failure. If a part becomes heavily distorted during a
build, the AM system being used could prematurely stop resulting in a build failure. To
mitigate the generation of residual stresses within a part, typically the substrate or “build
Design for metal additive manufacturing for aerospace applications 79

Figure 4.11 Typical surface roughness of a powder bed 15-5PH as-printed part.

plate,” on which an AM part is constructed, is heated to a specified temperature that can


be process (laser or EBAM) or powder dependent.
G
Build layout and support: The layout of parts on the build substrate as well as the alloca-
tion of support structure, if needed, are both highly critical to build success. Defining of
these build inputs requires a thorough understanding of the specific AM process to be
used, the desired part functionality, and the associated secondary operations that will be
needed to achieve part quality requirements.
G
Effect of powder reuse: In most builds with powder bed systems, powder usage per build
is less than 10%. In blown powder AM systems, the usage is still around 30% or less.
Therefore, a significant amount of powder that has been exposed is left for reuse after a
build. The powder size distribution, contamination and hence characteristics of the built
part may vary with the amount of reuse. Customers/manufactures typically put a limit on
how many times a powder exposed to the AM build process can be reused.
G
Open atmosphere systems: With efforts on reducing the costs of AM systems, there is a
recent trend toward print-head systems that can add AM capability to a conventional
Computer Numerical Control system. While lowering the costs significantly, they typi-
cally do not have a controlled atmosphere for builds, which is challenging for controlling
contamination in reactive metals like titanium alloys.
G
Geometric features: Certain features of a part can be more difficult to produce than others,
and as such a build can become inadvertently more complicated because of it. A way of
mitigating complexity of a build is choosing an AM build layout that simplifies cumber-
some features. An example of this could be reorienting a part to reduce overhanging fea-
tures, reducing the amount of necessary support needed for fabrication. As was mentioned
before, AM system resolution also plays a substantial role in the complexity of shapes and
geometries that can be produced, depending on the desired size and scale of the geometries.

4.3.3 Part evaluation: in-situ and after process nondestructive


evaluation (NDE)
To ensure a defect-free part, nondestructive techniques need to be applied both in-
situ and postbuild on an AM part. This is an important portion of quality control of
80 Additive Manufacturing for the Aerospace Industry

the part, and is often dictated by customer and part requirements. A complete
description of this topic for AM is beyond the scope of the chapter, but the follow-
ing are some key points of which to be aware:
G
Incoming powder characterization: This is critical to ensure quality and consistency of
input material. Parameters like particle size distribution, flow rate, chemistry, and mor-
phology are important, and should be measured and tracked with different material lots.
G
In-situ monitoring: This is critical for assessing parts while printing to detect and possibly
mitigate real-time defects. This includes features like melt pool control, thermal imaging
with each deposition layer, and closed loop controls.
G
Postprocess NDE: Techniques like computed tomography (CT) scan, X-ray, and
traditional microscopy are important to guarantee quality of a part. Fig. 4.12 shows an
example of how CT scanning can be used to detect defects in an AM part.

4.3.4 Post processing


AM is sometimes referred to as “3D printing.” This terminology often gives an
impression that we can easily fabricate a finished metal part, basically making a 3D
CAD digital model tangible merely with the push of a button. In most AM applica-
tions, though, this is not usually the case. What part manufacturers are realizing is
that just like traditional manufacturing, the actual process of printing itself is but a
small portion of tasks needed to make an AM part. The post processing of an AM
part turns out to include a significant portion of the overall cost of the part, and
thereby must be given equitable attention. Key points to keep in mind when evalu-
ating the amount of post processing needed for an AM part:
G
Ease of powder removal: This is an important consideration with powder bed AM parts.
Parts need to be designed such that powder in not entrapped in the final part. Build sup-
ports also need to be designed in such a way that it is easier to remove powder after the
build process has completed.

Figure 4.12 CT scan of an EBAM part showing linear lack-of-fusion defect in a


suboptimized Ti6Al4V part. EBAM, Electron beam additive manufacturing.
Design for metal additive manufacturing for aerospace applications 81

G
Minimizing postprocess machining: Most powder bed AM parts would need some level of
machining after printing. Part orientation and support structures should be designed such
that machining operations and related time required are minimized. For example,
orienting the part on the build plate such that the electrical discharge machining (EDM)
operation required to remove the part from the plate also gives the cutting surface of the
part the required specified finish.
G
Minimizing postprocess surface treatments: Due to fatigue, wear, and other performance
requirements, most parts have surface roughness requirements as mentioned in the
previous section. Since the attractiveness of AM is dependent on it being a near-net-shape
process, it is imperative that costly postprocess surface treatments are kept in mind to be
minimized while designing the build layout.
G
Heat treatment: Typically, most AM parts would need heat treatment either to reduce the
residual stress from the build, improve microstructure uniformity, or enhance other
microstructural/mechanical property characteristics. However, higher temperature heat
treatments or rapid cooling rates post heat treatment may cause distortion in the parts and
therefore should be addressed accordingly.
G
HIP: Most AM parts after heat treatment show lower fatigue properties as compared to
their wrought counterparts. One way to enhance fatigue properties in AM material is
through HIP’ing. The inclusion of this process can add significant cost to the part, in
which case the performance aspects of the application should be considered carefully prior
to the design and selection of fabrication and secondary processes.

4.4 Cost considerations


To find a successful commercial application, AM parts need to be both technically
and economically feasible. Most areas where AM currently brings value is with
expensive materials and highly complex parts where a significant amount of
machining is required. AM part cost breakdown for a typical powder bed AM pro-
cess is shown in Fig. 4.13. These costs can be higher or lower based on the specific
parts being printed, the material used, and what AM technology is employed.
Equipment and material costs continue to be significant cost drivers for AM. As
well, the labor involved with secondary operations having to do with part support
removal and additional machining needed to produce final part geometries, can also
have a substantial cost impact when evaluating the economic feasibility of produc-
ing a part using AM. However, with rapid advancements in the industry, the avail-
ability of newer faster machines, and the increasing customer demand for AM
material stock, these costs are beginning to come down significantly.
Some aspects about metal AM which should be considered when determining
whether it is a viable economic process for an application are:
G
If the application is for an industry that is heavily regulated, such as aircraft, what is the
economic impact of qualifying an AM process. This could mean qualifying the powder or
media used to fabricate the part, the specific AM machines that will be fabricating the
actual parts, and/or developing procedures and specifications governing the process
[19,20]. These are often the hidden costs of using/qualifying a new process for a part that
82 Additive Manufacturing for the Aerospace Industry

Figure 4.13 Typical cost breakdown of an AM part fabricated using a powder bed process
and has undergone secondary machining operations to produce final part geometries. AM,
additive manufacturing.

can go from a few thousand dollars to potentially millions of dollars for new materials,
and can easily throw off the economics of producing the part via AM.
G
Capital costs associated with purchasing and maintaining AM systems for manufacturing.
At current levels, this typically dominates the AM part costs [21].
G
Cost of the AM media from which the parts will be fabricated compared to wrought cost
of the same or comparable materials. Material costs can often be in the neighborhood of
20% of the total part costs.
G
Determining necessary inspection processes, both destructive and nondestructive methods,
required for evaluating part or product performance, and demonstrating that the product
meets the desired part specifications.
G
Secondary operations that will be needed after parts have been fabricated using an AM
process. These operations may include support removal, surface treatments, heat treat-
ment, or HIP.
These aspects as well as the inherent indirect costs associated with designing a
part and build layout for the AM process should be strongly considered when
determining the economic viability of implementing AM in a specific application.
The current trend in the industry is to evaluate the economic feasibility of
fabricating a part using AM, and comparing it to the existing incumbent fabrication
processes such as a casting or a forging. However, what is often missed in this
exercise is that the part being evaluated was designed for a casting or forging and
not for AM. A part designed specifically for AM may add significantly higher value
to the AM part. Also, just because a part can be fabricated using AM does not
mean that it should be. To justify the use of AM, the part should make both techni-
cal and economic sense.

4.5 Product and process design tools


AM as an emerging technology is currently undergoing several paths of develop-
ment in both process and technology. Current avenues of AM development include,
Design for metal additive manufacturing for aerospace applications 83

but are not limited to, additive machine development, process development, AM
material characterization and production, inspection methods both during process
and postprocess, design tools, and process synergy. In parallel with these direct
focus areas of AM development is allied technology development through accom-
panying software tools. Discussed in this section are some of the current capabilities
and areas of development for AM software tools.

4.5.1 Additive manufacturing design software


The development of AM design software has primarily been focused in two
areas: developing free-form design capabilities, and part shape and topography
optimization. These avenues are currently being addressed by many of the
industry computer-aided design (CAD) software producers as well as industry FE
analysis software companies [2223]. In terms of free-form design, CAD
programmers have begun to create tools and platforms allowing an AM part
designer to be able to create 3D bodies that do not constrain or inhibit the
capabilities of the AM fabrication process. Essentially this allows a CAD software
package to be able easily to design a part that can be fabricated using the full
breath of capabilities of the AM process. As well, some CAD packages are
beginning to develop software features where the AM part designer can identify
the AM process used to fabricate the part. The software will then apply specific
constraints, such as geometrical or material constraints, on the 3D model that are
representative of that process.
Shape and topological optimization, as previously mentioned in this chapter, are
design methodologies that are used heavily in AM part design because they
allow for tailored part performance to specified applications with the objective of
reducing part volume and weight. These methods of optimization, like free-form
CAD modeling, are not new tools, but there has been a recent push in their develop-
ment as applied to AM processes. These tools typically utilize existing numerical
methods and algorithms based on FE analysis or computational fluid dynamics, for
evaluating the performance of a part.
Development in both these areas of AM design software applications, free-form
design and part optimization, has been collaborative with many packages working
toward having capabilities in both areas to work in tandem. An ultimate goal of
development would be having the ability in a single environment to optimize and
refine the design of a part to its final form, and transfer the digital file to an AM
system for printing.

4.5.2 Additive manufacturing process software


The AM process is a multiphysics process involving the transformation of starting
powder or wire into a final product through heating, melting, and solidification
operations resulting in a layer-by-layer construction of a part or feature.
Understanding of this complex process is aided through the incorporation of
84 Additive Manufacturing for the Aerospace Industry

software tools, which use physics principles to model different aspects of the pro-
cess. Current software tools being developed to aide with the understanding of the
AM process have been focused on the following areas of interest, but are not lim-
ited only to these areas presented:
G
Modeling of residual stresses in an AM part or feature during a build, and having a com-
plete residual stress profile of the part at build completion.
G
Being able accurately to represent the microstructure of a part or feature being produced
using AM. Understanding how the melt pool and thermal gradients within a build, along
with the raw material properties used to fabricate an AM part, effect the final part’s
microstructure and chemistry.
G
Build layout design, and understanding the effects of building multiple parts versus a sin-
gle part in an AM build with respect to part functionality, induced residual stresses within
parts, and part microstructure.
G
Determining optimized part geometric orientation in a build layout both to ensure success-
ful build completion and reduce build time.
G
Modeling the effects of secondary operations performed on a part during the process of a
build or after build. Secondary operations can include machining/material removal, HIP,
surface treatment, and heat treatment.
Each of these focus areas entail their own complexity, but all have the general
goal of developing the sophistication necessary to understand the AM process in its
entirety, ability to predict a successful build, and predict part performance as a
function of process parameters.

4.6 Conclusions
In the present chapter, a review of the techniques used in DFAM, where the techni-
ques of topological optimization, part consolidation, and part integration were
discussed in some detail. Process aspects of AM design were reviewed, illustrating
the effects of material properties, part performance, and post processing operations
in relevance to part design. Current industry design tools for both part and process
design were summarized. The discussions emphasized that the traditional notions of
part design need to be updated to include key process elements when evaluating
design decisions for AM part fabrication.

Acknowledgments
The authors would like to thank all the members of Arconic Fastening Systems-New Product
Development Center, Arconic Engines, and the Arconic Technology Center, whose efforts
were critical in designing of parts, manufacturing prototypes, and testing of samples used in
the presented work. The authors would like to extend a special note of thanks to Luke
Haylock, Dr. Hasim Mulazimoglu, and Rodrigo Pinheiro for their advice and support through
different stages of the described work.
Design for metal additive manufacturing for aerospace applications 85

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Structure formation in A.M.
processes of Titanium and Ni-base 5
alloys
I.S. Polkin1, S.V. Skvortsova2, G.A. Turichin3 and M.B. Novikova1
1
All-Russia Institute of Light Alloys, JSC, Moscow, Russia, 2Moscow Aviation Institute
(National Research University), Moscow, Russia, 3St. Petersburg State Maritime Technical
University, St. Petersburg, Russia

Activities on the use of powder metallurgy methods for the manufacture of critical
structural components have been in progress for more than 40 years. Sufficiently
effective results were obtained for parts made of heat-resistant nickel and titanium
alloys. During this time, many important issues were solved to prove the possibility
of a significant reduction in the number of process stages and in the scope of
machining of parts obtained by powder technology as compared with conventional
deformation technologies. The achieved results speak for the possible decreasing of
metal consumption by 23 times, and that for disk titanium materials by up to 35
times [1].
Further progress of research work on achieving high solidification rates of pow-
der materials made it possible to start solving problems of increasing mechanical
properties. An increase in cooling rate allowed us to increase the content of alloying
elements in the solid solution and, due to this factor, to obtain higher mechanical
properties than those of parts made by using conventional technologies.
First, such advantages were obtained with the use of heat-resistant nickel alloys,
when high rate of crystallization of fine powders facilitates formation of a large
amount of the γ0 -phase during decomposition of the solid solution and refinement
of initial intermetallic compounds due to changes in their chemical composition.
In order to obtain such effects in titanium alloys it was necessary to achieve
higher cooling rates than those of nickel alloys, at the same time an improvement
in properties could be obtained only for special alloys of limited application. As for
titanium alloys, therefore, it was possible to concentrate on solving the first prob-
lem—decreasing the metal consumption and reducing the cost of manufacturing
parts.
At the same time, the calculations have revealed that in case of production of
titanium parts by conventional deformation technology, up to 30% of total costs of
the entire process accrue to the machining, whereas in the case of powder technol-
ogy, the cost of machining is much less (Fig. 5.1).
The next evolutionary stage in the development of the structural materials pro-
duction technology was the use of 3D printers to join individual particles (alloyed
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00006-6
© 2019 Elsevier Inc. All rights reserved.
88 Additive Manufacturing for the Aerospace Industry

Figure 5.1 Costs of production of Ti components by conventional technologies.

powders) into a finished part. This technology has “absorbed” all previous achieve-
ments in powder technology providing consolidation of particles in a hot isostatic
press (HIPer) under the action of temperature and pressure, and a metal can was
used as the shape-building element. As for the new additive manufacturing, the can,
as a shape-building element, was replaced with a 3D printer, which controls the
temperature beam in the 3D space and builds up the final part by joining the pow-
der particles.
The economic effect of application of additive technologies was caused by the
shortening of processes to make, fill, seal, and remove cans after HIPing, and
because of almost complete absence of machining. We can assume that the cost of
manufacturing parts by this technology will be approximately 30% lower than that
of conventional powder technology.
It should be taken into account that this method makes it possible to manufacture
parts with a shape that cannot be obtained by any other way, for example, hollow
spaces or lattice structures that allow achieving a significant reduction in weight.
Consideration of all methods of additive manufacturing, which have already
stood the test of time, allows us to identify three main ways that have proved their
usefulness:
G
direct deposition of metal powders on the forming surface of a part [direct metal deposi-
tions (DMDs)];
G
an action of a heat beam on the surface of the powder platform; only that part of powder
on the platform is consolidated, which is exposed to the beam [selective laser melting
(SLM)];
Structure formation in A.M. processes of Titanium and Ni-base alloys 89

G
and, finally, when a beam controlled by a 3D printer does not act on the powder, as it is
in the first two processes, but on a thin wire that is welded layer by layer and builds up a
desired shape of the part so called wire arc additive manufacturing (WAAM).
Having the same end goal, that is, to obtain the final 3D model of a part set by
the printer, these processes had different technological parameters: construction
rate, beam power, size of the initial material, metal temperature at different stages
of the process, the availability of additional equipment, and a number of other
differences.
In addition to provision of the final shape, overcoming these differences causes
one and probably the most important task of obtaining sufficiently high mechanical
properties that ensure reliability of the part working under operations conditions.
The achievement of necessary properties of parts made by additive manufacturing
is fully dependent on the absence of defects and on the microstructure
characteristics.
The solution of these tasks depends on the level of technology and the ability to
manage its parameters. For example, Fig. 5.2 shows the liquid bath dimensions for
two cases, that is, when the beam scanning speed changes from 50 up to 200 mm/s,
and the beam power increases from 100 to 200 W. In each case, the liquid bath
dimensions can vary approximately twofold, and the particles of 40 and 100 μm in
size can be completely liquid or be in a partially solid/partially liquid state.
The process of joining particles and layers formed from them occurs in both
cases, but the microstructure of the interface will be different, and therefore the
probability of formation of a defect on it will be different. Undoubtedly, the task of
technologists to build up a model will become more complicated, since the temper-
ature of the previous particle or layer will constantly change, depending on the size
of the part and other parameters of the construction. The knowledge of the nature
of changes in the structure during the production process of the part is extremely
necessary to achieve stable and high mechanical properties.
Let us consider the initial structure of powder particles and the nature of its
changes in the process of manufacturing 3D parts.

5.1 Evaluation of the structure of powder particles of


different sizes
Titanium and nickel alloy powders of 40120 μm in size produced by plasma
rotate electrode process (PREP) were used in the present work.
Electron microscope examination of the surface of powder particles of various
sizes showed that all particles had a smooth surface, strongly pronounced round
shape, and they were free of satellites, pores, and other defects that cause high flu-
idity and bulk density of such powders.
Examination of the surface structure made it possible to reveal the dendritic
structure of the surface for powder particles of all sizes, which was typical for both
titanium and nickel alloys (Fig. 5.3).
90 Additive Manufacturing for the Aerospace Industry

Figure 5.2 Changes in liquid bath dimensions in case of increasing of scanning rate and
laser power.

Investigation of the dendritic structure over the surface of powder particles of


various sizes made it possible to reveal a regular decrease in size of the dendritic
cells, accompanied by a refinement of powder particles. It was revealed most
clearly in cases of measuring the specific length of the dendritic cell boundaries,
which form the surface relief. No less than 25 powder particles of each size were
studied by a scanning electron microscope with magnification of 20003000.
It was also shown by studies that the more alloying elements in an alloy, for
example, Grade 5 (Ti6Al4V, 10% alloying elements), VT22 (18% alloying
Structure formation in A.M. processes of Titanium and Ni-base alloys 91

Figure 5.3 Surface structure of titanium and nickel-based alloys.

elements) and EI698 (30% alloying elements), the smaller are the dendritic cells
formed on the surface of powder particles of the same size, although the general
pattern of their dependence on the particle size is kept (Fig. 5.3).
Fig. 5.4 shows a dependence of the specific length of the dendritic cell bound-
aries on the powder particles surface on the size of powder particles (μm/μm2). As
it follows from the Fig. 5.4, a decrease in the average size of powder particles from
140 to 30 μm leads to an almost twofold increase in the specific surface of bound-
aries, that is, from 0.55 to 1 μm/μm2. It should be noted that the extreme growth of
92 Additive Manufacturing for the Aerospace Industry

Specific length of dendritic cell boundaries, μm/μm2


1.6

1.4
y = 4.57 x–0.42
R² = 0.843
1.2

0.8

0.6

0.4

0.2

0
0 50 100 150 200 250 300 350
Diameter of powder particles, μm

Figure 5.4 Dendritic structure parameters of the powder particle surface as a dependence on
the particle size by the example of TiAlMoZrSn alloy.

this value begins when the powder particle size is less than 40 μm, and, in case of
refining the particles from 300 to 140 μm, the change in the specific surface area of
the dendrite boundaries is rather small.
Analysis of the obtained data allows us to describe the data by the following
equation:

y 5 Ax2B ;

where y—specific length of the boundaries; x—diameter of the powder particles; A


—coefficient (3.95.6); B—coefficient (0.390.40).

5.2 A dependence of the microstructure of powder


particles in the initial state on their size
The microstructural study of Grade 5 alloy powder particles showed that the parti-
cles of less than 50 μm and within 150200 μm in size, being in the initial state,
have the martensite structure and the length of martensitic plates is equal to the
entire diameter of the particle (Fig. 5.5); almost exclusive presence of β-phase was
observed in powder particles of alloys with higher content of alloying elements,
such as VT22, which was confirmed by X-ray structure analysis.
Thus, it was difficult to determine the difference in the internal structure of pow-
der particles of different sizes in their initial state when they have been cooled at
B1 3 10241025 С/s, because the single-phase state is developed due to the high-
rate cooling.
Structure formation in A.M. processes of Titanium and Ni-base alloys 93

Figure 5.5 Microstructure of Grade 5 alloy powder particles of ,50 and .150 μm in size in
the initial state.

5.3 Determination of changes in the structure using


samples produced by different additive technologies
Two methods of production of a compact preform were used for preparation of
samples: high temperature DMD and consolidating of powder particles located on a
platform under the action of a thermal beam, that is, SLM.
The optimum temperature-time parameters of the process were chosen on the
base of investigation results of the compact preform structure.
Grade 5 alloy parts were obtained by the selective beam melting and by the
direct deposition of powders onto the part to be built up. In the first case, the pow-
der sizes were within 3040 μm, and in the second case—within 6080 μm.
Microstructure of samples in the initial state produced by DMD and SLM pro-
cesses is shown in Fig. 5.6A and B. The samples were cut out in the direction that
was transversed to the direction of the layer build up. The presented photos demon-
strate rather similar type of microstructure, which is characteristic for these produc-
tion processes. In both cases, the boundaries of deposited layers are decorated with
α-phase precipitations. Investigations of the longitudinal sections structure of the
built-up layers have revealed more clearly elongated boundaries of layers with
α-phase precipitations, while the structural directivity is not visible in the transverse
direction Fig. 5.6C and D.
In addition, metallographic studies showed that in the case of SLM, such defects
as individual pores or other small defects occur much more often than in the case of
direct deposition. Apparently, it can be explained by the increased energy of transfer
of particles onto the part to be built up in the course of DMD process, which allows
one to reach a higher degree of densification of the depositing metal particles.
The analysis of samples made by additive manufacturing showed that after
annealing (750 C, 2 hours in air) the microstructures in the initial state and after
annealing are quite similar for two cases of buildup of a part (Fig. 5.7).
94 Additive Manufacturing for the Aerospace Industry

Figure 5.6 Microstructure of Grade 5 alloy samples in initial state produced by SLM and
DMD ( 3 600): (A and B)—microstructure of samples cut out transversely; (C and D)—
microstructure of samples cut out longitudinally. SLM, selective laser melting; DMD, direct
metal deposition.

Figure 5.7 Microstructure of Grade 5 alloy samples ( 3 600) produced by (A) selective laser
melting and (B) direct metal deposition after annealing at 750 С, 2 h.

The absence of significant differences in the microstructure of the samples in the


initial state and after standard annealing can apparently be attributed to the time
and temperature sufficient for recrystallization processes already in the process of
building up the part, and the standard annealing temperature does not change
noticeably the structure of the alloy.
Structure formation in A.M. processes of Titanium and Ni-base alloys 95

Figure 5.8 Microstructure of Grade 5 alloy samples ( 3 600) produced by SLM:


(A) after annealing at 850 С, 1 h, in air
(B) HIPing at 950 С, 1.5 h, Р 5 142 MPa. SLM, Selective laser melting.

An increase in the annealing temperature of samples up to 950 C leads to a sig-


nificant increase in length and thickness of α-phase plates, both in longitudinal and
transverse directions. HIP treatment of samples produced by SLM eliminates reli-
ably pores and discontinuities, but increases additionally the dimensions of α-phase
plates (Fig. 5.8).
Investigation of microstructure of the samples produced by DMD and SLM
methods showed an identical type of the structure both in the initial and in heat-
treated states; it is also important that Grade 5 alloy powder particles of 6080 and
3040 μm in size were used for DMD and SLM, respectively.

5.4 Testing of mechanical properties of samples of parts


produced by direct metal deposition and selective
laser melting
Mechanical tests, i.e. ultimate tensile strength (UTS), and yield strength (YS), were
carried out using samples produced by DMD and SLM. Tests were carried out with
the use of samples in the initial state, after heat treatment and HIPing. Table 5.1
shows properties of Ti6Al4V alloy samples produced by SLM. It can be seen in
Table 5.1 that the initial material has a higher strength and reduced plasticity as
compared to the samples tested after heat treatment and HIP. It is probably related
to stress relieving and some increase in sizes of the α-plates, taking into account
that the heat treatment and HIP operations were carried out in the upper part of the
two-phase region (α 1 β).
A similar pattern of changes in structure and properties after heat treatment can
be observed with the use of samples obtained by DMD technology (Table 5.2).
Table 5.2 shows that the heat treatment, in comparison with the initial state,
causes a reduction in tensile strength by 40 MPa, in yield stress—by 50 MPa, and
reduction in area increases by approximately 6%.
96 Additive Manufacturing for the Aerospace Industry

Table 5.1 Mechanical properties of Grade 5 alloy samples produced by SLM

State Cutting UTS, 0.2% YS, δ, ϕ,


direction МPа МPа % %
Initial state Longitudinal 990 950 13 44
Transversal 980 965 11 38
Annealing: 850 С, 2 h Longitudinal 950 930 16 46
HIP: 950 С, Р-1400 atm, Transversal 930 920 17 48
holding 1.5 h

SLM, Selective laser melting; UTS, ultimate tensile strength; YS, yield strength.

Table 5.2 Mechanical properties of Grade 5 alloy samples produced by DMD

State Sample cutting Average value


direction
UTS, 0.2% YS, δ, Ψ,
МPа МPа % %
Initial state Longitudinal 1029 978 18 46
Heat treatment: 800 С, Longitudinal 992 927 19 52.5
1 h, in air
Heat treatment: 800 С, Transverse 1057 1017 14 34
1 h, in air
DMD, direct metal deposition.

Tests of samples cut out in the plane transversed to the growth direction of
layers produced by DMD showed higher strength values and a decrease in elonga-
tion as compared to samples cut out along the direction of the layers growth. The
reduced plastic properties obtained at the testing of samples are evidently associated
with a large number of grain boundaries presented in the cross section of the sam-
ple, possible defects and discontinuities occurring at the junction of layers, and
coarse α-phase interlayers.
In addition to the noted features in the structure and properties of samples cut
out in different directions, it is necessary to point out a large number of discontinu-
ities and pores formed in samples produced by SLM. That is indirectly confirmed
by the fatigue tests of these samples, fatigue resistance values of which, after
HIPing, are 1.31.5 times higher than those before HIPing, which is most probably
caused by the healing up of pores and discontinuities during HIPing.
Thus, consideration of mechanical properties of samples produced by DMD and
SLM methods showed that in both cases higher strength values are obtained in the
initial state as compared with properties of these samples after subsequent annealing
or HIPing.
Elongation characteristics after annealing are increased in comparison with the
initial state. It can be explained by the processes of stress relief and equalization of
the structure with increase in the size of α-phase plates by 12 μm; the plates are
Structure formation in A.M. processes of Titanium and Ni-base alloys 97

noticeably growing when annealing or HIPing is carried out at temperatures of the


upper part of the (α 1 β) region.
The second common property of the samples produced SLM and DMD is a dif-
ference in mechanical properties and structure of samples in different built-up direc-
tions. Unfortunately, this imperfection is inherent in the methods in question and
further research to achieve higher homogeneity of the built-up structure is needed.
The structure and properties obtained with the use of Grade 5 alloy samples
exceed significantly those of cast samples and are close to the values specific for
wrought material. There are some exception when defects in the form of cold shuts
can be formed, which are not completely eliminated by HIPing.

5.5 Conclusions
1. Investigations of the structure and properties of powders and parts produced from them by
additive technology have shown that the initial powder particles, as a rule, have a single-
phase structure, and temperature effects arisen in the course of additive manufacturing,
both by DMD and SLM, cause formation of a two-phase structure analogous to that of the
alloy in the annealed state.
2. The annealing leads to a slight change in properties and homogenization of the structure
and to a certain increase in the particle size of the α-phase.
3. The mechanical properties and structure of the samples manufactured by DMD and SLM
methods are similar and did not show differences when using powder particles of 6080
and 3040 μm in size for both methods.
4. Depending on the direction in which the layers are grown in the samples, the anisotropy
of properties necessitates the further improvement of the additive manufacturing
technology.

Acknowledgement
We would like to express our gratitude to the employees of Е.М. Golubeva, VILS OJSC,
М.А. German, Moscow Aviation Institute (National Research University), and F. Shamray
(St. Petersburg State Maritime Technical University) for their active participation and assis-
tance in the work.

Reference
[1] I.S. Polkin, V.N. Samarov, Advance in powder metallurgy of titanium, in: The 12th
World Conference on Titanium, June, 2011, Beijing, China Ti-2011.
98 Additive Manufacturing for the Aerospace Industry

Further reading
J.D. Cotton, R.D. Boyer, G.R. Weber, K.T. Slattery Technical Fellow, Titanium alloy devel-
opment needs for commercial airframes, in: Metallurgy Seattle, Washington, 2008.
I.S. Polkin, Additive manufacturing of titanium alloys, Technol. Light Alloys 3 (2015)
1116.
Measurement of powder
characteristics and quality for 6
additive manufacturing in
aerospace alloys
Thomas F. Murphy and Christopher T. Schade
Hoeganaes Specialty Metal Powders LLC, Cinnaminson, NJ, United States

6.1 Introduction
Titanium, superalloy, stainless steel, and tool steel powders used in the aerospace
industry are produced by a variety of methods that influence the particle morphol-
ogy and hence, their suitability for use in additive manufacturing (AM). These pow-
ders can be produced via gas atomization (GA), plasma spherodizing, plasma
rotating electrode process (PREP), or electrode induction melting GA (EIGA) [1].
Each of the AM processes such as selective laser melting (SLM), electron beam
melting (EBM), or direct energy disposition (DED) requires different powder
attributes to optimize their performance [2]. Metal injection molding (MIM) is also
used to produce parts for the aerospace industry and requires its own set of powder
characteristics to maximize the final part properties.
Characterization of metal powders for the aerospace industry (titanium, superalloys,
stainless steel, and high strength low alloy steels) involves documenting the average
particle size, particle size distribution, surface area, flowability, apparent density, tap
density, moisture content, and porosity in a powder. These attributes are, in many cases,
considered the minimum required information by the end user. Frequently, the
manufacturer of these powders provides a certificate of analysis which contains this
information. Additional characterization utilizing metallographic techniques is often
provided to allow optimization of the powder for each application. This chapter will
review basic powder testing used as quality control tools for powders as well as the
advanced metallographic techniques.

6.2 Quality control measurements


6.2.1 Particle size and distribution
Particle size and particle size distribution are important characteristics for each
batch of powder used for an application. As an example, Fig. 6.1 shows the particle
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00007-8
© 2019 Elsevier Inc. All rights reserved.
100 Additive Manufacturing for the Aerospace Industry

SLM EBM
10–45 μm 50–105 μm

100 1.8
90 1.6
Cumulative distribution Q3(x)/%

Densi ty distri bution q3l g(x)


80 1.4
70
1.2
60
1.0
50
0.8
40
0.6
30
20 0.4

10 0.2
0 0
4 6 8 10 20 40 60 80 100 200 400 600 800 1000
parti cle size/μm
MIM cut SLM
<20 μm 20–60 μm

Figure 6.1 Gas atomized Ti6Al4V particle size distribution utilized by different AM
techniques. AM, additive manufacturing.

size distribution for a Ti6Al4V powder made via the EIGA process. In many
cases the required particle size or particle size distribution is determined by the
powder delivery method utilized by the AM machine. In processes where a powder
bed is used (SLM), powder with particle size distribution in a range of 1060 μm
is required. In AM machines where the powder is carried by a gas or flows through
a hopper and powder feed system (such as EBM or DED), the distribution is typi-
cally coarser (50105 μm).
Particle size is a measurement of a specific dimension of the powder and
depends on the measurement technique used (for example, laser or light scattering)
[3]. Most devices measure a single geometric parameter from which an equivalent
circular diameter is calculated. Therefore, different methods of particle size analysis
do not generally agree, so the end user needs to be aware of the method used and
how it correlates to the process by which the powder is being used.
Typically, the powder is described by the mean particle size (d50), but the d90 and
d10 are also typically reported. In the case of the d10, (10% by weight, volume or
number of particles less than this diameter) it describes the finer powder that
typically needs to be minimized to ensure excellent flow of the powder. A d10 in the
range of 1020 μm is typical for SLM AM powders. If the d10 is below this size,
the finer particle size inhibits the flow and leads to poor packing in the powder bed.
If the d90 of the powder is to large, it indicates the powder may have very large
particles that will either be difficult to transport or not become fully melted by the
laser source. Particle size analysis is covered by various standards, such as ASTM
B822 or MPIF Standard 32 [4,5]. Typical particle sizes, as measured by laser analy-
sis for the different powders used in AM, are shown in Table 6.1.
Particle size distribution can also be measured by sieve analysis. Sieves are
made of metal, polymer, or cloth wire, which have a defined opening size (μm).
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 101

Table 6.1 Typical particle size distribution for AM techniques measured by laser analysis

Typical particle size (µm)


SLM powder bed SLM powder bed EB and powder blown
d10 717 2939 4858
d50 2737 4151 6887
d90 4050 5565 97125
SLM, selective laser melting; AM, additive manufacturing; EB, electron beam.

These sieves are used to screen and separate the powder into various size fractions.
The sieves are stacked in order of opening size, from largest to smallest and the
stack of sieves is typically set in motion by shaking or tapping to allow the powder
to percolate through the screens. The finest powder is collected in a “pan” at the
bottom of the sieve set. The weight retained on each screen represents a particle
size larger than the maximum opening in that screen. Particle size distribution can
be calculated in a similar fashion to that shown in Fig. 6.1. While sieve analysis is
an older method than light or laser scattering, it can provide a more physical repre-
sentation of the powder. For example, if the AM technique being used has an ori-
fice or flow distribution device that cannot tolerate a powder particle above a
certain size, a sieve analysis can ensure the powder particles do not exceed this
size. Table 6.2 shows typical sieve analysis for the common particle sizes currently
used in AM. Standards for testing powders by sieve analysis are ASTM B214 and
MPIF Standard 05 [4,5].

6.2.2 Apparent density and flow


Powder flow and packing characteristics are critical to all the AM methods. Flow
measurement is not only important for the bulk flow of the powder as it is
transported to the working area, but in cases where the powder is distributed by a
recoater, which places the individual particles in place before welding, the powder
must be able to flow evenly over the previous layer of powder that was fused. As
important as the measurement of flow is to the AM process, the measurement of
apparent density gives an indication of how the particles will pack in the powder
bed. If the powders are irregular in shape, the packing will be poor and the apparent
density low. On the other hand, if the particles are spherical and free of satellites,
the apparent density will be high. This is the preferred condition for powders used
in AM.
Flow of metal powders is determined by ASTM B213 and MPIF Standard 03
[4,5]. These methods are suitable only for powders that will flow freely through the
specified Hall funnel (Fig. 6.2). In practice, a specified mass of powder (50 g) is
placed in the funnel with a known orifice diameter at the bottom. The flow rate is
the time required for the 50 g to flow through the funnel. The lower the time (mea-
sured in seconds), the better flowability the powder has. In instances where the
Table 6.2 Sieve analysis for AM techniques

μm 250 177 149 105 74 62 44 32 25 20 ,20


AM process Mesh size 160 180 1100 1140 1200 1230 1325 1450 1500 1635 Pan
SLM 1045 μm 0 0 0 0 0 0 0.1 5.0 46.9 29.6 3.0
SLM 2063 μm 0 0 0 0 0 0 52.7 31.4 12.0 2.4 1.5
EB and powder blown 50105 μm 0 0 0 6.5 34 15.6 36.4 7.5 0 0 0
AM, additive manufacturing; SLM, selective laser melting; EB, electron beam.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 103

Figure 6.2 (A) Picture of Hall flowmeter and cup. (B) Schematic of Hall flowmeter and cup.

Figure 6.3 Titanium 6-2-4-2 (50105 μm) powder with satellites (indicated by red arrows).

powder is not free flowing, the funnel orifice diameter is doubled and this is called
the Carney test for flow (ASTM B417, B964, and MPIF Standard 28) [4,5]. In addi-
tion to the increase in orifice size, the mass of powder used in the Carney test is
increased from 50 g to 150 g.
The flowability of a powder is determined by several factors. Typically, coarser
particles flow better than finer powders. The fine powders have more surface area,
which creates friction and reduces the flow properties of the powder mass.
Spherical powders flow better than those that are irregular for the same reason.
When comparing spherical powders, if there are satellites on the powder, this will
also lead to poor flow relative to the spherical powder that is satellite free.
Satellites are smaller diameter particles that become attached to the larger particles
due to the recirculation of the atomizing gas (Fig. 6.3).
Moisture adsorption on the powder surface can contribute to poorly flowing
powders due to polarity effects and sometimes it is useful to heat the powders at
low temperatures or under vacuum to improve the flowability. In some alloys, a
104 Additive Manufacturing for the Aerospace Industry

7.0

6.0
Carney flow (s/50 g)

5.0
No flow
4.0

3.0

2.0

1.0

.0
.0 2.0 4.0 6.0 8.0 10.0 12.0 14.0 16.0 18.0
d10 of 316L stainless steel powder for SLM

Figure 6.4 Effect of percent of powder less than 10 μm on Carney flow.

thin hard oxide layer on the powder may improve the flow properties. A contrib-
utor to poor flow in powders used in SLM (typical particle size distribution
1060 μm) is the percentage of particles smaller than 1020 μm. This previously
mentioned d10 is the diameter at which 10% of the samples mass or volume
(depending on measurement) is comprised of particles with a diameter less than
this value. As the d10 of the powder size distribution decreases (meaning a finer
particle size), the Carney flow time starts to increase to a point below which
there is no flow (Fig. 6.4). It is for this reason that it is common in SLM to spec-
ify a minimum value of the d10, limiting the percentage of less than 10 μm
particles.
Apparent density of a metal powder is the mass of a loose powder per unit vol-
ume measured in g/cm3. It gives an indication how the powder will layer in the bed
of the AM process. Efficient packing is critical for heat transfer from particle to
particle. If the powder packs poorly, defects, such as porosity due to improper melt-
ing of powder, can occur. Higher packing densities lead to less shrinkage and there-
fore dimensional tolerances are improved. Powder packing can also be influenced
by powder properties, such as surface roughness and surface moisture. Finer parti-
cles tend to pack more efficiently; however, their propensity to agglomerate can
lead to balling and the laser or heat source that is running at a constant energy level
may not have enough energy to melt due to the increase in the localized mass.
Having a high packing density can also lead to lower levels of residual stress and
part distortion due to more uniform heat transfer.
The common method for measuring apparent density uses the Hall flowmeter
shown in Fig. 6.2 and is covered by ASTM B212 and MPIF Standard 04 [4,5].
A precisely calibrated cup fixes the volume and the powder flows through the fun-
nel and fills the cup. The powder is then leveled with a straight edge, taking
care not to apply any downward force to compress the powder. The apparent
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 105

35
30

Hall flow (s/50 g) 25


20
15
10
5
0
2.25 2.3 2.35 2.4 2.45 2.5
Apparent density (g/cm3)

Figure 6.5 Relationship between apparent density and Hall flow for Ti6Al4V,
50105 μm.

density (measured in g/cm3) is then calculated by dividing the mass of the powder
contained in the cup by the volume of the cup.
For nonflowing powders, ASTM B417 and MPIF Standard 28 are the applicable
standards [4,5]. Here the Carney funnel with a larger orifice (as described previ-
ously) is utilized. If the powder still does not flow through this larger orifice, provi-
sions are made to poke the powder with a wire, but at no time may the wire enter
the measurement cup.
Apparent density is also an indicator of particle shape. Particles with a low
apparent density tend to be irregular and may have satellite particles. Higher appar-
ent density powders are more spherical and tend to flow better. Fig. 6.5 shows the
relationship between apparent density and Hall flow for a Ti6Al4V powder
with a particle size of 50105 μm. As the apparent density increases, the Hall flow
time decreases. This graph shows the usefulness of these two measures as a quality
control tool to measure lot by lot variation.

6.2.3 Tap density


Tap density is the maximum density achieved when metal powder is vibrated or
tapped under specific conditions. The test method for tap density is covered under
ASTM B527 and MPIF Standard 46 [4,5].
In practice, a known mass of powder is placed in a graduated cylinder. The cyl-
inder is then lifted by a cam drive and abruptly lowered repeatedly (Fig. 6.6).
This “tapping”-induced movement and rearrangement of the powder reduces the
friction between particles and allows for more efficient packing. The tap density
measured by this test is always higher than the apparent density measured with
free-flowing powders. Tap density is a function of the powder shape, porosity,
and size distribution. How the tap density relates to the packing in a powder bed
for AM depends upon how much pressure and vibration is applied to the bed
106 Additive Manufacturing for the Aerospace Industry

Figure 6.6 Device for measuring Tap Density.

during the distribution of the powder. A more direct use of the tap density is in
combination with the apparent density. The change in density from the loose pow-
der (apparent density) to the rearranged powder (tap density) largely depends on
particle shape. Therefore, it is possible to get an estimation of the powder shape
by dividing the tap density by the apparent density. This is called the Hausner
ratio. For a spherical powder, the value would be lower than the value for a more
irregular powder. As a rule, powders with a Hausner ratio larger than 1.25 are
considered poor flowing powders; however, this depends on the particle size and
specific material under consideration. There are many variables affecting the pow-
der flow and the correlation with the Hausner ratio is limited, as shown in
Fig. 6.7. There is a general trend as the Hausner ratio increases the powder flow
decreases; however, there is considerable scatter in the data indicating there are
other variables influencing the flow.

6.2.4 Moisture analysis


The environment in which the metal powder is exposed has been shown to be rele-
vant to the performance of the powder in the AM process. If moisture is adsorbed
on the surface of the powder, it may have a negative impact on the flow behavior.
For alloys that are susceptible to oxygen and hydrogen pick-up, such as titanium,
the decomposition of hydrogen and oxygen from the water vapor during melting
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 107

Powder flow vs. Hausner ratio


7
Powder flow (Carney method s/50 g)

0
1 1.05 1.1 1.15 1.2 1.25 1.3 1.35 1.4
Hausner ratio (tap density/apparent density)

Figure 6.7 Carney flow plotted as a function of the Hausner ratio.

may lead to increases of these elements in solution, which may have an impact on
the mechanical properties. In other reactive metals, oxides may also form, which
may create nonmetallic inclusions in the metal.
There are several methods for determining the moisture content of a powder,
some which use weight loss measurements, and others that use titration (specifically
Karl Fischer Titration). Titration is selective for water because the titration reaction
consumes water and in doing so, can be used to determine the content. Titration is
very effective for measuring the water content in liquids, but care must be exercised
in solids to ensure water on the surface of the powder is in direct contact with the
solution and this may involve some method of mixing the powders and solution.
The affinity for oxygen with the base metal (such as titanium) is also a concern as
the solution must liberate water from the solid to measure the content. The appro-
priate standard governing this technique is ASTM E1868.
Another method, weight loss on drying (LOD), is a reliable and simple method
for measuring moisture content. It involves heating the metal powder so that the
moisture is evaporated. Like Thermogravimetric Analysis, the weight of the sample
is monitored and the difference between the starting weight and the final weight is
assumed to be the amount of lost moisture. LOD has been made even simpler by
replacing slow heating ovens with energy sources such as a small halogen lamps
(Fig. 6.8). In addition, known reference standards exist to ensure calibration of the
equipment. One issue with these devices is that the measurement of mass on drying
could also include any volatile elements on the powder, such as oil or organics.
However, most powders, such as titanium and superalloys, are not exposed to any
such material and, if they had, detecting it in this device would be useful.
108 Additive Manufacturing for the Aerospace Industry

Figure 6.8 LOD device for measuring moisture content of metal powders [6]. LOD, loss on
drying.

Fig. 6.9 shows the moisture level on Ti6Al4V stored in standard containers
in a nonclimate controlled environment over a 10-month period. The moisture con-
tent is stable and shows very little fluctuation over the time in which testing took
place. Measurements of the apparent density and flowability of the powder also
remained constant during this same time.

6.2.5 Inclusion analysis


One of the major concerns in producing powder, such as titanium or other alloys
typically used for aerospace applications, is the potential for inclusions of foreign
contaminants to be introduced into the powder during the melting or atomizing
processes. These inclusions can reduce fracture toughness, fatigue life, and ductil-
ity. Since this is difficult to predict, a method to measure the inclusion content of
the final atomized powder is sometimes necessary.
The most commonly used methods for examining the inclusions in powder are
X-ray computed tomography (CT) and light optical microscopy (LOM) coupled
with an automated image analysis (AIA) system. Since both techniques generate
and analyze images, the most accurate, reliable, and repeatable results are a conse-
quence of using images of the highest quality.
Both CT scans and AIA are vision-based systems using basically the same tech-
niques to generate digital images for analysis. Their respective samples are illumi-
nated by an appropriate form of energy, either high energy X-rays (CT scan) or
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 109

Ti-6AI-4V moisture analysis


0.500
0.450
0.400
wt % moisture

0.350
0.300
0.250 Ti 64 10–45 microns
0.200
Ti 64 20–60 microns
0.150
0.100 Ti 64 50–100 microns
0.050
0.000
1 2 3 4 5 6 7 8 9 10
Months of exposure

Figure 6.9 Weight percent moisture versus month for Ti6Al4V powder.

visible light (AIA), which interacts with the sample, causing changes to the inten-
sity or appearance of the energy. This altered energy, as either attenuated X-rays or
reflected light, is projected onto a flat panel detector that is sensitive to the specific
energy type. Both detector surfaces are covered by a planar array of picture
elements (pixels), and it is the intensity or characteristics of the energy falling on
the pixels that determines their digital brightness value. With the CT scans, the
attenuation of the X-rays is controlled by the local sample density, while with
the image analysis system, visible light reflected by the features on the metallo-
graphically prepared sample surface is captured for analysis.
Sample preparation for the two methods also differ. For CT scans, a small vol-
ume of powder is enclosed in a suitable container and placed in the system. The
sample is then scanned and individual layers are analyzed. Fig. 6.10 shows a single
layer of a Ti6Al4V powder (50100 μm in size). The red circle indicates the
presence of a high-density inclusion as a white spot in the powder.
For the technique using image analysis, a compacted sample of the powder is
sintered in a protective atmosphere to create a preform. This preform is then
reheated (in a protective atmosphere) and forged into a fully dense slug. After cool-
ing from the forging operation, the metallographic specimen is removed from the
forged slug by sectioning along the diameter of the cylinder. The rectangular sec-
tion is mounted using standard methods, then ground and polished using techniques
specific to the alloy being tested.
When viewed using the optical microscope, the presence of the darker nonmetal-
lic is determined by comparing the digital representation of the microstructure with
a predetermined grayscale range. Features falling within this gray-to-black range
are detected and separated from the remainder of the image and those located
within a specified distance of other detected feature(s) are joined, thus defining
inclusions as the combination of the joined individual features. These features are
measured and sorted into predefined size classes. The optical microscope magnifi-
cation and joining distances can be modified to match alloy and application
110 Additive Manufacturing for the Aerospace Industry

Figure 6.10 CT scan of Ti6Al4V powder layer showing the location of a high-density
inclusion. CT, computed tomography.

requirements. This technique follows the well-established ASTM B796 standard


used to analyze powder-forging grade ferrous powders [5].
An example of this technique is shown in Fig. 6.11, where an inclusion was
detected in Ti6Al4V powder. One of the advantages of forging a slug over per-
forming a CT scan on loose powder particles is that the inclusions can be located in
the metallographic sample and the chemical composition of the inclusions can be
determined by energy dispersive spectroscopy (EDS) on the scanning electron
microscope (SEM). The AIA-SEM results indicate that this inclusion was approxi-
mately 100 μm in length and comprised of nearly all carbon.

6.2.6 Shape factor


There are various shape factors measured by several instruments that can be used to
correlate with powder properties such as flow rate and packing density. More
recently, particle size analyzers with dynamic image analysis (DIA) are able to pro-
vide information on particle shape with very little sample preparation. DIA systems
are equipped with light sources, objective lenses and cameras that capture the
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 111

Figure 6.11 (A) SEM photomicrograph of inclusion found in Ti6Al4V gas atomized
powder. (B) Corresponding EDS showing that the inclusion was carbonaceous. SEM,
scanning electron microscope; EDS, energy dispersive spectroscopy.

particles as shadow projections as they pass through the system. From these projec-
tion measurements of particle shape, other geometric parameters can be calculated.
The simplest geometric parameter is the shape factor or particle roundness.
Fig. 6.12 shows the particle roundness (calculated by the aspect ratio: minimum
chord length/maximum chord length) measured from a light scattering instrument
(Retsch Technology-Camsizer X2). These data were collected from various produc-
tion lots of Ti6Al4V powder. The closer the roundness value is to unity, the
more circular the shape of particle projection. In this figure, the Carney flow rate is
plotted as a function of this roundness factor from DIA. The trend is that, as the
particle becomes irregular (roundness decreases), the Carney flow time increases.
Other methods to evaluate the shape and geometrical features of powder can
also be performed with metallographic techniques and image analysis. These meth-
ods will be discussed in subsequent sections.

6.2.7 Porosity
Porosity in many AM parts is generally avoided. In the aerospace industry, porosity
can lead to inferior mechanical properties such as reduced tensile and fatigue
strengths. The amount of porosity in the final AM part is directly correlated with
the amount of porosity in the powder and from processing parameters of the AM
process, such as power input, scan speed, scan hatching, and melt pool characteris-
tics. The production method of the powder has a direct influence on the amount of
porosity in the powder. For example, the PREP process involves liquid metal dro-
plets being thrown from a solid bar at very high revolutions per minute. There is lit-
tle or no entrainment of trapped gas and hence little to no porosity found in
powders made by this method. However, with the gas atomizing process, the turbu-
lence in the atomizing chamber can recirculate the atomizing gas entrapping it in
the solidifying particles. This can lead to trapped gas and porosity in the solidified
powder. If the powder contains porosity, the AM part that is manufactured from
112 Additive Manufacturing for the Aerospace Industry

Powder flow vs. particle roundness


8
Powder flow (Carney method s/50 g)

0
0.5 0.55 0.6 0.65 0.7 0.75 0.8 0.85 0.9
Particle roundess (Camsizer X2)

Figure 6.12 Carney flow versus powder roundness as measured by light scattering on a
Ti6Al4V powder (50100 μm).

this powder will also contain porosity. Therefore, quantifying the amount of poros-
ity in a powder is an important quality control tool. There are several commercial
methods for determining the amount of porosity in the powder particles, such as
pycnometry and CT scan; however, simpler metallographic techniques exist that are
generally faster and more cost effective.
To measure the porosity in a powder, metallographic mounts of loose powder
particles are made and analyzed using an AIA system. Loose powder samples are
mixed with a liquid epoxy and cured, encapsulating the individual particles in the
hard, stable epoxy. The composite mounts are ground to create cross sections of the
distributed particles, then polished using procedures designed to match the alloy.
When prepared, individual particle cross sections are revealed surrounded in the
mount by the epoxy.
The amount of porosity in the particles can be measured using image analysis
with these prepared mounts. This is accomplished by using the detected metallic
portion of the cross section and having the system software fill any darker,
undetected areas surrounded completely by metal. These filled regions are the
pores within the particles. By manipulating the various detected and stored
images, the filled regions can be further separated and both the volume percent
porosity in the particles and the percentage of particles containing pores can be
estimated.
Fig. 6.13 shows a light optical image of IN718 powder made via GA that shows
porosity in numerous particles. Using image analysis, the porosity as a percent of
powder cross-sectional area can be calculated as well as the percent of the particles
containing porosity (as a function of the total number of particles). This powder
was used in DED and porosity was shown to exist in the part built from this
powder.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 113

Figure 6.13 Light optical image of porosity and porosity level in IN718 GA powder.

6.3 Advanced metallographic techniques


The test methods described in the previous sections were considered routine, and in
many cases, the minimum battery of tests that is often performed by the manufac-
turer of the powder. However, in the development of a powder for specific AM
manufacturing processes, many times additional information is required to optimize
both the performance of the AM technique (SLM, EBM, or DED) and the quality
of the final part.
Since the morphology of the particles has a major impact on the behavior of the
powder, additional metallographic evaluation techniques are needed to evaluate the
characteristics of the different alloy powders. Unfortunately, many of the current
techniques used to generate relevant information were developed and standardized
for the larger, more irregular powder metallurgy (PM) and powder forging (PF)
powders [710]. These methods are often inappropriate for the fine, nearly spheri-
cal AM particles. The combination of the small size, spherical shape, and minimal
particle surface to material volume ratio (SV) often leads to difficulties in sample
preparation and requires modifications to AIA programs where well-defined surface
and edge details are essential for accurate estimation of particle size and shape
characteristics. While AIA techniques are used successfully for evaluating the PM,
PF, and AM particles, the finer particle size of the MIM powders often excludes
them from this type of LOM evaluation and AIA testing.
The AIA testing programs used to evaluate the shapes and sizes of the AM parti-
cles rely on meticulous metallographic sample preparation to ensure the cross
114 Additive Manufacturing for the Aerospace Industry

sections revealed on the mount surface are representative of the material volume.
The aim of the preparation sequence is to produce 2-dimensional (2D) surfaces that
contain faithful representations of both the surfaces and interiors of the encapsu-
lated particles without having an excessive number of particles pulled out of the
mount or rounding the particle edges during grinding and polishing. These negative
occurrences can create situations where fine particles are lost or details of the
surfaces are obscured. This unfavorable situation is compounded by the extracted
particles becoming embedded in the polishing cloths, thus creating scratches,
gouges, and deformation on the surfaces being prepared. Consequently, improve-
ments to the metallographic preparation procedure were needed to define accurate
particle cross sections [11].
Once the sample of mounted loose powder particles is prepared, several techni-
ques are employed to analyze the particle characteristics of size, shape, and surface
texture. In addition, the amount of internal porosity, entrapped nonmetallic inclu-
sions, and precipitated phases can be quantified using the same metallographically
prepared mounts. In many cases, AIA techniques are used for these tasks, although
manual methods are sometimes utilized where an automated system is not available.
Regardless of the testing method, accurate and reproducible metallographic prepara-
tion procedures are essential to the generation of meaningful data. In many cases,
the live or acquired digital images provide the best opportunity to evaluate these
attributes of shape and surface texture accurately.
All testing in this discussion focuses on the appearance, shape, and surface
texture of the particles evaluated on an individual particle basis, with the procedures
developed originally for titanium AM alloys. Consequently, with hundreds or thou-
sands of particle cross sections revealed and characterized on one sample surface,
statistical distributions of the shape and texture expressions can be calculated from
the acquired data. In many cases, reporting the distributions can be more meaning-
ful than simply determining average values. Also, while it is possible and accurate
to make size estimations using particle cross sections [12,13], none are made here.
Sieving and some of the laser measuring techniques are sometimes better suited to
the determination of size compared with using LOM on 2D sections of individual
particles.
An additional area of concern in the testing of the AM powders is the presence
of particles with dissimilar chemical composition in a specific powder volume (aka,
cross-product contamination). This situation occurs where several alloy types are
stored or used as feedstocks in one manufacturing location or AM machine. The
presence of these chemically dissimilar particles can lead to unwanted changes in
local microstructure, act as stress raisers, or cause other detrimental effects on a
built AM part. Determining their presence is essential to providing parts of uniform
quality with predictable properties.

6.3.1 Background
The fundamental differences between the AM and PM-PF powders are the size dis-
tribution and shape of the particles. In general, the AM particles are smaller, often
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 115

,60 μm in diameter, compared with the PM-PF powders that are ,150 μm. In
addition to the largest particles being  60 μm in diameter with the AM powders,
often the smallest particles (,5 μm) are removed. In comparing the relative particle
shapes, the AM powders are nearly spherical and the PM-PF powders are
irregularly shaped. The size and shape combination of each material is intended to
optimize powder behavior for processing of their respective parts. The AM powders
require fast, uniform mass flow and bed fill. Consequently, a sphere is desired
because the interparticle friction is lower and the particle arrangement is more
uniform and can be better controlled. In comparison, the irregular shape of the
PM-PF powders provides the important green strength that permits transfer of an
as-pressed PM part or preform from the compaction press to the sintering furnace
without damage. The powders designed for use in one process will not perform
satisfactorily in the other. Basically, smooth, spherical powders lack green strength
and irregularly shaped particles flow more slowly and fill the die cavity less
efficiently.
Where evaluating particle shape and surface texture are the aims of the testing,
acquiring images that accurately describe the individual particles and can be ana-
lyzed is of paramount importance. Fig. 6.14 shows examples of two nearly spherical
gas atomized AM powders. A Ti6Al4V is shown in Fig. 6.14A and a 316L
austenitic stainless steel in Fig. 6.14B. The shapes are sphere-like, but some of the
particles contain protrusions or satellites from the GA process. These irregularities
affect both the powder flow and the ability of the powder to fill the bed. The sizes
of these two powders are also somewhat different, although both are fine compared
with the PM-PF powders.
The shapes and sizes of typical PM-PF water atomized powders are illustrated in
Fig. 6.15. The (A) image is typical of an unalloyed iron or low-alloy steel and a
stainless steel powder is shown in the (B) image. The shape differences are obvious
compared with the particles in Fig. 6.14. Additionally, where the finest particles
have been removed from the samples in Fig. 6.14, none of the fine particles are
removed from the PM-PF powders.

Figure 6.14 Gas atomized (A) Ti6Al4V and (B) 316L stainless steel. SEM/SEI. SEM,
scanning electron microscope.
116 Additive Manufacturing for the Aerospace Industry

The differences in particle morphology between the powders observed in


Figs. 6.14 and 6.15 are apparent using secondary electron images (SEI) however,
using these images for quantitative analysis of shape is difficult since what is seen
is a projection of a three-dimensional (3D) particle onto a 2D plane. Furthermore,
quantification of surface details is difficult with projections due to overlapping and
the location of details on the original 3D surface.
A similar condition exists in LOM where transmitted light is sometimes used for
imaging particles. In practice, loose particles are distributed on a light transparent
substrate and the illuminating light is passed through this substrate into the micro-
scope objective lens. What is seen are shadows defining the particles and bright sur-
rounding regions where the light passed through unobstructed. As with the SEM
images, these are projections where only the extremes in particle surface provide
the shadow edges. Examples are seen in Fig. 6.16, where gas and water atomized
powders are compared. The gas atomized powder is a coarse titanium alloy powder
and the water atomized is an example of a ferrous PM-PF alloy.

Figure 6.15 Water atomized (A) Fe and (B) 316L stainless steel. SEM/SEI. SEM, scanning
electron microscope.

Figure 6.16 Transmitted light projections of gas atomized titanium powder (A) and water
atomized iron powder (B).
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 117

This transmitted light technique is limited in the capability to produce highly


detailed images of the fine AM powders. In using a light microscope to acquire the
image, the distance between the sample on the substrate surface and the front of the
objective lens must be larger than the particle size, which may be difficult if high
magnifications are required to enlarge the small AM particles and the position of
the in-focus plane requires the objective lens to be in contact with some of the pow-
der particles. Also, it cannot be assumed that what is imaged is randomly oriented.
The positioning and stability of the distributed powder is strongly affected by parti-
cle shape.
While using SEI and transmitted light may not be the most favorable techniques
for surface texture and some shape evaluations, using LOM to generate cross-
sectional images of loose powders in prepared metallographic mounts has proven to
be highly effective. Well-prepared planar surfaces provide the localized detail of
both the particle surfaces and interiors, which allows for accurate sample evaluation
using either manual or AIA techniques.
Although the SEM is not a preferred image source for the shape and texture
analysis, when SEI or backscattered electron imaging (BEI) is coupled with EDS, it
is effective in determining the presence of cross-product contamination. These are
visual imaging techniques where atomic number and chemical analysis on a local
scale can be used to distinguish one composition from another.

6.3.2 Metallographic sample preparation


6.3.2.1 Sampling
The first requirement in a metallographic evaluation of loose powder samples is the
acquisition of a representative sample for preparation and testing. Although many
techniques are used to select a random sample, the most reliable methods conform
to accepted standard practices [14,15]. The selected powder sample must be typical
of the powder mass and the sample size should be sufficiently large to allow for
preparation and analysis of multiple metallographic mounts.

6.3.2.2 Mounting
Once the sample is selected, the size and shape of the individual particles are usu-
ally the important characteristics in determining the most effective method for
mounting loose powder particles for the analysis of planar cross sections. The nor-
mal PM-PF grade particles (,150 μm in diameter) are often mounted successfully
using the standard fine compression mounting powders, for example, diallyl phthal-
ate, epoxy, or phenolic. This is accomplished by making a uniform physical mixture
of the metallic and mounting powders, pouring the mixture into the mount enclo-
sure, then processing the mixture using the pressure-temperature combination
appropriate for the specific mounting material. The combination of the large parti-
cle size and irregular shape of the metallic particles is often forgiving with these
mounting materials. More importantly, the irregular shape of the PM-PF particles
118 Additive Manufacturing for the Aerospace Industry

offers interlocking of the metal powder with the mounting material to anchor the
particles in the mount. This physical restraint is the only means of securing the
sample particles in the mounts with the compression mounting materials.
The situation with the titanium and other alloy AM powders is substantially
different. The particle size is often significantly smaller (, 60 μm in diameter) and
the shape is basically spherical with smooth surfaces. The spherical shape mini-
mizes the amount of surface area to the particle volume and the smooth surfaces
compound the mounting difficulties. With this combination of size and shape, no
physical interlocking occurs between the metallic powders and the compression
mounting materials. Consequently, for several reasons, the particles tend to pull-out
of the mount when ground and polished. These include, but are not limited to, pro-
cessing the surface past the location of the particle diameter, applying excessive
pressure to the mount during preparation, or if a heavily napped cloth is used during
final polishing.
Fig. 6.17 illustrates the difficulty preparing small spherical objects and retaining
them during grinding and polishing. In the top set of circles (simulated monosize
spheres), each circle is offset approximately 15% of the diameter length to a lower
position inside the textured mount. This offset shows an example of the random
positioning of the individual particles inside the rectangular mount volume. The
mount is then sectioned by grinding and polishing, with the location indicated using
the dashed line. This is seen in the lower group as flattened sections of the circles.
As the sectioning line approaches or passes the particle diameter, less of the particle
remains inside the mount and the likelihood for removal of the particle increases. In
this example, the two features on the left of the lower group will probably be
removed, the center two are in question, and the two on the right will probably be
retained.
One possible remedy for this situation is to use a liquid epoxy as the mounting
material. Liquid epoxies offer the advantage of having adhesive qualities that help
retain the low surface-area particles in the mount while maintaining the overall

Figure 6.17 Schematic example of particles being removed and retained in a mount after
grinding and polishing. Top: Simulated monosize spherical particles in the as-mounted
condition. Bottom: Particles after sectioning.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 119

hardness of the cured mount. Consequently, a greater percentage of the particles


will remain in the prepared mount.
To make the epoxy mounts, the epoxy is prepared first using the normal proce-
dure for the multicomponent mixture, then a small quantity of the subject metal
powder is introduced into the liquid mixture by stirring or folding until the distribu-
tion of the metallic particles is uniform and all the particles are coated with epoxy.
Care must be taken not to entrap air in the viscous liquid/metal mixture while fold-
ing or stirring. The presence of entrapped air bubbles in a cured mount is seen in
Fig. 6.18 as the large, dark, circular regions. After mixing, the epoxy/metal powder
composite mixture is poured into a mold. To finalize the mount, additional epoxy is
added to the top of the mount to ensure the proper mount height required for subse-
quent processing. The mold containing the epoxy/metal particle mixture is then
cured for the time recommended for the specific epoxy. After this time, it is often
useful to heat the cured mount to  100 C (  200 F) before starting preparation to
ensure the mount has cured fully. Due to the particle size distribution of the metal
powders and the high viscosity of the epoxy, segregation of the particles by size is
often not severe, with most of the particles remaining suspended in the viscous
epoxy. This helps ensure that a more representative selection of the particle size
distribution will remain in the mount and on the prepared surface for analysis.

Figure 6.18 Entrapped air bubbles in an epoxy mount of a gas atomized titanium alloy AM
particle cross sections. AM, additive manufacturing.
120 Additive Manufacturing for the Aerospace Industry

6.3.2.3 Grinding and polishing


The traditional progression of grinding metallographic mounts with successively
finer abrasives is often unnecessary and too aggressive for the preparation of
mounts containing loose powders. Where the initial grinding step is normally per-
formed to remove the deformation introduced by abrasive sectioning, the loose
powder samples have not undergone any deformation from sectioning prior to
mounting. Consequently, the purposes for grinding are to expose the particle cross
sections and establish the plane for polishing. In most cases, this is accomplished
using a single fine grinding step. Often, a CAMI 320 to 600 grit (FEPA P400 to
P1200) SiC paper with light pressure is sufficient to section the fine particles and
create a plane for the ensuing polishing steps. As with all sample preparation, the
abrasive type must match the alloy being prepared. With many titanium alloys,
grinding may be performed using a single 320 grit (P400) SiC paper step.
Regardless of the alloy, grinding may be accomplished manually, although it is
more frequently done using more automated methods.
The standardized manual and automated polishing procedures normally used in
the preparation of consolidated samples may not be appropriate for retaining small
particles in the defined planar cross sections. If these are the only options available,
the applied pressure, rotational speed of the polishing wheel, and polishing cloth
should be closely monitored and controlled to minimize particle pull-out. Cloth
type will affect the retention of the particles. Soft and napped cloths can promote
particle removal. Frequently, the hardness difference between the metal particles
and mounting material is significant and long polishing times, especially during
fine polishing with medium to heavily napped cloths, can remove an excessive
amount of mounting material, resulting in edge rounding and loss of particle sur-
face detail.
The number of steps and the time needed to achieve an excellent polished
surface is dependent on the condition of the surface after the final grinding step
and the alloy being prepared. For many titanium alloys, only two polishing steps
are required after the single grinding step, with the corresponding polishing
times being comparatively long [16]. For example, the first step is with a 6 or
9 μm diamond polish on a composite disk for 5 minutes and the second step is
with colloidal silica on a medium-hard nonporous cloth for .7 minutes. The
final polishing is aided through a small addition of H2O2 to the abrasive
suspension.
One alternative that has been used successfully is a two-step vibratory polishing
sequence. This is a combination of a long coarse polish on a “hard” cloth, followed
by a final polish on a short-napped cloth for a brief time. The drawback with this
method is the time needed for the first step. Usually hours, possibly 816, are
required to remove the evidence from the grinding step and reach the undisturbed
microstructure. The second step, the final polish, is normally accomplished in
,30 minutes; frequently 515 minutes is sufficient. The composition of the alloy
being prepared determines the type of polish used; however, alumina (Al2O3) in
two particle sizes has been used successfully with multiple materials.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 121

Particle removal from the mount can be a significant issue. If an excessive


number of particles are pulled out, it is advisable to either reprepare the sample
from the grinding step or create a new mount. One factor to consider is that
finest particles may be removed more frequently. These particles can have a
smoother surface compared with the coarser particles and the distance to the
location of the particle diameter is shorter. In a comparison of the relative
particle sizes, the coarse particles cool more slowly during atomization due to
their mass. This increases the possibility of impact with other particles while
solidifying, thus creating protrusions or satellites, or allowing precipitation of
phases or transformation products on the surfaces, which could microscopically
roughen the surface.
As an important reminder, all material and alloy-specific preparation practices
must be followed. The preparation procedures and materials are not universal across
the assortment of alloys used in AM.
An AM powder is used in Fig. 6.19 to illustrate the appearance of the powder
particle cross sections and particle pull-out. The sample has been mounted in epoxy,
manually ground, and vibratory polished. Despite these precautions, particle
pull-out still occurred. Image (A) shows the prepared field using normal image
brightness and contrast. Particle cross sections and edges are well defined and the
image appears satisfactory for AIA using LOM. The same field is shown in image
(B), where the brightness has been increased to show craters in the epoxy that were
the locations of particles removed during grinding and polishing (see arrows).
Consideration must be given to whether an excessive number of particles have been
removed, thus compromising the analysis due to a particle size bias. It is normal to
observe a small amount of particle pull-out, but a decision must be made whether
the number and density of particles remaining in the mount represent the volume
being analyzed.

Figure 6.19 Prepared cross section of an AM-grade powder. The illumination of image (A)
is suitable for analysis using automated imaging techniques, while image (B) has been
brightened to show locations where particles were pulled out during preparation. AM,
additive manufacturing.
122 Additive Manufacturing for the Aerospace Industry

6.3.3 Light optical microscopy—automated image analysis


Upon completion of sample preparation, an AIA system is used to generate the
shape and texture data. Customized testing routines have been developed to provide
the data needed to estimate the particle shape and surface texture using several cri-
teria. However, prior to any testing, decisions must be made to determine the mag-
nification needed to provide images in sufficient detail, the number of particles or
mount area to be examined, and other analysis details.
Considering the fine particle size of the of the various titanium, nickel-based,
iron-based, and other AM alloys, the magnifications most often used are determined
using a 20 3 or 50 3 objective lens on the light optical microscope. The require-
ments used for choosing the magnification are defining the particles with sufficient
pixels in the digital image and ensuring the number of analyzed particles exceeds a
minimum value. Revealing feature details, especially at the particle edges, is most
important in the decision process since the number of fields can be adjusted by
altering the stage pattern on the image analysis system. At the magnifications deter-
mined using the 20 3 or 50 3 lens and the attendant image resolution, the particle
cross sections and surface details are normally apparent and various measurements
can be made. In addition to the shape information, entrapped pores or other features
are also revealed and quantified on a routine basis. Fig. 6.20 shows a field from an
example titanium alloy powder mount within the described magnification range. In
addition, the sample was prepared using the three step sequence discussed previ-
ously and shows minimal particle pull-out.
Changes in image appearance resulting from adjustment in magnification are
seen in Fig. 6.21. This combination of images from the LOM-AIA system shows
several levels of magnification to illustrate how the pixel resolution and the ability

Figure 6.20 Cross sections of a titanium alloy powder metallographically prepared and
imaged using the automated system LOM, unetched. LOM, light optical microscopy.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 123

Figure 6.21 Light optical microscopy images acquired using the automated image analysis
system. The left images, (A), (C), and (E) are whole fields, while the right images (B), (D),
and (F) are the regions within the red rectangles enlarged 8 times. Although difficult to see,
the actual square representation of the pixel size is visible in B, D, and F.

to change magnification help in defining the features. The objective lens magnifica-
tion and image resolution are displayed on each pair of images. In photomicro-
graphs A, C, and E, the pixel array in the digital camera remains the same, but the
size of the features in the image are altered with changes in magnification.
Consequently, each feature is characterized by more pixels with increases in magni-
fication and more detail, especially at the edges, is defined.
124 Additive Manufacturing for the Aerospace Industry

The images in the left column, Fig. 6.21A, C, and E, show entire microscope
fields at three magnifications and resolutions. The right images, B, D, and F, are
the segments of the whole field images outlined with a red rectangle and subse-
quently digitally enlarged eight times to show the pixel size. While changing the
magnification introduces a requirement that more fields be examined to see
the same sample area (four times the fields for a doubling of the magnification), the
amount and quality of information available is improved to show more detail. This
is especially apparent at the feature edges where interparticle friction is important
to particle behavior during part build. Increasing the magnification, with the corre-
sponding increase in resolution, uses more pixels to define each particle, thus show-
ing more feature details.
Once the image is digitized, the process of separating the areas of interest from
the entire field must be accomplished accurately for the image processing and mea-
surements to be as close to the original sample as possible. This is done by compar-
ing the digital gray level or color value of each pixel with a predetermined gray or
color range and separating all pixels falling within this range from those outside.
With higher resolution, the ability to make this segmentation is more accurate in
defining the individual features. The AIA systems use automated and/or manual
methods for this process. Sometimes it is details in the sample that dictate the seg-
mentation method. After separation and storage of the desired information, all
image processing and measurement can be made.
In looking at the digital representations of the particle cross sections, examples
of touching particles are often seen in multiple locations within each magnified
field. These may be particles on the prepared surface that are touching due to coin-
cidence of location from the mounting process. To help separating these touching
particles, a sequence of image transformations can be written to separate particles
sharing a predefined linear distance, while particles with more common surface
remained joined. In this way, individual particles could be separated while satel-
lites, protrusions, and surface irregularities would remain connected. Provisions are
also written into the program to sort particles into size classes, eliminate specific
sizes from the analysis, or analyze particles by size classification. It is important to
remember the design of the program can be tailored to fit specific sample and data
requirements.

6.3.4 Shape and texture analysis


The physical characteristics of shape and texture are factors in the behavior of the
powder mass during the AM process. The shape affects the ability of the particles
to fill the powder bed and impact the flow, possibly slowing or creating a more
erratic flow behavior if the particles deviate from a near-spherical shape. Surface
texture influences interparticle friction and may significantly alter powder flow and
bed fill.
Examples of particle shape and surface texture are presented in Fig. 6.22. The
(A) image shows the basic particle shape of a gas atomized Ti6Al4V AM-grade
powder, with surface protrusions, satellites, and possibly a slight amount of
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 125

Figure 6.22 A gas atomized Ti6Al4V powder in (A) shows variation in particle shape
with a lower magnification image and detail of the surface texture of a single particle is seen
in the (B) image. SEM/SEI. SEM, scanning electron microscope.

Figure 6.23 Gas atomized titanium alloy particle (A) and an electrolytic copper particle (B).
SEM/SEI. SEM, scanning electron microscope.

secondary solidification. The surface texture of the same gas atomized Ti6Al4V
powder is seen in Fig. 6.22B. These shapes and surfaces are a result of solidifica-
tion of the liquid metal after contact with the gas stream.

6.3.4.1 Shape analysis


The concept of shape is somewhat subjective and, in these tests, is applied to the
2D representations of individual AM metal powder particle cross sections. With the
AM powders, the shapes of the particles and the shape variation within a powder
mass are dependent on the chemical composition of the alloys and the processes
used in their manufacture. In designing a shape analysis program, the testing para-
meters and conditions must be relevant to the features being studied. Not all test
measurements and expressions are necessarily useful to all powder types. For exam-
ple, it is doubtful the gas atomized titanium-based powder in Fig. 6.23A and the
electrolytic copper powder in Fig. 6.23B would be evaluated using the same shape
126 Additive Manufacturing for the Aerospace Industry

expressions. The particle shapes and end uses are too diverse. Consequently, the
tests should be designed to fit the powders and their intended applications to ensure
the data generated are both relevant and valuable. With AM, where powder flow
and apparent density are important, the shape testing should give an insight into
how these characteristics affect interparticle friction, flow of the powder mass,
particle packing, rearrangement, etc.
The literature contains numerous articles addressing the subject of analyzing
feature shapes, many of which can be applied to particle cross sections. These
include examples using measurement ratios, shape and form factors, comparison
with geometric shapes, Fourier analysis, the measurement of incrementally spaced
radii, and several mathematically intensive techniques [1728]. In addition, several
references incorporate quantitative microscopy (stereology) for analyzing geometric
properties, such as surface-to-volume ratios, calculated shapes, and curvature of
microstructural features [2941]. Using a slightly different approach, Hausner ana-
lyzed 12 different particle shapes through the combination of four individual mea-
surement criteria. He included illustrations of the particle perimeters for visual
comparison with the corresponding data [42].
Although the aforementioned references contained many methods for evaluating
shape, three approaches are discussed here. They are:
G
Combining individual measurements, that is, length, width, area, perimeter, various
diameters, etc., into ratios.
G
Using combinations of areas, perimeters, lengths, etc., in comparison with a geometric
shape, in this case, a circle.
G
Reduction of 2D feature data into a 1D graphic and statistical representation.
G
Measuring incrementally spaced radii from the feature centroid, plotting the results on
an x, y graph, and examining the data statistically (radius function).
Each approach was successfully accomplished in an automated fashion by
combining a series of commands in an AIA system and examples were examined in
more detail, as follows:
Ratios of individual measurements:

length
Aspect ratio 5 (6.1)
width

convex perimeter
Roughness 5 (6.2)
perimeter

Comparison with a geometric shape (circle):

4πA
Circularity 5 (6.3)
perimeter2

4πA
Compactness 5 (6.4)
convex perimeter2
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 127

4A
Roundness 5 (6.5)
π max Feret0 s diameter2

where A is the cross-sectional area of the particle, Feret’s diameter is a tangent or


caliper diameter.
 
Excess perimeter 5 perimeter  PAeq 3 100 (6.6)

where PAeq is the perimeter of an area equivalent circle.


In each of the above cases of geometric shape comparison, except for the Excess
Perimeter estimate, as the 2D feature approaches the shape of a circle, the value of
the expression increases to a maximum of 1. Features deviating from the circular
shape have a value ,1. The Excess Perimeter result is the percentage increase in
feature perimeter length compared with the area equivalent circle perimeter. In this
case, as the feature becomes rounder and smoother, the percentage drops to a mini-
mum value of 0.
Examining the radius function, the feature cross sections are defined using the
grayscale comparison and the centroid (center of gravity) of each, located using the
image analysis system. Radii are then drawn from the centroid to the feature perim-
eter. In these analyses, 30 radii were incrementally spaced at 12 degree intervals, as
seen in Fig. 6.24 with the 0 degree location highlighted. In this way, the shapes of
the features were determined by analyzing the variation in the radius lengths. The
lengths were plotted on x, y graphs and the statistics of mean (x), standard deviation
(s), and coefficient of variation (CV), ðs=x 3 100Þ calculated for each feature.

Figure 6.24 Example of the defined feature cross section containing the 30 radii. The 0
degree radius is located and the angular movement for measurement is counter-clockwise.
LOM, unetched. LOM, light optical microscopy.
128 Additive Manufacturing for the Aerospace Industry

There were several reasons for choosing 30 radii for these analyses. They were
related to the microscopy, the imaging process, and the size of the magnified parti-
cles. The choice of 30 was a compromise considering acquiring sufficient data for
the evaluation and the digital imaging process.
Once the particles are digitally imaged and the particle cross sections detected,
they are represented by a contiguous array of small raster points resembling
squares, that is, pixels. Within each particle, the centroid is located and radii drawn
from that point to the perimeter in 12 degree increments. Some of the pixels near
the feature center of gravity are used for multiple radii simply due to the proximity
of the individual radii to the origin or they are in contact with pixels from neighbor-
ing radii. As measurements are made, the image analysis system determines the pix-
els belonging to a feature by which are touching and which are not. As more radii
are used, the area at the center of each feature containing both pixels that are being
used multiple times and those that are touching neighboring pixels is enlarged.
Therefore, to measure each radius individually, a technique is needed to account for
the reused and touching pixels. This is done by creating a circle of known diameter
at the center of gravity sufficiently large to cover the area of multiple-use and
touching pixels. Prior to measurement, the circle is subtracted from the 30 radii and
each remaining radius then measured, see Fig. 6.25. The radius of the subtracted
circle is then added to each radius measurement to obtain the actual radius length.
If more radii are used, the size of the circle at the centroid must be enlarged to
account for the additional touching pixels and this could eliminate some shapes or
smaller particles from the analysis. The circle size used in Figs. 6.24 and 6.25 to
contain the touching pixels was sufficiently small to affect only the finest particle
cross sections and not have an impact on the analysis.
Experimentally, the collection of 30 data points for each particle appeared to be
sufficient to describe the particles. However, it is clear this technique could be used

Figure 6.25 A field prior to measurement showing the radii overlaid on the particle cross sections
with the circle at the center-of-gravity removed. LOM, unetched. LOM, light optical microscopy.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 129

successfully with more or fewer radii. Problems could be encountered with some
particle shapes. Examples are reentrant or overlapping surfaces where the center of
gravity, in extreme cases, might be near the edge or even outside the particle, peri-
odic or daisy-like shapes, or long, thin particles. Although these shapes are clearly
not satisfactory for AM, the radius technique could be used to analyze shapes other
than the desired convex particle cross sections.
It was also found that changing the number of radii had negligible effect on the
overall analysis time for a given sample. Most of the time used for the analysis is
accounted for with image acquisition and processing, which would be a constant in
the time required in the analysis. Changing the number of line lengths to be mea-
sured would shorten or lengthen the analysis time accordingly, but the change is
probably insignificant to the overall analysis time.
In determining the microscope magnification, the size of the AM particles is rela-
tively small in average diameter; consequently, a relatively high magnification is
needed to enlarge the particles sufficiently to see detail of the perimeters. For this rea-
son, the 50 3 objective lens was chosen for the example shown below. A lower mag-
nification could be used to examine the same number of particles in fewer fields and
in a shorter time, but with a possible unacceptable loss in surface information.
This selection of shape analyses parameters was performed on several powder
samples using the ratios and geometric comparisons mentioned above. It was found
that, although all the shape expressions are effective, some are more useful with
specific particle types. Additionally, some may be more robust than others.
Examples of both successful and less-than-successful analyses are presented in
Figs. 6.26 and 6.27. In both figures, two powder samples of gas atomized AM 316L

100
90 length/width
80 001
Cumulative percent

70
002
60
001 002
50
40
30
20
10
40 μm 40 μm

0
1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8 3.0
Aspect ratio

Figure 6.26 The aspect ratio results from the testing of gas atomized 316L powder samples
001 and 002 with the inset images showing examples of the particle cross sections. The
results are shown as cumulative plots of the frequency distributions. Inset images—LOM,
unetched. LOM, light optical microscopy.
130 Additive Manufacturing for the Aerospace Industry

100

90
001 Circularity
001 Compactness
80
002 Circularity
Cumulative percent

70
002 Compactness
60

50 Circularity = 4πA/P2
40 Compactness = 4πA/convex P2

30

20

10

0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0
Shape factor

Figure 6.27 The results of the circularity and compactness testing of gas atomized 316L
powder samples 001 and 002. The results are shown as cumulative plots of the frequency
distributions.

stainless steel were tested for comparison. The powders were produced by the same
manufacturer at different times and given the arbitrary designations of 001 and 002
for these tests. Both figures include the shape data from .1000 particle cross sec-
tions. During the analysis, numerous individual measurements were made and rela-
tionships calculated for each particle. From these data, several graphs were plotted
to characterize the two sample populations, with three shown here.
In Fig. 6.26, the results of the aspect ratio testing are compared. It is clear in this
cumulative percent plot that this ratio was not applicable to these powder samples
and, regardless of other shape differences, the ratio of length to width was not sig-
nificantly different with the population of particles examined in the two samples.
The two inset photomicrographs show examples of the particle cross sections for
comparison.
Measurements to calculate circularity and compactness were also made during
the characterization process of these two samples. Both are based on the shape of a
circle, with the actual and convex perimeters of the cross sections used to differenti-
ate the two expressions. Fig. 6.27 shows the comparison of the two powders based
on this difference in perimeter length, that is, surface texture. It shows the effect of
differences between the two perimeters resulting from the convex perimeter
smoothing small irregularities from the particle surface. Again, the graphs show
cumulative totals, with positioning of a curve to the right indicating a smoother,
rounder particle.
It is clear the “001 powder” sample is rounder when judged by circularity, with
the dashed blue line positioned a significant distance to the right of the dashed red
line. The difference in compactness is only seen at a shape factor value .0.65,
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 131

with the two solid lines diverging a measurable amount after that point. At com-
pactness values ,0.65, the samples are virtually identical.
Other measurement combinations were evaluated, with some appearing to be
more effective than others at differentiating these fine, relatively smooth, round par-
ticle cross sections.
The radius function evaluation was also performed using the image analysis sys-
tem. The basic sequence of image processing has been described earlier. The fields
for analysis were chosen randomly, with the selection of features made in several
ways. In some cases, particles were sorted into size groups, while specific sizes
were eliminated from consideration in others. An example of a processed field can
be seen in Fig. 6.28. This area was selected from a multifield automated analysis of
an AM maraging steel powder because it contained several particle shapes likely to
provide valuable insights into the radius function analysis. In Fig. 6.28A, the sepa-
rated and detected particles are the yellow features with four individuals selected
for further discussion. They are labeled 14. These were chosen for graphic repre-
sentation due to the variation in their individual shapes. Specifically, particle num-
ber 1 is pear-shaped, 2 appears to have secondary solidification on the lower right
side, 3 is nearly round, and 4 is roughly triangular. Fig. 6.28B shows the particle
cross sections with the centroids and radii appearing as the red overlay within the
detected features. Several small particles were eliminated from the analysis due to
their size and are radii-free. One defined particle appears to be an agglomeration of
two particles. During the automated sequence, guard and process frames were used
to control automated stage movement and eliminate partial particles from analysis,
while ensuring all particles were equally likely to be detected and analyzed.
Fig. 6.29 contains the results from the radius function analysis of the four
selected particles. It consists of particle images with the overlaid radii, x, y plots of
the 30 consecutive radius lengths, and the statistics of mean, standard deviation,
and CV. As expected, the graphs showing the change in radius length appear to be
characteristic of the basic feature shapes. For particle 1, the graph shows two peaks
and valleys in the description of the elongated, pear-shaped particle. The erratic

Figure 6.28 Field process for the radius function analysis. (A) is the detected, acquired
image and (B) is the detected features with the centroids and radii. The material is a
maraging steel powder. LOM, unetched. LOM, light optical microscopy.
132 Additive Manufacturing for the Aerospace Industry

1. 30

Radius length (μm)


25

20

15

10

5
Mean (μm): 20.87
0 Std. dev. (μm): 4.09
0 100 200 300 400
C.V. (%): 19.60

Angle (°)

2. 30

25
Radius length (μm)

20

15

10

5
Mean (μm): 20.79
0 Std. dev. (μm): 2.48
0 100 200 300 400 C.V. (%): 11.93

Angle (°)

3. 30

25
Radius length (μm)

20

15

10

5 Mean (μm): 19.10


0 Std. dev. (μm): 0.35
0 100 200 300 400 C.V. (%): 1.83

Angle (°)

30
4.
Radius length (μm)

25

20

15

10

5
Mean (μm): 12.80
0 Std. dev. (μm): 2.98
0 100 200 300 400
C.V. (%): 23.28
Angle (°)

Figure 6.29 Results of the radius function analysis for the four particles chosen from the
field in Fig. 6.28. LOM, unetched. LOM, light optical microscopy.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 133

shape of the graph for particle number 2 is characteristic of the irregular perimeter
from the secondary solidification region along the lower right edge. Particle 3 is
nearly round, with an almost flat graph. As with particle 1, the curve for particle 4
also appears to be nearly cyclic, although with a different period due to the triangu-
lar shape.
In looking at the statistics to the right of the graphs, the variation in radius length
is reflected in the standard deviation and CV for each particle. Particle 4 is the
smallest in size compared with the other three; however, the CV reflects a large
variation in the radii lengths. As a measure of the dispersion in the freqeuncy distri-
bution, the CV is comparable even though the particles are different sizes.
It is clear the x, y plots in Fig. 6.29 exhibit characteristic appearances in describ-
ing certain periodic or geometric cross-sectional shapes. While the measurement at
each angle is not important when taken alone, it is the overall shape of the curve
and the relationship of the local measurements that provides the shape and texture
information. Uniformity in the lengths indicates a round particle (Fig. 6.29-3) or a
round section of a particle surface, as is seen in the portion of Fig. 6.29-2 between
approximately 100 and 200 degrees. Large variations in the lengths show irregulari-
ties in the global shape and looking at the local angular progression of the values
can show whether the feature is relatively smooth or rough. Abrupt changes in
length depict roughness, while gradual changes, neutral, positive, or negative, indi-
cate a smooth surface, although not necessarily round.
The statistics generated from these data can be both useful and misleading. Both
the mean and standard deviation are related to size and, thus, cannot be compared
directly unless the particles are equivalent in size. Three of the four particles used
in Fig. 6.29 have basically the same size radius; as a result, the standard deviations
are comparable. Particle 4 is smaller and cannot be compared using the standard
deviation. However, with the CV as a ratio of the standard deviation to the mean, it
is valid for a variability comparison regardless of feature size. It should be noted, if
statistical comparisons within size classes are needed, the cross sections can be
sorted into classes before testing or the population measured and the data sorted by
a specific size parameter.
The AIA sequence of quantifying porosity entrapped within the particles can be
seen in the lower magnification/resolution series of photomicrographs in Fig. 6.30.
They demonstrate the sequence of image processing and how the separation of
pores from the particle cross sections can be made. In order of processing, step 1 is
acquisition of the grayscale image, followed by comparing the grayscale range of
the pixels with a predetermined grayscale, with those falling within the grayscale
shown as green and used for further processing and analysis. Next, touching parti-
cles are separated, with locations of created boundaries indicated with the small
yellow circles. If required, the algorithm used for this separation can be adjusted to
fit the amount of contact. The pore locations within the particles are located and,
finally, the pores defined for measurement are shown in red. This is gas atomized
titanium alloy AM powder imaged at a resolution of 0.69 μm/pixel. It is important
to note that, although the resolution used in this example is lower than what is used
in the shape analysis, the internal features are still detected and measured. With the
134 Additive Manufacturing for the Aerospace Industry

Figure 6.30 Image processing sequence for the analysis of porosity entrapped inside
particles.

pore analysis, multiple measurements and calculations can be made. They include
the area percent porosity contained in the total metallic area fraction, the percentage
of the particles containing pores, the pore size distribution, and others where
needed. It has also been shown that 2D AIA estimates of the porosity content in
AM materials compared well with 3D estimates from CT scanning [4346].
Questions often arise as to the time required for these tests. In regard to the test-
ing time with the AIA system to analyze shape, size, and internal porosity, once the
test method is developed, sample preparation requires 11.5 hours and the analysis
time is usually ,10 minutes/sample. In use, analysis of between 20,000 and 50,000
particles was accomplished in ,7 minutes during the research/method development
program. The variability in the number of particles was due to the particle size
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 135

distribution of the materials. At the conclusion of testing, averages and distribution


values are generated by the AIA system and the individual feature data is stored if
further manipulation is needed.

6.3.5 Microstructural analysis


Polished cross sections are also used to evaluate the microstructure of the as-
atomized particles. The same chemical etchants used for consolidated or cast tita-
nium products are used to reveal these microstructures. The most frequently used
etchants for the typical titanium alloy compositions are shown in Table 6.3 [47].
Examples of two as-gas atomized Ti alloy powder samples etched with Kroll’s
reagent are shown in Fig. 6.31.
It should be recognized the microstructure of the as-atomized particles is dis-
tinctly different compared with additively manufactured, PM, or cast titanium parts.

Table 6.3 Chemical etchants used for typical titanium alloys

Etchant name Typical composition Notes


Kroll’s reagent 1.5 mL HF Most commonly used
4 mL HNO3 etchant for Ti
94 mL H2O alloys
Oxalic reagent (tint) 20 mL HF Do not remove etch
20 g Oxalic acid products
98 mL H2O
ABF 1 g ammonium biflouride (NH2FHF) Do not remove etch
products
Lactic hydride Mix fresh 5 mL lactic acid and 5 mL Will etch
reagent stock solution of 3 mL HF and commercially pure
97 mL HNO3 titanium hydrides

ABF, ammonium biflouride.

Figure 6.31 Particle cross sections etched with Kroll’s reagent. Left image Ti6Al4V
right image Ti5Al5Mo5V3Cr.
136 Additive Manufacturing for the Aerospace Industry

The cooling rates experienced by the loose powders during atomization are substan-
tially faster than what is seen by a built or finished part. This results in a completely
different combination of phases and transformation products in the microstructure.
The utmost care should be exercised when etching any titanium alloy. Safety
procautions must be followed and personal protection equipment (PPE) must be
used. Hydroflouric acid, either as a direct component in the etchant or as produced
in the etching solution, is dangerous and extremely harmful to the operator and
metallographic equipment. Consult all available safety documents, that is, safety
data sheets, when using any ingredient in a chemical etching solution.

6.3.6 Chemical analysis


Chemical analysis is performed on AM powders to assure the particle-to-particle
uniformity in the powder mass. Variation in local alloy content may result in differ-
ences in microstructure, which could cause problems in part performance. In pro-
duction facilities and AM machines where multiple alloys are used, the possibility
exists that one alloy could accidentally contaminate another, aka, cross-product con-
tamination. In addition, powder transportation and handling could cause introduc-
tion of foreign materials. In both cases, accurate and reliable methods are needed to
determine the presence of contamination particles and if possible, identify them.
CT scans are sometimes used for these tests, however, because the CT scanner
relies on variations in density to determine alloy composition differences, the den-
sity difference must be fairly substantial to give a clear indication of the contamina-
tion. Historically, some of the original testing performed on titanium alloys in AM
was concentrated on detecting the presence of tungsten particles. This is relatively
simple since the density of a typical Ti6Al4V is approximately 4.5 g/cm3 while
tungsten is approximately 19.3 g/cm3. In this case, the W particles will appear as
bright particles in a mass of darker, lower density features in CT scans.
Unfortunately, no information on the actual chemical composition is generated.
Although detection of large differences in density, such as tungsten in a titanium
alloy, is possible using CT scans, problems arise when the contaminant composi-
tions are closer in density. The unintentional mixing of a titanium alloy with stain-
less steel, nickel-base alloys, or another titanium alloy may cause problems with
part performance through a variation in localized chemical composition and possi-
bly the microstructure. In these cases, the CT scan would possibly be unable to dis-
tinguish one material from another.
To improve on the ability to detect and identify chemically dissimilar contami-
nant particles in another alloy volume, an imaging and chemical analysis procedure
has been developed using a SEM equipped with EDS [48]. The goals of the testing
were to locate any contaminants that were present, determine their chemical compo-
siton, and find ways of displaying their presence that would be easily understand-
able and not subject to interpretation. Furthermore, these data and images could be
further analyzed for quantitative estimates of contamination composition and
amount.
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 137

Figure 6.32 Ti6Al4V alloy containing a large tungsten-rich contaminant. BEI unetched.

Initially, an SEM imaging technique using BEI was used to imitate the effect of
density used by the CT scan. These images are formed by the SEM based on atomic
number differences, where a higher atomic number feature will appear brighter than
one of lower atomic number. In looking at the comparision of titanium and tung-
sten, where the densities were vastly different and the basis for CT scan contrast
diferences, their atomic numbers are 22 for titanium and 74 for tungsten. It was
found that differences this great would not present a problem visually to differenti-
ate between these two elements, or alloys based on them, using an SEM imaging
technique. An example is shown in Fig. 6.32, which is a titanium alloy part contain-
ing a large tungsten contaminant particle. The tungsten particle is the lightest gray
feature in the image and the surrounding intermediate gray area is slightly higher in
atomic number than the darker gray, titanium alloy matrix.
Although finding the tungsten particles was accomplished using BEI, determining
the presence of particles closer in density, atomic number, and composition to the
base powders was also needed. Consequently, a test was designed for a contamination
study using a Ti6Al4V powder as the base. In the initial testing, samples of the
Ti6Al4V were doped with varying amounts of 316L stainless steel and Inconel
625 AM powders. The base powder and the contaminants had the same basic shape
distribution; however, the 316L was finer in particle size distribution. BE images
were acquired of both samples and elemental EDS maps constructed by designating
colors for each of the major elements present in the alloys. These colors were
combined either to create a distinctive color or to reinforce another color. What is
seen is the location of these elemental combinations separated by color through the
use of localized chemical anlaysis.
Sample preparation of the powders was simply to fix the loose powder particles
to a double-sided electrically conductive adhesive tape. It was also found that using
particle cross sections in metallographic mounts was possible, although the samples
would probably require coating with an electrically conductive material, most likely
carbon, thus increasing the testing time.
138 Additive Manufacturing for the Aerospace Industry

Figure 6.33 BEI of the particle distribution (left). Right image is an elemental map showing
the presence of the Inconel 625 contaminant (yellow) in the Ti6Al4V base (blue).

Figure 6.34 BEI of the particle distribution (left). Right image is an elemental map showing
the presence of the 316L contaminant (red) in the Ti6Al4V base (blue).

Fig. 6.33 shows the results of the Inconel contamination. With the BEI on the
left, a contrast difference is seen between the heavier nickel-base Inconel and
the titanium alloy. The monochrome BEI shows multiple particles slightly brighter
in grayscale compared with the background. The difficulty with this image is esti-
mating the percentage contamination since some of the particles are comparatively
fine in size. To improve this situation, the magnification would need to be
increased. With the chemical analysis, the colors in the elemental map were chosen
to represent the elements in both the base and contaminant alloys that would present
a distinction between the two. In the map image, the titanium alloy, seen as the
blue particles, is well contrasted with the yellow-colored Inconel particles. It is eas-
ily seen that the yellow particles in the elemental map correspond to the brighter
particles in the BEI.
The corresponding pair of images was made using the sample contaminated with
the 316L stainless steel. Images similar to those in Fig. 6.33 are used with the con-
taminated titanium alloy in Fig. 6.34. A similar blue color is again used to represent
titanium and the small stainless steel particles are displayed in red. The BEI was
not as clear in separating the two alloys as with the Inconel. This could be because
Measurement of powder characteristics and quality for additive manufacturing in aerospace alloys 139

the contaminant powders were small in particle size distribution and possibly
because the nickel-based Inconel is higher in atomic number compared with the
iron-based 316L. The situation could also benefit from an increase in magnification,
resulting in an enlargement in the particle projections. It would be particularly help-
ful to increase resolution for both the image and chemical anlaysis when faced with
contamination of a material finer in particle size distribution than the base powder.
To show further effectiveness of the test method, a test was performed using the
same Ti6Al4V base alloy, but with the contaminants as two other titanium
alloys. The two alloys chosen were a Beta 21S (Ti 1 15Mo 1 2.8Nb 1 3Al) and a
commercially pure (CP) titanium Grade 1 or 2. The CP Ti is basically Ti with
# 0.3 wt/o Fe and ,0.25 wt/o O. After unsuccessful attempts at creating well-
contrasted BEIs, these samples were imaged using SE.
Fig. 6.35 is the combination of particles with CP Ti used as the contaminant. In
this case, the base Ti6Al4V particles are a yellowish color while the CP Ti are
red. The Beta 21S results are shown in Fig. 6.36, where the Ti6Al4V base alloy
is an orange color and the contaminant (Beta 21S) is yellow.

Figure 6.35 SEI of the Ti6Al4V with added CP Ti. The right image is the elemental
map showing locations of particles of each composition—Ti6Al4V yellow, CP Ti red.

Figure 6.36 Left image, SEI of the Ti6Al4V with added Beta 21S. The right image is
the elemental map showing the locations of particles of each composition. Ti6Al4V
orange, Beta 21S yellow.
140 Additive Manufacturing for the Aerospace Industry

With these tests, it was found the magnifications could be varied to control the
number of particles imaged and the chemical analysis resolution. This resolution
may be vitally important if the contaminants are smaller in size compared with the
base powder. What is used in this document appears to be a good compromise
between defining the contaminants and showing a reasonable number of particles.
In addition, the resolution of the EDS spectra acquisition must be sufficiently high
to ensure multiple spectra are generated for each particle, regardless of size.
When making the elemental maps, knowledge of the EDS operation is essential
in determining a good combination of elements to be mapped and how to combine
the colors to distinguish one alloy from another. Colors can be chosen as compli-
mentary colors or to reinforce the color of another. It is important to remember,
when chemically dissimilar particles are found, the magnification can be increased
to isolate the contaminant particle and a chemical analysis performed on the single
particle if desired. The results can be qualitative, semi-quantitative, or quantitative
with the use of standards.

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zation of additive manufacturing powders, Int. J. Powder Metall. 54 (1) (2018) 4759.
The processing and heat
treatment of selective laser 7
melted Al-7Si-0.6Mg alloy
Jeremy H. Rao1,2, Paul Rometsch1,2, Xinhua Wu1,2 and Chris H.
J. Davies2,3
1
Department of Materials Science and Engineering, Monash University, Clayton, VIC,
Australia, 2Monash Centre for Additive Manufacturing (MCAM), Monash University,
Notting Hill, VIC, Australia, 3Department of Mechanical and Aerospace Engineering,
Monash University, Clayton, VIC, Australia

7.1 Selective laser melted Al alloy A357


7.1.1 Process control
Based on previous studies, although in a vacuum of a back-filled inert gas,
manufacturing fully dense aluminum alloy parts by selective laser melting (SLM) is
still quite difficult [13] because the build chamber atmosphere can contain
roughly 0.1% residual oxygen [1,4]. Also, SLMed aluminum samples can be porous
due to the high reflectivity and lower absorptivity of raw powder for the laser beam
[2,5], the high thermal conductivity through the solidified material far from the
melt pool, and the formation of oxide layers on the melt pools [68].
Considering the fast solidification rate in SLM with quite limited volume shrink-
age, there are two main causes for porosity: hydrogen and entrained gas [9]. In
SLM, the formation of oxide layers on the melt pools provides ready-made cavities
from which pores can grow at a reasonable pressure [68], making the formation
of pores much easier in SLMed materials. For relatively porous materials produced
by SLM, entrapped gas pores can expand and thus cause blistering during normal
solution heat treatment (SHT), which is detrimental to the mechanical properties
[10]. In SLM, hydrogen pores formed in liquid pools tend to be spherical due to the
surface tension, while those in tight interdendritic channels tend to take on irregular
shapes [2,11]. The irregular pores, in particular, can lead to extensive intercon-
nected porosity when coupled with very poor feeding of molten Al alloys [10,12].
Also, due to the high temperatures reached by laser melting, oxidation of the metal
close to the melt pools could occur [13]. As a result of the tenacity of the surface
oxide film, the metallurgical bonding across the aluminum powder layers can be
inhibited during SLM [14].

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00008-X


© 2019 Elsevier Inc. All rights reserved.
144 Additive Manufacturing for the Aerospace Industry

In SLM, the laser power, scan speed, hatch distance, powder layer thickness, and
substrate temperature are the common parameters adjusted to optimize the process,
changing the volumetric energy density available to heat and melt the powder
[6,7,15,16]. The laser power is the energy applied in a laser beam, and the substrate
temperature is simply the temperature applied on the plate where SLMed products
are built. The scan speed is the exposure time that the laser resides at each point,
and the hatch distance is the point distance between the focused laser spots during
scanning [8]. As one of the most important parameters in SLM, the energy density
controls the degree of consolidation of the powder particles and could potentially
aggravate the defect formation by creating turbulences in the melt pools that can
form defects at extreme conditions [11,17,18]. The energy density function Ψ is
given by

P
Ψ5
v3h3t

where P is the laser power, v is the scan speed, h is the hatch distance, and t is the
layer thickness [11]. Insufficient energy, usually due to a combination of low laser
power, high scan speed, and large layer thickness, also results in balling due to the
lack of molten pool wetting with the preceding layers [19,20]. Excessive balling
promotes the capture of the unmelted powder [2], leading to nonuniform melting by
laser beam and improper deposition of the top layer, inhomogeneity of the follow-
ing layers [21,22], and thus the formation of irregularities on the surface [2]. On the
contrary, a high laser power and a low scan speed may generate excessive energy
[23]. This can be detrimental to the surface finish due to extensive material evapo-
ration or powder sputtering [11,24,25].
For the purpose of SLM-processing parameter optimization, the main objective
is to minimize the porosity. Various SLM parameters toward processible Al alloys
have been collected from different literature and compared to study the specific
effects of laser power, scan speed, and hatch distance on the resultant porosity
[2,6,7,11]. The relative density of the SLMed aluminum and titanium samples
increases with the energy density (P/v 3 h 3 t), until roughly 50 and 100 J/mm3,
respectively, and the further increase in the energy density does not result in any
decrease in the porosity (Fig. 7.1) [2,7,21]. Hence, it appears that once the metal
powder is fully molten, further increasing the heat input is not beneficial and would
be a waste of energy and time [22]. For the SLMed samples built with similar
energy density, their relative density can be quite different (Fig. 7.1). On the other
hand, below this critical energy level, there is insufficient energy completely to
melt the powder, leading to increased porosity due to balling, as discussed above
[21]. Since all the parameters can individually influence the porosity, it is essential
properly to control them within the investigated processing window in order to
determine the best parameter combination to achieve the optimized energy input
and thus to produce dense SLMed parts.
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 145

Figure 7.1 Energy density versus relative density of (A) SLMed Al alloys and (B) SLMed
Ti6Al4V alloy based on the aggregation of data from literature [2,6,7,11,17,26]. SLM,
Selective laser melting.

7.1.2 Density optimization


The aim of this part is to demonstrate the feasibility of using aluminum alloy A357
as powder feedstock for SLM and to investigate the effects of SLM on the porosity
of aluminum alloy A357. The SLM-processing parameters were optimized to
achieve the maximum density, corresponding to an extremely fine microstructure
with very few pores [9]. For the prediction and determination of the most optimized
relative density of the SLMed Al alloy samples, the specific values obtained by
both experimental methods (Archimedes’ principle and Image J analysis) and
computational method (MATLAB) were quantitatively compared in parallel to
select the maximum data point achievable for samples from Groups A and B, as
illustrated by previous work [9]. With the same image analysis method used for
samples from Groups C to G, relative density versus laser power and scan speed
curves were also plotted by MATLAB, and the largest density regime ( . 90%) can
be obtained and marked by the dashed lines in the 2D process windows as well
(Fig. 7.2). Furthermore, based on the MATLAB limit diagrams from Groups C to
G, the surface model prediction of relative density with respect to laser power and
scan speed shows that decreasing the laser power and increasing the scan speed to a
large extent both result in a decreased relative density and thus increased porosity.
In this regard, the laser power affects porosity formation more significantly at high-
er scan speeds, and the scan speed affects the results more significantly at lower
laser powers.
In addition, based on the calculation of the laser power, scan speed, hatch dis-
tance, and layer thickness of each data point from Groups C to G, the specific
energy density corresponding to each relative density value can be determined. The
porosity formation seems to be triggered largely when the energy input into the
material is either reduced or largely increased (Fig. 7.3). In general, the relative
density of an as-SLMed part initially increases significantly with the energy density
146 Additive Manufacturing for the Aerospace Industry

Figure 7.2 3D plots and 2D processing windows showing the relationship among relative
density, laser speed, and laser power of the as-SLMed samples manufactured by Groups C to
G laser parameters. SLM, Selective laser melting.

before reaching the maximum value. This is because at the same substrate tempera-
ture, the reduction in the energy input leads to a decrease in the melt pool size and
then promotes the formation of pores due to incomplete consolidation and improper
powder melting [6,11,27]. At the maximum relative density, the laser energy input
is optimal, providing just enough power for full powder melting and bonding. In
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 147

Figure 7.2 (Continued).

this case, the sufficient energy input at a relatively slower scan speed and a higher
laser power leads to the formation of metallurgical pores with the elimination of
pores [2]. Afterward, the relative density either reaches a plateau before slightly
declining or drops straight away (Fig. 7.3). The experimental results all agree well
the literature review (Fig. 7.1A).
The optimal laser parameter points are summarized in Table 7.1 [9]. Within each
group, the hatch distance, powder layer thickness, and substrate temperature were
initially set as the independent variables. Then the SLMed samples were built with
varied laser power and scan speed to achieve the maximum relative density. Based
on the density results, the corresponding laser power and scan speed can be specifi-
cally determined as the dependent parameters.
Furthermore, since the laser power, scan speed, and hatch distance can individu-
ally control the heat input, it is conceivable that porosity formation can be mitigated
using one of these parameters (within the investigated process window) to control
the heat input and thus the relative density (e.g., use slow scan speed to consolidate
the melt pool fully). It is important to state that these modifications are only valid
within the investigated processing window when the porosity is higher than 90%,
since other mechanisms for porosity formation, such as melt pool turbulence or
evaporation, could also be triggered when they are outside this range investigated
148 Additive Manufacturing for the Aerospace Industry

Figure 7.3 Relative density versus energy density corresponding to the data in Fig. 7.2, with
the red dots showing the optimal laser parameters in each case from Groups C to G.

[11]. Based on the analysis of the microstructure and the mechanical properties in
previous work [9], point a in Table 7.1 was set as the optimized laser parameters
for sample building. Considering the manufacturing time required, point c in Group
C was not chosen in the end because the scan speed is too slow, although a rela-
tively high relative density can also be achieved. The manufacturing time is also a
key issue to be stressed to make SLM more cost effective. Also, as the laser para-
meters are properly tailored, an optimized energy input can ensure sufficient melt
spreading and at the same time prevent easy balling [28] and thus decrease the
overall porosity of the SLMed materials as well.
Table 7.1 Optimized laser processing parameters from Groups A to G corresponding to the maximum relative density and the standard
deviation [9]

Laser parameter group A B C D E F G


Hatch distance h (μm) 100 100 190 100 190 100 190
Layer thickness t (μm) 30 30 30 60 60 90 90
Substrate temperature ( C) 35 200 35 35 35 35 35
Relative density (%) 99.79 99.96 99.45 98.58 98.85 96.74 98.23
Standard deviation (%) 0.43 0.47 0.41 0.03 0.12 1.10 0.17
Laser power P (W) 300 370 225 370 370 370 370
Scan speed v (mm/s) 2000 2000 500 2000 1000 1000 1000
150 Additive Manufacturing for the Aerospace Industry

Table 7.2 Optimized HTPs applied on tensile samples

No. HTPs
1 Directly aged at 165 C for 2 h
2 Solution heat treated at 535 C for 1 h and aged at 165 C for 6 h
3 Stress relieved at 300 C for 2 h
4 Stress relieved at 300 C for 2 h and aged at 165 C for 2 h
5 Stress relieved at 300 C for 2 h, solution heat treated at 535 C for 1 h and aged
at 165 C for 6 h

HTPs, Heat treatment parameters.

7.2 Post selective laser melting heat treatment


For Al alloy A357, it has been reported that the rapid microstructure coarsening
occurs during SHT around the eutectic point of 540 C, and the rate of spheroidiza-
tion and coarsening increases with the solution treatment temperature [29,30]. In
this study, in order to prevent serious pore expansion in SLMed materials [31,32],
the standard T6 heat treatment temperature was slightly adjusted to 535 C, which
should also be sufficient for effective SHT [3133]. Microstructure coarsening
occurs more rapidly in modified aluminum alloys due to a much finer microstruc-
ture [34,35]. As a result, for manufacturing processes with high solidification rates
such as SLM, SHT time of 12 hours was found to be sufficient [36,37].
In order to cover the entire range of the heat treatment process, the postproces-
sing procedures have included complete precipitation hardening cycles over the
duration of ageing times at 165 C, as commonly used for conventional cast alloys
[36,3841]. In general, quite effective precipitation hardening can be achieved
[42,43]. On the other hand, since SLM is characterized by an extremely rapid melt-
ing and solidification process, a large amount of residual stresses are very likely to
be induced [44,45]. Therefore, apart from direct ageing, a high-temperature stress-
relief (SR) cycle at 300 C was also applied [4547]. In this regard, five sets of
HTPs were composed, as shown in Table 7.2 and applied on aluminum alloy A357
tensile samples to investigate the influence of those parameters on the correspond-
ing mechanical properties.

7.2.1 Tensile properties


By applying the postprocessing parameters above, the tensile properties of both hor-
izontal and vertical test samples can be obtained (Fig. 7.4). Based on the tensile
data, the directly aged sample at 165 C (HTP1) has the highest tensile strengths
and the lowest corresponding tensile strains in both directions. For the solution
heat-treated plus peak-aged sample (HTP2), however, it is less tough and more duc-
tile [48]. For these two types of samples, in particular, the uniform elongation is
quite close to the fracture strain (Fig. 7.4). On the contrary, for the stress-relieved
sample (HTP3), although it possesses the largest tensile strain, its strength is almost
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 151

Figure 7.4 The tensile data with standard deviation for SLMed samples heat treated at
different conditions in two directions, with the typical property standard of T6-cast alloy
A357 from the literature exhibited by the dashed lines [37,41], where UE standards for the
uniform elongation, YS the yield strength, and UTS the ultimate tensile strength. SLM,
Selective laser melting.
Source: Data from IMMA Handbook of Engineering Materials, Vol.1 Metals and Alloys,
Edition (1988) of AIM Metal Handbook, Published by Institute of Metals and Materials
Australasia Ltd and ASM Metals Handbook, 1985.

the lowest due to effective stress relaxation (Fig. 7.4) [32]. Furthermore, it should
be noted that the additional ageing process in the HTP4 sample only deteriorates
the corresponding tensile properties compared to the HTP3 sample. Finally, the ten-
sile properties for the HTP5 sample almost resemble those for the HTP2 sample
(Fig. 7.4), indicating that the strengthening kinetics in these two scenarios could be
quite similar. Considering tensile behaviors compared to the cast alloy standard,
both HTP2 and HTP5 can lead to optimized tensile properties.

7.2.2 Fractography
In general, defects tend to expose as large holes and unmelted powder, especially
after age hardening (Figs. 7.5 and 7.6). Also, although there exist more pores and
cavities in the horizontal direction (Fig. 7.5), the amount of unmelted powder is
larger in the fracture surfaces of the vertical direction samples (Fig. 7.6). In this
regard, those defects would be weak points for stresses to concentrate during tensile
152 Additive Manufacturing for the Aerospace Industry

Figure 7.5 SEM micrographs showing fracture surfaces of the horizontal direction tensile
samples heat treated by (A) HTP1, (B) HTP2, (C) HTP3, (D) HTP4, (E) HTP5. SEM,
Scanning electron microscopy.

Figure 7.6 SEM micrographs showing fracture surfaces of the vertical direction tensile
samples heat treated by (A) HTP1, (B) HTP2, (C) HTP3, (D) HTP4, (E) HTP5. SEM,
Scanning electron microscopy.

testing [11,24,25]. Furthermore, the fracture surfaces of the stress-relieved sample


seem more ductile than others with more dimples present (Figs. 7.5C and 7.6C),
and those of the directly aged sample are more brittle with large fracture facets
(Figs. 7.5A and 7.6A), since the Al matrix is largely strengthened by fine precipi-
tates such as βv [42,49,50]. These all agree well with the tensile data (Fig. 7.4).
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 153

7.3 Refinement of laser melting and postprocessing


parameters
7.3.1 The selection of optimized heat treatment parameters
With quite similar mechanical properties obtained, it is expected that the solution
treatment at 535 C for 1 hour should achieve similar SR effect compared to the
heat treatment at 300 C for 2 hours (Fig. 7.4). Consequently, the SR cycle might
not be necessary for solution heat treated samples, so that a large amount of time
and energy can be saved in the post heat treatment procedures. Therefore, SHT at
535 C for 1 hour plus peak-ageing (HTP2) at 165 C for 2 hours were selected as
the optimal heat treatment parameters, with the mechanical properties of the hori-
zontal test samples meeting or exceeding the cast alloy standard (Fig. 7.4) [37,41].
In addition, compared to HTP3 with the application of SR process only, the addi-
tional ageing process in HTP4 only deteriorates the corresponding tensile properties
of SLMed Al samples (Fig. 7.4). This is because after the SR process at 300 C, the
microstructure already becomes coarser compared to the as-SLMed sample
[5153]. The additional ageing treatment in HTP4 would only make the micro-
structure even coarser due to overageing, and therefore the strength and ductility
are further reduced (Fig. 7.4) [31,54].
Since both pores and nonmelted spots can be the crack initiation sites, break-
through cracks can start forming either from the surfaces in the horizontal direction
(Fig. 7.5) or from the subsurfaces along the melt pools in the vertical direction [16]
(Fig. 7.6). This indicates a similar detrimental effect of all defects on the tensile
properties regardless of their types and locations. Therefore, since there is no spe-
cific directional preference for crack propagation, it is the morphology of the forced
fracture areas determining the tensile strength of SLMed samples [16]. For instance,
apart from the defects in each direction, the horizontal direction fracture surfaces
(Fig. 7.5) show more dimples in the areas of forced fracture in comparison to the
vertical ones (Fig. 7.6) with more cleavage planes, suggesting a more ductile frac-
ture behavior for the horizontal test sample. Additionally, based on the fractography
of the tensile samples with further optimized relative densities to be discussed
below (Figs. 7.9 and 7.10), it can be confirmed the breakthrough cracks are still
irrelevant to the defect categories but related to the nature of the forced fracture
areas [16], and the defects are more likely to be exposed after certain heat treatment
due to the strengthened Al matrix [42,49,50].

7.3.2 The selection of optimized laser parameters


For the purpose of investigating the influence of further optimized relative density
on the resultant mechanical properties, some detailed tests were conducted. Based
on the relative density results obtained from Group A, its original optimized regime
was further narrowed to the benchmark within which the relative density is higher
than 98%, defined as Group A2 (Fig. 7.7A). The 2D projection benchmark is
154 Additive Manufacturing for the Aerospace Industry

Figure 7.7 (A) 3D plot and (B) 2D processing window showing the relationship among
relative density, laser speed, and laser power of the as-SLMed samples manufactured by
Group A2 parameters. SLM, Selective laser melting.

Table 7.3 LMPs applied on tensile samples

No. LMPs
1 100 μm hatching distance, 2000 mm/s laser speed, 300 W laser power
2 80 μm hatching distance, 2000 mm/s laser speed, 300 W laser power
3 100 μm hatching distance, 1400 mm/s laser speed, 300 W laser power
4 150 μm hatching distance, 500 mm/s laser speed, 200 W laser power

LMPs, Laser melting parameters.

highlighted by the dashed areas in Fig. 7.7B, with the optimized laser melting para-
meters (LMPs) from precious work defined as LMP1 [9].
In addition, in order to make the laser melting process more complete, the hatch
distance was reduced from 100 to 80 μm, defined as LMP2. In doing so, there is
10% more overlapping areas between two adjacent lasers generated compared to
LMP1 [9]. Also, the scan speed was decreased from 2000 to 1400 mm/s as LMP3
selected from Fig. 7.7 for a better powder melting scenario. For comparison,
another combination of laser parameters was selected from the literature, which
results in a very high tensile ductility of more than 25% of the SLMed sample after
modified heat treatment [32,55], defined as LMP4. Apart from the hatch distance
and scan speed, the rest of the parameters were all kept the same as LMP1, with
30 μm layer thickness, 0.1 mm beam diameter, and substrate temperature of 35 C.
These four sets of LMPs are shown in Table 7.3.
The relative density results retrieved from the Archimedes’ principle are com-
pared in Table 7.4 within the experimental uncertainty, with the corresponding
energy density determined as well. The SLMed sample manufactured by LMP1
with a high scan speed and hatch distance still exhibits the highest relative density.
Also, the energy density generated in each sample gradually increases from LMP1
to LMP4, and it is independent on the slight difference in the relative density, simi-
lar to what has been discussed before [9].
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 155

Table 7.4 Relative density and energy density results for SLMed Al A357 tensile samples
built by four sets of LMPs

LMP 1 2 3 4
Relative density (%) 99.79 6 0.01 98.57 6 0.01 99.64 6 0.01 98.93 6 0.01
Energy density (J/mm3) 50.0 62.5 71.4 133.3

SLM, Selective laser melting; LMP, laser melting parameters.

Figure 7.8 The tensile data showing the distinct difference between the horizontal and
vertical samples at the (A) and (C) as-built condition; (B) and (D) heat treated (HTP2)
condition.

7.3.3 Tensile properties


Four sets of parameters above were applied on both horizontal and vertical test
samples to determine the corresponding tensile properties. For comparison, the
SLMed sample manufactured by four sets of LMP also went through postprocessing
of HTP2. It is obvious that the tensile properties for all samples do not heavily
depend on the sample density, but rather the energy density (Fig. 7.8) as the relative
densities are within the optimized benchmark ( . 98%).
156 Additive Manufacturing for the Aerospace Industry

7.3.4 Fractography
Similarly, the defects are more obvious in the heat treated samples (Fig. 7.10) than
in the as-built ones (Fig. 7.9). Corresponding to the largest tensile properties before
and after heat treatment in both directions, the sample built by LMP1 exhibits the
most ductile fracture surfaces with the least amount of defects present [9], com-
pared to others built by LMP2, LMP3, or LMP4 (Figs. 7.9 and 7.10).

Figure 7.9 SEM micrographs showing fracture surfaces of the horizontal and vertical as-SLMed
tensile samples processed by (A) and (D) LMP2; (B) and (E) LMP3; (C) and (F) LMP4. SEM,
Scanning electron microscopy; SLM, Selective laser melting; LMP, Laser melting parameter.

Figure 7.10 SEM micrographs showing the corresponding fracture surfaces of the horizontal and
vertical tensile samples above heat treated by HTP2 afterward. SEM, Scanning electron microscopy.
The processing and heat treatment of selective laser melted Al-7Si-0.6Mg alloy 157

7.4 Conclusions
The SLM-processing and heat treatment parameters were successfully applied on
aluminum alloy A357. Based on the relative density analysis in this chapter, point a
in Group A (30 μm layer thickness, 100 μm hatching distance, 2000 mm/s laser
speed, 300 W laser power with beam diameter of 0.1 mm, and substrate temperature
of 35 C) were chosen from seven groups of samples as the optimized set of laser
parameters (Table 7.1). They were used as the target parameters for sample building
in this work. By using these parameters, SLM can be implemented to manufacture
3D aluminum alloy A357 parts with very low porosity. In addition, via the adjust-
ment of various modified parameters, SHT at 535 C for 1 hour plus peak-aging at
165 C for 6 hours have been selected as the optimized parameters for our SLMed
alloy, consuming much less energy and time. In this regard, relatively good
mechanical properties are achieved for SLMed materials, with their tensile beha-
viors of the horizontal test sample meeting or exceeding the typical property range
of T6-cast Al alloy A357 sample.
The purpose of reducing the hatch distance or scan speed for LMP2, LMP3, and
LMP4 is to make the laser melting process more complete. For instance, a high
laser speed in LMP2 is applied to compensate and balance the excessive energy
density coming from the reduced hatch distance. However, since the hatch distance
is too low in this situation, there is an excessive heat input, leading to powder sput-
tering and thus lower relative density. Although there is a much larger hatch dis-
tance in LMP4, since the scan speed is too small, similar balling effects would
occur due to the excessive energy input. Therefore, a change in one of the laser
parameters does not necessarily result in the specific increase/decrease in the rela-
tive density; it is the combination effect of the parameters that matters. In addition,
due to a poorer powder melting scenario for LMP2 and LMP4, a certain amount of
defects, such as the unmelted powder and large facets, can be observed in the corre-
sponding fractured samples (Figs. 7.9A, C, D, F and 7.10A, C, D, F). Therefore,
both as-SLMed and heat treated samples manufactured by LMP1 possess the best
mechanical properties in both directions (Fig. 7.4), although their corresponding rel-
ative density is not the highest. This means that powder melting scenarios, related
to the thermal history and the energy density, are more important.
For the SLMed materials manufactured by a series of optimized LMPs with quite
low porosity (,2%) (Table 7.4), the tensile behaviors are improved with the
decrease in the energy density from LMP1 to LMP4 regardless of heat treatment
(Fig. 7.8C, D). Therefore, based on the refinement of LMPs, LMP1 determined pre-
viously has been further confirmed as the most optimized parameters to build as-
SLMed parts with improved mechanical performance. As a result, there is a strong
correlation between mechanical properties and the energy density instead of the
optimized porosity. During tensile deformation, the SLMed Al matrix initially is
the dominant part bearing the load. After reaching the ultimate tensile strength
(UTS), however, defects such as small pores and unmelted powder would be the
weak points to cause a quicker failure during further extension. This is especially
158 Additive Manufacturing for the Aerospace Industry

typical for the artificially aged samples since their matrix is largely strengthened by
the fine precipitates, making the uniform elongations and fracture strains quite simi-
lar (Fig. 7.4).

Acknowledgments
This work was supported by Monash University (Australia), Science & Industry Endowment
Fund (SIEF) under the program [RP04153] “Manufacturing a small demonstrator aeroen-
gine entirely through additive manufacturing,” and Australia Research Council
[IH130100008] “Industrial Transformation Research Hub (ITRH) for Transforming
Australia’s Manufacturing Industry through High Value Additive Manufacturing,” including
financial support from Safran Power Units and Amaero Engineering. The authors are also
grateful for the access to the facilities at Monash Centre for Additive Manufacturing
(MCAM) and Monash Centre for Electron Microscopy (MCEM).

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Superalloys, powders, process
monitoring in additive 8
manufacturing
Kevin Minet1, Ankit Saharan2, Anja Loesser2 and Niko Raitanen1
1
EOS Finland Oy, 2EOS North America Inc

The term “superalloys” refers to a group of alloys based on nickel, cobalt, or iron-
nickel. Originally developed during WWII and in the early 1950s for military gas
turbines, they have since been continuously advanced and a large number of new
materials have been introduced. These materials are used for a wide range of applica-
tions, including aerospace, power generation, and multiple niche markets, such as
high-end automotive components (supercars, Formula 1, etc.). One of their most inter-
esting characteristics is their ability to maintain high mechanical strength at elevated
temperatures (typically up to 80% of their absolute melting temperature). Additionally,
they exhibit excellent hot corrosion and oxidation resistance, which makes them
suitable for applications with high service temperature requirements (up to 1000 C).
Superalloys are known to have rather complex chemical compositions and are
usually classified according to their base element and strengthening mechanisms, as
seen in Fig. 8.1.
The common feature in these alloys is their face-centered cubic (FCC) crystal struc-
ture, also called the gamma (ɣ) phase. Iron and Cobalt base alloys typically have a body-
centered cubic (BCC) structure at room temperature, but can also retain the austenitic
FCC structure by additions of nickel. All the nickel superalloys have an austenitic FCC
γ matrix phase at room temperature and variable amount of secondary phases including
FCC gamma prime γ 0 , and body-centered tetragonal (bct) gamma double prime γv.
For the most demanding applications, for example hot gas path components in
land-based and aeronautical gas turbines, nickel-base superalloys are omnipresent
as they outperform other superalloys classes. Their high mechanical performance is
based on two strengthening mechanisms:
- Solid-solution strengthening of the FCC gamma matrix.
- Precipitation-hardening by intermetallic γ 0 Ni3(Al, Ti) and/or γv Ni3(Nb) phases.

The ordered L12 Ni3(Al, Ti) structure of γ 0 .


Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00009-1
© 2019 Elsevier Inc. All rights reserved.
164 Additive Manufacturing for the Aerospace Industry

Figure 8.1 Classification of super alloys.

While alloys that are solely solid solution strengthened do not require heat treat-
ment to achieve their optimal strength, precipitation hardening alloys require spe-
cific heat treatments to reach their full performance.
Additionally, further strengthening can be provided by grain boundary strength-
ening mechanisms, through the use of Boron, Zirconium, and Carbon. These ele-
ments have extremely limited solubility in the γ and γ 0 phases, and tend to
segregate towards grain boundaries, becoming locally enriched in the intergranular
areas; borides, carbides, and, to some extent oxides that are formed at the grain
boundaries pin the interfaces and prevent grain boundary sliding. This strengthening
mechanism is of highest importance when creep resistance and mechanical strength
at high temperature are required.

8.1 Applications: materials in gas turbines


Superalloys have been developed to exhibit high mechanical strength, and stability
at high temperatures, above the temperature limits of steels. Nowadays, they find
their main applications in aeronautical and industrial/land-based and gas turbines.
For these two applications, the material requirements may change in turbine design
but the base requirements remain the same; typically high-temperature corrosion
resistance, dimensional stability, and high mechanical strength (especially tensile,
creep, and fatigue strengths).
One particularity of aero engines is the need for lightweight components, so
lower density materials are used whenever possible. A material of choice is tita-
nium, which is used for structural components as well as some engine parts.
Nevertheless, nickel alloys replace titanium in most applications where the service
temperature exceeds 600 C. The stress-rupture strength of different alloys is shown
in Fig. 8.2, and highlights the superior performance of nickel-base superalloys at
high temperature.
Superalloys, powders, process monitoring in additive manufacturing 165

Figure 8.2 Stress-rupture strength of different alloys at different temperatures.

Another particularity of aero engines is the rapid change in temperature condi-


tions caused by the different operating conditions encountered between take-off and
landing, which places heavy thermomechanical stress and dynamic loads on the
components. The criteria for land-based gas turbines are different, as the main focus
is on efficiency in continuous operation mode. There are fewer weight limitations,
therefore denser materials can be used.
An interesting example to highlight the extreme operational conditions in gas
turbines is the case of turbine blades: at the base of the blade, where it is clamped/
attached, high-temperature resistance, high stress-rupture ductility, high tensile
shear strength, and good low cycle fatigue are needed. In the upper area of the
blade, high creep and thermomechanical fatigue resistance are required due to the
steep thermal gradients. As the limiting factor of the service life of blades is usually
the long-time creep resistance, it is always considered one of the most critical fac-
tors to ensure component reliability. The materials developed for such applications
are, for example, polycrystalline IN713, MAR-M247, and their variants. Other
alloys, such as IN738 and IN939 exhibit better high-temperature corrosion resis-
tance. The tensile strength of some of these alloys can reach nearly 1400 MPa with
yield strengths above 1000 MPa.
Fig. 8.3 shows an overview of a gas turbine and a few examples of alloys used
in jet engine parts, where the hot sections are invariably manufactured with nickel
superalloys. Typical components include turbine blades, guide vanes, combustion
chamber, and fuel nozzles.
In the combustion chamber, which is the hottest part of the engine, hot gases
can reach a temperature as high as 2000 C. As the expanding gases escape
towards the exhaust, it is rather common in modern engines for the high pressure
166 Additive Manufacturing for the Aerospace Industry

Figure 8.3 Jet engine components and materials.

turbine components to see temperatures as high as 1600 C. Obviously, none of


the above mentioned materials are capable to withstand such temperatures, and
cooling and coating of the metallic components is necessary to ensure their per-
formance. Cooling technologies include steam or air streams, which are com-
bined with thermal barrier coatings. Fig. 8.4 shows the evolution of blade cooling
technologies since the 1960’s.
As seen above, the material choice is a critical factor to ensure part perfor-
mance. This has been the driving factor for development of new superalloys in
the last 60 years. Traditionally, nickel-base superalloys were developed to be
cast, and most of the critical turbine components are still manufactured this way.
Nevertheless, the recent emergence of new manufacturing techniques, in particu-
lar additive manufacturing, has been one of the biggest breakthroughs in modern
manufacturing and is now the main driver for the technology push when it
comes to component performance and efficiency improvements. There is a clear,
increasing demand from the industry for producing high-end components out of
nickel-base superalloys by additive manufacturing.
The key drivers of additive manufacturing include an outstanding freedom
of design, allowing the production of complex shape components without the
limitations of traditional manufacturing. Thus, component optimization, for
example the creation of complex internal structures and cooling channels that
allow even higher service temperatures (as seen in Fig. 8.4—evolution of blade
cooling technology), has triggered a high interest of turbine manufacturers for
additive manufacturing. Additionally, additive manufacturing offers extended
Superalloys, powders, process monitoring in additive manufacturing 167

Figure 8.4 Evolution of cooling technology in Turbine Blades  The Jet Engine  Rolls
Royce plc.

flexibility for weld repair and for the production of smaller batches without
the need to support high costs and lead times of cast manufacturing. Finally, for
very specific and complex applications, AM technology allows drastic reduction
in the need for component assembly, leading to further lead time and costs
reductions.
A hurdle in the adoption of additive manufacturing is that many nickel-base
superalloys are known to be difficult to process with additive manufacturing
technologies and numerous reports of severe cracking problems can be found in
literature. Usually attributed to y0 -strengthened alloys, this problem can also
exists for some yv-strengthened alloys, which are generally considered weldable.
Nevertheless, recent developments in the understanding of additive manufactur-
ing process mechanisms have contributed to solve these severe issues. A better
understanding of the role of the various alloying elements is also important
for elimination of cracking. Although recent studies have pointed out the effect
of alloying elements on cracking susceptibility, the underlying mechanisms
at play in additive manufacturing are still not fully understood. This is due to
the high chemical complexity of the alloys, the inter-relationships between
alloying elements, combined with the very fast process dynamics of additive
manufacturing processes, especially laser powder bed fusion technologies
(Direct Metal Laser Sintering (DMLS), Selective Laser Melting (SLM), Laser
Cusing, etc. . .).
168 Additive Manufacturing for the Aerospace Industry

Following are a few examples of successful AM application resulting from case


studies conducted by Electro Optical Systems for some key manufacturers in the
gas turbine industry:
- Hastelloy X: Owing to its excellent high-temperature corrosion resistance, solid-solution
strengthened Hastelloy X is particularly well-suited for components exposed to high ther-
mal stress, and will see applications with service temperature as high as 1200 C. Areas of
use include aerospace, for example, combustion chambers and their sub-components. This
material has been successfully used since 2013 in additive manufacturing by the gas tur-
bine manufacturer Siemens, for rapid manufacturing and rapid repair actions with the EOS
DMLS technology. Recently, Siemens has further evolved its use of the technology and
introduced its first fully AM-built gas burner. Using the EOS M400-4 system to produce
up to 8 burners at once, this technology has enabled Siemens to significantly cut lead times
and reduce production costs [11].
- INCONEL 718: Another very obvious material choice for hot structures with complex
geometries is the ubiquitous Inconel 718, which can be used to produce AM components
without any critical defects. Indeed, this alloy relies on a yv strengthening mechanism
(typically contains 18%20% of hardening phase), and its low amount of y0 forming
elements (Ti, Al) gives it an excellent weldability and weld-repair ability compared to
other y0 -strengthened alloys.
ArianeGroup has successfully taken IN718 and additive manufacturing technolo-
gies into use to solve a technical challenge related to a class 1 (mission critical)
component for the next generation of Ariane launchers. Thanks to EOS technology,
ArianeGroup successfully implemented a simplified propulsion module. Instead of
248 elements, the new injector head counts only one part, hence reducing technical
complexity and drastically cutting costs and production time, as compared to tradi-
tional casting [12].
Production process Construction time for 1 injector head
Casting and machining finishing 3 months
EOS M 400 (1 laser for 1 component) 65 h
EOS M 400-4 (4 lasers for 1 component) 35 h

Nevertheless, IN718 sees a detrimental coarsening of its yv hardening phase at high


temperatures, which limits its service temperature to about 650 C. The push for greater
efficiency and increased performance in land-based and aerospace gas turbines is driving
the need for increased service temperatures to very challenging levels. The next break-
through in improving their performance will be through the combination of additive
manufacturing and high-performance materials; AM designs which aim at optimizing
function through geometric complexity, combined with materials capable of sustaining
even higher service temperatures are also the key to reduce the environmental impact of
power production and air-transportation. It is clear that materials engineering for AM will
play a major role in the years to come to help the industry handle some of the biggest
challenges of the 21st century—energy and the environment. Therefore, there is a clear
need to develop solutions to process y0 -strengthened alloys with AM, as their inherent
higher temperature capabilities makes them uniquely desirable.
Superalloys, powders, process monitoring in additive manufacturing 169

Such alloys include, amongst others, IN939, IN738, and MAR-M247, which have
received significant interest for production by additive manufacturing. These materi-
als contain a much higher amount of aluminum and titanium leading to a very high
fraction of hardening phase (up to 80% of y0 by volume). However, formation of this
phase is also known to significantly hinder weldability, and makes their processing
by additive manufacturing highly challenging. Their typical behavior when processed
by laser powder bed fusion, for example, is a high sensitivity to weld and postweld
cracking, which causes manufactured components to be heavily defected. Several
cracking mechanisms have been suggested in the literature to explain the nonweld-
ability of this material class, which will be detailed in the following sections.

8.2 Material and processing challenges in additive


manufacturing of superalloys and different
approaches for solutions
8.2.1 Challenges with additive manufacturing—theory on
weldability issues
EOS additive manufacturing technology is based on laser powder bed fusion princi-
ples. As it uses a laser beam to selectively melt metal powder and weld it onto an
underlying substrate (made of previously solidified layers), process phenomena can
be, to a large extent related to the conventional laser welding. Therefore, a signifi-
cant share of the theory, applications and limitations of laser welding also apply to
laser powder bed fusion technology.
The crack susceptibility of high strength nickel superalloys is a vast a complex
subject. It has been widely investigated in the welding literature and can be used as
a basis to explain processability issues in additive manufacturing. However, in order
to fully understand the underlying mechanisms causing severe defect formation in
the case of y0 -strengthened nickel superalloys, the specificities of this manufacturing
method must also be taken into account to extend the theorization on weldability
issues. Thus, the following points must be considered:
- The complex metallurgy of nickel-base superalloys and factors contributing to crack forma-
tion, as well as the effect of individual elements on the material’s metallurgy (see Fig. 8.5).
- The nature of layer-wise manufacturing which causes multiple re-heating cycles and high stres-
ses, as well as the fast process dynamics which take the material very far from equilibrium.
- The complex interaction between laser beam and metal powder, as well as key input vari-
ables for successful processing of metal powder.

In the laser welding process, cracks are typically formed during solidification,
while the alloy undergoes rapid cooling. In additive manufacturing, where a thin
layer of powder (typ. 2080 μm) is selectively melted by a laser, solidification hap-
pens even faster, at rates up to 10^6 C/s. Cracking phenomena in welding encom-
pass four different mechanisms that this section will attempt to summarize.
170 Additive Manufacturing for the Aerospace Industry

Figure 8.5 Effect of various alloying elements on the metallurgy of y0 strengthened nickel
superalloys.

As discussed in the previous section, solid solution strengthened alloys (e.g.,


Hastelloy X), as well as low volume fraction precipitation hardened alloys (e.g.,
IN718) are generally considered weldable. Conversely, alloys containing high
amounts of titanium and aluminum (y0 forming elements), have been traditionally
referred to as “hard-to-weld” or “nonweldable” alloys. The weldability limit of
these materials has been empirically defined based on the combined content of tita-
nium and aluminum, as shown in Fig. 8.6.

8.2.2 Solidification cracking


Solidification cracking, also known as weld-centerline cracking, is a typical hot
cracking phenomenon which occurs in the fusion zone during the last stages of
solidification. As the melt pool solidifies from the edges towards its center, the
remaining liquid film is pulled apart by the tensile thermal strain occurring during
shrinkage, hence forming a crack in the middle of the fusion zone.
Solidification cracks are dependent on the width of the solidification range, as they
form when the material is in the so-called “brittle temperature range” (BTR), which is
the range between liquids and solidus [13]. Some alloying elements have been
observed to have an adverse effect on solidification cracking. Zirconium, Boron, and
Carbon, for example, are known for increasing susceptibility to solidification cracking,
as they segregate to liquid and form low melting point liquid films. Boron is also
Superalloys, powders, process monitoring in additive manufacturing 171

6 IN713C
B1900
CMSX-4
R108 IN100
Aluminum content, %

5 Mar-M-200

AF 2-1DA

Astrology
4 Udimet700
Udimet 600
IN738LC

3 GMR235
Inconel 700 Udimet 500

IN939
2 Unitemp 1753
Difficult to weld; weld and
Weldable Rene41
strain age cracking
Waspaloy
1 Rene62
Inconel X-750
Rene220C M252
C263 Inconel X
Inconel 718(x)
Inconel 909
0
1 2 3 4 5 6 7
Titanium content, %

Figure 8.6 Weldability diagram based on Ti and Al content.

known to change the solid/liquid surface energy by wetting the interdendritic regions
and grain boundaries, which increases cracking susceptibility. Other elements, such as
Phosphorus and Sulfur have the same effect, and must be kept to the lowest possible
level as they do not have any functional role in the alloy’s composition. Finally, nio-
bium is also known to segregate and form phases which can cause solidification crack-
ing (e.g., laves/y eutectics).

8.2.3 Liquation cracking (HAZ)


Liquation cracking, or heat affected zone (HAZ) fissuring, is another type of hot
crack formed when the low melting point phases (e.g., eutectic type constituents)
formed during solidification and segregated at the grain boundaries are re-melting
by subsequent scans of the laser. This results in a situation where the alloy is
locally molten below its true liquid us temperature. The inherent nature of additive
manufacturing can cause strong susceptibility to liquation cracking, as previously
solidified layers are typically re-melting during the melting fusion of the next few
layers of powder.
172 Additive Manufacturing for the Aerospace Industry

Literature suggests that HAZ liquation cracking might not be as detrimental


for yv alloys as for y0 strengthened alloys, because the kinetics of post-weld precipi-
tation in the heat affected zone are slower in the case of yv alloys, giving more time
for stresses to be relaxed [8].
Generally, materials processed in a way that produces a fine grain structure
(such as wrought or additively manufactured) are not overly sensitive to HAZ liqua-
tion cracking, as there is less time for low-melting-point phase forming elements to
segregate at grain boundaries.

8.2.4 Strain-age cracking


Strain-age cracking (SAC) is a phenomenon which is very specific to precipitation-
hardening nickel superalloys. Unlike the two above-mentioned cracking phenom-
ena, SAC is often referred to as a “cold-cracking” or “solid-state cracking” phe-
nomenon, as it doesn’t involve liquid phases but takes place during re-heating
cycles. The mechanisms behind SAC are rather complex and have been widely the-
orized, but no consensus yet exists. It involves not only y0 precipitation, but also
highly strained carbides, causing reduced ductility in the HAZ. Nevertheless, the
scientific community seems to agree that SAC comes from excessive stresses
formed during y0 precipitation and due to the y/y0 lattice mismatch, which cannot be
accommodated by grain boundaries. Fig. 8.7 shows a typical grain boundary crack
on a y0 strengthened alloy built by laser power bed fusion.
There are some attempts to monitor this phenomenon in the literature, for exam-
ple on René 41 alloy ([5] Sjöberg), with the definition of time-temperature crack
diagrams. Based on this study, a way to mitigate the problem is to minimize time
spent in the temperature range where rate of y0 precipitation is the highest. This is a
challenge in the case of AM due to the nature of layer-wise manufacturing, which
causes successive remelting and reheating cycles in the previously solidified layers,
as seen in Fig. 8.8.

Figure 8.7 Grain boundary crack on an additively manufactured IN939 component.


Superalloys, powders, process monitoring in additive manufacturing 173

Thermal cycle
TL : Liquidus temperature
TE : Eutectic reaction temperature
TS : Solidus temperature
Vulnerable stages for solidification cracking Tγ : γ precipitation temperature
TL
Vulnerable stages for liquation cracking
Temperature (ºC)

TS

TE Vulnerable stage for


ductility dip cracking

cycle 1 cycle 2 cycle 3 cycle 4 cycle 5

Time

Figure 8.8 Example of thermal cycling undergone by a given layer in DMLS.

Several studies suggest that SAC susceptibility is the reason why large volume
fraction y0 -strengthened nickel-base superalloys are nonweldable. The literature also
reports that the fast kinetics of y0 precipitation make y0 -strengthened alloys more
sensitive to SAC than yv strengthened alloys. In fact, IN718, with its slow yv precip-
itation kinetics, was developed specifically to solve the SAC issues in y0 alloys.

8.2.5 Ductility dip cracking


Ductility dip cracking (DDC) is another type of solid-state cracking that produces
intergranular cracking in the HAZ, even with alloys which are insensitive to solidi-
fication and liquation cracking (i.e., with low B, C, Zr, S, P content). Even though
austenitic materials can show tendency to DDC, this problem is not widely reported
in the case of nickel-base superalloys. However, as it appears in the heat affected
zone, it cannot be discounted as a potential cracking mechanisms when the alloy is
processed by additive manufacturing.
Generally, materials’ ductility is a function of temperature, where the highest
ductility is achieved close to the melting point. However, some materials can
exhibit a loss of ductility in the 0.5 Ts 20.9 Ts (solidus temperature) range,
called ductility dip that can lead to crack formation, as shown in Fig. 8.9. Since
DDC occurs due to sliding of grain boundaries from creep-like behaviour at high
temperature, all methods that can lock grain boundaries improve the resistance
to DDC.
174 Additive Manufacturing for the Aerospace Industry

Ductility-dip Segregation
cracking cracking

Ductility DTR BTR

Emin
0.5 Ts Ts TL

Temperature +

Normal Ductility-dip

Figure 8.9 DDC and BTR cracking areas. DDC, Ductility dip cracking; BTR, Brittle
temperature range.

8.3 Powder material properties


Like all other conventional manufacturing processes, additive manufacturing is no
different. There are various forms of feedstock used in these processes depending
on the type of technology, like wires/powder for direct energy deposition systems,
powder for laser/electron powder bed fusion systems, etc. Powder is inadvertently
the most common feedstock in metal additive technologies.
Hence, understanding powder material characteristics becomes essential. Let’s
take look at the most common powder characteristics especially true for laser pow-
der bed manufacturing. Please note that the criticality factor depends a lot on the
alloy used, powder delivery system, and other machine attributes like gas flow man-
agement inside the machine and optical and laser system of the machine.
1 Sampling: Sampling is key to getting repeatable and reliable measurements. Majority of
the sampling techniques and instruments were initially designed and geared toward indus-
tries, like pharmaceuticals and food. Ideally, one must take a sample of powder when it’s
flowing to get a representative sample from a batch. However, this may not be possible
when materials are getting atomized in through gas, plasma, water, etc., in long columns;
this is certainly not trivial when a batch of powder is received in containers from suppliers.
To alleviate this concern, powders may be sampled through existing standards like ASTM
B214, MPIF 1. These standards have alternative methods to obtain homogeneous and rep-
resentative samples with use of different devices like powder thieves, rifflers, and splitters.
2 Chemical composition: Chemical composition is one of the most important characteristics
of metal powders. Most material specifications clearly define the acceptable ranges for
alloying elements, including critical trace elements and also gas content (O/N/H).
Depending on the alloy, trace elements are crucial to the performance and processing of
these alloys. For example, traces of tungsten in Ti6Al4V is detrimental to mechanical and
fatigue properties of the alloy due to a very high gradient in liquidus temperature of the
base alloy and tungsten leading to un-melted tungsten particles that act as hard inclusions
Superalloys, powders, process monitoring in additive manufacturing 175

after the powder is processed to form an AM part. Also, different concentrations of gases
inside the powder can also affect critical properties of not only the powder but also of pro-
cessed AM parts. For example, higher oxygen ppm is Nitinol can affect its Af (austenite
finish) temperature. It is very important to understand and track the chemistry of the pow-
der feedstock and finished AM part. Tracking Mg loss is AlSi10Mg or O/N pickup in
Ti6Al4V can quickly determine if the feedstock is within specifications.
3 Particle size distribution (PSD): When an alloy is atomized in the atomizer, the resultant
powder has a wide PSD from fines (submicrons), to coarse (150200 1 μm). Laser pow-
der bed fusion commonly uses PSD in the range of 1563 μm, depending on the type of
alloy, processing parameters, and/or layer thickness. There are a number of ways to mea-
sure powder size distribution. The three main ways are sieving analysis, laser diffraction,
and dynamic image analysis. Both methods have their pros and cons, they also have
defined standards for each (ISO, DIN XXXX). Sieving analysis are a bit different from the
other two as they mainly classify powder sizes in specific class sizes that are often a range
rather than individual particle measurements, like the other two. However, the key is to
remain consistent with measurements across the process chain and ensure qualified instru-
ments to measure this characteristic. PSD impacts the AM process in a major way. A well-
balanced PSD with a normal distribution ensures better packing density that, in turn attri-
butes to better part quality. Having correct PSD for a defined process is also essential as
having too many fines increases the sintering kinetics because of increased surface area of
the fines, which is exposed to the laser energy. The chief characteristics for PSD measure-
ments typically are D10, D50, and D90, which are defined as follows,
a. D10: Particles with number distribution defined as passing 10% below this value.
b. D50: Particles with number distribution defined as passing 50% below this value. Since
this is the midpoint, this also indicates the number distributions where half is below
and above this specified value. Key thing to note here is the D50 is also the median
value and not the mean, as defined by certain ISO standards.
c. D90: Particles with number distribution defined as passing 90% below this value.
Please note that these values are can be number or volume distributions depending on
the technique used to measure the particles. For example, laser diffraction commonly uses
volume distributions to describe the D values, and dynamic image analysis uses number
distributions to describe the D values. Many software have the capability to convert
between the two distributions but one must always refer to the applicable ISO/ASTM stan-
dard to determine the appropriate technique.
4 Powder flowability: The main techniques to measure powder flowability are Hall flow
(ASTM B213-13), Carney flow (ASTM B964). Though flowability is a measured value,
it has not yet been correlated for all materials to part quality of powder bed fusion
machines which is directly affected by spreadability. Though similar terms spreadability
is quite different from flowability. Where, flowability on one side is affected solely by
powder characteristics such as morphology, PSD etc., spreadability on the other hand
depends not only the powder characteristics that affect flowability, but also other factors
like recoater geometry type (blade, roller, etc.), stiffness of recoater, speed of the recoa-
ter, friction of the underlying layer (or base plate in case of initial layer), layer thickness
to name a few. There are other tests like angle of repose etc. to test the flowability of the
powder but like Hall/Carney flow, they are also indirectly related to spreadability.
Efforts are ongoing in the industry today to quantify spreadability but so all the efforts
are still in progress with little real quantification in the literature at present.
5 Apparent/Tap density: There are a number of standards defined by the industry to measure
apparent (bulk) and tap density for metal powders. Apparent density is calculated by the
176 Additive Manufacturing for the Aerospace Industry

mass of the powder that can be contained in a specified volume without any external inter-
vention. Tap density is the density of the powder inside a specified volume after the pow-
der is tapped (self-settling). Both of these parameters along with the PSD drive the
packing density of the powder which not only determines part quality but can also lead to
build crashes. Improper packing density may lead to short feeding in powder bed fusion
machines.
6 Morphology: In general, spherical particles are optimum for laser powder bed fusion pro-
cess. The morphology not only affects the packing density of the powders but also the
energy absorption of the laser as well. Spherical morphology allows for more surface area
to be exposed which may increase the energy absorption of the laser which may result in a
more consistent meltpool. Nonspherical particles may result in energy trapped in the top
portion of the layer which may result in shallow penetration of the melt pool result in con-
duction type of weld between the powder layers. Nonspherical particles may also result in
poor spreading behavior leading to nonoptimal part quality. Fig. 8.10 shows morphology
of AM powder which is predominantly spherical.
With the use of Additive manufacturing technology in in production applications
for highly regulated industries like aerospace, medical; it becomes extremely impor-
tant to understand the behavior of these powders and how their intrinsic properties
change over time most commonly referred to as “aging of powders.” It is important
to understand that aging of powders not only depends on the type of alloy as some
alloys are more susceptible to chemistry change than others. Also, the aging
depends on the type of build you are doing in the AM machine.
Aging of the powders is not only linked to the powder specifications linked to a
particular application but also to the production of a particular build file.
There is a lot of concern with powder specifications especially regarding to
contaminants and possible degradation of powder chemistry. Fig. 8.11 provides a
holistic approach on how powder chemistry could be tracked and also specified.
The chemistry specification of the powder can be specified through master

Figure 8.10 SEM image of virgin Hastalloy powder.


Superalloys, powders, process monitoring in additive manufacturing 177

Figure 8.11 Powder chemistry specification.

specifications containing all the alloy chemistry including O/N/H specifications.


Through these master specifications, contaminants can easily be identified either
as trace elements or core chemistry depending on the contamination source/tech-
nique. Powder degradation in terms of O/N pickup or even moisture pickup could
be identified by referring back to the master specifications and using qualified
measuring techniques to quantify them.
ICP-OES:
XRF: X-ray fluoroscopy
IGF: Inert gas fusion
LOD: Loss on drying method
Fig. 8.12, illustrates a typical process to not only define the powder specifica-
tions according to the intended production job in the machine but also so that they
aging of powder could be taken into account as well.

8.4 Process monitoring


8.4.1 Quality assurance in AM
Manufacturers in markets with high-quality standards, particularly in serial produc-
tion, are reliant on trustworthy quality control and quality assurance systems.
Leading Additive Manufacturing system vendors such as EOS, SLM Solutions, and
Concept Laser are approaching these challenges with modular hardware and soft-
ware solutions (Dunsky, 2014). Generally, Quality control in AM can be structured
in three steps:
Preprocess: Machine acceptance tests, system maintenance, material quality control, pro-
cess parameter validation
In-process: System monitoring (laser power, oxygen content in process chamber, building plat-
form temperature, layer thickness, . . .) and in situ process monitoring of the melting process
Postprocess: Destructive testing methods (tensile testing, micrographs, . . .) and nonde-
structive (density, CT, X-ray, . . .) testing methods.
Figure 8.12 Powder specification plan for recyclability.
Superalloys, powders, process monitoring in additive manufacturing 179

8.4.2 Challenges with tradition postprocess inspection


techniques
Traditional destructive and nondestructive testing methods are expensive and lim-
ited in samples size, shape, and density of the material. Due to interbuild quality
variations it is not possible to test samples of one build in a destructive or nonde-
structive manner and make conclusions about the quality of the next build, even if
it is identical. Process parameters like shielding gas flow and laser power can vary
during the building process and affect the melting process. Variations of these
essential process parameters can induce that is lack of fusion based porosity even if
occurring in just a few layers of the build. Depending on the size of a part it can be
challenging to find this kind of processes failure with traditional inspection techni-
ques. Thus, the need for layer-wise, real-time process monitoring increased over the
past years.

8.4.3 Novel QA approaches


Due to the challenges with traditional inspection methods the need for in situ process
monitoring for additive manufacturing (AM) has arisen in the past years. Various
more or less critical process variations can occur during the layer-wise melting pro-
cess and can affect the properties of the solidified material. Process signatures like
melt pool geometry and emission from the melt pool and associated plasma plume
can be measured in real-time to assure stable process conditions ([9]).

8.5 Sensor types for in situ process monitoring


Certain process parameters can be monitored by vision-based, thermal or acoustical
sensors. Different sensors might reveal different process phenomena, which leads to
the implementation and combination of various sensor types to gain as much infor-
mation about the building process as possible. However, acquiring sensor data is
only the first step to process monitoring; the correlation between monitored data
and part quality is challenging due to that is self-healing phenomena occurring dur-
ing remelting of 34 previously exposed layers.

8.5.1 Optical in situ process monitoring systems for AM


Spatially integrated sensors like photodiodes and pyrometers, and spatially resolved
sensors like cameras can be used to monitor the melt pool and the HAZ surrounding it.
Optical monitoring systems can be further classified in terms of sensor integra-
tion. So-called onAxis sensors are mounted in the optical path of the laser beam to
monitor the melt pool with high resolution. OffAxis sensors on the other hand typi-
cally observe the melting process from the top of process chamber and monitor the
whole building area.
180 Additive Manufacturing for the Aerospace Industry

8.5.1.1 Photodiode-based process monitoring


EOSTATE MeltPool is a photodiode-based process monitoring system available for
EOS M290 systems. Two photodiodes are used to monitor the melt pool emission
both onAxis and offAxis. The photodiode in the optical path of the laser (Fig. 8.13,
Photodiode A) is restricted to a certain wavelength band close to the laser wave-
length. This is reasoned by spectral transmission of the scanner mirrors and the
optical characteristics of the beam splitter. The offAxis photodiode (Fig. 8.13,
Photodiode B) is mounted on top of the process chamber to observe the whole
building area. The wavelengths of visible light and laser emission are filtered by
band pass filters. Due to the wavelength restrictions, the on-axis photodiode mainly
measures melt pool emission, including plasma emission, metal vapor and thermal
radiation of the melt pool and the off-axis photodiode observes mainly metal vapor
and thermal radiation of the whole building area [3]. The hardware integration of
the monitoring system is illustrated in Fig. 8.13.
The photodiodes are capable of measuring the intensity of the melting process
with a bandwidth of approximately 30 kHz, therefore the sampling frequency is set
to 60 kHz. The sample rate provides an adequate temporal resolution to observe the
high dynamics of the melt pool that moves with scan speeds of 1 m/s and higher.
The high sample rate results in a resolution of approximately 50 μm/pixel
(Fig. 8.14).
The acquired monitoring data is analyzed in real-time by applying three different
algorithms to get information about the process stability or, for example, average
intensity of the melt pool.

8.5.1.2 Camera-based process monitoring


EOSTATE Exposure OT is a camera-based process monitoring system that utilizes
a sCMOS-based camera and specially designed optics to gather high resolution and
high focal depth images in the NIR wavelength range from the entire build platform
during laser processing. The light emitted by the laser interaction zone is focused

Figure 8.13 MeltPool, optical tomography (OT), and part surface correlation of a layer built
with reduced gas flow.
Superalloys, powders, process monitoring in additive manufacturing 181

Figure 8.14 Hardware setup of the EOSTATE MeltPool Monitoring System. Photodiode A
is in the optical path of the laser beam to observe the melt pool, Photodiode B is mounted on
top of the process chamber to monitor the whole building area [4].

on the camera chip after passing a neutral density filter and being spectrally filtered
in a narrow infrared wavelength band.
With a camera resolution of 2560 3 2160 pixel, a spatial resolution on the build-
ing platform of approximately 130 μm/pixel is achieved for an EOS M290 system.
The camera captures 10 frames per second, which are permanently super posi-
tioned to a holistic image of the layer. So, in the end of each layer, all images cap-
tured are integrated into one image, which represents a process map that can also
be correlated to the emitted process light.

8.5.1.3 Nonoptical sensor technologies


Acoustical sensors placed in the substrate plate can be used to detect cracking ([9]).
However, it is of acoustic anticipated that the 3D nature and complex acoustic envi-
ronment of the AM process would make implementation monitoring highly nontriv-
ial ([10]).

8.6 Quality assurance tie-in


Market segments typical for metal AM-like aerospace and biomedical industries
require high-quality parts with no significant variations in mechanical properties
and part integrity [1]. Ensuring the part quality and repeatability is one of the main
182 Additive Manufacturing for the Aerospace Industry

issues in transforming AM into a large-scale production technology, as the level of


complexity and amount of input parameters affecting the yield make understanding
the relationships between process parameters and defect formation difficult [5,6].
To qualify AM for production of, that is, aircraft parts is both costly and a lengthy
process, and therefore technological development in process monitoring is needed
to get parts faster to the market without compromises in mechanical performance
[3]. Different process monitoring techniques are being developed, as reaching
closed-loop control for AM requires established correlations between monitoring
data and part quality.

8.7 Defect data correlation automated, future closed-


loop control possibilities
The development of process monitoring systems and closed-loop control has not
yet reached a reliable and sufficiently accurate solution for defect detection.
Regardless of the hardware setup used in real-time process monitoring of additive
manufacturing, the main challenge remains in handling and analyzing the extensive
amount of recorded data. Process monitoring is one of the obvious applications for
machine learning, as loads of monitoring data is produced to correlate with certain
quality metrics. The input values fed to the learning algorithm are the features
derived from signal or processed images, depending on the monitoring system, and
the output is the outcome to be predicted without expensive postprocess inspection.
Machine learning aims to automate the statistical inference of data [2] and therefore
reduces the work intensity of the process. The additive process is at its current state
robust in a sense that the response to certain anomalies and their probabilities of
occurrence in parts is often consistent with changes in process conditions.
As the measured signal data from EOSTATE MeltPool correlates with the
amount of material defects, such as porosity, data from both monitoring and labora-
tory analysis can be leveraged simultaneously. One approach is to train a supervised
learning algorithm to include certain signal features layer-wise as training data
input and the fraction of defects determined via material analysis as the output.
Ideally, the output would be a layer-wise fraction to consider variations between
layers. Then, the model can be used to predict the porosity of monitored layers to
evaluate the part quality on macro level with a certain level of confidence. For an
illustration of the approach and the relationship between measured part crosscut
defects and arithmetic mean of predictions for each part with rather scarce amount
of data (n 5 30), see Figs. 8.15 and 8.16.
One of the difficulties in achieving straight correlation between in-process mea-
surements and emerging defects is the healing effect, which refers to remelting dur-
ing the exposure of subsequent layers and consolidating areas where pores have
already formed. Practically, this means that observed deviations in monitoring data
may not reflect the state of the resulting material and its integrity. Even though the
signal can be correlated with overall level of porosity or inclusions in a material by
Superalloys, powders, process monitoring in additive manufacturing 183

Figure 8.15 Arithmetic means of layer-wise defect fraction predictions and measured
crosscut defect fractions of EOS IN718. The predictions are made for unclassified test data
not used by the training algorithm, and the parts are processed with varying process
parameters [4].

Figure 8.16 Evaluation in three dimensions based on monitoring signal. The layers are
colored by predicted defect fractions with darker shade referring to elevated number of
defects [4]. (A) nominal part; (B) part with defects.

using predictive algorithms, an efficient closed-loop system would need a viable


solution for deriving the spatial locations of defects. A plausible explanation to for-
mation of rather unpredictable pores is that constant heat input might not be able to
melt fully the local spots where a large spatter has been redeposited, subsequently
resulting in a lack of fusion or a gas pore [7]. Therefore, reliable detection of resul-
tant porosity hindering, that is, fatigue performance of produced material would
184 Additive Manufacturing for the Aerospace Industry

need experimentally derived thresholds to build up confidence in indications flag-


ging the process anomalies.
Another challenge is generalization of any interpretations made from the in-
process measurements. First, postprocess analysis of produced materials sets its lim-
itations in geometries of parts with which to be correlated. Process monitoring
needs to be able to produce reliable results and analysis independent of the size or
shape of produced part and therefore should be accounting for the type of laser
exposure and, i.e., hatch length. Second, the signal depends on the emissivity of the
material. Signal processing methods are needed to remove noise from collected
monitoring data and to extract correlating features, which would ideally be as gen-
eralized as possible to exclude the effects of varying part geometry and hatch
length, machine, and possibly material.
It is unlikely that one sensor could detect all possible process defects deteriorat-
ing the mechanical performance of produced material, such as pores and cracking
after solidification. Finding a single predictor variable having strictly linear correla-
tion with the level of defects is difficult due to the vast catalog of defect mechan-
isms. Moreover, the different predictors should be accounted for that may exhibit
nonlinear correlations with defects and interactions among the variables. This com-
plexity encoded to the additive process promotes the use of data-driven modeling
and machine learning fully to exploit the sensor data in proactive quality control.
Many of the state-of-the-art learning algorithms are designed to count for nonlinear
patterns and higher-order interactions hidden in vast amount of data. Supervised
learning methods offer structured ways to combine extracted features or derived
indications to the results of laboratory analysis. The accuracy of defect detection in
such an approach would depend on how the available predictors reflect the reality,
resolution of monitoring system, and postprocess analysis method, and inevitably
there will be a limit in size of defects that can be detected. The upside is that pro-
duced indications would be based on patterns in experimental data known likely to
result in a pore or other detectable defect.
Achieving accurate defect detection is not the end of the line in striving for
closed-loop control, however. To avoid cracking associated with excessive local
thermal gradients, the potential overheated locations need to be detected before any
cracking occurs. The machine architecture needs to be able to vary the heat input
accordingly. When a pore is detected, corrective actions need to be taken and that
prompts a whole new research subject on how the defect area can be melted again
to achieve full consolidation without unwanted changes in the microstructure.
Healing effect may be then used as an advantage with locally varying energy den-
sity delivered into materials during the exposure of subsequent layers. Compiling
all predictive outputs and classifications together is not a trivial task, either; thus,
more investigation on process monitoring is needed to achieve mature solutions for
reducing need for extensive postprocess inspection. However, machine learning has
the potential to combine the monitoring features from different systems to corre-
sponding quality metrics together for rather accurate nondestructive evaluation of
additively manufactured parts.
Superalloys, powders, process monitoring in additive manufacturing 185

References
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Fusion and/or solid state additive
manufacturing for aerospace 9
applications
James C. Withers
ATS-MER, LLC, Tucson, AZ, United States

9.1 Introduction
The traditional approach to manufacturing a metal part is subtractive machining to
a final shape from a cast ingot or a forged billet, or the metal cast to a near net
shape and finally machined to tolerance. Castings typically have residual porosity
and, depending on thickness, have variable mechanical properties through the cross
section due to the variable cooling rate through the casting cross section. The sub-
tractive machining from a block results in very poor material utilization. In contrast,
fusion metal additive manufacturing (AM) consists of adding material through a
directional programmed molten pool in a layer-by-layer fashion to produce a near/
net shape part, thus reducing material waste, lead times, design constraints, and
potentially the finished part cost. Fusion AM enables novel product designs that
cannot be fabricated using conventional subtractive processing. AM can also extend
the life of in-service parts through innovative repair methodologies. There are mul-
tiple approaches to AM to produce metallic parts.
The first reported patent literature of metal AM was by Baker [1] in 1926 that
built parts via electric arc melt/fusion processing to generate 3-dimensional (3D)
objects, as shown in Fig. 9.1. In 1971, Mitsubishi patented [2,3] processing utilizing
welding of multi-wire to produce a functionally graded wall that was followed in
the early 80s by Kussmaul [4] manufacturing very large steel parts weighing 79 t at
a build rate of 80 kg/h. With the advent of computer aided design (CAD) systems,
the capability of fabrication layer-by-layer from a digital design package has gener-
ated a paradigm in the capabilities of metal AM. There are a family of AM pro-
cesses in which parts are first modeled into a CAD program that slices them into
thin layers where specialized machines then build-up parts layer-by-layer according
to the pattern in the program by injecting metal powder or wire into a high tempera-
ture plasma, laser beam, or electron beam where the feed metal is melted into a
pool that builds the layer; or by laser-sintering a powder within a thin layer of pow-
der onto a substrate or previously built layer. Metal AM has become increasingly
important in the context of next generation manufacturing from both prealloyed and
a blend of elemental powders, or alloy wire feedstocks to achieve properties super-
ior to conventionally processed counterparts. Metal AM processes allow for
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00010-8
© 2019 Elsevier Inc. All rights reserved.
188 Additive Manufacturing for the Aerospace Industry

Figure 9.1 Illustration from Baker patent US 1,533,300.

previously unthinkable designs and dramatic reduction in lead times producing


metals at equivalent to superior mechanical properties to conventionally processed
counterparts. AM is a frontier that is a transforming manufacturing technology.
Transforming a computer-generated file into a physical object is something border-
ing upon science fiction come to life. AM technology is revolutionizing the ways
products are conceptualized, developed, and realized. AM translates back to design,
thereby enabling breakthroughs that are not possible in traditional manufacturing in
subtracting material from a block. Fusion AM can provide small run economic pro-
duction, lowering environmental impacts, wasting less material, improving effi-
ciency that expends less energy than conventional subtractive processes. AM can be
envisioned as a process that builds parts from scratch that means the end product
does not emerge from a solid block, instead it is produced layer-by-layer into a near
net shape. The building in a mapped layer-by-layer architecture removes many con-
straints imposed by traditional machining from a block.
The fusion metals AM process begins with a CAD file of a 3D component,
which is split into a series of layers with a predetermined layer/build/line spacing/
thickness on the order of 0.56.0 mm. Each layer contains a tool path, which is fol-
lowed by the multiaxes stage while powder or wire is injected into a melt pool pro-
duced by a focused power beam generated by plasma, laser, or e-beam.
It is well known that the myriad of properties of both wrought and cast metals
are not the same for different test orientations, such as anisotropic behavior, in
many metals and particularly titanium alloys relative to structural performance.
Directionality in these alloys can be attributed to the basic fusion processing pro-
ducing crystallographic texturing and alignment of structured discontinuities,
including pores, inclusions, and second-phase particles. Anisotropic properties are
observed in fusion beam AM materials, with properties varying with sample orien-
tation relative to the building direction. In beam fusion AM, the high solidification
rates combined with the high thermal gradients present in the solidifying melt pool
results in a highly textured structure such as shown in Fig. 9.2. The line-by-line and
layer-by-layer fashion in which beam fusion AM builds causes directional varia-
tions and heterogeneity of the grain structure and structural discontinuities that
affect performance in some applications.
Fusion and/or solid state additive manufacturing for aerospace applications 189

Figure 9.2 Typical large columnar microstructure in fusion AM processing. AM, Additive
manufacturing.

Figure 9.3 Types of defects that can occur in addition to pores in beam fusion AM [5]. AM,
Additive manufacturing.

Fusion AM results in high thermal residual stress generating distortion/warping


in large pieces and cross sections. The cooling from the molten pool can generate
cracking in the build, such as shown in Fig. 9.3 [5], which cracks are in addition to
pore defects from gas absorption as well as lack of fusion. The high residual stres-
ses in as-formed beam fusion AM can bring down the service life of a component
quite significantly. The stresses in the melt are mostly tensile, which can be as high
as the yield strength of the material. Having the means of controlling grain orienta-
tion in fusion AM produced metals in a manner to generate equiaxed fine grains as
needed based on application is not only beneficial, it is enabling to assure exem-
plary performance over conventionally processed metals.
Distortion and cracking in addition to pore/defects generation during a fusion
metals AM build is a major adversity to overcome [6] before satisfactory qualified
parts can be realized. Distortion in fusion AM is an unavoidable result of a small
molten pool of metal on a much colder body [7] that solidifies in a continuously
190 Additive Manufacturing for the Aerospace Industry

moving build path, creating expansion and contraction stresses of such magnitude
the body deforms and may also crack. Distortion can be mitigated to some extent
through implementing physical restraints on the substrate and part being built and
by decreasing the severity of the thermal gradients through heating of the body dur-
ing the build to which there are limits to base heating and the extent of the expan-
sions and contractions. Restraints do not dissipate the distorting forces and may
cause higher residual forces. Modeling simulation of the build process has a capa-
bility to predict the distortion and provide a basis to mitigate the distortion and
even to a major extent mitigate or possibly prevent the distortion and/or cracking of
a fusion build. Some alloys, such as high strength steels and titanium alloys, are
more susceptible to cracking in addition to distortion. Crack modeling requires
more detail in material properties and sophistication than distortion modeling.
Some cracks as well as pores can be healed in post hot isostatic processing that can
also relieve stresses and refine microstructure when coupled with annealing and
quenching. In some cases, forging post processing can close pores and cracks as
well as eliminate distortion, but is at added cost.
Among the multiple advantages cited for fusion metal AM is reduced cost due to
reduced material waste and producing to near net shape, requiring minimal machin-
ing for ready use. Within any given alloy, cost is related to initial CAD profiling,
feed materials cost, build rate, build atmosphere of a shield, tent or isolation cham-
ber, AM machine cost rate, labor rate, postheat processing, and machining in-situ
during processing or post machining to final tolerance and finish. Modeling of the
cost can provide a first estimate that must include how many trial builds will be
necessary to produce a qualified part ready for use. One example cost model for an
arc beam fusion AM process has been provided by Canfield University [8] that
compares AM processing to conventional machining from a solid piece. In the
Canfield analysis, AM is more economical than conventional processing of machin-
ing from a solid; but, surprisingly, the rate of build has little effect on cost in this
particular model. The Canfield analysis predicts the powder bed AM sintering pro-
cess is always more expensive than machining from a solid.
There are large and numerous opportunities as well as major hurdles for fusion
AM. Most often the opportunity is to take this part and make it with one of the
fusion power beam processes, don’t change anything; but this often does not work,
which does not approach the full potential of fusion AM. The sense of urgency to
implement fusion AM processing is driven not only by fusion AMs potential, but
also by AMs many successes. With the proper design options to meet the part use
requirements, such as load constraints and weight requirements relative to location
within the part, instead of shape only, then AM maximum effectiveness results cou-
pled with cost and delivery time. Original design to take advantage of AM proces-
sing has been shown to reduce part count in some systems by a factor of 70. In
some Department of Defense (DoD) components casting lead time is up to 700
days whereas fusion AM lead times can be only a few days. Certification of fusion
AM built parts remains a hurdle that is rapidly being addressed with quality control
standards and certification being rapidly introduced. One Navy program [9] is pro-
ducing specification blocks by fusion plasma beam processing that provide a
Fusion and/or solid state additive manufacturing for aerospace applications 191

standard for comparative processing to certify parts for engine/aerospace applica-


tion. Qualification can be a big barrier, even though fusion AM can produce things
of the highest quality, but getting them into application can be an uphill battle.
Variations of the fusion power beam AM process has been the dominant AM
process to produce parts in spite of the aforementioned limitation of distortion,
cracking, and textured microstructure. However, variations of friction stir welding
(FSW), termed friction stir processing (FSP), can be adapted to AM (FSAM) that
produces material substantially free of the fusion AM limitations. FSP is a solid
state, nonmelt process that has been shown to produce very fine grain equiaxed
microstructures that have exhibited exemplary properties well above fusion AM or
standard wrought-processed metals. The principle of FSW/FSP is relatively simple.
It consists of a nonconsumable rotating tool, made of a material stronger and harder
than the work piece in a configuration of a pin and a shoulder, as shown in Fig. 9.4.
The tool at spinning rates of a few hundred to a few thousand revolutions per min-
ute (rpm) is downwardly forced into the work piece, similar to drilling. Friction is
generated between the nonconsumable pin and the work piece generating sufficient
heat plastically to deform the work piece. The shoulder of the tool also generates
friction heat and, with the downward force, the shoulder also forges the plastic state
of the material as the material in its plastic state rotates from the front to the back
of the pin. Another source of heat comes from the adiabatic heat produced during
the plastic deformation of work piece material around the rotating tool pin. The

Figure 9.4 Nonconsumable FSAM tool. FSAM, Friction stir additive manufacturing.
192 Additive Manufacturing for the Aerospace Industry

softened material in back of the pin cools as the rotating tool traverses along a
defined line that completes the weld. The larger diameter of the tool shoulder with
its downward force contains the softer plastic material as it spins from the front to
back of the pin that the softer plastic material could otherwise flow out easily to
form flash as well as resulting in defects in the weld, like segregation, dentritic tex-
tured structure, porosity, and hot cracking associated with the fusion-based AM
technologies. Relative to the nonmelt solid state, FSAM has much lower residual
stress that mitigates distortion and eliminates solidification cracking. One example
of FSP is illustrated in Fig. 9.5 with a process operation in Fig. 9.6.
Having the means through FSP of controlling grain size and orientation in a
manner to generate equiaxed fine grains as needed in prescribed locations in AM
produced metals based on application is not only beneficial, it is enabling to assure

Figure 9.5 Illustration of FSAM. FSAM, Friction stir additive manufacturing.

Figure 9.6 Friction stir machine in operation.


Fusion and/or solid state additive manufacturing for aerospace applications 193

exemplary performance over conventionally processed metals. FSAM has the


potential to revolutionize the field of AM. FSAM may be the most significant
development in metal processing in decades. A comparative example of FSP over
fusion beam AM is shown in Table 9.1 [10].
FSP has demonstrated in some cases an increase in yield strength as shown in
Figs. 9.7 and 9.8 [1113]. Yield strength and microstructure directly affects fatigue
life. When FSAM produces enhancement in yield strengths, an increase in fatigue
life can be anticipated over fusion AM produced material or standard wrought
material; or the same fatigue life at an increased applied load.

Table 9.1 Key benefits of FSP process over beam fusion AMa

Advantages Disadvantages

Metallurgical Process related


No melting No shielding gas High process forces—clamping often
No solidification No filler material required
cracking
No gas porosities No harmful emissions Exit hole at the end of the weld
No loss of alloying No work (arc) hazard
element
Low distortion Low surface
preparation
Weld all basic alloys No postweld milling
Excellent required
repeatability
Nonconsumable tool
a
Italics constitutes editing for this application.

(A) (B)
1600 1600
Engineering stress (MPa)

Engineering stress (MPa)

FSAM Ti-6-4 over Ti-6-4 FSAM Ti-6-2-4-6 over Ti-6-4


1400 1400

1200 1200

1000 1000

800 800

600 600

400 400
200 200
0 0
0.00 0.05 0.10 0.15 0.20 0.000 0.025 0.050 0.075 0.100

Engineering strain Engineering strain

Figure 9.7 Tensile properties of FSP treated titanium (A) Ti6Al4V, and (B)Ti-6-2-46
over Ti-6-4. FSP, Friction stir processing.
194 Additive Manufacturing for the Aerospace Industry

(A) (B)
1800
Engineering stress (MPa)

1500
1200 Yield strength Tensile %
Condition
(MPa) strength (MPa) Elongation
900
Base 610 720 14
600 FSAM 500/1
FSAM 500/1 PCBN tool 1616 1747 12
(PCBN)
300
P92 Base Material
0
0.00 0.05 0.10 0.15 0.20
Engineering strain

Figure 9.8 Example of FSAM of P92 steel showing strength increase of more than 250%
over base steel produced by standard processing. FSAM, Friction stir additive manufacturing.

Many variations can be envisioned for FSP to customize material properties and
to AM build shapes. The FSP process illustrated in Fig. 9.5 utilizes a foil welded
onto a base where build-up is achieved with multiple layers of foil. It is also possi-
ble to decouple the pin and shoulder that can operate at different rpms and down-
ward force, as illustrated in Fig. 9.10, which can operate at different rpms to
optimize properties in some cases. The quality of the weld/build has a relationship
to the rotation speed of the tool. High speed of the tip can be desirable to generate
friction/heat that generates plasticity of the metal that relates to producing a defect
free, high quality weld. However, slower speeds of the shoulder can retain the
movement of the metal from the front to rear of the tip and produce a smooth weld
surface. This can be accomplished with a tool, as illustrated in Fig. 9.9. Speed ratios
of tip 1.25:1 shoulder; tip 2:1 shoulder and tip 4:1 shoulder have produced good
welds in metals such as Mg, Al, Ti, and steels.
To enhance the build quality of FSP processing, multiple tools can be utilized in
tandem, such as illustrated in Fig. 9.10. This concept assures high transference
speed and a defect-free fine microstructure in the weld that enhances mechanical
properties in the weld/build. Similarly, tools can be placed side-by-side that
increases the rate of FSP processing. Side-by-side and in tandem assures rapid pro-
cessing and high-quality processed metal.
An alternative in FSP processing of utilizing foil feed to build on a backing or
previously built layer is to feed powder or wire through the tool as illustrated in
Fig. 9.11. The tool in this case, as contrasted from Figs. 9.4 and 9.5, does not utilize
a pin, but might utilize a slight indention.
The underside of the tool is configured to smear and weld the feed metal mate-
rial to the surface of the substrate. This tool configuration is excellent to repair
scratches and gouges in the surface of componentry that has high value, such as
integrally bladed disks of aluminum and titanium. Powder or wire feed down the
tool center provides the metal to repair. Since the FSP processing is nonmelt solid
state, the surrounding parent metal is primarily unaffected as would occur in a
fusion weld repair. In addition to surface repair, this configuration of FSP can be
Fusion and/or solid state additive manufacturing for aerospace applications 195

Figure 9.9 Illustration of a tool that provides the capability for the tip and shoulder to rotate
at different speeds. The shoulder is grooved to provide a smooth surface finish.

Figure 9.10 Dual tools running in tandem to produce a single multiple pass weld.
196 Additive Manufacturing for the Aerospace Industry

Figure 9.11 FSP/FSAM cladding using a powder feed to clad a surface. FSP, Friction stir
processing; FSAM, Friction stir additive manufacturing.

Table 9.2 Mechanical properties of FSAM jointed Ti-6Al-4V at ATS-MER

# Ultimate tensile Yield Elongation on 1v

Strength, ksi Strength, ksi %

FSW weld Ti6Al4Va FSW weld Ti6Al4Va FSW weld Ti6Al4Va


1 159 120 135 110 5.2 15
2 160 132 6.6
FSW, Friction stir welding.
a
Handbook value.

termed FSAM, which is somewhat akin to fusion power beam AM using analogous
feeds but the build remains in the solid state, non-melt producing microstructures
that can exhibit higher mechanical properties, such as shown in Figs. 9.7 and 9.8
and Table 9.2. This configuration of FSAM can produce composites via a feed of
metal powders and ceramic particulate that opens additional product areas.
No matter the FSP tooling configuration, the processing is dependent on friction
heating to raise the temperature to a plastic state. This means the metal material
must be raised from the ambient to a plastic state suitable for processing that is gen-
erally at least 0.5 Tm to as high as 0.75 Tm, which time to temperature has a limita-
tion on the rate of processing; that is, the linear rate of the tool to produce a defect-
free microstructure. Rate can be enhanced by reducing the time to raise the material
from ambient to the optimum plastic state. This can be accomplished by adding
heat to raise the ambient in front of the FSW weld so that the FSP processing only
has to raise the temperature to produce a weld a minimum amount. The added heat
Fusion and/or solid state additive manufacturing for aerospace applications 197

Figure 9.12 Illustration of laser preheating in front of the FSAM tool [14]. FSAM, Friction
stir additive manufacturing.

Figure 9.13 Illustration of PTA in a hybrid couple with FSP. PTA, Plasma transferred arc;
FSP, Friction stir processing.

in front of the tool can be provided by standard processing, such as laser, plasma
torch, radiation, induction, etc., to a select value such as 0.40.6 Tm, leaving only
a minimum temperature rise required via the FSP operation. Processing rates can be
substantially enhanced via the auxiliary temperature additive processing. An illus-
tration of laser preheat in front of an FSP tool is shown in Fig. 9.12 [14].
The FSP operation can be combined as a hybrid with fusion power beam AM
processing, such as illustrated in Fig. 9.13, that provides the attribute of FSP to
198 Additive Manufacturing for the Aerospace Industry

transform the columnar microstructure shown in Fig. 9.2 to an equiaxed fine micro-
structure that enhances mechanical properties. Such laboratory experimental hybrid
systems have demonstrated feasibility. Hybrid AM systems of building the metal
that includes inspection of the build as it grows with in-situ feedback control to the
AM build operating parameters as well as integrating subtractive machining on the
same platform triggered by the inspection systems, which remove and patch any
defect on that layer before the next layer build begins, provides a basis to produce
parts that meet certification for direct use after build. Advanced integrated AM sys-
tems are now capable of meeting these requirements.

9.2 Experimental examples


There is a value of AM produced parts based on virtually unlimited capability of
part complexity, versatility, and speed for just-in-time producing mechanical prop-
erties comparable to superior-to-conventional fabricated metallic parts. Although
fusion metallic AM by definition includes powder bed processing, this rendition
excludes fusion AM powder bed and includes only powder or wire feed to a molten
pool generated by a plasma, laser, or electron power beam. In the case of laser
power beams, depending on the metal composition and its reflectivity from its mol-
ten surface in the wave length of the laser beam, most of the laser radiation power
can be reflected, resulting in low power efficiency. The reflected radiation often
damages the componentry of the system. Green light versus infrared minimizes
reflectivity. Nonbeam via solid state nonmelt FSP is also included independently as
an AM process as well as a hybrid jointly with fusion AM processing.
In the case of fusion metallic AM, the build can be vertical or horizontal, which
may include both types of build in the same part depending upon part complexity.
The cost of build encompasses the entire value chain of powders; processing equip-
ment, including its cost and build rate; amount of post machining to tolerance and
surface finish; post heat treatments, if any; inspection; and certification. The fixed
costs of metallic AM are one-tenth of those of conventional subtractive manufactur-
ing, but the recurring costs of AM are higher by up to 2 3 [15]. The cost of feeds,
prealloyed powders, mixed elemental powders to in-situ form the alloy, or preal-
loyed wire are a major recurring cost and the methodology of preventing distortion/
warping during the build, especially for large and variable thick cross-section parts
strongly influences the cost to produce a fusion metallic AM part. In the case of
nonmelt FSP part fabrication, the feed can be powder, wire, or sheet, and due to
lack of fusion distortion/warping is substantially mitigated. An example of parts
produced by FSP is shown in Fig. 9.14 [16].
Figs. 9.7 and 9.8 are examples of mechanical properties achievable with FSP
processing in titanium and steel. Another example of using FSP to produce hybrid
dissimilar titanium alloy combinations, which is unique to FSP processing, is shown
in Table 9.3 [17]. In addition to these titanium alloy dissimilar combinations, other
dissimilar combinations include aluminum alloys pairing corrosion resistance with
Fusion and/or solid state additive manufacturing for aerospace applications 199

Figure 9.14 Aluminum deck lid FSP joined to galvanized steel [16]. FSP, Friction stir
processing.

Table 9.3 Tensile values of samples extracted from joint regions

Sample Yield strength Tensile strength Ductility


(GPa) (GPa) (%)
Ti-6-4 over Ti-6-4 1.1 1.2 17
Ti-6-2-46 over Ti- 1.3 1.4 9
6-4
Ti-6-4 Base 0.9 1.0 23
Ti-6-2-46 Base 1.1 1.2 18
Note: Bold text indicates substrate onto which the Ti-6Al-4 was deposited.

Figure 9.15 (A) Example of a tool with a long thin tip, (B) a medium length and larger
diameter tip, and (C) a minor/short tip which the latter is for filling minor damages.

high mechanical properties and steels such as soft and hard steels for golf club
applications.
The FSP processing is excellent to repair virtually any metal in any application.
Depending on depth of damage that needs repair, tools with different length tips, as
shown in Fig. 9.15, may be used as well as tools with no tip. Repairs in high value
200 Additive Manufacturing for the Aerospace Industry

Figure 9.16 Example of FSP damage repair. FSP, Friction stir processing.

Figure 9.17 Surface of fusion AM at high build rates. AM, Additive manufacturing.

parts, such as turbine blades, provide a major economic incentive. An advantage of


FSP repair is the surrounding metal is not degraded as a result of the solid state
nonmelt processing that would result from fusion AM. FSP with proper shoulder
design can produce a very smooth surface, as shown in Fig. 9.16, which requires lit-
tle to no final surface finishing. FSP following fusion AM (Fig. 9.13) that can build
at a very fast rate resulting in a rough surface, such as Fig. 9.17, can not only trans-
form the textured microstructure to provide enhanced mechanical properties but
also smooths the rough build surface up to the smoothness, such as shown in
Fig. 9.16.
How the power beam is generated in fusion processes plays a significant role in
the cost and properties achieved in an AM build. The plasma beam, which is
Fusion and/or solid state additive manufacturing for aerospace applications 201

Figure 9.18 Example of PTA plasma beam in AM build. PTA, Plasma transferred arc; AM,
Additive manufacturing.

analogous with welding, is by far the most economical system and has thus far
demonstrated building the largest parts at high build rates. Welding is a metalwork-
ing operation that is commonplace, well established, and widely employed.
Welding provides the promise of fusion metallic AM to meet the ultimate goal of
AM manufacturing. An example of plasma transferred arc (PTA) plasma beam is
shown in Figs. 9.18 and 9.19.
An illustration of the PTA AM process is shown in Fig. 9.20.
Two example PTA AM systems are shown in Fig. 9.21.
The cost of such plasma welding type systems are one-third to one-fifth laser
and e-beam systems and contain closed-loop feedback control from multiple camera
wavelength systems, including reference probes similar to computer numerical con-
trol (CNC) machining as well as in-situ subtractive machining and grinding built-in
with the PTA-AM processing. Such systems have been operational for over a
decade, producing build rates in the range of 570 cc/min, depending on density
and melting point of the metal. Some example large-scale components produced by
PTA AM are shown in Figs. 9.229.24.
Other example fabricated componentry is shown in Figs. 9.25 and 9.26.
As shown in Fig. 9.20, metal powders and/or wire are fed into the molten pool,
which can also include ceramic particulate to produce cermets, such as shown in
Figs. 9.279.29. The PTA AM system can produce foams with a skin such as
shown in Fig. 9.30, as well as some ceramics such as shown in Fig. 9.31.
202 Additive Manufacturing for the Aerospace Industry

Figure 9.19 Example of a finer PTA torch in operation producing an approximately 10 mm


diameter melt pool. PTA, Plasma transferred arc.

Figure 9.20 Illustration of PTA AM system. PTA, Plasma transferred arc; AM, Additive
manufacturing.
Fusion and/or solid state additive manufacturing for aerospace applications 203

Figure 9.21 Examples of a large vertical and robotic PTA system at ATS-MER. PTA,
Plasma transferred arc.

Figure 9.22 (A) Large titanium blocks made by PTA beam fusion AM processing (20 3 30
3 4v), (B) Ti64 large armor plate. PTA, Plasma transferred arc. AM, Additive
manufacturing.

Figure 9.23 (A) Front shield and (B) Gunner Canopy (5 3 6 feet free of warping) produced
by PTA beam fusion AM in TiB2/Ti components. PTA, Plasma transferred arc; AM, Additive
manufacturing.
204 Additive Manufacturing for the Aerospace Industry

Figure 9.24 Example of 2 m length refractory metal clad C18150 copper rails for rail gun.

Figure 9.25 A sampling of architecture produced by PTA AM. PTA, Plasma transferred arc;
AM, Additive manufacturing.
Fusion and/or solid state additive manufacturing for aerospace applications 205

Figure 9.26 Cylindrical bar preform in custom titanium alloy forged into connector rods.

Figure 9.27 Mg-B4C cermet microstructures.

Varieties of torch sizes and configurations are available that provide the capabil-
ity for PTA AM processing to produce coatings on the inside of pipe as illustrated
in Fig. 9.32, such as supplying Inconel compositions inside low cost steel pipe.
It is clear the low-cost systems of PTA have substantial versatility to AM build
parts. Coupling FSP with fusion AM in a hybrid with PTA, such as illustrated in
206 Additive Manufacturing for the Aerospace Industry

Figure 9.28 TiB2/Ti composite integrally built on a Ti6Al4V base by PTA beam fusion
AM processing. PTA, Plasma transferred arc; AM, Additive manufacturing.

Figure 9.29 TiB2/Ti cermet armor after hit by APM2 muzzle velocity (no cracking after
hit).
Fusion and/or solid state additive manufacturing for aerospace applications 207

Foam with a solid layer Final formed foamed part

PTA AM produced
titanium foam

Foam with encapsulating skins


of different thicknesses

Figure 9.30 Example of foams produced from fusion PTA AM processing. PTA, Plasma
transferred arc; AM, Additive manufacturing.

Fig. 9.13, provides a capability to transition the typical isotropic textured micro-
structure to very fine anisotropic microstructures that exhibit excellent mechanical
properties. With FSP just behind the solidified molten mini-pool while the metal is
hot, FSP proceeds at the high build rate of the PTA AM processing.
After demonstration of producing parts that overcome the challenges of distor-
tion/warping, post inspection and processing that verifies defect free with all
mechanical properties at least equivalent to wrought comparison properties at
acceptable economics, qualification, and certification for usage for flight hardware
is a major hurdle. One example is Ti6Al4V parts, such as shown in Fig. 9.33.
Certification of a part can cost millions of dollars and take over a decade to accom-
plish [17]. The old traditional means of qualification and certification is less than
satisfactory for AM manufacturing, which is now becoming the new norm. A more
integrated compositional material engineering (ICME) approach is appropriate. The
ICME tools must account for all the AM key process parameters and their interac-
tion that processing history and post inspections combine to provide part qualifica-
tion and certification for use as flight hardware as well as certified for virtually any
208 Additive Manufacturing for the Aerospace Industry

A boule of HfC-C eutectic cut in half by SEM of a broken flexure test specimen of HfC-C eutectic
EDM machinery (Note: Lacks of columnar microstructure)

The HfC-C withstood cyclic oxidation at 2600°C

Figure 9.31 A boule of HfC-C eutectic that melts above 4000 C and its crystal structure
produced by fusion PTA AM. PTA, Plasma transferred arc; AM, Additive manufacturing.

Figure 9.32 Illustration of PTA AM coating inside pipe. PTA, Plasma transferred arc; AM,
Additive manufacturing.
Fusion and/or solid state additive manufacturing for aerospace applications 209

Figure 9.33 Ti-6Al-4V produced from sponge powder plus aluminum and vanadium powder
using fusion PTA AM to near net shape and final machine.

application. It is now possible to in-situ detect flaws in a fusion AM build down to


approximately 12.5 μm, which is the resolution of the optical sensor/detection sys-
tem. A short wave infrared imaging camera system coupled with a visible imaging
and a separate pyrometer provides diagnostic signatures in real time to in-situ detect
defects. These monitoring capabilities are coupled with a closed-loop control algo-
rithm capable of controlling the AM processing system to produce metal deposits
with assurance that no defect, if any, is greater than 12.5 μm. The actual tempera-
ture of the melt pool, surrounding area, and previous deposit layers, which is the
body of the component, is queued by the emissivity correction which is generally
not known for most molten metal surfaces in a relatively high purity containment,
but, nonetheless, possibly a molecular oxidation layer on the surface of the melt
pool. Therefore, the actual temperature of the melt pool and the immediate sur-
roundings is not precisely known since an accurate emissivity is not known.
Nonetheless, this temperature detection is highly valuable as a real-time control
coupled with the closed-loop control algorithm that controls the beam power that
melts the pool. This in-situ control system coupled with a real-time subtractive
machining system that can be used to stop the build and machine out any detected
defect following restarting the build provides a basis to confirm builds can be made
defect free or at least with defects less than 12.5 μm. Such a system with in-situ
detection, closed-loop real time feedback, and a subtractive machining system has
been producing builds in titanium, steels, superalloys, and, in some cases, in alumi-
num and magnesium for nearly a decade. Post processing of the in-situ certified
210 Additive Manufacturing for the Aerospace Industry

part may also include select heat treatments as well as multiple nondestructive char-
acterization that can augment the in-situ certification to certifying quality of a build
part, providing a qualification basis for the AM produced part. At the rate of devel-
opment advancement of metal fusion AM processing, such processing will become
commonplace. AM of metals and metal composites has transformed AM into a
robust manufacturing paradigm and enabled producing highly customized parts
with significantly improved mechanical properties, compared to standard wrought
produced materials.

References
[1] R. Baker, Method of making decorative articles, in: US 1,533,300, Apr 14, 1925.
[2] U. Akira, Method of and apparatus for constructing substantially circular cross section
vessel by welding, in: US 3,558,846A, Jan 26, 1971.
[3] H.R. Edgecomb, Device for testing plastic materials, in: US118,437A, Aug 22, 1913.
[4] K. Kussmaul, F.W. Schoch, H. Luckow, High quality large components ‘Shape
Welded’ by a SAW process, Weld. J. 62 (1983) 1724.
[5] R.S. Mishra, H. Sidhar, Oct Friction Stir Welding of 2XXX Aluminum Alloys
Including Al-Li Alloys, Elsevier, Amsterdam, 2016.
[6] E.R. Denlinger, et al., Effect of inter-layer dwell time on distortion and residual stress
in additive manufacturing of titanium and nickel alloys, J. Mater. Process. Technol. 215
(2015) 123131.
[7] M. Gouge, P. Michaleris, Distortion in metal additive manufacturing: modelling and
mitigation, Met. Add. Manuf. 3 (1) (2017) 6171. Spring.
[8] F. Martina, S. Williams, Wire 1 arc Additive Manufacturing vs. Traditional Machining
From Solid: A Cost Comparision, Report Ver. 1.0, Cranfield University, 2015.
[9] DoD, Navy Contract No. N68335-15-C-0408, Inducing Known, Controlled Flaws in
Electron Beam Wire Fed Additive Manufactured Material for the Purpose of Creating
Non-Destructive Inspection Standards, ATS-MER, LLC, 2016.
[10] R.S. Mishra, Z. Ma, Friction stir welding and processing, Mater. Sci. Eng 50 (12)
(2005) 178.
[11] DoD, Army Contract no. W15QKN-16-C-0093, Friction Stir Additive Manufacturing
of Titanium Alloys for High Performance Military Applications, ATS-MER, LLC,
2017.
[12] R.S. Mishra, UNT, Materials Science & Engineering, Denton, TX.
[13] DOE, Contract Nos. DE-SC0013783, Alternate Additive Manufacturing to Produce
and/or Join Nuclear Quality Components, and DE-SC0013788, Alternative Additive
Manufacturing to Produce Fossil Energy Critical Systems, 2017.
[14] R.S. Mishra, Friction stir additive manufacturing as a potential route to achieve high
performing structures, in: Presented at the US DOE Workshop on Advanced Methods
for Manufacturing (AMM), September 29, 2015.
[15] W. Frazier, Metal additive manufacturing: a review, J. Mater. Eng. Perform. 23 (2014)
19171928.
[16] J. Saumyadeep, R.S. Mishra, G.J. Grant, Friction Stir Casting Modification for
Enhanced Structural Efficiency, Elsevier, Amsterdam, 2016.
Fusion and/or solid state additive manufacturing for aerospace applications 211

[17] DoD Army Contract No. W15QKN-16-C-0093, Friction Stir Additive Manufacturing
of Titanium Alloys for High Performance Military Applications, ATS-MER, LLC,
2017.

Further reading
N. Kumar, W. Yuan, R.S. Mishra, Friction Stir Welding of Dissimilar Alloys and Materials,
Elsevier, Amsterdam, 2015.
S. Das, et al., Metallic materials for 3D printing, MRS Bull. 41 (2016) 729741.
This page intentionally left blank
Profile electron beam 3D metal
printing 10
Dmytro Kovalchuk1 and Orest Ivasishin2
1
JSC NVO Chervona Hvilya, Kyiv, Ukraine, 2G.V. Kurdyumov Institute for Metal Physics,
Kyiv, Ukraine

Additive manufacturing (AM) over the past decade has become one of the most
important directions for the development of world industry. AM technologies offer
the opportunity quickly and accurately to manufacture products according to the
individual requirements of the customer, which is the old dream of any manufac-
turer. Thanks to this unique ability, AM, along with robotics and information tech-
nologies, is even called the third industrial revolution [13]. AM is defined as the
process of manufacturing a product according to a three-dimensional (3D) model
by layer-by-layer joining of materials using automatic computer control (CAD/
CAM). AM technologies are also called industrial 3D printing, and equipment for
their implementation is 3D printers [46].
AM of metal products is especially important because metals and alloys are still
the main industrial construction materials [7].
A number of different AM technologies for metals have been developed through
the present time, differing in:
G
consumable material—powder, wire or powder-binder mixture;
G
the source of heating—laser, electron beam, plasma, electric arc etc.; and
G
method of layer formation—selective melting (sintering) of the prepared powder bed,
direct deposition of powder or wire on the previous layer (direct energy deposition), and
metal injection molding (binder jetting) as well [4,5,8].

But, despite constant research and numerous experiments, the metal AM technol-
ogies developed to date still have a number of problems that hinder their wide-
spread introduction into the industry. The following are main drawbacks of existing
metal AM technologies [9,10]:
G
complex and expensive equipment;
G
expensive consumable materials;
G
limited sizes of manufactured 3D products and low productivity (for technologies using
powder);
G
thick walls of products and rough surface of manufactured 3D parts (for technologies
using wire);
G
residual porosity, uneven structure, residual stresses, and deformations;

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00012-1


© 2019 Elsevier Inc. All rights reserved.
214 Additive Manufacturing for the Aerospace Industry

G
the need for additional postprocess operations;
G
complex control of running of the process, requiring highly skilled personnel; and
G
lack of certified processes for inspection of the material for defects.
All this ultimately leads to a high production cost of products, which highly lim-
its the really wide and deep penetration of AM technologies into the world indus-
trial production chains [11].
Specialists of the JSC NVO Chervona Hvilya have developed a new method and
system for manufacturing 3D objects [12], comprising forming of a molten pool on
the substrate under influence of an electron beam, feeding of feedstock material to
a melting zone where it is melted by the same electron beam, deposition of received
additional molten material onto the substrate forming of solid deposited layer along
specified trajectory due to solidification of molten feedstock material together with
molten pool as soon as melting zone has left zone of heating by electron beam,
repeating this process the necessary number of times upon previously deposited
layers up to complete forming of specified 3D object, wherein a profile electron
beam in the shape of hollow inverted cone with the apex located near the melting
zone is used for forming of a molten pool on the substrate and for melting of feed-
stock material, and feedstock material is fed to melting zone through feedstock
guide directed along the axis of said hollow conical electron beam (Fig. 10.1).
The new AM technology was called “xBeam 3D Metal Printing” due to charac-
ter view of a profile electron beam. This process belongs to direct energy deposition
processes according to the generally accepted classification of various types of AM
technologies, where they are defined as AM processes in which the focused thermal
energy is used to melt materials during their deposition [4,5] (real view of the
hollow conical electron beam is presented on the Fig.10.2).

Figure 10.1 The scheme of the system for running of the invented process.
Profile electron beam 3D metal printing 215

Figure 10.2 Profile electron beam in the form of hollow inverted cone.

The development of the new method is based on the unique ability of gas-
discharge electron beam guns to generate the profile electron beam by direct emis-
sion from the cathode and without the use of additional deflecting and focusing
means [13].
In more widespread conventional thermionic electron beam guns [14], the source
of electron emission is a cathode made of a material with high emission properties,
which is heated to high temperatures (sometimes above 3000 C). It is necessary to
provide its reliable protection against the influence of the residual atmosphere in
the operating chamber to ensure a long-term operation of such a cathode; otherwise
it will quickly collapse. This is achieved by maintaining the highest possible vac-
uum in the operating chamber (usually at least 1024 mbar), and even higher vacuum
in the electron gun itself by means of additional evacuation from the beam transmit-
ter along the path of the electron beam from the cathode to the working camera. It
is clear that this is possible only if the electron beam is formed with the minimum
possible diameter. Thus, forming of shaped electron beams by traditional therm-
ionic electron beam guns is practically impossible.
In gas-discharge electron beam guns, an electron beam is formed by secondary
electron emission in the following manner. Internal space of gas-discharge electron
beam (EB) gun is evacuated by general vacuum system of technological installation
wherein this gun is installed directly through the exit hole or gap where the electron
beam leaves the internal space of the gun. Accelerating voltage within limits
216 Additive Manufacturing for the Aerospace Industry

545 kV is applied on the cathode of the gas-discharge electron beam gun when
vacuum in operating chamber reaches the necessary operating level (usually within
the range 10241021 mbar). Operating gas, for example, helium, hydrogen, oxy-
gen, or other gases is supplied to discharge chamber of the gas-discharge EB gun
through an inlet nipple. High voltage glow discharge with anode plasma is initiated
inside gun’s discharge chamber between cathode and anode under above conditions.
Said anode plasma serves as a source of ions that are accelerated by electric field at
zone of cathode potential drop and bombard surface of cold cathode, causing elec-
tron emission. The same electric field at zone of cathode potential drop accelerates
electrons emitted from cathode surface and forms an electron beam the shape of
which is determined by configuration of cathode emission surface because emitted
electrons fly away from the cathode surface exactly perpendicular to this surface at
each point of emission. Thus, for example, if cold cathode has shape of a circle
located between two circular anode electrodes oriented coaxially to the cathode and
emission surface of this cathode has a shape of a segment of a sphere with the cen-
ter on the axes of gas-discharge electron beam gun, the electron beam with the
shape of hollow inverted cone will be formed as a result of electron emission from
the cathode, and the apex of the cone will coincide with position of the center of
said imaginary sphere. Accordingly, primary focusing of the electron beam of such
an electron beam gun is provided by geometry of emission surface of the cathode
and does not require application of separate focusing system. Power of electron
beam generated by gas-discharge electron beam gun is regulated by change of elec-
tron beam current, which is controlled by change of pressure inside discharge cham-
ber of the gun by means of increase or reduction of operating gas supply rate.
Other character features of gas-discharge electron beam guns are also important
for the effective implementation and usage of this technology and the achievement
of positive technological and economic effects particularly such features as the abil-
ity to work stably in a wide range of residual pressures in the operating chamber
(10241021 mbar), including partial pressure of different gases, the ability to gen-
erate and form an accurate electron beam under influence of relatively low acceler-
ation voltage (30 kV and less), will result in a simple and compact design,
convenient service and maintenance, long life time of the cathode, and easy and
flexible control of process parameters.
Special static experiments were executed to check the quality of the profile elec-
tron beam formed without the use of focusing lenses and deflecting coils. In these
experiments, a hollow conical electron beam was directed to various sections of a
static titanium wire fixed coaxially with this beam, as shown in Fig. 10.3—first the
apex of the cone was directed to the upper end of the wire (A), then under the root
near the base plate (B), and then to the middle of the wire (C). In all three cases,
the melting of the wire occurred only in a narrow zone of intersection of the beam
with the wire, with practically no noticeable thermal effect on the nearest zones.
Such character view of places where electron beam effected the target has con-
firmed quite high concentration of the energy in the profile electron beam.
Such form of an electron beam and the mutual arrangement of this beam and the
fed consumable material with respect to the substrate provide a number of critically
Profile electron beam 3D metal printing 217

Figure 10.3 The effect of a hollow conical electron beam on an aligned coaxial titanium wire:
(A) on the upper end; (B) under the root near the base; and (C) in the middle of the wire.

Figure 10.4 Schematic view of deposition process.

important physical and metallurgical conditions for the deposition of the molten
material and the formation of deposited bead that should result in a controlled for-
mation of the next layer with certain geometric parameters and the desired structure
of the deposited material.
First, it is necessary to note the following technological features of xBeam 3D
Metal Printing.
1. The round configuration of the molten pool and the vertical feeding of the consumable
material in the exact center of the molten pool (Fig. 10.4) provide:
a. the absence of shaded areas on the substrate that prevents the occurrence of lack-of-
fusion defects and porosity in the deposited layers;
b. the possibility of forming a weld bead with the width only slightly greater than the
diameter of consumable wire, which makes it possible to manufacture parts with thin
and precise walls; and
c. general high process efficiency due to effective usage of practically all power supplied
to the deposition zone.
Such an axisymmetric configuration of heat flow and mass transfer greatly simplifies
the mathematical modeling of the process, which is very important for improving the con-
trol of the technological process in order to predict and to obtain the specified properties
of the material [15].
2. The consumable material is completely enveloped by precisely and flexibly regulated
energy flow (Fig. 10.5), which provides absolutely axisymmetric and uniform preheating
218 Additive Manufacturing for the Aerospace Industry

Figure 10.5 Image of influence of the hollow conical beam on the consumable wire.

and controlled melting of the consumable material. It is important to emphasize that the
hollow configuration of the beam obtained without the use of scanning ensures very con-
stant and uniform heating of both the wire and the substrate. This property, among other
things, also opens interesting technological possibilities, for example, the use of complex
configurations of consumable material, such as cored wire or a bundle of several wires of
various materials.
3. Continuous stationary transfer of liquid metal from the end of consumable wire to the sub-
strate is reliably held by surface tension forces (Fig. 10.6). As soon as liquid metal formed
at the end of the fed wire touches the liquid metal in the pool on the substrate a fluid
neck-way is immediately formed between the end of the wire and the substrate. This liq-
uid metal flow formed and maintained under influence of surface tension forces serves as
a reliable channel for smooth and steady transfer of additive material from the consum-
able material onto the substrate. The gravity force also influences the liquid metal flow.
Additive liquid metal spreads within the boundaries of the currently existing melt pool as
soon as it arrives due to complete adhesion between similar liquids. Boundaries of spread-
ing additive material are determined by the limits of the exposure area of the electron
beam on the substrate. Once the liquid metal reaches the solid metal on the substrate out-
side the pool, it immediately solidifies. Thus, a reliable and flexible mechanism for form-
ing deposition bead of specified width, and, correspondingly, the thickness of the wall of
the 3D object to be produced, is realized.

It is necessary separately to emphasize that this property of continuous liquid


metal transfer from the end of the wire to the substrate ensures the workability of
xBeam 3D Metal Printing technology in Zero gravity due to the fact that surface
tension forces act in the same way as on the Earth. The need for AM of metal parts
in Zero gravity on the board of spacecraft, as well as in the missions for the devel-
opment of the Moon and Mars, is permanently emphasized in the plans of relevant
organizations and companies such as NASA, ESA, SpaceX, and others [16,17]. In
this case AM powder methods are not applicable, and in known wire-based AM
methods there is a danger of formation and detachment of droplets due to the pulse
nature of wire heating.
Another extremely important property of xBeam 3D Metal Printing technology
is the significantly lower power concentration of the heating source (the electron
Profile electron beam 3D metal printing 219

Figure 10.6 Photo of the spreading of liquid metal from the end of the wire along the
substrate: (A) direct photo image and (B) photo image through a dark glass.

beam) generated by the low-voltage gas-discharge electron beam gun in comparison


with other heating sources of currently known additive metal production processes.
Usually developers of metal 3D printers are trying to apply the devices designed for
welding applications like traditional thermionic electron beam guns, lasers, and
plasma torches as the source of heating, where the minimum possible focus spot
(usually from tens to hundreds of microns) and high-power concentration (up to
105106 kW/cm2) were important technological parameters. In AM, an excessive
power concentration can lead to deep penetration onto the previous layers, resulting
in the formation of defects in the produced 3D parts. Therefore, the power of high
concentration must be distributed over the surface by means of scanning with
extremely high frequency, which is a complicated technical problem first, and, sec-
ond, it breaks the continuity of the process of formation of the deposited layer.
The ability to avoid deep heat penetration into the previous layer provides a
technologically important opportunity to deposit the next layer with an overhang
without supporting structures and without tilting of the substrate plate. Fig. 10.7
shows samples of parts obtained using this strategy—substrate plate was horizontal
and wire Ø3 mm was fed vertically during all deposition process. Both internal and
external surfaces of the parts have practically the same texture in spite of solidifica-
tion of overhangs, maintaining high manufacturing accuracy and minimal losses for
machining. This ability opens additional flexibility in design of parts to be produced
220 Additive Manufacturing for the Aerospace Industry

Figure 10.7 (A) Experiment with gradual increase of shift up to 2.0 mm from previous layer
resulting in ultimate achieved overhang 60 from vertical and (B) experiment with forming
of Ø150 mm cylindrical curve.

by 3D printing. Also, such declined walls can be used as supports for forming of
next layers upon them instead of substrate.
Appearance of residual stresses during deposition is one of the major problems
of most of the known metal AM methods. In the worst case, this problem can cause
formation of significant residual distortions that disrupt the geometry of the pro-
duced 3D parts and lead to significant additional material losses during final
machining. Significantly lower temperature gradients on the substrate or/and in the
previous layers provided by xBeam 3D Metal Printing technology significantly
reduce the level of residual stresses and distortions. A mathematical model of the
formation of a 3D sample by layer-by-layer deposition using xBeam 3D Metal
Printing technology was developed to study the 3D kinetics of temperature fields
and the stressstrain state of 3D objects [14]. The calculations have demonstrated
Profile electron beam 3D metal printing 221

Figure 10.8 (A) Dependence of substrate bending (residual distortion) from the length of the
sample according to mathematical model (B) Sample made by deposition of Ti6Al4V
wire Ø2.0 mm, base plate 12.7 mm.

the possibility of providing a relatively small level of residual distortion in the sub-
strate (Fig. 10.8A), which is also confirmed by experiments (Fig. 10.8B).
The very soft and controllable character of thermal action of a low-voltage hol-
low conical electron beam on the substrate is well demonstrated by the following
experiment in which a wire was used as a substrate instead of the traditional thick
plate. A Ti6Al4V wire with diameter of 3 mm was used as consumable material
for deposition and CP Ti wire with diameter of 3.2 mm was used as the substrate in
this experiment accordingly. Setup process parameters were the following: power
of the electron beam gun—3 kW at an accelerating voltage of 15 kV, the wire feed
rate 14 mm/s, and the substrate translation speed 14 mm/s. Preliminary heating of
the substrate was not applied. In one experiment, the single-bead and the double-
bead walls were built along the substrate wires (Fig. 10.9A). In another experiment,
two single-bead walls were built across substrate wires and also one cylinder was
built upon the same substrate wires (see Fig. 10.9B). These figures (walls and cylin-
der) have similar main dimensions (width and height of the walls, layer thickness)
and the general view of side surfaces with the same figures built upon the thick
solid substrate under the same process parameters. But, in this case, the base wire-
substrate looks practically straight. It means formation of very low residual stresses
and distortions in the substrate that is almost unavoidable when using a massive
222 Additive Manufacturing for the Aerospace Industry

Figure 10.9 Samples obtained using a wire as a substrate for deposition: (A) deposition
along substrate wires and (B) deposition across substrate wires.

plate [14]. The application of such an approach can be very effective in cases of
production of 3D objects in which the base plate is not a part of the final product
and must be completely removed by machining.
Loss of volatile alloying elements due to evaporation from the liquid phase dur-
ing deposition is one of the serious problems of a number of existing metal AM
technologies. For example, it is the loss of aluminum from titanium alloys, the loss
of titanium from niobium alloys, etc. Sometimes the reduction in the content of
such volatile elements is so high that the chemical composition of the material
received by 3D printing falls out of the requirements of the standards for these
grades. In such cases, specially produced raw materials (powders or wires) with sig-
nificantly increased content of some alloying elements are used in order to compen-
sate for subsequent losses of these elements and to maintain the required ratio of all
alloying elements in the material of the final product. This leads to significant
increase in the cost of raw materials, and hence the final product.
Profile electron beam 3D metal printing 223

xBeam 3D Metal Printing technology significantly reduces the specific amount


of material that remains in the liquid phase per unit time, thereby significantly
reducing the loss of alloying elements due to evaporation. For example, exploration
study of the change in the chemical composition of the titanium alloy Ti6Al4V
because of the deposition process using xBeam 3D Metal Printing technology
showed only a small or minor decrease in the aluminum content from 5.99% in the
initial wire to 5.72%5.93% (depending on the process parameters) in the depos-
ited material, which ensures compliance with the requirements of all standards for
this grade. This property allows the usage of standard industrial wire available in a
free competitive market as a material for deposition.
An important operating feature of xBeam 3D Metal Printing technology is a
small number of basic process parameters and their easy control. It is very impor-
tant for providing of reliable process repeatability and overall production efficiency.
The main parameters of the process are:
G
power of the electron beam gun;
G
the gap Z between the wire outlet hole and the substrate (Fig. 10.10);
G
feed rate of the consumed wire; and
G
translation speed of substrate (linear movement rate of deposition point).
This means that the one predefined wire diameter is used for one 3D printing
process.
The gap Z between the wire exit hole and the substrate is the key parameter that
determines the main characteristics of the xBeam 3D Metal Printing process. The
value of the gap Z determines the distribution of the power of the electron beam
between the consumed wire and the substrate, and also the width of the area of
effect of the electron beam on the substrate that determines the diameter of the melt
pool on the substrate and the corresponding width of the deposited bead. Thus,
maintaining a stable gap Z value provides a stable deposition rate under constant
electron beam power, that is, constant productivity of the deposition process.
An important advantage of the technology is that this key process parameter is
controlled simply by ensuring a constant geometric configuration of the equipment

Figure 10.10 The gap Z between the wire exit hole and the substrate.
224 Additive Manufacturing for the Aerospace Industry

components, which is easily realized by mechanical means and is also easily


regulated.
Further, at constant values of electron beam power and the gap Z, that is, at a
constant deposition rate and the width of the resulting deposited bead, the height of
the deposited layer can be regulated by changing the linear translation speed of the
substrate because, in this case, the same amount of incoming liquid metal will be
distributed in another area in direct proportion to the change in the linear translation
speed of the substrate. Fig. 10.11 schematically shows the change in the configura-
tion of the deposited bead with a decrease in the speed of substrate movement
(from the upper to the lower figure) at a constant deposition rate and the width of
the deposited bead. Fig 10.12 shows the walls with different parameters of the
deposited layers, formed from the wire of the same diameter.
Thus, control of just a few simple parameters of the equipment provides flexible
control over the formation of 3D objects and guarantees the repeatability of the
main deposition parameters of each layer (Fig. 10.13).
Other process parameters, like vacuum level in the operating chamber, accelerat-
ing voltage, type of operating gas in the gas-discharge EB gun, and substrate tem-
perature as well must be also taken into account and appropriately controlled in
determining the complete set of essential process parameters.
The ability to maintain a shallow pool of molten metal on the substrate during
the deposition process together with the possibility to form very thin layers of
deposited material provides a much higher rate of cooling and solidification of the
initial and additive material on the substrate, resulting in better structure of solidi-
fied material. This feature is especially important for refractory materials, such as
titanium and niobium alloys where heat radiation prevails in the balance of distribu-
tion of cooling flows.

Figure 10.11 Configuration of the deposited bead depending on deposition parameters.


Profile electron beam 3D metal printing 225

Figure 10.12 Deposited layers formed from the wire with diameter 2 mm: (A) stainless steel
304L, layer thickness 0.6 mm and (B) titanium alloy Ti6Al4V, layer thickness 1.2 mm.

Figure 10.13 Cup made from CP Ti Grade 4 wire Ø3 mm, 50 layers, productivity 2.5 kg/h.
(A) image of the completely 3D printed cup, (B) image of the 3D printing process

The formation of a columnar structure in deposited metallic materials, when


columnar grains sometimes grow through all deposited layers, is one of the serious
problems of the existing processes of metal AM. Such type of metal structure is
highly undesirable, since it leads to nonuniform properties in different directions.
xBeam 3D Metal Printing technology has demonstrated the ability to prevent the
formation of a columnar structure in 3D deposited metal parts thanks to flexible
capabilities of controlling power distribution and due to very dynamic character of
deposition process that provides high rates of crystallization and subsequent cool-
ing. Fig. 10.14 shows a structure of the sample made of titanium alloy Ti6Al4V
226 Additive Manufacturing for the Aerospace Industry

Figure 10.14 Structure of the specimen made of Ti6Al4V. (A) full cross-section, (B)
enlargment 1 (C) enlargment 2.

by xBeam 3D Metal Printing. A casting type structure with equiaxed type grains
growing through the one to two nearest layers boundaries was obtained, which demon-
strates absence of any interlayer character differences, segregations, and defects.
The similar character of metal structure is observed in all directions of the
cross section of Ti6Al4V samples manufactured using xBeam 3D Metal
Printing technology—in the plane YZ across growing wall, in the plane XY
where layers are deposited, and in the plane ZX along the growing wall from the
side (Fig. 10.15).
The choice of the diameter of the consumed wire is an important factor in choos-
ing the right deposition strategy of production of 3D parts by xBeam 3D Metal
Printing. xBeam 3D Metal Printing technology was developed for preferable usage
of industrial wire of standard grades with diameters from 1 to 3 mm. This is an
important argument in favor of increasing the economic efficiency of the technol-
ogy, because standard industrial wire is much cheaper than the special wire pro-
duced by customized order. In addition, the price of the wire is significantly
reduced when increasing its diameter for the same grade. It is obvious that it is
more convenient to form thin walls with a lower roughness from the consumed
wire of smaller diameters. At the same time, the smallest wall thickness provided
by xBeam 3D Metal Printing technology is about 1.5 mm, which is approximately
equal to minimum diameter of the focal spot at the top of the hollow conical elec-
tron beam. Therefore, usage of wire diameter less than 1 mm for deposition is not
reasonable. As for upper limitation of wire diameter, it is limited mainly by ability
to make wire straight and applicable for accurate coaxial feeding to the deposition
point through guide direction of the special EB gun. Consumable material in the
form of straight rods can be used instead wire for high strength and rigid materials.
3D parts with walls of which the thickness is larger than ultimate thickness of
the one deposited bead provided by xBeam 3D Metal Printing technology are
formed by deposition of several parallel beads with some overlap between them in
each layer, as shown in Fig. 10.16.
Profile electron beam 3D metal printing 227

Figure 10.15 Structure of the specimen made of Ti6Al4V: (A) in the plane XY and (B)
in the plane ZX.

Figure 10.16 Formation of walls of different thicknesses. Titanium alloy Ti6Al4V, wire
Ø2 mm, walls 1 and 3—single-bead, wall 2—triple-beads, wall 4—double-beads deposition
strategy.
228 Additive Manufacturing for the Aerospace Industry

It is possible to apply a wire with the most suitable diameter, the multiplicity of
which will ensure the smallest permissible allowance for subsequent machining.
The macrostructure of a thick wall formed by strategy with a several parallel passes
is shown in Fig. 10.17.
In general, the optimal choice of the diameter of the deposited wire and of the
basic process parameters makes it possible flexibly to form the deposition strategy
and to achieve very high output yields even for products with very different walls,
including very thin walls (as low as 1 mm of final size). Thanks to this technology,
xBeam 3D Metal Printing confidently shows the best efficiency in the manufacture
of metal products with walls from 1 to 10 mm, thus occupying a niche between the
accurate but low-productivity powder-based AM technologies and the productive
but rough wire-based AM processes.
The experimentally demonstrated capabilities of xBeam 3D Metal Printing technol-
ogy to form a defect-free equiaxed structure of deposited metal materials are expected
to provide good mechanical properties of the resulting products. The primary results
of exploration of the basic mechanical properties of titanium alloy Ti6Al4V (ten-
sile strength, yield strength, elongation, and reduction of area, as well) demonstrated
complete meeting of the requirements of the basic standards for Ti6Al4V pro-
duced both by conventional thermomechanical processing chain and by AM. The
properties in the direction of deposition of the layers (horizontal direction) and across
the layers (in the vertical direction) are almost identicalsee Table 10.1.

Figure 10.17 The macrostructure of a thick wall (20 mm) formed by five parallel beads,
titanium alloy Ti6Al4V, wire Ø3 mm.
Table 10.1 Results of mechanical testing of Ti6Al4V

Specification Tensile strength, MPa (ksi) 0.2% Yield strength, MPa (ksi) Elongation (%)

(XY) (Z) (XY) (Z) (XY) (Z)


AMS 4999 (min) 889 (129) 855 (124) 800 (116) 765 (111) 6 5
AMS 4928 (Forging 896 (130) 827 (120) 10
Annealed)
AMS 4905 (Beta 841 (122) 745 (108)
Annealed)
xBeam 3D Metal 940949 (136138) 913926 (132134) 848873 (123127) 829842 (120122) 1217 1217
Printing
230 Additive Manufacturing for the Aerospace Industry

The pilot installation xBeam-01 was designed and built for exploration study of
capabilities of xBeam 3D Metal Printing technology and for testing of the devel-
oped engineering, monitoring, and control solutions—see Fig. 10.18. The installa-
tion is simple and compact in design—its footprint does not exceed 10 m2, allowing
possibility to install it in any university laboratory. The loading of consumable wire
can be done without opening of the operating chamber, which is very convenient
for carrying out research work. Deposition processing can be carried out within a
vacuum range 10221021 mbar thanks to ability of a gas-discharge electron beam
gun to operate in a low vacuum, so the installation is equipped only by one
mechanical fore-pump. Operating of special gas-discharge electron beam gun under
low accelerating voltage about 1015 kV provides safety working conditions for
staff from X-ray radiation from the operating chamber.
Technical data of the pilot installation xBeam-01 are presented in Table 10.2:
Deposition rates up to 700 cm3/h were achieved during experimental operation
of the pilot installation xBeam-01 that corresponds to more than 3 kg/h for titanium

Figure 10.18 Installation xBeam-01.


Profile electron beam 3D metal printing 231

Table 10.2 Technical data of the pilot installation xBeam-01

AM process type Electron beam direct energy deposition


Building volume (W 3 D 3 H) (mm) 300 3 300 3 300
Positioning system Three-axis, linear
Ultimate power (kW) 20
Ultimate accelerating voltage (kV) 20
Maximum power consumption (kW) 30
Ultimate vacuum (mbar) 5  1023
Operating vacuum (mbar) 1  10225  1021
Permissible feedstock type Wire, rods, cored wire with
diameters 13 mm
Operating gas (helium) consumption, 2.5
at 0.1 MPa (L/min)
Recommended installation 3300 3 3000 3 2400
space (L 3 W) (mm)
Total weight, approximate (kg) 1500

alloys. This productivity was provided by nominal power of special gas-discharge


EB gun about 5 kW. This allows us to expect productivity of at least 2000 cm3/h at
the maximum rated power of the gun, which corresponds to the maximum indica-
tors in the market of metal AM technologies demonstrated to date.
Accuracy and surface roughness of 3D parts manufactured at the pilot installa-
tion of xBeam-01 has demonstrated that required tolerance for machining is not
more than 1 mm on each wall surface, which is much better than any of existing
wire-based metal AM technologies.
The prototypes of serial xBeam 3D metal printers of laboratory and industrial
scale are developing now on the basis of pilot operation of the installation xBeam-01.
Evaluation of direct and indirect operation costs of manufacturing of 3D parts by
xBeam 3D Metal Printing technology were made during trial production of real
industrial parts as well as calculation of yield and general material balance through
complete production chain. The obtained estimation showed the operating cost
(without material balance) for titanium alloys at a rate of about $40 per kg of fin-
ished product, taking into account the final machining to bring the part to its final
form. This corresponds to less than $0.01 per 1 cm3 of deposited material, which is
the lowest indicator among all currently existing metal AM processes.

Summary
The xBeam 3D Metal Printing is a relatively new AM technology. Although a few
AM technologies using wire for deposition are already known, including those in
which the electron beam is used as the heating source, the xBeam 3D Metal
Printing has very different physical and metallurgical character of liquid metal
232 Additive Manufacturing for the Aerospace Industry

transferring and spreading onto the substrate due to specific power distribution in
deposition area provided by profile electron beam. Therefore, further progress of
this technology development still requires additional investigations and modeling of
interconnections between process parameters and subsequent experimental
approval.
Nevertheless, exploration study of this process performed until the present time
has demonstrated the great potential of xBeam 3D Metal Printing both for R&D
works and industrial application. Already validated capability of high productive
manufacturing of quite precise parts made of defect-free metal with good metal
structure and properties opens very encouraging prospects for this technology to
become the solution of many technical and technological problems of existing
metal AM technologies.
xBeam 3D Metal Printing can drastically bring down the production cost of 3D
metal products thanks to significant reduction of material losses, possibility to use
cheaper materials for deposition, and affordable equipment prices as well. In addi-
tion, this process does not have technological limitations in size of produced parts.
All together, these can give a strong impetus to a wide industrial application of
metal AM, including applications for the most popular and nonexpensive industrial
materials, like stainless steel and others.
But, first of all, xBeam 3D Metal Printing can become the reliable technology
for the aerospace industry. Exclusive possibility of control deposition conditions
provided by the profile electron beam, including flexible regulation of deposited
bead configuration, allows good control of thermal distribution during the deposi-
tion process, resulting in formation of predictable and repeatable metal structure
and properties. Some special features provided by xBeam 3D Metal Printing can
open new prospects in parts design. Finally, these key technical capabilities are sup-
ported by low buy-to-fly ratio, which is very important for basic expensive aero-
space materials like titanium-, nickel-, niobium-based alloys.
The xBeam 3D Metal Printing technology and 3D printers of the xBeam 3D
family promise to become a reliable, efficient, and friendly equipment for the wid-
est industrial and scientific circles.

References
[1] The Economist, A third industrial revolution, The Economist April 21 (2012). ,http://
www.economist.com/node/21552901..
[2] TechCrunch, Is 3D printing the next industrial revolution? TechCrunch February 26
(2016). ,https://techcrunch.com/2016/02/26/is-3d-printing-the-next-industrial-revolution/..
[3] Roland Berger Strategy Consultants GmbH, Additive manufacturing market outlook.
Value chain—market size—key players—business models, in: Additive Manufacturing.
A Game Changer for the Manufacturing Industry? Roland Berger Strategy Consultants
GmbH, 2013.
[4] ISO/ASTM 52900:2015, Additive manufacturing—General principles—Terminology, in:
ASTM F2792, 2015.
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[5] Wohlers Report, 3D Printing and Additive Manufacturing State of the Industry Annual
Worldwide Progress Report, 2017. ISBN 978-0-9913332-3-3.
[6] AdditiveManufacturing.com, What Is Additive Manufacturing? AdditiveManufacturing.
com. ,http://additivemanufacturing.com/basics/..
[7] A. Zaleski, Here’s why 3D printing needs more metal, Fortune November 11 (2015).
[8] 3dprintingindustry.com, 3D Printing Processes: The Free Beginner’s Guide. ,http://
3dprintingindustry.com/3d-printing-basics-free-beginners-guide/processes/..
[9] C. Chaplais. 7 Challenges to a Wider Adoption of Additive Manufacturing in the
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[10] Gao, W., Zhang, Y., Ramanujan, D., Ramani, K., Chen, Y., Williams, C.B., Wang, C.
C.L., Shin, Y.C., Zhang, S., Zavattieri, P.D. The status, challenges, and future of addi-
tive manufacturing in engineering, Comput. Aided Des. 69 (December 2015) 6589.
[11] D.S. Thomas, S.W. Gilbert, Costs and cost effectiveness of additive manufacturing. A
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[12] JSC NVO Chervona Hvilya, 2016 Method and apparatus for manufacturing of three
dimensional objects. Patent of Ukraine No.112682. Issued on October 10, 2016.
[13] D. Kovalchuk, V. Melnyk, I. Melnyk, B. Tugai, Prospects of application of gas-
discharge electron beam guns in additive manufacturing, Electrotechnic. Electron.
(E 1 E) 56 (2016) 3642.
[14] S. Schiller, U. Heisig, S. Panzer, Electron Beam Technology, Wiley, 1995.
[15] O.V. Makhnenko, A.S. Milenin, E.A. Velikoivanenko, N.I. Pivtorak, D.V. Kovalchuk,
Modelling of temperature fields and stressstrain state of small 3D sample in its layer-
by-layer forming, Paton Welding J. 3 (2017) 714.
[16] T. Ghidini, An overview of current AM activities at the European Space Agency. 3D
printing and additive manufacturing—industrial applications, in: Global Summit 2013
—London, UK, November 11, 2013.
[17] R.G. Clinton Jr., NASA Marshall space flight center additive manufacturing: rocket
engines and in space manufacturing, in: Second International Symposium Additive
Manufacturing, February 89, 2017, Dresden, Germany.
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Additive manufacturing of
titanium aluminides 11
Wei Chen and Zhiqiang Li
AVIC Manufacturing Technology Institute, Beijing, P.R. China

11.1 Applications of TiAl


It has been more than a decade since TiAl (Ti48Al2Cr2Nb) blades were
first introduced into the low pressure turbine (LPT) of GEnx engines in 2006
(Fig. 11.1A). The primary driving force was to replace Ni-based superalloys
for weight savings due to the low density, high modulus, and good creep strength
of TiAl [15]. The lower centrifugal loading of the lighter TiAl blades
further reduces the size of the Ni-based superalloy disc, which contributes a
significant proportion of the weight saving. Two stages of TiAl LPT blades allow
about 100 kg of weight to be removed for each engine (Fig. 11.1B), which is
unprecedented for a single material change in the aero-engine industry.
Comparing with prior engines in its class, the GEnx engines deliver a 20%
increase of fuel efficiency, a 50% reduction of noise, and an 80% reduction of
NOx emission. At present, there are approximately 190,000 TiAl blades flying
daily throughout the world on 229 Boeing 787s and 101 Boeing 747-8s [6]. The
new LEAP engines jointly developed by GE and Snecma will also use TiAl for
the LPT blades.
In addition to the effort of GE, Pratt & Whitney, along with MTU, are using a
TiAl alloy (TNM) as an LPT material for the last stage of the PW1100G Geared-
TurboFan (GTF) engine [710]. In September 2014, the Airbus 320neo aircraft
equipped with two GTF engines completed its maiden flight, in which hot-forged
TNM turbine blades were implemented. Besides, Rolls-Royce has also announced
its plan to use TiAl LPT blades for the future medium-thrust engines named
Advance and UltraFan [11]. Other than LPT blades, Pratt & Whitney and Volvo
have been developing TiAl components, such as compressor blades and shrouds,
blade retainers, and turbine dampers [12]. Snecma and Turbomeca also performed
several feasibility studies to make a TiAl high-pressure compressor casing via
powder metallurgy (PM). However, until now, GE’s Ti-48Al-2Cr-2Nb LPT blade
is still the only intermetallic component that is in revenue service.

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00013-3


© 2019 Elsevier Inc. All rights reserved.
236 Additive Manufacturing for the Aerospace Industry

Figure 11.1 (A) Last two stages of GEnx low pressure turbine, (B) TiAl-4822 blades on one
stage.

11.2 Fundamentals of TiAl


TiAl alloys usually consist of two major phases. The α2 phase (Ti3Al) has the hex-
agonal DO19 structure and the γ phase (TiAl) has the tetragonal L10 structure.
These two ordered phases exhibit very low ductility, especially in the binary state.
For the α2 phase, the long-range order affects the deformation modes for α-Ti, with
the result that fewer modes are readily activated [5,13]. In particular, twinning is
not observed in this phase and c 1 a slip is much less frequently observed.
The presence of long-range order also inhibits cross slip, so dislocation pile-ups
in the front of the slip bands and the associated stresses can initiate cleavage [5].
Both the reduction in slip systems and the occurrence of planar slip are responsible
for the low ductility of the α2 phase up to about 600 C. For the tetragonal γ phase,
the ordering also decreases the plastic deformation capability and the ductility is
quite low up to about 750 C.
Alloying has been shown to improve ductility and fracture toughness. The first
benefit of alloying is to relax the restriction on slip modes; the second is to retard the
kinetics of ordering or to change the degree of long-range order; the third is to alter
the alloy constitution by introducing the β or β2 phase as a ductile second phase that
can arrest or hinder the growth of microcracks that form in the brittle α2 and γ
phases; the fourth is to alter the transformation behavior during heat treatment and
processing to permit microstructural refinement and control [5]. Typical TiAl alloys
with potential engineering applications can be described by: Ti(4249)Al
(0.110)X, with X designating alloying elements such as Nb, Cr, V, Ta, Mo, Zr, W,
Si, C, and B. The constitution of these alloys may involve a variety of stable and
metastable phases, depending on the detailed composition and processing conditions.
Detailed review of TiAl alloy design can be found elsewhere [5,1315].
TiAl alloys can be thermal-mechanically processed to 4 types of microstruc-
tures: equiaxed (near γ), duplex, nearly lamellar, and fully lamellar.
Microstructural variables like equiaxed γ volume fraction and grain size, α2/γ
colony size and orientation, and α2/γ lamellae width all have a significant
influence on mechanical properties [1623]. Similar to Ti6Al4V, lamellar
Additive manufacturing of titanium aluminides 237

microstructure exhibits better fracture toughness and creep resistance, while


duplex or equiaxed microstructure exhibits higher ductility and fatigue properties.
It is well acknowledged that there is no universal alloy composition that is
suitable for all applications; rather alloy composition must be tailored together with
processing to achieve the required properties for specific components.

11.3 Processings of TiAl


Similar to conventional Ti alloys, the processing routes established for TiAl-based
alloys on an industrial scale can be divided into four categories (Fig. 11.2): casting,
wrought processing, PM, and additive manufacturing (AM) [2428].

11.3.1 Casting
Casting offers the most cost-effective route for TiAl components, primarily because
the well-established infrastructure for investment casting of conventional Ti alloys
[2]. The centrifugal casting process offers the advantage of shaping complex parts by
minimizing gas porosities and misruns. At present, this process is capable of mass
producing high-quality TiAl components, such as the Ti48Al2Cr2Nb LPT

Figure 11.2 Processing routes for TiAl components.


238 Additive Manufacturing for the Aerospace Industry

blades in GEnx engines, and the 45XD LPT blades in Rolls Royce’s Trent-XWB
engines. Depending on the engine type, 90150 LPT blades per stage are required
[2729].
However, the solidification during the casting process often results in macro-
scopic columnar grains and micro-segregation of the alloying elements. The growth
of columnar grains in preferential crystallographic orientations with respect to the
heat flow direction can further create a strong texture, which leads to structural het-
erogeneities in the castings [13,30,31]. These features are very difficult to alleviate
by subsequent heat treatments. Even though the morphological texture could be
anticipated for simple parts, it is not trivial for complex parts like turbine blades.
This morphological texture and the ordered structure of TiAl lead to a strong anisot-
ropy of the mechanical properties [32,33].

11.3.2 Wrought processing


In order to avoid heterogeneous structures or to induce a favorable texture in
the direction of the highest constraints, forging or extrusion generates a more homo-
geneous and refined structure [34,35]. Wrought processing of TiAl has been shown
possible and the benefit is that greater microstructural flexibility can be achieved
by thermalmechanical processing, so finer duplex or equiaxed microstructures can
be obtained for improved ductility. In general, hot-working of TiAl alloys is per-
formed well above their brittle-to-ductile transition temperature and can be divided
into two steps. The primary hot-working refines the ingots to a fine-grained uniform
microstructure suitable for subsequent wrought processing or heat treatments.
This is accomplished at temperatures between the eutectoid and the γ-solvus by
employing relatively low deformation rates, during which dynamic recrystallization
is prevalent and strain-induced porosity can be avoided.
Wrought processing routes involving closed-die forging are of interest for
making various components, in particular jet engine parts that have to withstand

Figure 11.3 Compressor blades of Ti-45Al-8Nb-0.5(B,C) produced using extrusion and


forging process by Thyssen, GfE, Leistritz for Rolls Royce.
Source: Courtesy of X. Wu, Review of alloy and process development of TiAl alloys,
Intermetallics 14 (1011) (2006) 11141122.
Additive manufacturing of titanium aluminides 239

severe loading conditions. Small Ti45Al8Nb0.5(B,C) compressor blades


have been produced using an ingot extrusion and multistep isothermal forging
process (Fig. 11.3) by Thyssen, Gesellschaft für Elektrometallurgie mbH (GfE),
Leistritz AG [24]. Some wrought Ti47Al3.7(Nb, Cr, Mn, Si)0.5B high-
pressure compressor blades have also been made [36]. The processing involved
ingot extrusion (1250 C), isothermal forging, and final heat treatment. Recently,
Pratt & Whitney has used forged LPT blades for the last stage in their GTF
engine. Isothermal forging with subsequent annealing was chosen [36].
It should be pointed out that, due to its intrinsic brittleness, wrought processing
of TiAl needs to be performed at high temperatures (usually above 1100 C) and
low deformation rates through multistep operations. Hot working also requires the
use of dedicated tools under a neutral gas atmosphere. The productivity and tool
life tend to restrict the volume of wrought processing, although the mechanical
properties of wrought TiAl are superior to the casted counterparts. These factors
will ultimately be an economic hardship if TiAl components are processed this way
for production applications.
In the 1990s, a number of technical programs were initiated to evaluate
the potential of TiAl sheet and foil for aerospace applications. Forgings or powder
billets were used as the prematerials for rolling. During the PM route, gas-
atomized powders were canned, evacuated at elevated temperatures, sealed, and
hot isostatically pressed (HIPed) to a billet of full density. This is attractive
because HIPed TiAl powder billets can be directly rolled without homogenization
and forging. Ti46.5Al4(Cr,Nb,Ta,B) and Ti48Al2Cr2Nb sheets up to
2000 3 500 3 1.0 mm were successfully rolled using this PM route [3741].
Although the R&D work on TiAl rolling has been going on [4244], no real
application in aerospace was found. However, the groundwork of producing high-
quality TiAl powder has been laid.

11.3.3 Powder metallurgy


PM is a longstanding method of producing Ni-based alloy components used in tur-
bine engines. The difficulties of wrought processing motivated the exploration of
PM to produce TiAl products. The advantage of the PM technique is that high-
quality, near-net-shape, and homogeneous parts can be made with substantially
reduced machining and scrap. The near-net-shape PM method can make various
TiAl components with complex shapes. Dimensions of the final components are
calculated based on the finite element modeling of powder shrinkage during HIP.
This technique has matured to a state of designing and making aerospace compo-
nents with high precision (Fig. 11.4).
In recent years, other PM methods have been applied to TiAl alloys, such as
combustion synthesis [45], spark plasma sintering [46,47], and microwave
sintering [48]. Components have been made and the mechanical properties were
evaluated [49].
240 Additive Manufacturing for the Aerospace Industry

Figure 11.4 PM net-shape Ti48Al2Cr2Nb aero engine component. PM, Powder


metallurgy.
Source: Courtesy of D. Liu from IMR.

11.3.4 Additive manufacturing


AM has gained increasing attention since 2010 and the advantages have been
widely recognized [50]. Its ability to directly produce intricate shapes is quite
remarkable. Complex shapes have been made from spherical powder using both
laser and electron beam AM methods [51]. These parts are essentially in-situ cast-
ings with high solidification rates. Therefore, the tensile properties, in particular
yield strength, of these parts are expected to lie somewhere between those of a
forging and a large investment casting. The ability of making TiAl LPT blades has
been demonstrated using electron beam melting (EBM) technology (Fig. 11.5).
Other AM methods, such as selective laser melting (SLM) and laser metal
deposition (LMD) have also been tried for making TiAl components. Although
these techniques show reasonable promise in making simple-shaped samples,
current research is being directed toward the optimization of processing parameters
to form fully dense components with minimal defects. In the following sections, the
processingmicrostructureproperties relationship of TiAl made by these AM
methods will be reviewed and discussed.

11.4 Laser metal deposition of TiAl


The study on laser AM of TiAl is very limited, but the pioneered work dates back
to 1999 [52,53]. In early days, only LMD process was adopted. In this process, the
gas-atomized powder is injected directly into the focused laser beam, and the laser
delivery column and powder nozzle move as an integral unit (Fig. 11.6). This is a
multilayer deposition process, where the preceding layers are partially melted or
Additive manufacturing of titanium aluminides 241

Figure 11.5 EBM Ti48Al2Cr2Nb LPT blades made by AVIC MTI. EBM, Electron
beam melting; LPT, Low pressure turbine.

Figure 11.6 Laser metal deposition process.

heated in the subsequent deposition. The size of heat-affected zone in every subse-
quent deposition will be determined by the choice of processing parameters, such
as laser power, scanning speed, etc. Therefore, the cooling rate and hence the
microstructure evolution are strongly affected.
242 Additive Manufacturing for the Aerospace Industry

The biggest challenge of making bulk TiAl is its crack sensitivity, especially
during the rapid heating-cooling of LMD process. To guarantee a stable deposition
process and good bonding with the substrate, the focus of the powders is
suggested to be below the deposition plane [54]. A parametrical study on
Ti47Al2Cr2Nb shows that cracks can be avoided if a continuous deposition
was assured [52]. Occasionally pores up to 10 μm were observed within the mate-
rial. The composition of the builds was nearly identical to the powder, indicating
no Al loss or oxygen pickup. The as-build material exhibited an inhomogeneous
microstructure and layered nature of the parts was apparent, with each individually
deposited layer containing columnar and equiaxed grains of different sizes as a
result of variations in the solidification rate. However, a subsequent microstructure
homogenization above the α-transus did not improve the tensile properties with
respect to the as-build condition.
In the meantime, Srivastava et al. [53,55,56] investigated the effect of LMD
processing parameters on the Ti48Al2Mn2Nb alloy. The heterogeneous
microstructure was associated with the remelting and thermal cycles as the succes-
sive layers were deposited [53]. In a later study, the key processing parameters that
have significant effects on the build quality were identified [55]. The laser energy
input and powder feed rate were found to determine the processability and therefore
the build quality [56]. However, crack-free samples and surface finish with a good
quality were not achieved in their work.
Changing the laser power strongly affected the microstructure uniformity,
and the grain morphology varied from equiaxed to columnar to dendritic [56].
Lamellar (α2 1 γ) and equiaxed γ phase regions were observed. All the LMD
Ti48Al2Mn2Nb samples exhibited a much finer microstructure compared
with the cast material (Fig. 11.7A). This was due to the high cooling rate associ-
ated with the laser melting process. A slow laser scanning speed and/or high laser
power led to a large heat input and a superheated molten pool. Therefore, it took
a longer time for solidification to start and the temperature of the base material
became higher, which resulted in a lower temperature gradient of the interface
and a lower cooling rate. Thus, a coarse dendritic microstructure was expected
(Fig. 11.7D). For the sample processed with low heat input, small superheating
and large temperature gradient at the interface led to a faster cooling rate and a
finer microstructure (Fig. 11.7B and C). However, inhomogeneity was found in
the as-deposited material, and post-processing heat treatments were not able to
acquire a good compositional homogeneity without too much microstructure
coarsening [56].
Attempts further to describe the metastable and heterogeneous microstructure
of the as-deposited Ti48Al2Cr2Nb were made by Zhang et al. [54]. It is
found that each deposited layer exhibited a metastable microstructure with the
massive γ phase on top, while the high temperature α-phase, which transformed
to α2 phase after cooling down, was retained on the bottom. This was attributed to
the much higher cooling rate at the bottom of the layer due to the rapid heat
extraction from the substrate. The thermal gradients along the build direction also
tend to favor texture effects. For the stoichiometric binary TiAl alloy, sequential
Additive manufacturing of titanium aluminides 243

Figure 11.7 OM microstructure of Ti48Al2Mn2Nb processed by (A) conventionally


cast, (B)(D) LMD samples fabricated with laser power 300, 360 and 400 W, respectively.
LMD, Laser metal deposition; OM, Optical microscope.
Source: Courtesy of D. Srivastava, I.T.H. Chang, M.H. Loretto, The effect of process
parameters and heat treatment on the microstructure of direct laser fabricated TiAl alloy
samples, Intermetallics 9 (2001) 10031013.

laser remelting created the epitaxial growth of γ phase with (1 1 1) plane perpen-
dicular to the build direction, and hence a columnar grain structure was favored
along the build axis [57]. Similarly, a directionally solidified columnar grain
structure formed in the deposition direction of an LMD Ti47Al2.5V1Cr
[58]. Subsequent solid state phase transformation took place and a fully lamellar
microstructure with (α2 1 γ) colony size of 50100 μm and lamellar spacing of
0.30.5 μm formed.
One of the main challenges of LMD process is the brittleness and susceptibility
to oxygen pick-up of TiAl. A recent attempt of making Ti48Al2Cr2Nb by
LMD was performed in an argon-purged chamber with a substrate (cast
Ti48Al2Cr2Nb) preheated to 750 C [59]. The oxygen content in the chamber
was reduced to less than 10 ppm. The preheating improved the bonding between
the deposit and the substrate, and also reduced the propensity for cracking. Thin-
walled samples free of cracks reached over 99% density.
It has been demonstrated recently that optimal processing parameters can be
determined to prevent cracking due to accumulated residual stresses. Thomas et al.
[60] introduced a second laser source at the side of the nozzle, which can create a
heating area surrounding the focal spot of the laser that fuses the powder. This
244 Additive Manufacturing for the Aerospace Industry

Table 11.1 Processing parameters for LMD TiAl samples [60]

Process parameters Min. values Max. values


Powder size, μm 80 125
Laser power, W 200 700
Powder feed rate, g/min 0.5 2.2
Deposition rate, mm/min 60 4000
Z-Increment, mm 0.05 1.5
Number of layers 20 50

LMD, Laser metal deposition.

Table 11.2 Room temperature tensile properties of LMD Ti47Al2.5V1Cr and


Ti40Al2Cr [58,61]

Materials Condition UTS, MPa Elongation, %


Ti47Al2.5V1Cr As-deposited 550 0.3
1100 C/30 min/AC 620 0.4
1100 C/30 min/WQ 630 0.4
1125 C/30 min/WQ 650 0.6
Ti40Al2Cr As-deposited 560 0.2
1100 C/30 min/AC 560 0.3
1100 C/30 min/WQ 580 0.4
1125 C/30 min/WQ 600 0.6
LMD, Laser metal deposition.

complementary heating source, when running at low energy density, slows the cool-
ing rate and diminishes the thermal gradient in the part. Experiments were con-
ducted under controlled atmosphere by changing the processing parameters
(Table 11.1) to manufacture a series of Ti47Al2Cr2Nb beads, thin walls, and
massive blocks. A processing window regarding laser power and scan rate was
established. Varying the laser scan rate can tailor the sample microstructure, with
dendritic microstructures for low scan rate and finer ones for high scan rate.
Conventional postprocessing heat treatments can fully restore homogeneous micro-
structures to either duplex or fully lamellar.
The mechanical properties of LMD TiAl have not been studied very much. A
low tensile ductility of as-deposited Ti47Al2.5V1Cr and Ti40Al2Cr were
reported. Although the ultimate tensile strength (UTS) is close to the forgings, the
tensile elongation is still lower even after heat treatment (Table 11.2) [58,61]. For
the Ti47Al2.5V1Cr alloy, ductility lower than 0.6% was observed along both
XY and Z directions in the as-deposited samples, which was attributed to the
columnar grains in a fully lamellar microstructure [7]. Rittinghaus [59] mentioned
the oxidation problem during the LMD process in a very qualitative way. This
could be a reason for the low ductility other than defects, but none of the studies
measured the oxygen content of the deposited material.
Additive manufacturing of titanium aluminides 245

Most recently, using the optimized processing parameters and heat treatments,
room temperature tensile properties of LMD Ti47Al2Cr2Nb have shown a
very good balance in terms of strength and ductility [60]. In particular, a lower scat-
ter in tensile ductility was obtained with a minimum value of 1% as opposed to the
same alloy processed by cast 1 HIP. Tensile tests of heat-treated samples showed a
UTS of 539 6 15 MPa with elongation of 1.7 6 0.2% along the XY direction, and a
UTS of 519 6 23 MPa with elongation of 1.2 6 0.2% along the Z direction. An
early work by Moll et al. [52] also reported a room-temperature tensile strength
around 500 MPa with 1%2% elongation.
For other mechanical properties, such as fracture toughness, creep, or fatigue, no
public information has been found.

11.5 Selective laser melting of TiAl


SLM has been using to fabricate aerospace components of various materials, such
as steels, Ti alloys, and Ni-based superalloys. Especially when GE Aviation
announced its plan for producing 100,000 fuel nozzles for the LEAP engines by
2020, SLM has become the first AM technology being used for making critical
components in a jet engine. However, SLM has not been demonstrated as a
suitable process for the γ-TiAl alloys so far.
The first attempt of making Ti48Al2Cr2Nb alloy by SLM was per-
formed in 2011 and samples without cracks cannot be obtained [62]. In 2014,
Löber et al. [63] used a TNM alloy with a 4563 μm powder size range and a
75 μm layer thickness for parametrical study. The build chamber was filled with
high purity Ar gas and a residual oxygen level of # 200 ppm was guaranteed.
Laser power and scanning speed were adapted to stabilize the process and to
obtain the best morphology for single beads. A detailed study was performed by
varying the scanning speed (50100, 3502100 mm/s) and laser power
(50250 W) to build a processing map for the TNM alloy. Pronounced cracking
due to high cooling rate during solidification was observed at low power and
low scanning speed.
It is found that the optimized parameter set of laser power and scanning speed
consist of: 100 W, 50 mm/s for the volume contour, 175 W and 1000 mm/s for the
outer contour, a hatching of 0.3 mm, and a layer thickness of 75 μm. The scanning
strategy was a stripe hatching. These optimized parameters were used for produc-
ing small cylinders and dodecahedron cells as shown in Fig. 11.8. A relative den-
sity of around 99% and a fine grained nearly lamellar β microstructure was
achieved. The microstructure of the as-build material was inhomogeneous due to
the nonuniform cooling rate (Fig. 11.9A). A two-step heat treatment at 1230 C
followed by 950 C introduced a uniform duplex microstructure consisting of β and
α2 grains with some γ lamellae in α2/γ colonies (Fig. 11.9B). In addition, compres-
sion tests on SLMed TNM alloy were performed and the strength was found to be
close to cast samples.
246 Additive Manufacturing for the Aerospace Industry

Figure 11.8 Produced TNM-B1 3D-dodecahedron structures with optimized parameter set.
Source: Courtesy of L. Löber, F.P. Schimansky, U. Kühn, F. Pyczak, J. Eckert, Selective
laser melting of a beta-solidifying TNM-B1 titanium aluminide alloy, J. Mater. Process.
Technol. 214 (2014) 18521860.

Figure 11.9 SEM pictures of the SLM produced TNM sample (A) as-build, (B) 950 C heat
treated. SLM, Selective laser melting; TNM, TiAl alloy; SEM, Scanning electron microscope.
Source: Courtesy of L. Löber, F.P. Schimansky, U. Kühn, F. Pyczak, J. Eckert, Selective
laser melting of a beta-solidifying TNM-B1 titanium aluminide alloy, J. Mater. Process.
Technol. 214 (2014) 18521860.

Thomas et al. [64] investigated the influence of the SLM process parameters on
Ti47Al2Cr2Nb. High scanning speeds induced an instability of the melt pool
and more cracks after solidification. The processing has been optimized, but the
range of parameters in the study did not completely suppress the cracking effect
due to the high cooling rate of the SLM process.
The microstructure and tensile properties of Ti44.8Al6Nb1.0Mo0.1B
were studied by Gussone et al. [65,66]. Samples of 99% density could be achieved
when the laser energy input was above 55 J/mm3. The Al loss is directly related to
Additive manufacturing of titanium aluminides 247

Figure 11.10 Typical microstructures (SEM) of samples produced at TPH 5 800 C (top row
and middle row) and TPH 5 1000 C (bottom row). SEM, Scanning electron microscope.
Source: Courtesy of J. Gussone, Y.C. Hagedorn, H. Gherekhloo, G. Kasperovich, T.
Merzouk, J. Hausmann, Microstructure of γ-titanium aluminide processed by selective laser
melting at elevated temperatures, Intermetallics 66 (2015) 133140.

laser energy input and high Al losses at high energy densities indicate significant
overheating. Samples manufactured with the highest energy input (300 J/mm3)
exhibited acicular or platelet structures (α2 within β/B2) as shown in the left column
of Fig. 11.10. At medium energy input (110 J/mm3) similar needles/platelets can be
observed which, however, exhibited a lamellar α2/γ substructure (Fig. 11.10 top
row, middle column). Typical for low energy densities (60 J/mm3) are globular
248 Additive Manufacturing for the Aerospace Industry

shaped ultrafine lamellar α2/γ colonies with β/B2 and γ grains in the submicron
range at the colony boundaries (Fig. 11.10 middle row, right column). Furthermore,
the microstructure of samples manufactured at TPH 5 1000 C were coarser than
samples produced at 800 C.
Li et al. [67] studied the microstructure features, phase transformation, and
nano-hardness of the SLM Ti45Al2Cr5Nb processed by SLM under laser
scanning speed of 500800 mm/s. A higher scanning speed led to finer grains, and
increased volume fraction of γ and B2 phases. The SLMed materials exhibited a
much higher nano-hardness than its traditional casting counterpart and the hardness
value increased with the preheating temperature [68]. Although the compression
strength of the SLM Ti45Al2Cr5Nb alloy was over 1000 MPa [68], the only
study on tensile properties available in public about SLM TiAl alloys reported a
very unstable strength [65]. After HIPing at 1200 C/200 MPa/4 h, tensile strength
of Ti44.8Al6Nb1.0Mo0.1B can be up to 900 MPa as well as below
400 MPa. The poor ductility of all samples was attributed to the high oxygen
pickup during the SLM process as well as the defects that were not removed by
HIPing. The tensile strength at 850 C was between 541 and 545 MPa.

11.6 Electron beam melting of TiAl


The EBM process has the highest technical readiness level among all AM methods
for fabricating TiAl. Various components, such as LPT blades and turbocharger
wheels, have already been made (Fig. 11.11). One important reason is that the sub-
strate is kept above 1000 C during the whole EBM process, so cracks due to resid-
ual stress can be minimized.
The earliest study of making a Ti47Al2Cr2Nb sample by EBM was per-
formed by Cormier et al. [69]. A 7.4 at.% loss of Al was found by comparing the

Figure 11.11 An EBM Ti45Al8Nb impeller. EBM, Electron beam melting.


Source: Courtesy of H. Peng from Beihang University.
Additive manufacturing of titanium aluminides 249

Figure 11.12 The element mappings obtained by microprobe measurements show, the
inhomogeneous distribution of Al due to evaporation taking place in the top region of the
melt pool.
Source: Courtesy of J. Schwerdtfeger, C. Körner, Selective electron beam melting of
Ti48Al2Nb2Cr: microstructure and aluminium loss, Intermetallics 49 (2014) 2935.

as-build sample with the original powder. This is related to the evaporation of Al
during the EBM process in vacuum, but no detailed analysis was performed.
Schwerdtfeger et al. [70] did a comprehensive parametric study of Al loss and build
quality in the EBM Ti48Al2Cr2Nb alloy. It is found that lower beam currents
and the reduced overheating of the melt pool are critical to decrease Al evaporation.
By adjusting the processing parameters, Al loss down to 0.5 at.% was achieved.
However, a slightly uneven distribution of Al was found in samples (Fig. 11.12).
This local variation in Al concentration can affect the solidification pathway and
hence the microstructure. Biamino et al. [71] reported about 1 at.% of Al loss in the
build, but did not give details on the beam parameters used. The strong influence of
energy input on Al evaporation for Ti47Al2Cr2Nb powders was also reported
by Ge et al. [72].
Using a numerical model based on a lattice Boltzmann method that includes
hydrodynamics, thermodynamics, and multicomponent evaporation [73,74], the
relation between energy input, evaporation, and residual porosity was numerically
investigated for the EBM Ti48Al2Cr2Nb (Fig. 11.13) [75]. The chemical dis-
tribution in the build was dominated by the advection of melt driven by the surface
tension and evaporative recoil. The line energy strongly affected the peak tempera-
ture during processing, and thus the element evaporation. It is demonstrated that
significant reductions in evaporation losses can be achieved by applying a
suitable beam scanning strategy. These numerical results were consistent with
experimental data.
250 Additive Manufacturing for the Aerospace Industry

Figure 11.13 Physical effects during the selective melting of a metal powder using a
focused electron beam. In the schematic, the beam is deflected from left to right. The
direction of gravity is indicated by g.
Source: Courtesy of A. Klassen, V.E. Forster, V. Juechter, C. Körner, Numerical simulation
of multi-component evaporation during selective electron beam melting of TiAl, J. Mater.
Processing Tech. 247 (2017) 280288.

In addition, Chen et al. [76] reported an uneven distribution of Al caused by dif-


ferent processing parameters in one EBM Ti48Al2Cr2Nb sample. The cross
section of a rod (the build direction is pointing out of the picture) shows that the
“contour” zone exhibited a lower Al content than the “hatch” zone. This has further
caused microstructure difference in these two zones.
Biamino et al. [71] investigated the possibility to produce fully dense
Ti48Al2Cr2Nb. A process optimization was able to eliminate defects caused by
lack-of-fusion between two subsequent layers, but random spherical pores below
20 μm were still found. These pores were due to the argon gas entrapment inside the
powders during the atomization process. Recently, Mohammad et al. [77] examined
the defects distribution using micro-CT in the as-build Ti48Al2Cr2Nb fabri-
cated with three different energy inputs. The total number and volume fraction of
defects decreased with the increase of energy input. Large defects were more preva-
lent in the samples produced with low energy density, indicating a lack-of-fusion
between layers.
The as-build EBM TiAl material exhibited a fine-grained equiaxed γ microstruc-
ture and this microstructure was due to the small melt pool and the rapid cooling.
Based on the XRD 2θ scan, Murr et al. [78] and Mohammad et al. [77] both reported
a higher volume fraction of α2 phase than γ phase in the powder comparing with the
EBM as-build samples. Electron BackScattered Diffraction (EBSD) shows that 90%
of the material is composed of γ phase, and there is no preferred crystalgraphic orien-
tation in this phase. However, the α2 phase exhibited a strong texture (over 12 times
random) with its c axis parallel to the build direction [76].
In the as-build Ti48Al2Cr2Nb [76,79], Ti48Al2Nb0.7Cr0.3Si [80],
and Ti(4748)Al2Cr8Nb [81] alloys, there is a layered microstructure with
large γ bands and fine duplex bands distributed intermittently along the build direc-
tion (Fig. 11.14).
Additive manufacturing of titanium aluminides 251

Figure 11.14 Microstructure of the vertical cross section of at θ 5 0 (A), (D), 45 (B), (E)
and 90 (C), (F). (A)-(C) at low magnification, (D)(F) at high magnification.
Source: Courtesy of M. Todai, T. Nakano, T.Q. Liu, H.Y. Ysuda, K. Hagihara, K. Cho, et al.,
Effect of building direction on the microstructure and tensile properties of
Ti48Al2Cr2Nb alloy additively manufactured by electron beam melting, Add. Manuf.
13 (2017) 6170.

It is suggested by Baudana et al. [80] that the large γ grains were due to local
overheating, the heat diffusion phenomena during the melting of the new powder
layer, and contemporary remelting of a portion of the substrate during the EBM
process. Todai et al. [79] found that the sum of one duplex and one γ band is
approximately 90 μm, which is the thickness of each powder layer. In addition,
with increasing distance from the top surface, the microstructure of the as-build
EBM Ti48Al2Cr2Nb sample varied gradually from full-lamellar, near-
lamellar, to duplex to γ/duplex layers (Fig. 11.15). These different microstructures
were caused by heat-treatment effect of the electron beam and the stored energy in
the material caused by the rapid solidification. During the EBM process, an electron
beam melts the powder layer and part of the layer beneath it. Therefore, the mate-
rial below the melting pool is reheated to different temperatures, depending on the
distance along the build direction. The fully lamellar and nearly lamellar regions
form in the vicinity of the top surface. With the increase of build cycles, the anneal-
ing temperature for the lamellar regions decreases gradually to form the duplex
microstructure. Finally, part of the duplex region subjected to the annealing just
above the eutectoid temperature transforms into γ bands. This is how the periodic γ
bands formed [79].
252 Additive Manufacturing for the Aerospace Industry

Figure 11.15 Schematic illustrations showing the microstructure evolution and the unique
layered microstructure formation during the EBM process. (A) A snapshot during the EBM
process, (B) feed a powder layer, (C) fusion several layers, (D) feed the next layer, and (E)
fusion several layers again. EBM, Electron beam melting.
Source: Courtesy of M. Todai, T. Nakano, T.Q. Liu, H.Y. Ysuda, K. Hagihara, K. Cho, et al.,
Effect of building direction on the microstructure and tensile properties of
Ti48Al2Cr2Nb alloy additively manufactured by electron beam melting, Add. Manuf.
13 (2017) 6170.

With a subsequent heat treatment, the equiaxed microstructure can easily


transform to fully lamellar through all duplex ratios [71,76,79,80] (Fig. 11.16). It
is worthy to notice that the bands of coarse γ grains do not disappear unless the
annealing temperature is above α-transus. These γ grains pin the grain boundary
to avoid the over grow of lamellar grains. Besides, a strong dependence of the
microstructure on process parameters was observed by Schwerdtfeger et al. [70].
It appears that a higher line energy leads to a fully lamellar microstructure,
while only very few lamellar regions can be observed for the sample produced
with lower line energies.
Due to its intrinsic brittleness, TiAl is much more difficult to build by EBM com-
pared with conventional Ti alloys, such as Ti6Al4V. The chamber has to be kept
at B1050 C to minimize cracking. The room temperature tensile strength of the as-
build EBM Ti48Al2Cr2Nb was measured to be 503 6 18 MPa (Table 11.3). A
Additive manufacturing of titanium aluminides 253

Figure 11.16 Microstructure of EBM Ti48Al2Cr2Nb heat-treated to different vol.% of


equiaxed γ phase (A) 90% equiaxed γ, (B) 60% equiaxed γ, (C) 25% equiaxed γ, (D) near
fully lamellar. EBM, Electron beam melting.
Source: Courtesy of GE Avio Aero.

similar tensile strength was also reported by Mohammad [77]. However, the ductility
was essentially 0 due to the defects such as small pores and occasional lack-of-fusion
inside the material [76]. The fracture surface exhibited defects such as unmelted pow-
der and spherical pores [77]. Recently, Todai [79] reported a very high strength for
the as-build EBM TiAl-4822 based on flat tensile samples of 5 mm long and
0.8 3 1.5 mm for the gauge cross section (Table 11.3). The room temperature tensile
strength along the build direction is B640 MPa and the tensile elongation is B0.5%.
The tensile strength 45 and 90 away from the build direction is similar to that of
the build direction, but the average tensile elongations are both above 2%.
Preliminary study on the fracture toughness and fatigue crack growth properties of
EBM TiAl-4822 was also performed [82].
Isolated microcracks are occasionally found in the as-build Ti48Al2Cr2Nb
material, so HIPing is typically performed to remove defects. The average tensile
properties versus temperature of EBM Ti48Al2Cr2Nb heat treated to equiaxed
(HIP at 1200 C), duplex (HIP 1 1260 C/2 h), nearly lamellar (HIP 1 1300 C/2 h),
and fully lamellar (HIP 1 1360 C/2 h) microstructure are shown in Fig. 11.17 [83].
The tensile strength appears to be fairly temperature independent up to 800 C. The
microstructure-property relationship of EBM Ti48Al2Cr2Nb is similar to the
material processed by conventional methods. The RT tensile strength of the HIPped
254

Table 11.3 Room temperature tensile properties of EBM TiAl-4822 along the build (z) direction

Material condition Gauge cross-section size Microstructure type YS, MPa UTS, MPa A, %
As-build (AVIC MTI) Cylindrical (Φ5 mm) Equiaxed  503 6 18 0
As-build (Osaka Univ.) [79] Flat (0.8 3 1.5 mm) Equiaxed B605 B640 B0.5
1200 C HIP (AVIC MTI) Cylindrical (Φ5 mm) Equiaxed 467 6 15 501 6 25 1.3 6 0.7
1260 C HIP (GE Avio) [71] Cylindrical (Φ8 mm) Equiaxed B375 B430 B1.2
HIP 1 1260 C/2 h (AVIC MTI) Cylindrical (Φ5 mm) Duplex 382 6 11 474 6 23 1.3 6 0.3
HIP 1 1300 C/2 h (AVIC MTI) Cylindrical (Φ5 mm) Near lamella 377 6 10 441 6 9 1 6 0.2
HIP 1 1360 C/2 h (AVIC MTI) Cylindrical (Φ5 mm) Fully lamella 373 6 13 429 6 26 0.8 6 0.2

EBM, Electron beam melting.


Additive manufacturing of titanium aluminides 255

600 15

500

Elongation, %
10
UTS, MPa

400

300

200 5

100

0 0
0 200 400 600 800
Temperature, ºC
Equiax Duplex NearL FullL
Equiax Duplex NearL FullL

Figure 11.17 Tensile properties versus temperature of EBM Ti48Al2Cr2Nb with


different microstructure. EBM, Electron beam melting.

Table 11.4 Creep properties of EBM Ti48Al2Nb0.7Cr0.3Si with near lamellar


microstructure [80]

Creep stress, Final creep Rupture LarsonMiller


MPa strain, % time, h parameter
200 5.72 372 24.22
300 8.32 23.7 22.93
EBM, Electron beam melting.

material is equivalent to the as-build material, but the ductility increased from 0%
to 1.3% due to the closing of pores and microcracks inside the material.
The duplex microstructure exhibited a lower strength but the ductility improved
a little. Biamino et al. [71] also reported similar properties for the EBM
Ti48Al2Cr2Nb heat treated to 40% of lamella phase. When the volume fraction
of lamella phase increases further, the tensile strength and ductility both decrease. The
tensile properties of fully lamellar material are close to Ti48Al2Cr2Nb castings
with similar grain size. When tensile tests were performed on samples aged at 650 C
in air for 10 hours, there was an evident loss of ductility at room temperature, but the
loss diminished with the increase of temperature [71]. This surface oxidation induced
phenomenon is the same as in the TiAl processed by conventional methods.
Tensile properties of other EBM TiAl are only available for the
Ti48Al2Nb0.7Cr0.3Si heat treated (1360 C/2 h) to nearly lamellar micro-
structure. The UTS and elongation are 336 6 26 MPa/0.27 6 0.1 % at room temper-
ature, and 426 6 22 MPa/1.96 6 0.5 % at 800 C, respectively. The creep properties
were also reported (Table 11.4).
256 Additive Manufacturing for the Aerospace Industry

Figure 11.18 Fatigue crack initiated from a ceramic particle (circled in the figure) in an
EBM Ti48Al2Cr2Nb. EBM, Electron beam melting.

The fatigue data of EBM TiAl are very limited in open literature. A Haigh dia-
gram shows that the EBM TiAl-4822 outperforms its casting counterpart at various
temperature/stress conditions [84]. The fatigue crack growth threshold was mea-
sured to be 6.136.7 MPa m1/2, which is more than 30% higher than the value in
GE’s reference data. The material with equiaxed microstructure (HIPed at 1200 C)
exhibited a room-temperature fatigue limit of 450 MPa [83]. This is a very high
value for the TiAl-4822 alloy, but there is a very large life scatter at higher stress
levels. On the fracture surface of many samples, the fatigue cracks were found to
initiate from tiny ceramic particles (oxides of Al and Si) (Fig. 11.18), which is
likely the crucible debris mixed up during the gas atomization process. No other
types of defects were found to be the crack initiation sites. For a material with low
ductility like TiAl, defects control the mechanical properties and microstructure is
secondary. Therefore, understanding the defect tolerance and defect management is
critical for parts produced by AM.

11.7 Summary and prospects


The general challenges or issues of AM also apply to TiAl alloys. This section
attempts to identify some specific challenges and opportunities that affect the future
of TiAl AM. Some of these factors are related to market size and cost, but these
factors are every bit as important to the acceptance of new production methods as
the technology itself.
Among the three AM methods mentioned above, EBM has the highest technical
readiness level. Because of the low substrate temperature and high cooling rate, it
seems that LMD and SLM are not suitable for the production of TiAl end-use parts,
but LMD may find use in niche applications, such as blade tipping. EBM has shown
Additive manufacturing of titanium aluminides 257

the potential to make TiAl materials with good mechanical properties, and GE
Aviation has committed to the production of TiAl turbine blades for the GEnx engine
using this method [85]. However, TiAl has reduced tolerance for flaws, and hence a
greater sensitivity to chemical, microstructural, manufacturing, and service disconti-
nuities. The evaporation and uneven distribution of Al after AM will also create
instability of mechanical properties. This is why AM process control is more impor-
tant when making TiAl components. A high fidelity model that is independent of
geometry and size should be developed to set up a fixed practice. In addition, compo-
nent design and lifing methodologies for AM TiAl need to be developed. At the
implementation stage, no unforeseen technical problems concerning the AM proces-
sing or component behavior, which may be very costly to remedy, should arise.
In the present competitive aerospace market, component cost is the primary
driver for adoption. TiAl alloys have found limited, but very challenging commer-
cial applications in the aerospace industry. The much smaller production volumes
of TiAl powder are disruptive to the shop floor and procedures, which keeps the
powder price at a high level and makes quality consistency between batches
difficult. Each new material or processing requires millions of dollars to develop,
mature, and qualify. Because casting is able to cover most of the TiAl market appli-
cations, the niche has been filled adequately and is difficult to displace. There is
inadequate reason to develop new processing routes on the basis of known alloys
unless there is a performance boost or a clear cost reduction opportunity.
Influenced by “thought inertia,” the LPT blade is considered the first AM TiAl

Figure 11.19 EBM Ti48Al2Cr2Nb honeycomb made at AVIC MTI. EBM, Electron
beam melting.
258 Additive Manufacturing for the Aerospace Industry

component that can be commercialized. The machining of TiAl is very difficult and
expensive. Therefore, considering the current ownership cost of an AM equipment
(B$800,000/set and additional maintenance fee per year), feedstock price (B$400/
kg), and production rate (B10 h/blade), the AM TiAl blade has to be much closer
to “net shape” than the casted blade in order to justify the cost.
The complexity of part geometry is critical in determining the point at which
AM becomes an economically viable production pathway. Actually, the shape-
making capability of AM has not been fully utilized for the TiAl components. For
example, NASA’s reusable launch vehicle program selected TiAl honeycomb as
the primary thermal protection system for the leeward side of the VentureStar [86].
The sheet forming and joining process of making these honeycombs are very
expensive but can be readily replaced by EBM AM (Fig. 11.19). TiAl honeycomb
panels can also be used in hot ducts and doors in jet engines. Hollow or even lattice
structures can be a future direction for the TiAl AM.

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Further reading
M.H. Loretto, D. Horspool, R. Botten, D. Hu, Y.G. Li, D. Srivastava, et al., Controlling the
properties of some ordered Ti-based alloys, Mater. Sci. Eng. A 329-331 (2002) 16.
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Aerospace applications of the SLM
process of functional and 12
functional graded metal matrix
composites based on NiCr
superalloys
Shishkovsky Igor
Center for Design, Manufacturing and Materials, Skolkovo Institute of Science and
Technology, Moscow, Russia

12.1 Introduction
Increasing requirements for the machine details operating under aggressive environ-
mental conditions—ultrahigh or ultralow temperatures and/or pressures encourage
the search of new materials and methods for their processing. On the other hand,
the task of reducing weight and cost of these manufacturing materials while pre-
serving their functionality remains relevant. Therefore, the development of metal
matrix composites (MMCs) is an important innovation in the field of materials sci-
ence over the past three decades. Composites made of metal matrix offer a number
of attractive advantages over traditional engineering materials due to their excellent
properties [13].
A huge selection of potentially hardening phases gives new opportunities in
improving mechanical and physical properties of the MMC. The strengthening
inclusions have different morphology (e.g., long or short fibers, particles) and size
(micro- or nanosize) [3,4]. The inclusions can also be combined in a hybrid com-
posite [1,5,6]. The most widely used inclusions are carbides of chromium (CrxCy)
[79], titanium (TiC) [1012], tungsten (WC) [1319], and silicon (SiC)
[2023]. Their high hardness makes them a good choice for increasing the wear
resistance of MMC. Other popular types of inclusions are oxides, borides, or
nitrides [2431] also provide satisfactory hardening, as well as intermetallides
[3237]. Composites with reinforcing particles in a metal matrix have received a
worthy interest among all the mentioned possibilities because of their excellent
properties and low production costs.
MMC hardened by solid inclusions are known to belong to the category of the
so-called hard alloys or cermets if the volume content of the solid phase exceeds
50% [1,38]. With such a solid content, solid alloys usually cannot form a homoge-
neous and single-phase melt congruent in chemical composition, which makes the
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00014-5
© 2019 Elsevier Inc. All rights reserved.
266 Additive Manufacturing for the Aerospace Industry

casting technology inapplicable to the cermets. Solid alloys are traditionally pro-
duced by methods of powder metallurgy, and products are limited to the simplest
shapes [39,40]. Particles of the powder bind together as the temperature rises
through the liquid-phase sintering mechanism. In contrast to hard alloys, the so-
called dispersion-hardened alloys (DHA) contain no more than a dozen volume per-
cents of the solid phase, and casting methods are already applicable to them. In this
chapter, attention is paid to the region of transition from the cermets to the DHA by
percentage content of reinforcing inclusions in MMC.
In powder metallurgy, MMCs are usually prepared in ball mills to achieve uni-
form mixing and grinding (including the use of mechanical activation or even
microspinning of particles). The plasticizers are added to the powder mixtures and
molded by pressing methods, injection molding, then the preforms are kept in fur-
naces at temperatures above the melting point of the low melting phase of the
MMC. Thus, in order to create the actual 3D parts, additional substrate processing
methods (milling, cutting, etc.) are required.
The heat resistance of the MMC is largely determined by the metal matrix (in
our case, the alloys were nickel-based) and presence of deoxidizers. High-
temperature strength is the result of the fastening of dislocations, and is achieved
by doping and proper dispersion hardening. Reduction of grain size and use of
nanostructure additives is not less promising for improving the mechanical proper-
ties of the MMC. Prior to the development of additive technologies (AT) by com-
paction methods that did not lead to grain growth, plasma-spark sintering, high-
frequency induction heating, hot isostatic pressing (HIP), pulsed magnetic compac-
tion, and self-propagated high-temperature synthesis were considered [41].
Thus, nanoscale inclusions play an important role in improving the physical and
mechanical properties that can be achieved by adding small-volume fractions
(#2%), whereas for micron particles reinforcing the metal matrix, the composites
contain larger volume fractions ( . 10%) which are significant [42]. However, a
considerable increase of the hardening inclusions concentration can lead to degrada-
tion of the MMC properties due to possible agglomeration and clustering of inclu-
sions and/or microporosity development in nanocomposites. Therefore, at the
present time, there has been a significant growth of interest for manufacturing of
nanocomposites in a metal matrix, when nanoparticles are included in the base
matrix [43]. It should be mentioned that, compared to the composites with micron-
sized reinforcing inclusions, nanocomposites exhibit comparable or even better
mechanical properties using fewer inclusions [44].

12.2 Metal matrix composites fabrication via additive


technologies
When it comes to the use of the MMC in products, powder AT demonstrate a con-
siderable potential. Among the methods of the powdered AT, the following should
be distinguished: [45] (1) the processes of a laser deposition of powders in which
the laser beam is coaxial with the powder(s) flow and is used to melt the powder
Aerospace applications of the SLM process 267

mixture when it delivers the substrate; (2) approaches where a focused (laser or e-
beam) energy source is used to melt the locally selected zones of the powder layer
predistributed on the base platform. The first category is called direct energy depo-
sition (DED) processes and includes processes known as the 3D laser cladding
(LC), laser engineered net shaping, or direct metal deposition (DMD) technologies
[41,45]. At the same time, the LC can be used as a method of restoring the worn
surfaces of machine parts. The selective laser melting (SLM), laser beam
manufacturing, or selective electron beam melting are examples of the second AT
group, which has name of powder bed fusing (PBF) process [3,41,45,46].
In practical implementation, in the laser melting processes of the powder layer,
the two components of the composite material (i.e., the matrix and reinforcing addi-
tives) are required to be mixed prior to their distribution along the platform in the
powder layer [41,45]. On the other hand, in the DMD505 (Trumpf Co), it is possi-
ble to feed up to 4 powders in one bundle simultaneously from separate hoppers
without preliminary mixing [41]. This option seems to be optimal because it allows
avoiding any segregation of the mixture constituents due to differences in the densi-
ties of the powders, which can spoil the accurate control of the MMC [32,41]. It
also gives a possibility of gradual change of the matrix and reinforcing powders
ratio during layered cladding to make functionally graded materials (FGM) and 3D
parts based on them [21,32,35,37,47].
Another point to consider is that the LC of premixed powders is favorable in
cases of applying a composite layer on a substrate with very high reflectivity [32].
It also should be mentioned that while a huge number of studies on MMC
manufacturing using the DED processes have focused on the methods of powder
feeding, there are some studies in the field of hybrid ATs where the combination of
a wire material with the supply of an alloying and/or hardening powder of ceramics
[4850] is used.
Materials science aspects of the MMC manufacturing, reinforced by the ceramic
particles in the AT should include analysis of the following processes. The absorp-
tion capacity of laser radiation by ceramic particles can substantially differ from the
absorptance of the matrix powder, which affects the character of the energy transfer
from the laser to the MMC when the 3D part is formed [20,32,47]. Under interac-
tion of laser beam with ceramic particles, the hardening particles can melt or decay
[2427]. Consequently, it may be important to regulate the parameters of the laser
treatment carefully, depending on the volume content of ceramic particles under the
FGM and tools manufacture [32,47]. At times, ceramic particles can partially dis-
solve in the melt [8,24,29,32], and the dissolution process itself is generally deter-
mined by the phase diagram in the matrix-ceramic system, and there are examples
for which the dissolution of hardening particles in the melt bath stays at the low
level [29,32]. Then, new phases can develop from secondary precipitation of these
particles within the metallic matrix during crystallization. Because of the ultrafast
thermal heatingcooling cycles, usually realized with the AT, these new phases
can turn out to be metastable, to exhibit the properties of ultrafine structures, which
leads to increased solidity and endurance [20,24]. The strengthening phase can be
synthesized in MMC in situ by interphase reactions, dissolution, and secondary pre-
cipitation. In this case, the laser energy is not only used for the melting of powder
268 Additive Manufacturing for the Aerospace Industry

mixtures, but also for overcoming the energy barrier of the reaction activation and
the formation of novel chemical compounds [20,32,41,46]. In any case, both in ex
situ and in situ MMC creation, a precise control of the AT processes is necessary to
ensure fabrication of MMC with improved properties.

12.3 Metal matrix composites on the nickel alloy based


Tungsten carbides are by far the most vastly applied ceramic hardening inclusions
in Ni-based MMC. The WC has lower reactivity in Ni-based alloys [51].
Consequently, Ni is occasionally used to coat W ceramic powder particles before
using them as reinforcing inclusion to decelerate the dissolution of ceramic particles
[5155] and to diminish their ability to absorb the laser to that of the matrix. Low
reactivity of the WC with Ni-based alloys makes it quite simple to regulate the dis-
solution rate of the particles in the composites by optimizing the parameters of the
process (e.g., changing the scan velocity or power of the laser beam) [52,53].
In the literature, the WC partial dissolution into Ni alloys is reported, which
leads to the precipitation of secondary tungsten carbides of various stoichiometry
(secondary WxC), and mixed carbides (MxCy) [51]. In the NiW system, interme-
tallic phases (NixWy) were also found in NiCrBSi 1 WC compositions under the
high laser power LC and on substrate preheated up to 400 C [53]. The WC rein-
forced MMC have been successfully obtained in a vast range of Ni-based alloys:
NiCrBSi alloys [5254] or NiCo band [55].
Adding chromium carbide (Cr3C2) in the Inconel 625 alloy provides satisfying
outcome in terms of endurance because of partial dissolution of this carbide in the
MMC and the liberation of small carbides, which were at the same time enriched
with Cr [8]. Titanium carbides (TiC) also show great promise as hardening addi-
tives in Inconel 625 [5658] and Inconel 690 [12]. Minimal dissolution of TiC was
observed in a study [12] and very low dissolution of TiC was shown, so that a car-
bide having fine dendrite structure could form.
Other reinforcing inclusions suitable for use in Ni-based MMC include titanium
diboride (TiB2) and rare earth metal oxides, like CeO2 or Y2O3 nanoparticles
[27,55,59], are also applicable for Ni-based MMC. The oxide nanoparticles were
considered very effective in purifying the microstructure and ameliorating the cor-
rosive resistance of the composites.
Thus, a large amount of studies [5,7,8,11,1619,6062] are devoted to the LC
of the MMC on the basis of nickel alloys, including ceramic additives (TiC, WC,
Cr2C3, Mo) on the surface of steels to restore their operability. Those applied pro-
blems of meaningful improvement of physic-mechanical properties of nickel alloys
worn surfaces were the main focus. There are a number of studies specifically on
the layerwise SLM and/or 3D LC (PBFDED processes) of nickel superalloys
[10,1315,6365]. However, in these works, the question of producing the
functional-gradient (FG) structures and/or parts is not being discussed, which is the
main goal of this chapter. We should also pay attention to the numerical studies
Aerospace applications of the SLM process 269

[66,67], which contains the calculation of the metal crystallization after the
PBFDED processes and resonates with our model and numerical approaches [68].
Of interest are the papers [69,70] that set out some of our approaches to creation of
the FG parts from the MMC.
It should also be noted that the SLM technology, especially in conjunction with
the combinatorial approach developed in recent years [7174], can immediately
solve many problems of the MMC manufacturing and treatment that are not pro-
cessed by traditional methods. The SLM is not limited by complexity of the geo-
metric shape of future 3D parts and/or the refractory properties of the material.
High rates of heating and cooling guarantee the production of fine-grained, nano-
scale and/or even nonequilibrium structures with increased strength and wear resis-
tance, which, undoubtedly, should be in demand when developing new transport
and space systems, creating innovative technologies for rocket, aerospace and/or
nuclear equipment of a new generation.

12.4 Methods and materials


In our works, a powder of NiCrBSi alloy was chosen as the nickel superalloy clad-
ding alloy (12%18% Cr, 2.0%4.5% Si, 1.5%3.8% B, ,5% Fe, 0.6%1% C,
0.04% P, 0.04% S, Ni bal.,% by weight, 55 HRC) with a dispersion of 6080 μm.
The following powders were used in the experiments by the SLM and the MMC
synthesis, based on the nickelchromium matrix of the NiCrBSi alloy with harden-
ing inclusions in the following systems: NiCrBSi 1 TiC (5%10%15% by vol-
ume), NiCrBSi 1 TiB2 (5%10%15% by vol.), and NiCrBSi 1 WC (5%10%
15% by vol.). For all systems (NiCrBSi 1 TiC 1 TiB2 or WC), nanosized TiC and
WC particles and submicron TiB2 particles were used. For all systems, the SLM
regimes were tested on a steel substrate, in an argon medium, both without heating
the substrate, and with additional heating up to 300 C. In the experiments, nano
titanium carbide powders—TiC (99 1 %, 4060 nm, cubic), titanium diboride-TiB2
(98 1 %, 212 μm) were used, which were both produced (US Research
Nanomaterials Inc., Houston, United States) and nano tungsten carbide 2 WC
(99 1 %, 5080 nm, hex) produced by Plasmotherm (Moscow, Russia). The distri-
bution of all the aforementioned powders by size was analyzed by means of an opti-
cal granulometer ALPAGA 500NANO (OCCHIO s.a., Belgium).
A unique experimental-technological setup for the PBF process of powder FG
MMCs based on the nickel alloy NiCrBSi matrix was constructed in the Samara
branch of the LPI (Fig. 12.1) and included [32,41]: two lasers on YAG: Nd13
(Kwant-60, radiation wavelength 1.064 μm, power up to 25 W), and ytterbium fiber
laser LK-100-B (radiation wavelength 1.07 μm, power up to 100 W), operating in a
continuous mode independently from each other; own deflectors for each wave-
length for realizing the laser influence (LI) scanning over the powder surface; soft
process management via a personal computer; interchangeable focusing lenses;
mechanism for delivering and leveling several types of powder mixtures
270 Additive Manufacturing for the Aerospace Industry

Figure 12.1 Scheme of the MMC fabrication via the SLM process. SLM, Selective laser
melting; MMC, metal matrix composites.

simultaneously; cylindrical platform moving in the vertical direction, on which a


3D parts are layerwise fabricated; and in situ diagnostics of the SLM process.
The procedure for the FGS creation and gradient 3D parts, based on the MMC
with the NiCrBSi alloy matrix, is shown in Fig. 12.1 and was developed before
[29,32,37].
The following analysis techniques were used in the framework of this study. The
composition and crystal structure of the MMC submicron and nanoscale structures
were determined from X-ray diffraction (XRD) on a DRON-3M diffractometer (Cu
Kα radiation). The phase composition of the samples was determined using the X-
ray database PDF2, 1999 release, and the computer program—SearchMatch ver.
3.010. The quantitative analysis of the diffractograms was carried out using the
Rietveld program PowderCell 2.0.
Morphological studies were carried out on a scanning electron microscope
(SEM) (Carl Zeiss, Germany). Using the attachment for the energy dispersive anal-
ysis (EDX) (Inca Energy 300, Oxford Instruments, United Kingdom), a microele-
ment analysis of the obtained 3D samples was also performed. Electron
microscopic photographs were processed by the SIAMS-600 computer image analy-
sis software.

12.5 Results and discussion


Our studies began with the experimental determination of the optimal SLM regimes
for individual passages of the NiCrBSi alloy, the regime of layer-by-layer synthesis
during scanning with a laser beam along the meander, zigzag, and a meander rota-
tion on 90 on each subsequent layer, and then all the above mentioned techniques
were repeated, but with the platform heated up to Tp 5 300 C.
Fig. 12.2AC shows the appearance of the 3D cubes from the NiCrBSi alloy
after the SLM in argon: (A) the power of the LI changed from 95 to 50 W from the
substrate to the top, but without heating the platform; (B) the regime did not include
Aerospace applications of the SLM process 271

Figure 12.2 Side view of the 3D NiCrBSi nickel alloy cubes. (A) P 5 9550 W; v 5 20 cm/
s. (B) P 5 80 W; v 5 20 cm/s. (C) P 5 80 W; v 5 20 cm/s, Тp 5 300 С.

Figure 12.3 Side view of the gradient 3D cubes from the MMC based on the NiCrBSi
nickel alloy with nano additives (P 5 80 W; v 5 10 cm/s; argon; Tp 5 300 C). (A)
NiCrBSi 1 TiC (51015 vol.%). (B) NiCrBSi 1 TiB2 (51015 vol.%). (C)
NiCrBSi 1 WC (51015 vol.%). MMC, Metal matrix composites.

heating of the platform, the power of LI was constant; (C) the regime included heat-
ing of the platform Tp 5 300 C.
Finally, Fig. 12.3 shows the appearance of gradient 3D cubes from the MMC
based on the nickel alloy NiCrBSi in which the content of the nanoceramic doping
additive from 5% by volume at the base, 10% by volume, increases from platform
to top in the middle and further to 15% by volume, according to the scheme shown
in Fig. 12.1. As noted earlier, in this study we worked with: (1) TiC; (2) TiB2; and
(3) WC nanoceramics.
It is clearly visible that structure of all 3D parts received is far from perfect.
There is a significant porosity and roughness of the fused structure without addi-
tional HIP (result will be presented in a separate contribution), the shape of 3D
parts has significant deviations from the claimed (cube, the base area is
5 3 5 mm2). In the sample of Fig. 12.2B, there is a significant shrinkage (the regime
without heating of the platform). Based on the results of optimizing the SLM
272 Additive Manufacturing for the Aerospace Industry

regimes for nickel superalloys, we concluded that there is no alternative to addi-


tional heating in the SLM chamber up to 500700 C, as it was done us earlier in
Ref. [32].
The results of optical metallography (OM) of cast structures after the SLM in
the materials are shown in Figs. 12.4 and 12.5. Fig. 12.4 shows the microstructures
after the SLM of the NiCrBSi alloy (the upper row—the structure of the middle
layers of 3D products from Fig. 12.2, the lower row—at the bottom). The darker
areas in Fig. 12.4 correspond to the structures obtained by turning by 90 relative to
the previous layers. They were characterized by higher microhardness. In the modes
with base heating (Fig. 12.4C), the structures turned out to be more ordered.
Heating by laser source (at the base—95 W, at the top—50 W, Fig. 12.4A) stabilizes
the structure only to the surface of the sample. Finally, a complete lack of heating
(Fig. 12.4B) gives extremely heterogeneous, but stronger (i.e., high-speed laser hard-
ening) structures. On the average, microhardness of the samples was: (Fig. 12.4A)
345650 HV0.1; (Fig. 12.4B) 365728 HV0.1; (Fig. 12.4C) 409649 HV0.1.
OM of the MMC based on nickel alloy NiCrBSi with nanoceramics are shown
in Fig. 12.5 (upper layers B15%, middle layers B10%, and at the base B5% addi-
tions of the corresponding nanoceramics). FGS in the NiCrBSi 1 TiC system
(Fig. 12.5A) are fairly uniform with “coarsening” to the surface of the 3D sample.
Measurements of microhardness of MMC give an average value of B571 HV0.1
with a variation from 462 (at the base) to 700 (at the surface) HV0.1. In the FGS of
the NiCrBSi 1 TiB2 system (Fig. 12.5B), inclusions of secondary titanium borides
in the lower and middle layers are clearly visible. Apparently, to the 3D surface,
the sample is finally “heated” by the LC, which leads to complete dissolution of the
borides; however, high-speed cooling does not have time to homogenize the FGS.

Figure 12.4 OM after the SLM for the NiCrBSi nickel alloy (AC regimes see in
Fig. 12.2). (A) P 5 9550 W; v 5 20 cm/s. (B) P 5 80 W; v 5 20 cm/s. (C) P 5 80 W;
v 5 20 cm/s, Тp 5 200 С. SLM, Selective laser melting; OM, optical metallography.
Aerospace applications of the SLM process 273

Figure 12.5 OM after the SLM of the MMC, based on nickel alloy NiCrBSi. (A)
NiCrBSi 1 TiC (51015 vol.%). (B) NiCrBSi 1 TiB2 (51015 vol.%). (C)
NiCrBSi 1 WC (51015 vol.%). SLM, Selective laser melting; MMC, metal matrix
composites; OM, optical metallography.

The average microhardness was about 651 HV0.1, with a variation from 425 (at the
base) to 757 (to the surface) HV0.1. Finally, Fig. 12.5C shows the FGS in the
NiCrBSi 1 WC system. We have observed both the large dendrites of the nickel
matrix and the release of chromium carbides (white point inclusions) and the
recrystallized (reduced) WC particles. A similar picture was observed in [53]: aver-
age microhardness in the NiCrBSi 1 WC B513 HV0.1 system with a variation from
355 (at the base) to 728 (to the surface) HV0.1. If we compare these data with the
above given microhardness values of pure NiCrBSi after the SLM, it is obvious that
the creation of a concentration gradient in the MMC gives rise to microhardness.
The main thing about the MMC is that the microhardness really depends on the
concentration of the nano ceramic additive, which means that it can be controlled,
as well as the future properties of the 3D product.
Further, we performed the XRD measurements of the MMC obtained on the
basis of the nickel alloy after the SLM.
274 Additive Manufacturing for the Aerospace Industry

Fig. 12.6 shows the results of qualitative XRD in the MMC based on the
NiCrBSi after the SLM. Below the X axis, the diffractograms of the original pow-
ders are shown without the LI treatment, and above the X axis after the SLM. It
should be noted that even 15% of the addition of nanoceramics is satisfactory with
a slight change in the arrangement and intensity of the peaks in the original
NiCrBSi alloy up to the LI. Everywhere (Fig. 12.6) we fix pure nickel (04-0850,
JCPDS, PCPDFWIN version 2.02 1999), as well as phases—Ni16Cr6Si7 (17-
0332), Cr15.58Fe7.42C6 (78-1502, PDF2) and Ni49Ti14Si37 (29-0942, PDF2).
After the SLM in the MMC with nano titanium carbide (Fig. 12.6A), TiC lines (71-
0298, PDF2) are practically not visible. We have already observed similar patterns
earlier [29,75] in the development of a Ti 1 nano TiC based MMC, when carbon
forms a solid solution with titanium without clear precipitation into the carbide
phase. Now we observe a similar picture not only in the NiCrBSi 1 TiC system, but
also in the MMC based on NiCrBSi 1 WC (Fig. 12.6C). Nano tungsten carbide
apparently also dissolves in the SLM and forms a solid solution; however, the OM

Figure 12.6 The XRD after the SLM in the MMC, based on the NiCrBSi: (A)
NiCrBSi 1 TiC; (B) NiCrBSi 1 TiB2; (C) NiCrBSi 1 WC. SLM, Selective laser melting;
MMC, metal matrix composites; XRD, X-ray diffraction.
Aerospace applications of the SLM process 275

and SEM (Figs. 12.5C and 12.7C) show it fixed in the upper layers. We also
observe the release of chromium carbides—Cr23C6 (85-1281, PDF2) after the LI.
And only in the MMC NiCrBSi 1 TiB2, where there micron particles of TiB2 were
initially larger, titanium borides are clearly visible throughout the 3D volume. The
change in microhardness noted above correlates with the results of XRD.
Fig. 12.7 shows the characteristic images of substructures in the FG MMC based
on the NiCrBSi alloy with a gradient of the concentration of nanoceramics in the
matrix of this nickel superalloy. The upper row of Fig. 12.7 contains the data of the
microelement EDX analysis of the corresponding images. The Fig. 12.7A is an
enlarged photo of OM (see Fig. 12.4A, upper row).
The dendritic structure of the nickel matrix and the submicron particles of the
strengthening phase, TiC, are visible, which was confirmed by EDX data.
Fig. 12.7B is similar to Fig. 12.4B (upper row). The darker micro region in the
photo corresponds to the apparently TiB2 microparticle. SEM in the NiCrBSi 1 WC
system (Fig. 12.7C and Fig. 12.4C, top) shows a multitude of microparticles of
tungsten carbide (see EDX data in Fig. 12.7C). From the still unexplained here, it is
necessary to single out a large amount of oxygen (EDX, Fig. 12.7A) and practically
complete absence of boron (i.e., the NiCrBSi alloy contains up to 3.8 wt% B) in the
nickel glory matrix. Note that boron was not registered with the XRD (see
Fig. 12.6). In general, the substructures of the SEM will repeat the results of the
OM (Fig. 12.4).

Figure 12.7 SEM after the SLM in the MMC, based on nickel alloy NiCrBSi. (A)
NiCrBSi 1 TiC (51015 vol.%). (B) NiCrBSi 1 TiB2 (51015 vol.%). (C)
NiCrBSi 1 WC (51015 vol.%). SLM, Selective laser melting; MMC, metal matrix
composites; SEM, scanning electron microscope.
276 Additive Manufacturing for the Aerospace Industry

12.6 Conclusions
The main goal of the work was to show the principle possibility of creating func-
tional structures for layered SLM in systems: NiCrBSi matrix 1 ceramic additives
(TiC, TiB2, WC). The following results were obtained:
1. optimal regimes of the layer-by-layer SLM in NiCrBSi matrix 1 TiC, WC, and/or TiB2
inclusions in argon medium according to the planned scheme and
2. SEM 1 EDX and XRD data on the structural and phase composition of functional (and
FG) MMC based on the NiCrBSi matrix, microhardness measurements.

Actually, the MMC with nano inclusions were successfully manufactured with
the SLM. However, we recommended a significant increase in temperature (up to
500700 C) in the synthesis chamber to improve the manufacturability and repro-
ducibility of 3D products to avoid the propensity of nanoparticles to agglomeration
and mesoporosity, and also the tendency to cracking. Laser synthesis in situ MMC
is a very interesting alternative, allowing uniform distribution of nanoparticles in
the nickel superalloy matrix.

Acknowledgments
This study was supported by the Russian Foundation of Basis Researches (grants 1429-
10193 ofi-m and 1748-630290 Povolzh’ye_a). The part of study was funded Ministry of
Education and Science of the Russian Federation (RFMEFI58317X0062) and MOST (No.
2017YFE0100100) under the BRICS project.

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manufacturing, Steel Res. Int. (2017). Available from: https://doi.org/10.1002/
srin.201600416.
[75] I. Shishkovsky, V. Scherbakov, Selective laser fusion of titanium based gradient alloy
reinforced by nano sized TiC ceramic, Mater. Sci. Forum. 916 (2018) 8590.
Available from: https://doi.org/10.4028/www.scientific.net/MSF.916.85.

Further reading
X.B. Liu, S.H. Shi, J. Guo, G.Y. Fu, M.D. Wang, Microstructure and wear behavior of
gamma/Al4C3/TiC/CaF2 composite coating on gamma-TiAl intermetalllic alloy pre-
pared by Nd:YAG laser cladding, Appl. Surf. Sci. 255 (2009) 56625668. Available
from: https://doi.org/10.1016/j.apsusc.2008.11.023.
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Surface roughness and fatigue
properties of selective laser 13
melted Ti6Al4V alloy
Zhuoer Chen1,2, Sheng Cao2,3, Xinhua Wu2,4 and Chris H.J. Davies1,2
1
Department of Mechanical and Aerospace Engineering, Monash University, Clayton,
VIC, Australia, 2Monash Centre for Additive Manufacturing (MCAM), Monash University,
Notting Hill, VIC, Australia, 3School of Materials Science and Engineering, University of
Shanghai for Science and Technology, Shanghai, P.R. China, 4Department of Materials
Science and Engineering, Monash University, Clayton, VIC, Australia

13.1 Introduction
Additive manufacturing (AM) of titanium and its alloys is of utmost interest due to
wide industrial applications of titanium alloys and the substantial cost advantages
AM offers over conventional processing methods that require high machining costs
and lead times [1]. Selective laser melting (SLM) process is a powder bed fusion
technology; it uses a focused laser beam to melt consecutive layers of fine metal
powder particles according to the cross-sectional profiles of a 3D computer aided
design to manufacture three-dimensional components. One advantage of the SLM
process is the ability to manufacture geometrically complex structures with high
resolution. However, the surface roughness of SLMed parts remains a drawback of
the SLM process for applications in the aerospace industry where the parts are sub-
ject to fluid flow [2] or cyclic loading [3].
In general, surfaces of different orientations can be classified into horizontal
(top) surfaces, vertical (side) surfaces, upward-facing surfaces (up-skin), and
downward-facing surfaces (down-skin) (refer to Fig. 13.1 for illustration).

13.1.1 Surface roughness of selective laser melted metallic


components
The processing conditions of SLM process has a significant influence on the rough-
ness on horizontal and vertical planes of SLMed metallic parts. The effects of layer
thickness and laser scan speed on the side surface of a one-pass thin wall sample
were explored experimentally [4], a low-speed and a small-layer thickness produced
rough side surface due to excess heat input; on the other hand, surface become
porous when scan speed and layer thickness exceeded a certain value. In another
study of one-pass thin-wall sample [5], the optimum linear energy density
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00015-7
© 2019 Elsevier Inc. All rights reserved.
284 Additive Manufacturing for the Aerospace Industry

Figure 13.1 Schematic drawings of SLM specimens with surfaces of different orientations
to the build platform. For inclined surface ((A) up-skin and (B) down-skin surfaces), an
inclination angle θ is used to describe the orientation. SLM, Selective laser melting.

(laser power divided by scan speed) for top surface did not produce minimum side
surface roughness, while a relatively lower linear energy density is preferred for
side surface in order to minimize attached particles. The Ra value of the top surface
of SLMed cubic samples were found to decrease monotonically with energy density
(laser power divided by the product of hatch distance and layer thickness) for the
experimented processing parameters in [6]. According to a physical model of SLM
process that takes into account Marangoni flow and evaporation in the melt pool,
an optimum linear energy density was determined for minimum top surface rough-
ness while top surfaces made with too low or too high laser energy input were
roughened by Marangoni flow and recoil pressure due to material evaporation,
respectively [7]. In addition to SLM machine parameters, other factors, such as par-
ticle size distribution and part spacing, can also affect surface roughness. A powder
feedstock that is rich in coarse particles and sparse in fine particles results in large
effective layer thickness and low powder layer density during SLM, and conse-
quently produces rough top surface [8]. A finite element thermal analysis [9] pre-
dicts that an increase in the spacing between thin wall parts on the build platform
alleviates the heat accumulation effect, which is related to the less-partially melted
particles attached to the side surfaces.
Up-skin surfaces and down-skin surfaces are both affected by the staircase
effect, which arises from the discrepancy between the stacked 2D layers by layer-
wise deposition process and the original 3D digital design. Additionally, the rough-
ness of up-skin and down-skin are formed by different mechanisms. Both the
transition boundaries between layers and partially melted powder particles attached
to the step edge of each layer contributes to the overall roughness of up-skin
surfaces. As the inclination angle increases, the effect of layer boundaries (staircase
effect) on surface roughness gradually decreases, which results in a lower Ra value
[10,11]. Meanwhile, the coverage of partially melted particles on up-skin surfaces
increase as the inclination angle increases, and becomes the primary cause of sur-
face roughness when inclination angle is close to 90 degrees [11].
Down-skin surfaces are also known as overhanging surfaces since the area
scanned is supported by a powder bed instead of solidified metal of the previous
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 285

deposition layers. The heat transfer from overhanging areas are slower due to lower
effective thermal conductivity of the powder bed. The excessive heat input in over-
hanging areas causes a much larger melt pool to form and extend into the powder
bed by the action of gravity and capillary force [12,13], which results in high sur-
face roughness on down-skin. Another type of defect associated with overhanging
structure is thermal warping due to the thermal stress induced by rapid solidification
and lack of support structure underneath the overhangs to restrict the thermal defor-
mation [14]. The thermal warping effect forms an elevated edge on the SLMed part
that protrudes from the powder bed surface and hampers powder re-coating process.
The warping effect can develop through deposition layers to such an extent that the
building process has to be terminated due to the severe collision between the
elevated edge and the re-coater arm. In this case, a support structure has to be added
to anchor the overhanging structure. The lowest allowable inclination angle for a
downward-facing surface to be made without support structure is around 30 degrees
[13,14].

13.1.2 Post-selective laser melting surface treatment


The surface of additive manufactured parts can be treated with mechanical polish-
ing, electrochemical polishing, chemical etching, and laser polishing. Mechanical
polishing methods, such as milling, polishing, and blasting, have limited accessi-
bility to geometrically complex structures made by AM processes [15]. Chemical
polishing/etching can penetrate into intricate internal structure, such as SLMed
lattice; however it requires careful control of chemical solutions and etching time
to achieve effective reduction in roughness while retaining the desired geometry
of the parts [16]. In particular to chemical etching of Titanium alloys, some con-
tent of hydrofluoric acid is needed, which raises safety concerns and is not
environmentally friendly. Laser polishing/remelting technology is another option
to enhance surface quality of AM parts. A pulsed or continuous wave laser beam
is used to re-melt the surface of additive manufactured parts to improve surface
finish. For SLMed parts, laser remelting must be conducted after the removal of
unfused powder surrounding the fabricated parts [17]. The achievable surface fin-
ish by laser polishing is dependent on the initial topology of the surface [18].
Surfaces of various orientations to the build direction possess different surface
texture, and therefore respond differently to the laser remelting process [19].
Multiple stages of laser polishing with different laser parameters need to be opti-
mized, according to the initial surface topology and material [20]. In summary,
although the aforementioned surface finishing techniques have shown some poten-
tial in reducing the surface roughness of SLMed products, there are limitations to
each of the techniques. It is therefore desirable to minimize surface roughness in
as-built condition through the control of processing conditions so that the neces-
sary post-SLM surface finishing can be avoided or minimized. It is also important
to understand to what extent the surface roughness can affect the performance of
the parts such as fatigue life.
286 Additive Manufacturing for the Aerospace Industry

13.1.3 Fatigue performance of selective laser melted Ti6AL4V


Fatigue performance of SLMed Ti6Al4V is influenced by defects related to the
SLM process, such as surface roughness, residual stress, and porosity. The fatigue
life-limiting effect of these defects overshadows the influence of microstructure
[3,2123].
Surface defects serve as stress concentrators in fatigue testing of Ti6Al4V
alloy made by SLM, which limits the fatigue life of the specimens, especially for
high-cycle fatigue (HCF). Surface finishing treatments can significantly improve
the fatigue life due to the reduction in surface roughness. Wycisk et al. [24]
reported that the polishing of SLMed Ti6Al4V sample reduced the Ra value
from 13 to 0.5 μm and significantly enhanced the fatigue limit from 210 MPa in as-
built condition to 510 MPa in polished condition. A doubled fatigue strength after
surface polishing and machining (Ra B0.2 μm) was also found in [25]. Bagehorn
et al. [15] studied the fatigue performance of SLMed Ti6Al4V specimens after
different mechanical surface treatments, including milling, abrasive blasting, vibra-
tory grinding, and micro-machining; among them, milling achieved the lowest Ra
value (0.3 μm) and the highest fatigue run-out strength at 107 cycles (R 5 0.1). The
scatter in fatigue life observed in samples after different treatments was attributed
the variable remaining surface roughness valleys achieved [15].
The high temperature gradient during SLM process results in high residual stress
in the parts in as-built condition. A tensile residual stress on surface accelerates
fatigue crack initiation during HCF testing [22]. Therefore, a post-SLM stress relief
heat treatment is necessary before the parts are cut off from the build platform.
Further annealing heat treatment or hot isostatic pressing (HIPing) can transform
the fine martensitic microstructure of SLMed Ti6Al4V into α 1 β lamellar
microstructure. The α 1 β lamellar microstructure increases the ductility and delay
crack propagation by introducing plastic deformation in front of the crack [26]. In
addition to microstructural transformation, HIP also closes some internal pores of
SLMed products, which might benefit the fatigue endurance [23,25,26].

13.2 Experimental procedure


13.2.1 Material
The material used in the present study is gas-atomized pre-alloyed Ti6Al4V
alloy powder. The powder was sieved through 65 μm aperture and used as feed-
stock. The powder particles after sieving were spherical in shape. The D10, D50,
and D90 are 16, 30, and 50 μm, respectively.

13.2.2 Selective laser melting of Ti6Al4V specimens


A Concept Laser X-line 1000R machine with a fiber laser of maximum powder of
1 kW was used to fabricate the samples. Laser beam spot was fixed at 100 μm in
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 287

Table 13.1 Three sets of core scan parameters for building samples at three different build
rates

Parameter Layer Laser Scan Hatch Build Relative


set thickness power speed distance rate density
(µm) (W) (mm/s) (mm) (cm3/h) (%)
Performance 50 350 770 0.18 25 99.6
Intermediate 50 750 1925 0.20 69 99.2
Speed 100 1000 1400 0.23 116 98.5

Relative density is measured by Archimedes method.

Figure 13.2 Schematic drawing of contour scan. Solid lines represents zig-zag core scan
vectors; dashed lines represents contour scan, which is shifted outward from the position of
core scan vector closest to the surface (dotted lines).

diameter throughout this study. The build chamber was circulated with Argon gas
to reach an oxygen level less than 1000 ppm before the SLM job was initiated.
Three sets of pre-developed SLM parameters termed as “Performance,”
“Intermediate,” and “Speed” were applied to make the samples [27] (Table 13.1).
“Performance” parameter set was designed for making parts with maximum relative
density; “Speed” parameter set aimed to build parts with highest feasible production
rate; “Intermediate” parameter set was a balance of the former two.
To study the effect of different inclination angle on surface roughness, cuboid
samples with two parallel inclined surfaces to the substrate were fabricated. Each
sample possesses a pair of up-skin and down-skin surfaces with the same θ angle to
the substrate (Fig. 13.1). As a means to improve surface finish and dimensional
accuracy, a contour scan over the edge of the scan area was performed for each
layer after the laser exposure of the core area (Fig. 13.2). Same contour parameters
were applied for “Performance” and “Intermediate” samples because these two
groups shared the same layer thickness (Table 13.2).
288 Additive Manufacturing for the Aerospace Industry

Table 13.2 Contour parameters for samples with three different core scan parameters

Parameter set Laser power Scan speed Contour offset


(W) (mm/s) (mm)
Performance and intermediate 350 770 0.18
Speed 800 1765 0.18

Figure 13.3 Geometry of tension-compression rotating fatigue (R 5 21) sample.

13.2.3 Surface roughness measurements


A Mitutoyo Surftest SJ410 machine was used to conduct the surface roughness
measurements by stylus contact method. The stylus traverse direction was set to be
perpendicular to the layer boundaries for all the measurements. For surface rough-
ness measurement of fatigue samples, three measurements were conducted on each
sample with 120-degree rotation in between.

13.2.4 Postselective laser melting heat treatment of fatigue


samples
For both “Performance” and “Intermediate” fatigue samples, the first stage post-
SLM treatment was stress-relieve heat treatment at 650 C for 1 hour in a vacuum.
The “Performance” samples then went through an annealing treatment at 800 C for
2 hours. After stress-relieve heat treatment, “Intermediate” samples were Hot
Isostatic Pressed (HIPed) at 850 C under 150 MPa Argon gas pressure for 4 hours.

13.2.5 Fatigue testing


A tension-compression rotating fatigue test with a stress ratio R 5 21 was carried
out on a GUNT WP140s tester. Machined samples (Ra ,1 μm) and net-shaped
sample (Ra .7 μm depending on SLM processing parameter) after SLM and post-
SLM treatments were adopted for the fatigue test (Fig. 13.3). Fatigue strength was
determined at the run-out 107 cycles.
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 289

13.3 Results and discussion


13.3.1 Surface roughness
13.3.1.1 Ra versus inclination angle and processing parameters
The Ra values were measured from surfaces with various inclination angle θ are plot-
ted in Fig. 13.4. Based on the staircase effect, the theoretical Ra values can be calcu-
lated, assuming the step edge of each layer is rectilinear (Eq. 13.1). According to this
simplified prediction, the roughness of an inclined surface increases with layer thick-
ness and cosine of inclination angle θ. “Speed” samples were fabricated with a layer
thickness (100 μm) that is two times the layer thickness for “Performance” and
“Intermediate” samples (50 μm). Therefore, the roughness of inclined surface for
“Speed” samples is expected to be higher due to the large layer thickness while dif-
ferences in laser processing parameter also contribute to different roughness.

Layer thickness 3 cosθ


RaðstaircaseÞ 5 (13.1)
4

Figure 13.4 Ra values of surfaces with different inclination angle to the build platform. The
samples were fabricated with different processing parameters. (A) results for “Performance”
and “Intermediate” samples, (B) result for “Speed” samples. The numerical predictions of Ra
values based on staircase effect (according to Eq. 13.1) are presented for comparison.
290 Additive Manufacturing for the Aerospace Industry

It is clear for all groups (“Performance,” “Intermediate,” and “Speed,” with and
without contour) that the experimental data does not agree with the staircase predic-
tion or follow the trend predicted. All the measured Ra values are higher than the
prediction by staircase effect.
Meanwhile, the experimental Ra value is asymmetric about the middle line
(inclination angle 5 90 degrees), which also differs from the staircase effect predic-
tion. Ra values for up-skin surfaces are generally lower than the Ra values for
down-skin surfaces, especially for smaller θ angles.
For “Performance” samples, the up-skin surface roughness does not change sig-
nificantly with inclination angle, but the down-skin surface roughness rises dramati-
cally as the inclination angle departs from 90 degrees. The “Intermediate” and
“Speed” samples share a similar trend. Up-skin surface Ra is lowest at the small
inclination angle (4045 degrees), increases sharply and enters a plateau from mid-
dle range (5060 degrees) to 90 degrees. The down-skin roughness for all groups
increases dramatically as the inclination angle decrease from 60 to 40 degrees.

13.3.1.2 Effect of contour scan on surface texture


In general, the contour scan improves the surface finish of inclined surfaces. The
improvement is not significant for up-skin surfaces but becomes more pronounced
for down-skin surfaces, compared to up-skin surfaces. For all samples without con-
tour scan, Ra value is particularly high on the down-skin with inclination angle
ranging from 40 to 60 degrees.
To understand the effect of contour scan in smoothing the surfaces, we investi-
gate the surface texture of the samples. The scanning electron microscope (SEM)
images in Fig. 13.5, taken from the horizontal surface (top surface) of the samples,
show the difference in scan track instability due to the different core scan para-
meters applied (“Performance,” “Intermediate,” and “Speed”). The top surface of
the “Performance” sample (Fig. 13.5A) features scan track with uniform width and
good wetting between neighboring tracks, and a small amount of unmelted, small,
and spherical particles attach to the top surface. By contrast, the top surfaces of
“Intermediate” and “Speed” samples show highly unstable track morphology, which
was referred to as balling phenomenon in previous studies [28,29]. The remelting/
overlapping between scan tracks is inconsistent and therefore some voids appear
between scan tracks. Apart from small spherical particles (,50 μm), some irregu-
larly shaped particles with larger size also appear on the top surface for
“Intermediate” and “Speed” samples. These particles were ejected from the melt
pool during SLM process as a result of surface tension driven fluid flow and recoil
pressure caused by excessive material vaporization [7,30].
According to the SEM images at the edge of the sample (Fig. 13.5B, D, and F),
the individual scan tracks merge to a wider track as they approach the edge. The
formation of this feature relates to the control of laser beam at the edge of scanned
area by the SLM machine. During SLM, the laser scan vector travels in a zig-zag
pattern over an area designated by 2D profiles of the digital part design, encounter-
ing a turn every time it reaches the edge of the 2D profile (Fig. 13.2). In the
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 291

Figure 13.5 SEM images from top surfaces of “Performance” (A, B), “Intermediate” (C, D),
and “Speed” (E, F) samples. The left column images (A, C, E) were taken from the middle
of the core scan area, while the right column images (B, D, F) were taken from the contour/
core interaction zone.

Concept Laser 1000R machine, the laser beam was kept on while making this turn
at the edge during which the laser beam decelerates, arriving the edge and acceler-
ates leaving the edge. Therefore, the actual heat input close to the edge is higher
than that in the middle of the scan area. The unusually high energy input at the
edges can result in a difference in surface roughness. As the laser power increases
in the order of “Performance,” “Intermediate,” and “Speed” samples, the decelera-
tion of the laser beam at the edge yields a different extent of overheating at the
edge and hence results in different roughness. The outer edge of the contour in
“Performance” sample is straight and free of large attached particles (Fig. 13.5B),
292 Additive Manufacturing for the Aerospace Industry

Figure 13.6 SEM images from vertical surfaces of (A) “Performance,” (B) “Intermediate,”
and (C) “Speed” samples applied with contour scan. Black arrows point to large spatter
particles. White arrows point to surface voids.

while the outer edge of the contour in “Intermediate” sample appears (Fig. 13.5D)
corrugated due to the presence of surface irregularities. The roughness of outer
edge is even higher in the “Speed” sample (Fig. 13.5E).
The roughness at the outer edge of contour translates into the roughness on verti-
cal surfaces (θ 5 90 degrees). In the “Performance” sample, the surface is fully
dense with some semi-melted particles evenly distributed over the surface
(Fig. 13.6A). By comparison, in “Intermediate” and “Speed” samples (Fig. 13.6B
and C), small particles often appear in clusters connected by re-solidified metal;
and spatter particles of diameter B200 μm are present. In addition, large surface
cavities are present in “Intermediate” and “Speed” sample. All of these features fac-
tor into the overall roughness.
To make a qualitative analysis of the effect of contour scan on inclined surfaces,
the “Performance” samples are selected for further study on inclined surfaces as the
“Performance” group are not complicated by the presence of spatters and severe
melt pool instabilities.
For up-skin at 40-degree inclination angle, the application of contour scan
slightly increased the Ra value from 13 to 19 μm, which is not as expected. For the
sample without contour, the semi-circular features formed by the laser turning
points (Figs. 13.7A and 13.9A) are closely packed on up-skin surface, which
appears as small steps at cross section (Fig. 13.7C). For the sample with contour
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 293

Figure 13.7 SEM images and cross-sectional optical micrographs of 40-degree up-skin
surface sample made by “Performance” parameters. Parts (A) and (C) are from sample
without contour, (B) and (D) are from sample with contour.

scan, the up-skin surface shows regularly spaced layer boundaries and semi-melted
particles preferentially located at the layer boundaries (Fig. 13.7B). Judging from
the cross section of contour scanned up-skin (Fig. 13.7D), the contour scan merges
several layers together and forms a periodic surface fluctuation with larger
wavelength.
For down-skin at 40-degree inclination angle, some vertically connected peaks
and grooves emerge on surfaces of the samples with no contour (Figs. 13.11A and
13.12C). This is also a result of high energy input at laser beam turning points.
However, during the SLM process, the melt pool at down-skin is surrounded by
powder bed, whose heat conductivity is significantly lower. The combination of
high local energy input and slow heat dissipation from the laser beam turning points
at down-skin causes significant local overheating, thereby forming a larger melt
pool that extends into the powder bed to form the dross materials on down-skin
(Fig. 13.8A). The melt pool extension is also evident from the cross section
(Fig. 13.8B). When a contour scan was applied, the materials between peaks and
valleys are redistributed (Fig. 13.8C) and the melt pool extension is less significant
(Fig. 13.8D).

13.3.2 Fatigue properties


Fatigue tests were carried out to “Performance” and “Intermediate” samples after
post-SLM heat treatments. Since the “Intermediate” samples possess a moderate
294 Additive Manufacturing for the Aerospace Industry

Figure 13.8 SEM images and cross-sectional optical micrographs of 40-degree down-skin
surface sample made by “Performance” parameters. Parts (A) and (C) are from sample
without contour, (B) and (D) are from sample with contour.

Figure 13.9 Backscattered electron images of (A) “Performance” sample after stress-relieve
and annealing heat treatment and (B) “Intermediate” sample after stress relieve and HIPing.

level of porosity, a HIPing treatment were carried out to close up the remaining
pores. After post-SLM heat treatments, α 1 β two-phase lamellar microstructure
were obtained in both “Performance” and “Intermediate” samples (Fig. 13.9).
To assess the effect of surface roughness on fatigue performance of SLMed
Ti6Al4V, two pairs of comparisons are made. The first comparison is between
the un-machined (as-built surface condition) samples made with “Performance” and
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 295

Figure 13.10 Fatigue properties of SLMed Ti6Al4V alloy samples. Data points with a
black arrows means the fatigue tests were interrupted since a 107 cycle fatigue life has been
reached. SLM, Selective laser melting.

“Intermediate” parameters, which exhibit different roughness on vertical surfaces


(Fig. 13.6). The Ra values, measured from fatigue samples, are in the range of
720 μm for “Performance” group, 2030 μm for “Intermediate” group. With un-
machined surface condition, “Performance” samples in general have longer fatigue
life than “Intermediate” samples (Fig. 13.10). None of the “Intermediate” samples
reached a fatigue life higher than 105 cycles, even under stress of 200 MPa, while
half “Performance” samples in the maximum stress range of 250350 MPa sur-
passed 105 cycles in fatigue life. For both “Performance” and “Intermediate” sam-
ples in as-built surface condition, crack initiated from the surfaces. However, the
crack initiation site at “Performance” is isolated (Fig. 13.11), while in the
“Intermediate” sample, multiple fatigue crack initiation sites from surface defects
that are connected to one another (Fig. 13.12). Some unmelted powder particles are
found at the crack initiation site (Fig. 13.12C), suggesting that the pores connected
to the free surface in “Intermediate” samples were not closed by HIPing.
The second comparison is made between un-machined samples and machined
samples. The Ra values of the machined surfaces fall in the range of 0.51 μm.
The fatigue performance of machined samples for both “Performance” and
“Intermediate” groups was improved compared to their un-machined counterparts.
Unlike the un-machined samples whose fatigue crack initiated from surfaces, the
machined samples exhibit fatigue cracks initiated from the interior defects
(Fig. 13.13).
296 Additive Manufacturing for the Aerospace Industry

Figure 13.11 Fracture surface of an un-machined fatigue sample applied with


“Performance” machine parameters. (B) is an enlarged image of the circled areas in (A).

Figure 13.12 Fracture surface of an un-machined fatigue sample applied with


“Intermediate” machine parameters. Parts (B) and (C) are enlarged images of the circled
areas in (A).
Surface roughness and fatigue properties of selective laser melted Ti6Al4V alloy 297

Figure 13.13 Fracture surface of a machined fatigue sample applied with “Intermediate”
machine parameters. Parts (B) and (C) are enlarged images of the circled areas in (A).

13.4 Conclusions
Surface roughness of SLMed Ti6Al4V strongly depends on the orientation of
surface to the build platform. The laser processing parameters developed for achiev-
ing high relative density does not always yield lowest overall surface roughness.
Application of a contour scan with appropriate selection of parameters generally
improves surface finish. The machine-specific control of laser scan path at the edge
of the profile can generate specific surface texture, which might not be
repeatable for other machine systems. A fundamental understanding of the forma-
tion of various surface features, such as the amount and distribution of attached par-
ticles, inter-layer wetting on inclined surfaces, melt pool extension in overhanging
areas (down-skin) is needed for minimization of surface roughness of SLMed
components.
Surface roughness is the most dominant fatigue life-limiting factor for SLMed
Ti6Al4V alloy samples. This is not only confirmed by the improvement in
fatigue life after surface machining, but also evident in the different fatigue perfor-
mance of samples with different as-built surface condition (“Performance” and
298 Additive Manufacturing for the Aerospace Industry

“Intermediate”). This also justifies the need for SLM process optimization and con-
trol to minimize as-built surface roughness.

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Aluminum alloys for selective
laser melting  towards improved 14
performance
Paul Rometsch1,2,3, Qingbo Jia1,2, Kun V. Yang1,2,4 and Xinhua Wu1,2
1
Department of Materials Science and Engineering, Monash University, Clayton, VIC,
Australia, 2Monash Centre for Additive Manufacturing (MCAM), Monash University,
Notting Hill, VIC, Australia, 3Rio Tinto Arvida Research and Development Centre,
Jonquière, QC, Canada, 4CSIRO Manufacturing, Clayton, VIC, Australia

14.1 Introduction
Additive manufacturing (AM) of metallic materials has attracted growing interest
since its invention and has developed rapidly with the evolution of advanced laser
technology and mechanical control systems [1]. In recent years, AM of metal parts
has transitioned from prototype design to the fabrication of real parts for industrial
applications. Various fields, including aerospace, automotive, marine, and medical
industries have witnessed the benefits offered by AM technologies [2]. A typical
example is that general electric (GE) has successfully printed an aircraft fuel nozzle
that passed certification in 2015 [3]. By utilizing the advantages of AM technolo-
gies, the complex nozzle structures, which would normally require the assembly of
more than 20 traditionally manufactured parts, have now been re-designed for a sin-
gle selective laser melting (SLM) operation that resulted in a further 25% weight
reduction. Such AM processes also provide benefits of high material utilization and
short lead times for both new product development and real applications. The AM
technologies are now especially attractive for high value bespoke components with
complex geometries and short production runs, as in the aerospace sector.
The energy source for AM is normally a laser beam, electron beam, or electric
arc, and feedstock types include metal powder or wire. This contribution will focus
on powder-based laser AM, which is the most common type of AM for making net-
shape aluminum alloy components. More specifically, the focus herein is on SLM,
also known as powder bed fusion. So far, SLM has been applied to various metal
material systems, including Ti-based materials (commercial purity Ti, Ti6Al4V, Ti-
5533 [46]), Fe-based materials (304 stainless steel, maraging steel, tool steels
[79]), Al-based materials (AlSi10Mg, AlSi12, AlSi7Mg [10]), Ni-based materials
(IN 718, Hastelloy X [11]), and Co-based materials (CoCrMo [12]).
Among all the AM technologies, SLM has been regarded as the most promising
process for fabricating engineering components. The size of the components is lim-
ited mainly by the size of the powder bed in the machine, but the machines are
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00016-9
© 2019 Elsevier Inc. All rights reserved.
302 Additive Manufacturing for the Aerospace Industry

evolving rapidly. Due to the rapid powder melting and solidification characteristics
of the SLM process, very high cooling rates up to B105106K/s can be achieved
within a single molten pool [13]. One may therefore view SLM as a form of rapid
solidification casting or welding with countless re-melting and heat affected zones
(HAZs) between adjacent scan tracks and successive build layers. The non-
equilibrium nature of the SLM process endows the fabricated parts with very fine
microstructures and properties that are comparable to or even better than those of
traditional cast or wrought products, depending on the degree to which alloys are
designed to capture the benefits of the SLM process.
Due to the significant design freedom, manufacturing flexibility, and concomi-
tant light-weighting opportunities offered by the SLM process, there is now a grow-
ing demand for critical lightweight components to be built in this manner, such as
high performance Al alloy components for aerospace applications. However, the
most widely used Al alloys for SLM are still based on the AlSi eutectic system
(i.e., AlSi7Mg, AlSi10Mg, AlSi12) due to their good castability and weldability
[10,14]. These alloys have been borrowed from the casting industry and typically
achieve mechanical properties that are not much better than those of their cast
counterparts, though significant variations may occur depending on SLM process
parameters, building orientation, and post-heat-treatment parameters.
On the other hand, attempts at adapting high strength Al alloys, such as the 2xxx
and 7xxx series wrought alloys that are commonly used in aerospace applications,
to SLM have often resulted in cracking since such alloys are less castable and more
prone to hot tearing during the building process [14,15]. By contrast, some alloys
with rare earth (RE) and/or transition metal (TM) element additions appear to hold
more promise for achieving better performance in terms of tensile properties and
thermal resistance [16].
There is now widespread interest to increase the number of Al alloys that can be
produced by SLM and to improve their mechanical properties both in terms of
absolute values and consistency. There is also a growing realization within the
industry, including at the Aluminum Association, that Al alloy composition, temper,
and property specifications cannot simply be borrowed from existing cast or
wrought product designations but should be tailored specifically to SLM. This con-
tribution will focus on what has been done and what further opportunities exist with
respect to Al alloy and process design to meet the growing demand for higher per-
forming Al alloy components made by SLM.

14.2 Processingmicrostructureproperty
considerations for current alloys in selective laser
melting
Among all the material systems used for SLM, Al alloys are regarded as one of the
more challenging materials due to their high reflectivity, thermal conductivity, and
oxidation susceptibility. As mentioned above, the currently applied Al alloys for
Aluminum alloys for selective laser melting  towards improved performance 303

SLM are still mainly based around the near-eutectic AlSi casting alloys, that is,
AlSi7Mg, AlSi10Mg, and AlSi12. By carefully adjusting the process parameters,
such as laser power (P), scanning speed (v), layer thickness (t), hatch distance (h),
and scan strategy, a wide range of components can be fabricated very successfully
from these alloys with more than 99.5% relative density.
Porosity issues have been widely investigated for SLM fabricated Al alloys, and
it is now commonly accepted that porosity levels below 0.5% can be regarded as
acceptable for most applications.
However, if the processing parameters are poorly controlled, various defects
may occur, such as irregularly shaped pores due to insufficient melting at low
energy densities, small round gas pores due to moisture, and large round pores asso-
ciated with the keyhole effect in deep V-shaped melt-pools at high laser power
levels [17]. Many studies report on how processing parameters, especially the
applied volumetric energy density (VED 5 P/vth), may be optimized to minimize
porosity [1823]. Gas pores due to moisture, also called hydrogen pores, tend to be
smaller than the other types of pores, but may be enlarged significantly during sub-
sequent solution heat treatment. Such porosity can be reduced by pre-drying the
powders to remove moisture from the Al oxide/hydroxide on the powder surface
[17,24,25].
Spatter and smoke formed as by-products during laser-material interaction may
also influence the densification and the final mechanical properties of SLM-
fabricated parts [26]. Adjusting the gas flow velocity, the direction of the laser scan
with respect to gas flow and the part placement on the build platform can signifi-
cantly reduce accumulated spatter and smoke particles. Studies on the processing
atmosphere in the chamber showed that no obvious difference could be found
between argon and nitrogen, but that helium tends to give more porosity [27].
Processing parameters and build design characteristics also play an important role
in determining the surface roughness, which may be considered as a defect in some
applications, such as those requiring smooth surfaces for enhanced fatigue perfor-
mance, tight tolerances, mating surfaces, friction, fluid flow, corrosion resistance,
or esthetic appeal.
Since it is well known that appreciable quantities of porosity-related defects will
influence the properties, especially the ductility, ultimate tensile strength, conduc-
tivity, and fatigue performance, it is taken for granted herein that a quest toward
improved performance for any alloy must start with process optimizations to mini-
mize porosity-related defects. It has, for example, been demonstrated that while the
fatigue performance of AlSi7Mg made by SLM is broadly similar to that of its cast
counterparts, the fatigue performance is clearly deteriorated by a rough surface and
sub-surface porosity [17]. The principles of such defect formation as outlined above
are similar for all Al alloys and will therefore not be elaborated on here. Similarly,
the powder characteristics also play an important role in determining the final prop-
erties of SLM-fabricated parts, but this will not be discussed much further in this
contribution. From a processing perspective, it is important to achieve good powder
spreading and packing in each layer of the powder bed, which is influenced by
304 Additive Manufacturing for the Aerospace Industry

factors such as the particle size distribution, packing density, flowability, and how
spherical the powder particles are.
Furthermore, since the SLM process is based on layer-by-layer building princi-
ples, most of the heat generated during SLM will be conducted downward toward
the solid metal substrate (rather than into the surrounding powder or atmosphere),
which triggers columnar grain growth in the build direction with epitaxial grain
growth from layer to layer. Along with the layer-wise build nature of the SLM pro-
cess, this results in some mechanical property anisotropy in fabricated Al alloy
parts, which can be reduced or eliminated if the alloy and process have been
designed to promote fine equiaxed grains instead of the commonly occurring large
columnar grains. Such grain refinement also helps to avoid hot tearing, where
cracks grow preferentially along grain boundaries between the large columnar
grains oriented in the build direction.
Due to the very high cooling rates in the SLM manufacturing process, unique
metastable microstructures can be achieved in the fabricated parts, but these are
easily transformed toward an equilibrium state if high temperature post heat treat-
ments are carried out. For industrial production, it is normally essential to carry out
at least a stress relieving heat treatment after SLM to reduce the risk of distortion
or cracking. For some alloys, the post heat treatment may include various combina-
tions of hot isostatic pressing (HIP), solution heat treatment, quenching, and/or
aging to achieve the desired mechanical properties. It is important to note that post
heat treatments are an important consideration when choosing an Al alloy for SLM
as they may influence the microstructure, mechanical properties, defects, and over-
all processing cost appreciably.
Based on the above discussion, it is important to note that a quest toward
improved performance requires attention to the following key processing considera-
tions to start with:
1. Optimize powder characteristics to achieve good layer-wise spreading in the powder bed;
2. Optimize SLM processing parameters to achieve near 100% relative density;
3. Identify possible defects and adjust processing conditions to minimize them;
4. Optimize post heat treatments to achieve the desired combination of stress relief and
microstructure and mechanical properties.
It goes without saying that there are many design considerations that impact on
the processing and performance of SLM components (e.g., design of complex com-
ponent geometries, support structures, build orientations, build strategies), but these
are best left to discussions about specific components.
Fig. 14.1 shows a typical grain structure of an AlSi7Mg alloy fabricated by
SLM. Columnar grains are found to grow from the molten pool boundary toward
the melt pool center (opposite to the main heat flow direction), and some of the
larger columnar grains can grow across several molten pools. This results in some
preferred growth orientations and the development of a crystallographic texture. By
rotating the scan vectors between each layer, the strong fibrous texture can be chan-
ged into a weak cube texture.
Aluminum alloys for selective laser melting  towards improved performance 305

Figure 14.1 Typical grain structure, determined by electron backscattered diffraction, of an


AlSi7Mg alloy made by SLM on a Concept Laser X-Line 1000 machine (build
direction 5 Z). SLM, Selective laser melting.

From a top view of the last build layer, grain sizes are found to vary across dif-
ferent molten pool positions. The grain size decreases gradually from the molten
pool center to the boundary, and grains tend to be more randomly orientated at the
molten pool boundary. It is generally believed that the solidification mode and crys-
tal growth morphology depend on the classical constitutional cooling theory in
terms of thermal gradient (G) and solidification rate (R) [28]. The G/R ratio deter-
mines the solidification front stability and the resultant solidification mode and
microstructure, while the G 3 R product gives the cooling rate and the correspond-
ing microstructural fineness. In the upper parts of the molten pool, the thermal gra-
dients are lower and the chances of forming equiaxed grains are a little higher. In
general, finer and more equiaxed grains are more likely to be observed around melt
pool boundaries due to changing thermal conditions across the melt pool, which
includes re-melting and heat affected zones (HAZs) along melt pool boundaries.
The shape, size, and distribution of AlSi eutectics influence the final mechani-
cal properties. In the as-fabricated condition, the eutectic Si particles and dendrite
or cell spacings are typically 12 orders of magnitude finer than in a conventional
casting [29,30]. This is due to the much faster solidification rate in SLM. During
casting, the cooling rate is slow and the resultant undercooling is also limited. The
306 Additive Manufacturing for the Aerospace Industry

prolonged solidification time allows Si particles to grow along their preferred crys-
tallographic orientations to form rod or needle shaped morphologies when modifiers
are not used [31].
According to a previous study, cooling rates of up to 106K/s with very high G
can be achieved in the molten pool of SLM-processed AlSi alloys [32]. This
explains why the dendritic cell spacing is of the order of 1 μm while the interden-
dritic regions are decorated with an almost continuous network of extremely fine
rounded Si particles, many of which are of the order of 100 nm or less in size, as
shown in Fig. 14.2A. Careful investigations revealed that the cellular structure and
Si particle size varies across the molten pool and can be divided into three zones:
the fine region, coarse region, and HAZ. Since the border and the upper part of the
molten pool are re-melted repeatedly by the adjacent scan track and the subsequent
build layer, residual heat from the previous scan pass can lower the solidification
rate and result in the formation of coarsened cellular structures. Within the HAZ
areas, Si will precipitate out from the supersaturated Al matrix, which, in turn,
forms more finely dispersed Si particles. The cellular microstructures formed in
SLM fabricated alloys have been observed in AlSi based alloys, CoCrMo alloys,
and stainless steel alloys [3337]. The unique cellular microstructure formation
mechanisms have been investigated and elucidated in detail [38,39].
For the AlSi based alloy system, variations in Si characteristics can influence
the mechanical properties and fracture characteristics. This is especially evident
after heat treatment, which causes dramatic changes in Si and other intermetallic
particle characteristics. If samples are stress relieved at 300 C, the semi-continuous
interdendritic Si network breaks up and the Si particles coarsen, as shown in

Figure 14.2 Secondary electron images of an AlSi7Mg alloy made by SLM on a Concept
Laser X-Line 1000 machine (A) in the as-fabricated condition, (B) after stress relieving at
300 C, and (C) after solution heat treating at 543 C. Fractographs of conditions (B) and (C)
are shown in (D) and (E), respectively. SLM, Selective laser melting.
Aluminum alloys for selective laser melting  towards improved performance 307

Fig. 14.2B. On the other hand, Fig. 14.2C shows that if the samples are solution
treated, the fine Si particles are dramatically coarsened to polygonal particles
.1 μm in size and the spacing between them is also increased. In addition,
Fig. 14.2C also shows that some needle-like particles have precipitated and grown
to .1 μm in length during the solution treatment. These high-aspect ratio particles
are Fe-containing intermetallics, which are hard to find in the as-fabricated or stress
relieved conditions.
A comparison between Fig. 14.2A, B and C reveals that solution treatment
results in a significant coarsening of the microstructure. This is also evident on the
corresponding fracture surfaces, which show much larger dimples and cracks on the
tensile fracture surface after solution treating at 543 C (Fig. 14.2E) than after stress
relieving at 300 C (Fig. 14.2D). As expected, the stress-relieved condition with the
finer microstructure gave more than double the elongation to fracture, but only
about half the yield strength compared to the solution treated and aged condition.
While a solution treatment may be necessary to increase the strength of some
alloys, care must be taken to avoid excessive coarsening of the microstructure,
expansion of gas pores into large defects, and/or undesirable residual stresses with
possible distortion during quenching after solution treatment.
The AlSi based alloys typically show a relatively high strength and low ductil-
ity in the as-fabricated condition, though the ductility improved at the expense of
strength after heat treatment [21,30,3947]. Due to the very rapid cooling rate in
the SLM process, a significant amount of solute remains in solution, which contri-
butes to significant solid solution strengthening and strain hardening effects in the
as-SLM condition. Some researchers also found rod-type Si precipitates embedded
in the Al matrix with a size of around 45 nm in width and 20 nm in length [48].
By means of in situ mechanical testing within a transmission electron microscope
(TEM), it has been shown that the fine-scale cellular dendritic structure itself, Si
particles within the cells, as well as Si particles at the cell boundaries, can all effec-
tively prevent dislocation movement and thus contribute to strengthening in the as-
fabricated condition [49].
In some cases, SLM fabricated samples possess lower ductility compared to con-
ventionally cast samples. This is most likely the case when porosity or unmelted
powders are present due to insufficient energy input during the SLM process [42].
During tensile testing, such defects act as crack initiation sites and promote quick
crack propagation, leading to a lower ductility. In addition, molten pool boundaries
or scan track overlaps with weak bonding areas are also believed to cause early fail-
ures [50]. However, depending on the scan strategy employed in the SLM building
process, crack propagation undergoes different paths before final failure, suggesting
that the final ductility can also be tailored by optimizing the scan strategy. On the
other hand, contour scans can decrease the ductility if the interface between the
core and contour is weakened, whereas base plate heating can improve the ductility
by effectively annealing the material.
Fatigue performance is one of the important mechanical properties as it deter-
mines the stress level and endurance limit of parts under dynamic loading. The
fatigue performance of SLM-fabricated samples is influenced by various factors,
308 Additive Manufacturing for the Aerospace Industry

such as internal and surface defects, the microstructure, strength, residual stress,
and surface roughness. This includes spatter, oxide inclusions, and porosity, but
especially large irregularly shaped pores due to un-melted powders. In general,
defects that cause stress concentrations, especially on the surface, are particularly
detrimental to the fatigue performance. So far, samples made by SLM still suffer
from a high surface roughness, especially in overhanging, or downskin, areas. It is
well known that machined/polished samples show obvious fatigue performance
improvements compared to samples with as-built rough surfaces, especially at the
lower stress levels where the fatigue life is influenced more by crack initiation at
defects [31]. It has been demonstrated that the fatigue performance can be improved
by machining off defects from the surface or sub-surface regions [17], and by heat
treatment to improve the mechanical properties [47]. Although the fatigue perfor-
mance of AlSi based alloys made by SLM is broadly similar to that of castings,
the SLM materials can outperform castings in fatigue if the defects can be reduced
or eliminated, such as by HIP and surface treatment.
Use of substrate heating during the SLM building process can also improve the
fatigue performance. The reasons are fourfold: First, heating up the substrate can
effectively inhibit porosity and splash formation, because lower thermal gradients
can be achieved that can contribute to degassing and maintaining the molten pool
stability. Second, base plate heating can reduce residual stresses and thereby con-
tribute to higher fatigue resistance. Third, base-plate heating contributes to micro-
structural evolution due to reduced thermal gradients and effective heat treatment.
The previously mentioned cellular structures will decompose and form fine sepa-
rated Si particles, much like the stress relieving heat treatment effect shown in the
progression from Fig. 14.2A to B. Fourth, the crystallographic texture developed as
a result of the layer-by-layer building process will also be weakened due to base-
plate heating, thereby contributing to an enhancement of the fatigue performance.
However, it is important to note that care must be taken before embarking on sub-
strate heating for Al alloys, since this can cause other problems, such as increased
microstructure and property variations in the build direction as material closer to
the substrate has effectively received more heat treatment than material deposited
further up.
In general, the growing body of literature reporting on the mechanical properties
of Al alloys after SLM indicates that the mechanical properties of AlSi based
foundry alloys are broadly similar to what is achieved after casting. It is difficult,
for example, to achieve a yield strength of much more than about 280 MPa for
AlSi7Mg or AlSi10Mg alloys, unless steps are taken to design the alloys and their
post heat treatments specifically for SLM.
One of the challenges facing the fabrication of industrial components by SLM is
how to reduce the residual stress to prevent distortion and/or cracking. If AlSiMg
foundry alloys or other heat treatable alloys are stress relieved in the range of
250400 C, they will undergo significant over-aging and softening. The large
amount of solute remaining in solid solution after SLM will precipitate out and the
microstructure will coarsen. As a result, the alloy will need to be solution treated,
quenched, and aged if any significant age hardening is to be achieved after the
Aluminum alloys for selective laser melting  towards improved performance 309

stress relieving treatment. As implied earlier with reference to Fig. 14.2C, such a
solution treatment causes the cellular AlSi eutectic networks from the as-
fabricated condition to disappear while the Si particles coarsen significantly [51].
Although the coarse angular Si and elongated Fe intermetallic particles may act to
decrease the ductility, an observed increase in ductility has been attributed to a
decrease in residual stress [51,52]. As a result, a T6 heat treatment is often specified
after SLM [53,54].
While the T6 treatment is geared toward achieving a good balance between
strength and ductility, it does not capture the benefits of the rapid solidification
nature of the SLM process since it coarsens the microstructure and decreases the
attainable level of solute supersaturation. Some researchers have attempted direct
isothermal heating at 263 C, but questions still remain about the duration and effi-
cacy of such a treatment [55]. Direct annealing between 200 and 450 C shows that
the tensile strength decreases while the ductility improves with increasing heat
treatment temperatures [42], but the cellular microstructure and eutectic Si particle
characteristics hardly change at temperatures lower than 200 C [30]. Other
researchers found that HIP of SLM fabricated AlSi10Mg alloys decreased the
strength, whereas a combined HIP 1 T6 treatment gave better mechanical properties
compared with a normal T6 treatment [49].
Mechanical anisotropy is believed to be another important factor that determines
the applicability of some SLM fabricated parts. Various studies have shown that the
tensile properties tend to be higher in the horizontal direction (xy plane) than in
the vertical (z), or build direction, and that this anisotropy varies from machine to
machine and is more significant for ductility than for strength [21,5661]. It is gen-
erally believed that the reason for these problems can be attributed to the following:
1. Fusion defects and porosity alignment along the build direction. Due to the layer-by-layer
nature of the SLM process, insufficient fusion bonding or powder spreading could intro-
duce weaknesses in the build direction.
2. Crystallographic texture or microstructure variations. Columnar grains are obtained in
SLM fabricated AlSi based alloys and an h0 0 1i texture is obtained due to the epitaxial
grain growth. Therefore, horizontally oriented samples tend to possess higher properties
due to more grain boundaries and effectively smaller grains in that plane.
3. Interface effects between scan tracks and layers can cause different intermetallic particle
characteristics along different directions [62]. It should also be noted that the inclined
angle of the build parts can influence the microstructural homogeneity and the resultant
properties [63].
The above discussion has highlighted some of the challenges and limitations
faced when borrowing existing alloys and attempting to apply them to SLM. In
short, the mechanical properties are not much better than those of castings made
from the same alloys, and improvements tend to be incremental. The remaining dis-
cussion will focus on pathways toward more significantly improved performance by
more intentional design or adaptation of alloy compositions and processing specifi-
cally for the SLM process.
310 Additive Manufacturing for the Aerospace Industry

14.3 Alloy and process design for improved performance


There has been a growing move in recent years to design or adapt alloys specifi-
cally for SLM for the purpose of improving the mechanical properties. Three of the
main alloy and process design approaches will be discussed here:
1. Design of new alloys for SLM, based primarily on transition metal (TM) and/or rare earth
(RE) element additions. This approach utilizes the rapid solidification nature of SLM to
place more solute in solution, which enables new compositional space to be explored that
is out of reach of conventional ingot metallurgy. Functional elements with limited solid
solubility and relatively slow diffusion rates (e.g., Sc, Zr) are of particular interest.
2. Adaptation of existing high strength alloys for SLM. This approach seeks to borrow exist-
ing high performance wrought alloys (e.g., 2024, 7075) and adapt them to SLM by modi-
fying them in some way to make them less susceptible to hot tearing. It also includes the
application of existing high-strength foundry alloys such as A205/A20X to SLM.
3. Development of composite materials for SLM. This approach seeks to add ceramic, car-
bon, or intermetallic particles to reinforce Al alloys on either the micron scale or nano
scale.
The plot of yield strength against elongation in Fig. 14.3 shows how alloys that
are designed or adapted specifically for SLM (in any of the above three categories)
can attain yield strengths in the range of 300600 MPa compared to only

Figure 14.3 Tensile properties of a wide range of aluminum alloys fabricated by SLM, with
or without various post heat treatments, showing alloys borrowed from among AlSi(Mg)
foundry alloys (blue) and alloys adapted for or designed specifically for SLM (red). SLM,
Selective laser melting.
Aluminum alloys for selective laser melting  towards improved performance 311

100300 MPa for alloys that are borrowed from among the AlSi(Mg) foundry
alloys. In both cases, a comparable broad range of elongations to fracture is achiev-
able, and the strength generally decreases with increasing elongation as expected.
This plot clearly shows that the commonly used AlSi(Mg) alloys are not optimized
for high performance and that there is significant scope to develop alloys with dou-
ble the yield strength for a given elongation.
Although designers normally feel more comfortable with existing materials, and
the qualification of new materials is a major effort, it should be pointed out that
even a well-established aerospace alloy such as AlSi7Mg already has a significantly
different microstructure and hence a potentially different mechanical performance
after SLM than after casting. While the previous discussion has provided a founda-
tion of how the basic performance of any alloy can be improved incrementally, the
remaining discussion will therefore focus on the above three alloy and process
design approaches aimed at achieving a step-change in the mechanical properties. It
should be noted at the outset that there is some overlap among the three categories
and that hybrid solutions are also possible.

14.3.1 Design of new alloys for selective laser melting


This section will focus on scandium (Sc), which is regarded as one of the most
effective alloying elements for controlling the structure and improving the proper-
ties of Al alloys [64]. Some similar beneficial effects may be achieved with other
TM and/or RE element additions, though perhaps to a lesser degree. The low
atomic number and density of Sc makes it an interesting alloying addition for high
performance Al alloys in the aerospace industry, especially for high-value proces-
sing by SLM where there is negligible material waste and material costs comprise
only a small fraction of the total cost of a component. There has been great interest
in studying the benefits offered by Sc additions, especially for 5xxx and 7xxx high-
strength wrought alloys [65], due to the following three primary reasons:
1. Sc provides outstanding grain refinement effects. During the solidification process in cast-
ing or welding, primary Sc-containing particles will form and act as heterogeneous nucle-
ation sites for crystallization. Such grain refinement can also mitigate hot cracking and
improve the weldability of Al alloys, which is of particular interest for SLM since high
strength Al alloys tend to be very susceptible to solidification cracking.
2. Sc provides significant precipitation hardening to Al, but this is normally limited by a sol-
ubility of ,0.4 wt%. Due to the rapid solidification in the SLM process, more than double
that amount of Sc can be placed into solution and then precipitated out as nano-scale
Al3Sc hardening precipitates during subsequent aging in a temperature range of about
250350 C [66].
3. Sc improves the recrystallization and grain growth resistance of Al alloys since the Al3Sc
dispersoids are very effective at pinning grain boundaries and stabilizing the grain or sub-
grain structures [67]. This helps to maintain fine grains even at high temperatures.
Grain refinement leading to fine equiaxed grains is desirable since it can offer
many benefits, such as reduced shrinkage porosity, less mechanical anisotropy,
higher strength, and reduced hot tearing susceptibility. As previously reported, the
312 Additive Manufacturing for the Aerospace Industry

Al3Sc particles can form at high temperatures in the melt with a lattice parameter
of 0.4103 nm, which is very close to the 0.4049 nm for pure Al and therefore makes
them very effective nucleation sites for α-Al grains during solidification [68,69].
For binary AlSc alloys, this normally requires a hypereutectic composition, but
for ternary or higher-order alloy systems, lower levels of Sc may already achieve
significant grain refinement. It must be noted here that the grain refinement effect
can be further enhanced by adding TM elements such as Ti and Zr [70], which can
replace some of the Sc atoms in Al3Sc particles and thereby further decrease the lat-
tice misfit [71].
The grain refinement effect of Sc additions has also been verified for normal
casting, where it was found that by introducing 0.2 and 0.4 wt% Sc into alloy
A356, the secondary dendrite arm spacing (SDAS) decreased by 50% and the Si
particles were simultaneously spheroidized, which, in turn, improved the hardness
and wear resistance [72]. Investigations on Sc additions to alloy F357 revealed that
multi-refinement effects could be obtained for grain structures, SDAS, eutectic Si
morphologies, as well as the Al5FeSi intermetallic morphologies [73]. However, Sc
was found to combine easily with Si to form V-phase (AlSc2Si2) precipitates that
can weaken or poison the grain refinement effect [74] and also reduce the amount
of Sc that is available for precipitation hardening.
Introducing 0.66 wt% Sc into aerospace wrought alloy AA2139 resulted in a sig-
nificant decrease in grain size, and this phenomenon could also be achieved by
replacing some Sc with Zr [75]. However, the resulting mechanical properties were
lower compared with the Sc-free version of the alloy. This was attributed to the for-
mation of AlCuSc W-phase particles that lowered the effective Cu concentration,
resulting in the formation of a smaller amount of θ (Al2Cu) strengthening phase.
On the contrary, other researchers reported that no W phase can be found in Al
(0.74.4)Cu0.48Sc and Sc-modified AA2618 alloys [76]. Interestingly, Sc addi-
tions to an AlLi based alloy showed obvious grain refinement and revealed core/
double shell Al3(Li,Sc,Zr) structured precipitates due to the different diffusion rates
of the various elements in that alloy system [77,78]. Aerospace 5xxx and 7xxx
series wrought alloys are also quite amenable to Sc additions since no ternary
AlMgSc or AlZnSc tend to form in these alloys. It has also been demonstrated that
the addition of Zr works very well together with Sc in these alloy systems [79,80].
The high hot tearing susceptibility of most high strength Al wrought alloys is
often related to the enlarged solidification temperature ranges in these alloys.
However, Sc-modified alloys can effectively resist such hot cracking since fine
equiaxed grains can help to accommodate thermal stresses and provide enhanced
feeding of remaining eutectic liquid along grain boundaries during the final stages
of solidification [81]. In the welding industry, it is known that Sc containing fillers
(e.g., AA5556) provide pronounced grain refinement and improved weld properties
[82]. This is useful information since SLM is effectively a form of high-speed mul-
ti-layer laser welding.
Precipitation hardening is regarded as one of the important strengthening
mechanisms in Al alloys. The degree of precipitation strengthening is related to the
volume fraction, size, type, and distribution of hardening precipitates as these
Aluminum alloys for selective laser melting  towards improved performance 313

factors determine how effectively dislocation motion is obstructed [83,84]. In gen-


eral, if more solute can be placed into solution during rapid solidification or
quenching, a higher volume fraction of hardening precipitates can be formed during
subsequent aging and the strength can be tailored by optimizing the processing
conditions.
It has been stated that Sc provides the highest strengthening increment per
atomic percent addition to Al compared with any other alloying element [85]. In
fact, Sc can provide a 4050 MPa yield strength increment per 0.1 wt% Sc addition
due to the formation of fine L12 coherent Al3Sc precipitates during heat treatment
[86]. However, this strengthening potential is limited because the phase diagrams
show a maximum equilibrium solubility of B0.38 wt% Sc for binary alloys and
generally less for multi-component alloys [87]. By increasing the cooling rate dur-
ing solidification, it has been found that the solubility can be improved significantly
and hence a higher age hardening effect is observed after aging [88]. In binary
alloys, a peak hardness is achieved after aging for several hours at around 300 C
[89]. However, if slower diffusing TM elements, such as Zr, Hf, Ti or V, are added,
they can partially replace the Sc atoms in Al3Sc precipitates and form a shell
around the precipitates [90]. The resulting core-shell structured precipitates are very
resistant to coarsening, so the aging temperature can be further increased and the
alloys have the added benefit of being stable at much higher temperatures than nor-
mal precipitation hardening Al alloys. The combined addition of Sc and Zr works
particularly well in this respect. Alloys without Sc can also be made as the rapid
solidification nature of the SLM process allows more TM or RE elements to be
placed into solution and provide similar effects, though the dispersion strengthening
contribution from Al3(TM/RE)-type trialuminide precipitates without Sc will nor-
mally be less than that of similar Sc-containing precipitates. This is supported by
recent work where it was shown that the AlEr system provides less hardening
than the AlSc system after laser melting and aging [91].
The aging curves in Fig. 14.4 show a number of interesting effects after SLM.
First, an AlMgMnZr alloy (with 4.2 wt% Mg, 0.4 wt% Mn, and 0.2 wt% Zr)
achieved a hardness of 60 HV in the as-SLM state with no change in hardness after
aging for 2 hours at 300 C. By contrast, an AlMgScZr alloy (with 3.4 wt% Mg,
1.1 wt% Sc, 0.5 wt% Mn, and 0.2 wt% Zr) achieved almost twice the hardness in
the as-SLM condition (112 HV), .170 HV after 2 hours at 300 C, and still .160
HV after aging for a full 7 days at 300 C. The peak hardness of this alloy is compa-
rable to that of high-strength 7xxx alloys peak aged around 150 C. This demon-
strates both a significant age hardening capability in the alloy with Sc and a high
thermal stability at 300 C.
Aging curves for a standard AlSi7Mg alloy are shown for comparison in
Fig. 14.4. This alloy achieves a similar hardness in the as-SLM condition (B115
HV), but then keeps softening with increasing holding time at 300 C as this is a
typical annealing temperature for conventional Al alloys (i.e., the material is stress
relieved and the supersaturated solid solution decomposes into non-hardening preci-
pitates that continue to coarsen/over-age). If the same AlSi7Mg alloy is then solu-
tion treated at 543 C and quenched (after stress relieving at 300 C), the as-
314 Additive Manufacturing for the Aerospace Industry

Figure 14.4 Aging curve comparisons for AlSi7Mg, AlMgMnZr, and AlMgScZr for
different heat treatment conditions after SLM, where SR refers to stress relieving at 300 C
and ST refers to solution treating at 543 C. SLM, Selective laser melting.

quenched hardness is close to half of what it is in the as-SLM condition. Upon sub-
sequent aging at a more typical aging temperature of 165 C, the alloy then reaches
a peak hardness of B120 HV and already starts over-aging after just 6 hours at
165 C. Interestingly, this peak aged hardness is not much higher than the as-SLM
hardness, though if the alloy had been aged at 165 C directly after SLM, then the
peak-aged hardness would have been closer to 145 HV (but this would be followed
by even more rapid over-aging after just 23 hours at 165 C). However, while
such a direct ageing treatment gives an attractive hardness, it generally results in a
low ductility and insufficient stress relieving to prevent distortion in complex
components.
Attempts at combining Sc-containing precipitates with conventional hardening
precipitates have not progressed very far due to the B150 C difference in aging
temperature. If a precipitation hardening wrought alloy containing Sc were aged at
300 C, then the conventional hardening precipitates would coarsen/over-age in a
very short time [92]. Furthermore, the loss of Sc to non-hardening phases such as
W-AlCuSc or V-AlSi2Sc2 would make it wasteful to add Sc to alloys that are rich
in Cu or Si. Since the required heat treatment temperature range to achieve the opti-
mum Al3Sc precipitation is located between the solution treatment and aging tem-
perature regimes for normal heat treatable Al alloys, it may therefore be more
feasible to add Sc into non-heat treatable alloys to utilize simultaneous solid solu-
tion strengthening and Al3Sc precipitation hardening while also keeping the post
Aluminum alloys for selective laser melting  towards improved performance 315

treatment more simple and cost-effective (and ideally with simultaneous stress
relieving at the elevated aging temperatures). For example, Sc modified 5xxx series
AlMg based alloys exhibit higher hardness and strength levels compared with Sc
free samples [93]. Similarly, adding Sc into an AlMn based 3xxx series alloy also
resulted in higher hardness values after simple isothermal heat treatment [94].
Probably the first alloy that was designed specifically for the rapid solidification
conditions in the SLM process is Scalmalloy from the Airbus Group, which was
made by adding about 0.8 wt% Sc and 0.3 wt% Zr to alloy AA5083 [95,96].
Microstructural analyses revealed that the SLM-fabricated Scalmalloy is composed
of a typical bimodal microstructure in which superfine equiaxed grain regions are
separated by slightly coarser columnar grain regions. As a result, there is very little
anisotropy in the mechanical properties, which is attributed to very few preferred
orientations in the microstructure. For the as-SLM condition, a yield strength of
290 MPa, an ultimate tensile strength of 430 MPa and an elongation of .15% have
been reported [96]. Upon aging at 325 C for 4 hours, a distinct age hardening effect
was observed whereby the microhardness increased greatly from 105 to 177 HV0.3
[97]. Tensile tests showed that the heat-treated samples obtained a yield strength
over 470 MPa, a tensile strength of around 515 MPa, and a ductility of around 14%,
while some further subtle changes were observed if the alloy was subjected to a
HIP treatment [98].
Scalmalloy has captured the attention of both researchers and industry in recent
years. This has led to growth in industrial application and also to the publication of
numerous papers seeking to explain various aspects of the unique microstructure
and properties of Scalmalloy and related alloys [14,96102]. In fact, the AlMgScZr
alloy in Fig. 14.4 is a variant of Scalmalloy that achieves a peak aged yield strength
of about 480 MPa. This alloy was investigated in some detail after SLM at Monash
University, and further results are shown in Figs. 14.5 and 14.6. The electron back-
scattered diffraction (EBSD) results in Fig. 14.5C show the bimodal grain structure
with colonies of fine columnar grains separated by regions of sub-micron sized
equiaxed grains. By comparison, a similar AlMgMnZr alloy, but without Sc (as in
Fig. 14.4), resulted in very coarse columnar grains growing epitaxially through mul-
tiple melt pools in the build direction and exhibiting severe hot tearing with cracks
extending along the grain boundaries between the columnar grains (Fig. 14.5B).
Typical microstructures for an AlSi7Mg alloy fabricated on the same EOS M280
machine shown for comparison in Fig. 14.5A also reveal columnar grains, but there
are no cracks and the grain size is between the extremes of the two 5xxx-based
alloys with and without Sc shown in Fig. 14.5C and B, respectively.
The results in Fig. 14.6 reveal how difficult it is to change the grain structure by
means of processing effects alone since the high thermal gradients in the SLM pro-
cess trigger columnar grain growth for most alloys. However, when powerful grain
refiners such as Sc are added and the processing parameters are pushed to condi-
tions that decrease the thermal gradients and increase the remelting zone volumes
as in Fig. 14.6H, then it is possible to trigger a columnar-to-equiaxed transition and
achieve an almost fully equiaxed grain structure [100]. Fully equiaxed grain struc-
tures are rare in SLM, but this work shows that it is not impossible if powerful
316 Additive Manufacturing for the Aerospace Industry

Figure 14.5 Microstructural comparisons among three different alloys made by SLM on an
EOS M280 machine: (A) AlSi7Mg alloy EBSD image showing columnar grain structure at
top, and scanning electron microscopy (SEM) image showing cellular dendritic eutectic
microstructure at bottom; (B) AlMgMnZr alloy EBSD image showing coarse columnar grain
structure with intergranular cracking at top, and light optical microscopy image showing melt
pools with vertical cracks at bottom; and (C) AlMgScZr alloy EBSD image showing fine
bimodal grain structure at top, EBSD image showing superfine equiaxed grains in the
middle, and SEM image showing fine particles in both columnar and equiaxed grain regions
at bottom. SLM, Selective laser melting.

grain refiners are used together with appropriate processing conditions. Such micro-
structures also tend to resist hot tearing, but careful alloy and process design is still
needed to achieve the desired mechanical properties.

14.3.2 Adaptation of existing high strength alloys for selective


laser melting
It goes without saying that wrought alloys are designed to undergo thermo-
mechanical processing rather than laser melting. The work hardening alloys (i.e.,
1xxx, 3xxx, 5xxx) will remain soft after SLM since no cold work is deliberately
applied. If higher strengths are desired after SLM, then extra alloying elements
should be added to induce solid solution hardening and/or precipitation hardening
(as in the case of Scalmalloy). For precipitation hardening alloys (i.e., 2xxx, 6xxx,
7xxx, 8xxx), it is possible to achieve precipitation strengthening either by aging
directly after SLM or by solution treating, quenching, and aging after SLM.
However, the main issue with most of the wrought alloys is that they are highly sus-
ceptible to hot tearing during the SLM process, with cracks commonly occurring
between columnar grains as shown in Fig. 14.5B.
Aluminum alloys for selective laser melting  towards improved performance 317

Figure 14.6 EBSD grain structure comparisons between two different alloys made by SLM
on an EOS M280 machine with (AD, top) showing results for an AlMgMnZr alloy, and
(EH, bottom) for an AlMgScZr alloy. Processing conditions were varied from left to right
as follows:
(A and E) 35 C platform temperature with VED 5 77 J/mm3, (B and F) 35 C platform
temperature with VED 5 154 J/mm3, (C and G) 200 C platform temperature with
VED 5 77 J/mm3, and (D and H) 200 C platform temperature with VED 5 154 J/mm3. SLM,
Selective laser melting; VED, volumetric energy density.
Source: Adapted from work published by the current authors: K.V. Yang, Y. Shi, F. Palm, X.
Wu, P. Rometsch, Scr. Mater. 145 (2018) 113117.

The 2xxx series alloys are widely used in aerospace applications and are known
to be susceptible to cracking during casting and welding [103]. Alloys 2022 and
2024 have been studied under various SLM processing conditions and a reduction
in cracking was observed when samples were built on thin wall support structures
[104,105]. However, cracks were still found on the first several layers above the
support structures. For alloys 2618 and 2219, it has also been found that crack-free
samples are difficult to make by SLM despite trying different scan strategies and
hatch distances [106,107]. However, by careful control of SLM process parameters
within a narrow window, some researchers have succeeded in eliminating cracks in
alloys based on 2024 and 2618 [108,109], though such improvements often corre-
spond to reduced productivity or increased porosity. A very recent paper reports
that an Al3.5Cu1.5Mg1Si alloy was successfully made by SLM without
cracks and achieved a yield strength of 368 MPa after post-SLM T6 heat treatment,
but it had to be fabricated with a low power of 200 W and a low speed of 200 mm/
s to avoid cracking [110].
Severe cracking has also been found in SLM-fabricated 6061 samples, but the
cracking characteristics can be influenced significantly by varying the process para-
meters, especially laser power and scan speed [111,112]. In comparison with
AlSi10Mg, 6061 has a significantly larger solidification range (by about 50K),
which contributes to its increased hot tearing susceptibility. It is now well known
that such cracking occurs along grain boundaries in the final stages of solidification,
318 Additive Manufacturing for the Aerospace Industry

so any attempts to eliminate hot tearing should focus on alloy chemistry, grain
refinement, and stress-relieving during the solidification cooling process.
The high strength 7xxx series wrought Al alloys are also widely used in the aero-
space industry. It has been found that these alloys are very difficult to make by
SLM without large columnar grains and solidification cracking [113,114]. Despite
varying the laser defocusing distance and scanning speed, cracks could still not be
successfully eliminated and cracks were found to propagate along grain boundaries
in both keyhole and conductive melting modes [115]. It is believed that during the
final solidification stages in the SLM process, the shrinkage behavior and lack of
liquid feeding along the columnar grain boundaries caused the occurrence of the
solidification cracks [115].
Dedicated work on reducing cracking has revealed that the SLM processability
of wrought Al alloys can be effectively improved by introducing powerful nucleants
for grain refinement and/or decreasing the solidification temperature range. By add-
ing a significant amount of Si into alloy 7050, solidification cracks were effectively
eliminated and the final T6 hardness was improved [116]. It was found that Si could
decrease the solidification range, improve the fluidity, cause the formation of a
low-temperature eutectic that promotes the backfilling effect of liquid material
between grain boundaries, and promote the formation of very fine equiaxed grains
at the molten pool boundaries. Similar effects have also been observed by blending
Si with 6061, leading to dense parts without solidification cracks [49].
Perhaps two of the most significant achievements in this category are due to the
addition of Zr to a 2xxx alloy and separately to a 7xxx alloy for the purpose of
eliminating hot tearing by means of grain refinement. When a gas atomized
Al4Cu2Mg0.5Mn powder that cracks upon SLM was blended with a 2 wt%
addition of pure Zr powder, there was no cracking after SLM and a yield strength
of B445 MPa was achieved [117]. This could also be categorized as new alloy
development due to the high level of Zr that was added. In the other development,
hydrogen-stabilized nano-Zr particles were added to gas atomized 7075 powder,
which resulted in significant grain refinement and elimination of cracks, though the
SLM 1 T6 yield strength of 325373 MPa was lower than that for wrought 7075-
T6 plate [15].
In the context of existing alloys, it should also be mentioned that extensive work
was conducted on rapidly solidified powder metallurgy alloys several decades ago,
which resulted in the development of numerous alloys such as AlFeX and
AlZnMgCuX. It is worth noting here that after compaction, extrusion, and
heat treatment, the rapidly solidified powder alloys X7090
(Al8Zn2.5Mg1Cu1.5Co) and X7091 (Al6.5Zn2.5Mg1.5Cu0.4Co)
achieved tensile yield strengths of about 540590 MPa with elongations to fracture
of around 8%12% [118,119]. Such alloys have hardly been evaluated for SLM to
date, but are perhaps worthy of investigation if hot tearing can be avoided.
This section has focused mainly on wrought alloys since they generally have
higher strengths than cast alloys. However, it should be mentioned here that high-
strength casting alloys also have significant potential for SLM and perhaps provide
an even better starting point for alloy development due to their improved castability
Aluminum alloys for selective laser melting  towards improved performance 319

and resistance to hot tearing. If high-strength casting alloys are to be adapted for
SLM, then the focus will shift from crack avoidance to improving the mechanical
properties. One noteworthy example in this respect is the AlCu based casting
alloy A205, also known as A20X in the aerospace casting industry. This alloy,
sometimes also referred to as AM205 in powder form, has recently been applied to
SLM. There is not much data available yet, but early indications are that the TiB2
particles cause significant grain refinement and that the alloy could achieve a yield
strength in the vicinity of about 340420 MPa after SLM, depending on alloy
chemistry, SLM processing parameters, and post-heat treatment conditions. Due to
its high content of micron-scale TiB2 particles, this alloy could also be categorized
as a metal matrix composite (MMC), which is the subject of the next section.

14.3.3 Development of composite materials for selective laser


melting
MMCs can exhibit unique combinations of properties and provide another way of
increasing the strength after SLM. As a result, there has been a growing interest in
exploring the potential of producing Al-based MMCs by SLM [120,121]. These
MMCs may also be of interest for aerospace applications, especially if care is taken
to ensure that the reinforcement particles do not act as crack initiation sites for
fatigue failure.
In one investigation, high-energy ball milling was used to synthesize Al2O3/Al
nanocomposites, which were then characterized for SLM fabrication purposes
[122]. With the use of TEM, it was found that the nano-sized Al2O3 particles can
be tailored by control of milling parameters to be homogeneously distributed across
the Al powder surface, which is generally regarded as a suitable form for SLM pro-
cessing in terms of flowability and laser absorptivity. Afterward, the composite
powders were subjected to SLM fabrication and near full density samples could be
obtained with optimized process parameters [123,124]. The Al2O3 reinforcements
were found to be distributed uniformly within the Al matrix, which contributed to a
significant improvement of yield strength, microhardness, and wear resistance.
In order further to increase the strength of the widely used AlSi10Mg alloy after
SLM, pure Ni powders were mixed in with a ratio that can guarantee a chemical
composition close to the eutectic point in order to decrease the solidification range
and avoid solidification cracking [125]. Except for a few agglomerations of micron
sized Al3Ni particles, most of the sub-micron sized Al3Ni particles obtained by in
situ reaction were found to be distributed uniformly across the matrix. The precipi-
tated Al3Ni particles have a high coherency with the Al matrix and the properties
of the SLM-fabricated parts were greatly enhanced due to Orowan strengthening or
stacking fault mechanisms. When trying directly to incorporate ceramic particles
like SiC or TiC into AlSi10Mg through ball milling, a reasonably uniform distribu-
tion of these reinforcing particles could be realized with optimized parameters, and
improved mechanical properties could be achieved after SLM [126,127]. For exam-
ple, SLM-processed SiC/AlSi10Mg parts showed two types of reinforcing phases
320 Additive Manufacturing for the Aerospace Industry

(unmelted SiC particles and in situ formed Al4SiC4 strips), and the fraction of one
could be increased by changing the process parameters. In this case, the Al4SiC4
phase is believed mainly to be responsible for the elevated mechanical properties
due to its improved wettability with the Al matrix. On the other hand, novel ring-
structured nanoscale TiC particles were obtained in SLM-fabricated TiC/AlSi10Mg
parts, and the formation mechanisms are attributed to the rearrangement of TiC par-
ticles driven by the Marangoni flow and capillary forces. As a result, an elevated
microhardness and tensile strength with no obvious decrease in ductility were
obtained compared with unreinforced samples.
Carbon nanotubes are regarded as potential reinforcements for SLM fabricated
Al matrix composites due to their outstanding advantages of high elastic
modulus, mechanical strength, and electrical conductivity [128,129]. However,
mechanical mixing of carbon nanotubes is believed to be difficult due to their
high tendency to agglomerate, and thus a slurry ball milling method was pro-
posed, which achieved a relatively uniform distribution of carbon nanotubes on
the AlSi10Mg powder surface under appropriate milling parameters. However,
one problem is that decomposition and evaporation of carbon nanotubes were
found to occur during SLM. Some carbon atoms diffused to the molten pool and
dispersed into the AlSi10Mg matrix, which slightly enhanced the tensile strength
but lowered the ductility.
It is well known that TiB2 has a low lattice mismatch with the Al matrix and
also plays an important role in the grain refinement of Al alloys. Therefore, incor-
porating non-deformable TiB2 particles into AlSi10Mg alloys is regarded as an
effective way of improving the mechanical properties. However, as the nano-sized
TiB2 particles have a high tendency to agglomerate, the resulting strengthening
effect can be compromised. Recently, researchers proposed a novel way of dispers-
ing the reinforcements among the Al alloy powders [130]. By melting reactive salts
of K2TiF6 and KBF4 into the pure Al, improved nano-TiB2 reinforced Al compo-
sites were obtained. This composite was then remelted together with AlSi master
alloys to achieve the desired composition. The melted metal was then gas atomized
into powder, which contained homogeneously dispersed nano-sized TiB2 particles
within the AlSi10Mg alloy.
When this composite powder was used in SLM with optimized processing para-
meters, a near fully dense nano-TiB2 reinforced AlSi10Mg composite was success-
fully made [131]. The nano-particles are also believed to improve the laser
absorptivity and the resulting processability compared with AlSi10Mg powders.
Microstructure observation revealed fine equiaxed grains and a random texture,
which was attributed to the combined effect of both grain refinement by nano-TiB2
particles and the high cooling rate of the SLM process. It was found that the nano-
TiB2 and Si particles are coherent with the Al matrix, which results in strong inter-
facial bonding. As a result, the SLM-fabricated TiB2/AlSi10Mg nano-composites
achieved a yield strength of B430 MPa together with an elongation to fracture of
15.5%, which is much higher than AlSi10Mg made by SLM.
Aluminum alloys for selective laser melting  towards improved performance 321

14.4 Summary and outlook


The AlSiMg alloys have been borrowed from the foundry industry and are now the
most widely studied and used aluminum alloys for SLM. These alloys are well
suited for SLM since they have been designed for solidification processing.
However, the mechanical properties after SLM are not much better than after cast-
ing, suggesting that the potential benefits offered by the SLM process are not fully
captured. On the other hand, the traditional high-strength wrought Al alloys cannot
be easily manufactured by SLM due to their high susceptibilities to hot tearing.
Efforts made on reducing the hot cracking susceptibility, such as by adding power-
ful grain refiners, have resulted in significant improvements, but the mechanical
properties are still not particularly outstanding. Research into the addition of rein-
forcement particles to form composite or nano-composite materials has progressed
a long way, though the wettability and bonding between the reinforcements and the
Al matrix tends to be a weak spot. There is also a need for more work on improving
the surface roughness, property consistency/isotropy, and fatigue performance for
SLM in general, especially for aerospace applications. Nevertheless, it has been
shown that there is already a significant body of knowledge related to controlling
the grain structure, reducing defects, and optimizing processing conditions (includ-
ing post heat treatments) to achieve improved microstructures and properties for
existing alloys.
While much of the work related to AlSiMg alloys represents only incremental
improvements, the purpose of this contribution has been to demonstrate that a step-
change in mechanical properties is possible if alloys are designed specifically to
capture the benefits offered by the SLM process. It has been demonstrated that
while opportunities exist to achieve significant improvements in mechanical proper-
ties (over those of AlSiMg alloys) by adapting high-strength wrought or cast alloys
to SLM, even greater improvements can be realized if new compositional space out
of the reach of conventional ingot metallurgy is targeted. So far, the alloys with the
highest strength after SLM are those that have been designed to place more solute
into solution via the rapid solidification conditions in the SLM process than is pos-
sible by conventional casting or solution treatment and quenching. This includes
the AlMgScZr Scalmalloy from the Airbus Group (yield strength .450 MPa) and
the AlMnScZr alloys from Monash University (yield strength .550 MPa), both of
which achieve great properties due to unique combinations of precipitation harden-
ing, solid solution hardening and ultrafine grains that are hard to achieve in more
conventionally processed alloys.
The rapid solidification conditions in the SLM process now enables the use of
larger amounts of slow diffusing TM elements and/or RE elements, which also pre-
sents interesting new opportunities to achieve high-strength alloys with significant
thermal stability (e.g., NanoAl alloys). In the end, a hybrid approach incorporating
the best aspects from the various approaches discussed herein may yet bring about
the greatest improvements. Meanwhile, the number of Al alloys for SLM is increas-
ing and there is rapid progress toward improved performance.
322 Additive Manufacturing for the Aerospace Industry

Acknowledgments
This work was supported by the Australian Research Council (Grant No. IH130100008). The
authors acknowledge use of the facilities at the Monash Centre for Additive Manufacturing
and the Monash Centre for Electron Microscopy. Jeremy Rao, Elena Labelle, Stephanie Giet,
Ariel Dingjan, Arthur Li, Yunjia Shi, Mengying Wang, Tom Jarvis, and John Shurvinton are
also thanked for various contributions.

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Additive aerospace considered as
a business 15
Lawrence Gasman
SmarTech Markets Publishing Crozet, Virginia, United States

Additive manufacturing (AM) seems to have found some role in almost every
industry, but aerospace stands out. Aerospace is still the only sizeable industry in
which AM has become mainstream technology and SmarTech Publishing (www.
smartechpublishing.com) anticipates that the market for AM hardware in 2018 will
exceed $380 million, growing to $1.4 billion by 2027. For materials used in “AM
Aerospace, industry analyst firm SmarTech Publishing expects sales of almost $180
million in 2018 to $1.3 billion in 2027.”
The clearest indication of the direction of the AM aerospace industry is the
acquisition initiated by General Electric (GE)—a market leading company in AM
adoption for aerospace applications—of Arcam AB and Concept Laser in summer
2016. These two leading manufacturers of metal powder bed fusion technologies
were acquired for US$1.4 billion combined. Within a few weeks after Concept
Laser’s acquisition was completed, the company had grown from 200 to 244
employees and is now expected to reach 400 by 2018.
Since GE is the company that has conducted the most extensive studies to date
on the cost-effectiveness of AM for aerospace production, it seems logical to con-
clude that the $1.4 billion investment was considered by the company as a fairly
safe bet on the future of manufacturing in aerospace primarily, but also in several
other industrial segments.
AM production volumes in aerospace remain fairly low, but the industry is readying
for much greater levels of adoption. All that said, the implementation of AM in aero-
space continues to be frustrated to some extent by the lack of availability of software
capable of fully supporting all phases of the AM process in the aerospace industry.
Because of the high degree of specialization required, along with the potential for a
high revenue stream, several firms have been building up their AM system capabilities,
targeting production in aerospace and—to a lesser degree at this time—automotive.
These can be either pure AM facilities or large Tier One suppliers that are
investing significantly into expanding their AM offerings. The Additive Factory
concept is based on a fully integrated process, from powder manufacturing to
metrology and finishing processes—leveraging “farms” of automated AM pro-
duction systems.
At the present time, additive factories are owned by major aerospace groups. This
is the case, for example, for Premium Aerotech (a 100% subsidiary of the Airbus
Group) and Avio Aero, now a fully owned subsidiary of General Electric. Avio Aero
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00017-0
© 2019 Elsevier Inc. All rights reserved.
328 Additive Manufacturing for the Aerospace Industry

has production sites in Poland, with more than 4600 employees worldwide. Now part
of the GE Additive network, the company provides clients with technological solu-
tions to respond quickly to the constant changes demanded by the market.
Specialized service bureaus have been launched in the United States with the spe-
cific aim of producing 3D-printed components for aerospace customers. Two of these
are Addaero Manufacturing and Sintavia. Addaero was founded by former Pratt &
Whitney employees, and claims to specialize in both electron beam manufacturing
(EBM) and direct metal laser sintering (DMLS) metal manufacturing. The company’s
most notable case study to date is in space components manufactured for NASA.
Sintavia is reported to utilize three SLM Solutions metal powder bed fusion systems.

15.1 3D printing technologies for tooling and


prototyping
For the short- to medium-term future, the primary application of AM in aviation will
remain tied to prototyping and tooling. This opens the doors to implementation of
several 3D-printing technologies and materials, such as photopolymerization based
stereolithography and material jetting processes. These are processes cannot be used
for end-use production because most materials tend to deteriorate with time, but—for
a limited period—they can offer excellent characteristics. Furthermore, material jet-
ting technologies can uniquely offer multi-material capabilities.
Other new technologies, such as the continuous DLP (CLIP) high-speed stereo-
lithography process from US-based carbon, or the highly affordable metal extrusion
and binder jetting combination of processes recently introduced by US-based start-
up desktop metal, could also find their way in civil aviation prototyping and even
part production, although for the time being they are both focusing on automotive,
offering lower costs and higher production speeds for less demanding parts.

15.2 Factors driving additive manufacturing in the


aerospace industry
By removing constraints related to traditional manufacturing processes, both physi-
cal limitations and financial feasibility constraints, AM has brought forth the poten-
tial for numerous design-related improvements in aircraft. With regard to
commercial aircraft, these design improvements are, or will be, manifested primar-
ily in terms of weight reduction and increased performance characteristics.

15.2.1 Weight reduction


In the short term, the most critical of these improvements is weight reduction.
Weight is especially crucial for modern aircraft. Although a Boeing 737 weighs
approximately 65 MT, eliminating only one pound in weight can generate savings
of hundreds of thousands of dollars each year for airline companies. Spread that
Additive aerospace considered as a business 329

number out to include all aircraft worldwide and the savings are upwards of $10
million, according to GE Aircraft. In a study by EADS Innovation Works and EOS,
it was estimated that replacing the engine cowling hinge with an AM part could
reduce the overall weight of the aircraft by 10 kg.
The next level of weight reduction will be fueled by a number of new technolo-
gies and new materials within the AM field. Metal powder-bed AM systems can offer
substantial weight reductions to titanium parts, which make up around 15% of a
plane’s total weight. A new generation of composite materials has now been engi-
neered for 3D printing, both by extrusion and plastic powder bed fusion technologies,
which possess mechanical properties comparable or superior to milled aluminum.
Weight benefits are also starting to be quantified in more cost-efficient manufactur-
ing as well, thanks in part to steep growth in adoption of metal powder bed technolo-
gies with very high deposition rates and hybrid computer numerical control (CNC)
capabilities. Boeing and Norsk Titanium—a metal fed AM system manufacturer—
have estimated that implementation of the first federal aviation agency (FAA)-
approved additively manufactured structural titanium component will result in savings
of $23 million off the $265 million price tag for its newest 787 Dreamliner model.

15.2.2 Additive manufacturing and improved aircraft design


AM can also lead to significant improvements in aerospace design. AM technologies,
in the most optimal circumstances, are the manifestation of the benefits of computer
aided design/computer aided manufacturing (CAD/CAM) modeling. Next generation
generative software is also enabling engineers seamlessly to optimize designs to ben-
efit specifically from AM processes. These improvements can reduce the life-cycle
cost of the plane by increasing engine efficiency, reducing drag, and reducing mass.

15.2.3 Software as a limiting factor on additive manufacturing


aerospace
One key element that has limited AM adoption in the aerospace industry is the
availability of practical software solutions to exploit fully the benefits of AM in
the design, workflow, and supply-chain phases. But this has changed radically
over the past 2 years:
G
Airbus Group has extended its use of Dassault Systèmes’ 3DEXPERIENCE platform to
its AM programs, integrating design, simulation, and production. This was done as part of
the “Co-Design to Target” industry solution and provided Airbus with digital continuity
to optimize its conceptual designs by virtually validating each phase of the AM process.
G
solidThinking publisher Altair has entered a non-exclusive partnership with aerospace
part supplier RUAG and 3D printing service bureau Morf3D for cooperation in advancing
AM for aerospace applications.
G
Autodesk has continued to evolve its Dreamcatcher generative design tools, which was
used to design a topologically optimized Airbus A320 cabin bracket that was additively
manufactured (by metal powder bed technology) as a proof of concept. The AM bracket
was significantly lighter than the previously used partition. It was also strong enough to
anchor two jump seats for flight attendants during take-offs and landings, was less than
one inch thick, and could be attached to the plane’s airframe in just four places.
330 Additive Manufacturing for the Aerospace Industry

15.3 How additive manufacturing is improving the


supply chain the aerospace industry
Because aircraft demand is characterized by long lead times, production schedules,
and production backlogs that may last years, the risk of investment in new equip-
ment and infrastructure such as represented by AM has some of the supply chain
worried. Fears that elevated production rates from AM will still not last long
enough to pay for the investment is the concern.

15.3.1 Service providers


With so many major aerospace companies exploring AM solutions, some 3D printing
service providers that print volumes from aerospace customers may eventually erode
as manufacturing operations move in house. This is, of course, a distinct possibility.
On the other hand, there may be short- to medium-term opportunities for 3D
printing service providers to become integrated into the aerospace supply chain as a
means to provide flexible production solutions. In fact, some specialized service
bureaus are already making investments in more production-level equipment based
on the level of growth of AM aerospace.
This trend will alleviate the pressures on aerospace firms to make heavy invest-
ments in AM equipment. Relatively few service providers may be equipped world-
wide to handle a large influx of demand; however, as potential aerospace
applications for AM have grown, there already has been an increase in the number
of specialized 3D printing service providers targeting the aerospace industry.
Print services providers have been serving the aerospace industry for some time;
however, the market for service providers is now changing to meet the growing trend
of final parts manufacturing utilizing 3D printing. Across several influential adopting
industries, a growth in specialty service bureaus serving a specific industry with
advanced 3D printing services has been observed. This has been true recently in aero-
space, where several existing and entirely new firms are shifting business models to
capitalize on the opportunities specifically associated with aerospace applications.
Several firms seem to be particularly heavily involved as service providers for the
aerospace industry. These include Materialise [has an agreement with Airbus to supply
parts 3D printed in high performance ULTEM with Stratasys fused deposition model-
ing (FDM) technology], Stratasys Direct Manufacturing, ProtoLabs, and 3D Systems-
on-Demand (has worked with Thales Alenia on metal aerospace applications).

15.3.2 Siemens
In early 2017, Siemens rolled out its product name (PLM) solution for AM.
Benefiting the aerospace industry in particular, this solution enables automated gen-
erative design using the new topology optimization capabilities that enable organic
shapes that would be difficult for a human designer to envision. The ability to 3D
print an optimized part shape could reduce the number of parts in an assembly,
Additive aerospace considered as a business 331

thereby decreasing weight and increasing strength. As a result, industries, such as


aerospace, could realize dramatic value.

15.3.3 SAP
SAP has signed a co-innovation agreement with APWorks, a subsidiary of Airbus
Defence and Space, which aims to accelerate the adoption and standardization of
industrial 3D printing initiatives aerospace and defense. The goal here is to manu-
facture 3D-printed components such as armrests and brackets, improve fuel effi-
ciency and reduce CO2 emissions. APWorks can also better manage spare part
orders in real time to deliver qualified products for safety-critical applications in
aerospace and other industries.

15.4 Materials for additive manufacturing aerospace


15.4.1 Metals
Metal AM technologies are now being used for structural parts that go beyond air-
craft engines. One clear indication came from the agreement, signed mid-2016,
between Airbus and Dassault Systèmes regarding the 3DEXPERIENCE PLM plat-
form. Airbus Group will deploy Dassault Systèmes’ collaborative design and simu-
lation applications as part of the “Co-Design to Target” industry solution
experience, for the AM of tooling, prototyping, and parts for test flights and for pro-
duction use on commercial aircraft.
Metal powder bed fusion technology and the aviation industry have developed
what is likely to be the most significant 3D printing technology/end-user relation-
ship in 3D printing history. The aerospace industry continues to push the develop-
ment of various forms of metal powder bed fusion systems further in capability
through commitment to developing real, viable, serial manufacturing opportunities
for the technology previously seen only in the medical and dental industries.
Metal powder bed fusion systems have continued to evolve out of their largely
research-related roles and into true strategic manufacturing tools for the early lea-
ders in aerospace engines. From a handful of different aerospace engine parts that
were in pre-production and testing for serial manufacture at various aerospace sup-
pliers, the market for AM metal parts has now expanded to include safety-critical
structural components, with research being conducted on the industrialization of
production for large-size parts.
Several significant names in aerospace continue to experiment with these sys-
tems producing viable test components being incorporated into experimental test
aircraft or test engines. GE—and to a minor degree Rolls-Royce—has been driving
innovation within AM for engine parts. Airbus has been leading the way on struc-
tural and safety-critical components, both directly through its own internal AM-
focused R&D activities and indirectly through fully owned Tier 1 suppliers such as
Premium Aerotech.
332 Additive Manufacturing for the Aerospace Industry

The overall capabilities of metal powder bed fusion systems have increased sig-
nificantly within the context of aerospace; however, there is still much development
left to do. The process for validating an AM part for flight—especially in structural
and flight/safety critical components—is extremely long, with some major projects
coming to fruition in recent months that have taken as long as 10 years since they
were first envisioned.
A lot remains to be done on process optimization. While the machines have
evolved significantly, most adopters do not consider them as yet fully able to sus-
tain serial manufacturing processes. While speed and size are now considered more
than adequate for most requirements, much remains to be done on process optimi-
zation, automation, repeatability, and integration of AM systems in the industrial
manufacturing workflow.
This involves requirements that are significantly different from those of the pro-
totyping lab, where an AM system can function as a standalone machine. In the
industrial manufacturing workflow, more automation is required in the phases
before and after the actual build process, with automated powder management, pro-
cess simulation, process control, and finishing stations.
A number of key trends in metal powder bed fusion equipment are heavily influ-
enced by use from aerospace users. Several of these trends have played a critical
role in expanding the final part applications now underway today in aerospace
engines. These are summarized in the Exhibit below.
Evolution of recently identified key trends in metal powder bed fusion systems
Trend Effect Impact on recent
aerospace market
development
Improved operational Streamline total machine operation Minor/negligible
safety standards process chain
Build envelope Expand addressable applications and Moderate
expansion improve scalability for higher volume
production
Automatic powder Improves cost profile of metal powder Moderate
delivery and bed AM
recycling
Multiple melt pool Improves overall ability of metal Moderate to significant
technology powder bed AM systems to meet true
manufacturing requirements
Modular system Improves metal AM’s ability to Significant
design integrate into existing manufacturing
environments
Process monitoring Allowing for increased efficiency and Potentially significant
and quality applicability in total aerospace (ongoing)
assurance systems manufacturing chain
AM, Additive manufacturing.
Source: SmarTech Publishing.
Additive aerospace considered as a business 333

In general, technology upgrades in metal powder bed systems related to increas-


ing throughput of parts (such as multiple melt pools, powder delivery and recycling,
build envelope expansion) are having less effect in advancing adoption from aero-
space manufacturers when compared to efforts for improved quality assurance and
modularity or flexibility of various systems.
Throughput upgrades are highly valued as the perception and critical acceptance
factors for metal AM in aerospace are improved—which is largely happening and
will continue to happen through better process monitoring technology, standards
development, and flexible AM systems that can accommodate innovations specific
to aviation end users.
Metal powder bed fusion hardware systems have evolved significantly over the
past 2 years both in terms of machine capabilities and process automation. Two
trends that are especially relevant to aerospace are a focus on faster speeds and a
focus on larger sizes.

15.4.2 Directed energy deposition


Other approaches to the AM of metal components involve a relatively broad
group of processes known collectively as directed energy deposition (DED).
These systems offer a much different value proposition to the aerospace industry
by being typically of very high cost, but with the ability to serve much larger
part sizes in metal, with much higher deposition rates, as well as the ability to
fabricate in a freeform nature by depositing material onto existing objects or
surfaces.
Many DED systems have very rapid deposition speed at the cost of the high
degree of accuracy and small feature size that powder for which bed systems are
known. Wire-based DED systems take this principle to the extreme, while blown
powder systems can resemble powder bed output to a relatively close degree. This
is advantageous in certain applications where machining is already expected to
arrive at final tolerances, surface finish quality, or other considerations. Additional
time and cost for machining operations can be offset by the extremely rapid build
rates, especially when compared to the traditional manufacturing alternative for
many aerospace components.
The compelling short-term opportunity for DED systems in aerospace is in
remanufacturing and repair of existing parts, which can repair critical compo-
nents that would otherwise be very costly to replace, or can augment existing
structures to add new features or capabilities. The longer term potential for
DED technologies is the rapid manufacture of large metal aerospace components
in a highly cost-effective manner, with greatly reduced lead times and material
consumption.
One element that is likely to drive adoption of this technology in civil aviation
manufacturing—and in all manufacturing, that involves large metallic parts—is
that DED systems are not only available as Cartesian deposition systems but
also can easily be implemented as a single “deposition engine tool” that can be
built into standard industrial CNC and laser-cutting systems. Optomec and
334 Additive Manufacturing for the Aerospace Industry

Trumpf already offer this option. The Exhibit below details the opportunities for
DED technology.
Opportunities for directed energy deposition in civil aviation manufacturing
Opportunity Benefit Powder bed Wire vs powder
competition
Large near net Build volume for Minor—powder Wire is most
shape fuselage very large bed limited by advantageous
components components build size where near net
shape is acceptable
Turbine blades Rapid deposition Moderate—powder Wire
speed bed can compete
with smaller
blades
Remanufacture Ability to deposit No Powder is most
(repair) metal on existing advantageous
structures and where precision
surfaces may be a concern
Remanufacture Ability to deposit No Powder systems
(feature addition) metal on existing currently have
structures and much higher
surfaces material flexibility
Source: SmarTech Publishing.

15.4.3 Polymers
While real metal applications for flying parts in civil aviation are still rather
scarce, the opposite is true of plastic-based parts, practical examples of production
certified flying parts abound and continue to multiply, within and beyond proto-
typing. Performance characteristics of components made via several polymer 3D
printing processes are generally very good, as long as considerations of the nature
of each individual print process are taken into account and matched to proper
application.
Conceptually speaking, one clear example of what can be achieved with poly-
mers in AM was offered by the (Testing High-tech Objectives in Reality) project,
where a team at Airbus designed and fully 3D printed a small-sized pilotless air-
craft. China’s COMAC is also working on similar largely 3D printed aircraft
demonstrators. The Lingqueshan (Bird Spirit) B project features several composite
and 3D printed parts, including sub-bearing parts and landing gear.
Several commercial case studies now exist that involve large commercial craft
with hundreds—and sometimes thousands—of 3D-printed polymer parts through-
out the cabin, environmental control systems, cockpit and electronic systems, and
other areas. These parts, while generally not considered as revolutionary as
printed metal engine parts or key structural components that loom on the horizon
for AM, represent a critical portion of the current market for AM as a production
Additive aerospace considered as a business 335

technology for aircraft. Building the value case for AM in the present, with real,
quantifiable benefits that can be observed today, are absolutely paramount to fur-
thering the overall use of AM in the future—where much of the expected value
currently lives.
Use of polymers such as thermoplastic filaments, thermoplastic powders, and
photosensitive resins also have a strong foundation in prototyping applications in
commercial aerospace spanning the last 20 years. These activities have steadily
increased, helping to reduce product lead times and costs associated with aircraft
design.
In all, polymer materials, print technologies, and, ultimately, parts, stand to
become an equally significant opportunity as the much more often championed
activities in metal aerospace printing. Material standards and qualifications are
much more developed, and print technologies have decades of commercial use
within aerospace organizations, already creating a wealth of experience from which
to draw. Although few in the industry today are likely utilizing polymer 3D printing
to manufacture aircraft components in a manner that is representative of AM’s
highest potential, in time the competencies will develop right alongside activities in
metals.
Given the significance of polymers and, more importantly, composites manufac-
tured for aircraft through traditional processes, a very significant addressable mar-
ket exists for 3D printing in polymer. The Exhibit below summarizes opportunities
and timelines for polymer 3D printing in commercial aerospace.

Evolution in polymer 3D printing applications in aerospace


Application Current popular Evolutionary path Current
category application adoption trend
Prototypes Fit and assembly testing More iterations per part Moderate and
increasing
Tools Assembly jigs, fixtures, Lifecycle tooling, Moderate and
guides castable tooling increasing
Flight parts Low volume production, Serial production Minimal and
spare parts increasing
Source: SmarTech Publishing.

Production of polymer-based AM parts is now underway at several aircraft


manufacturers and Tier 1/Tier 2 suppliers all over the world. Most cases revolve
around the use of Stratasys industrial FDM technology, based on its Fortus
900mc and Fortus 450 systems, which are capable of reliably producing parts in
high performance ULTEM 9085. One of the first major official operations on
AM of polymer flying parts was launched by Materialise in late 2015 when the
company signed a commercial agreement with Airbus to use its Belgium-based
additive factory to deliver airworthy end-use parts for Airbus’ new A350 XWB
aircraft.
336 Additive Manufacturing for the Aerospace Industry

Meanwhile, material extrusion systems are the most adopted technology


worldwide, primarily thanks to abilities in rapid prototyping and tooling, and the
aerospace industry is no exception. Material extrusion is a widely applicable
print technology in aerospace, primarily because of its good cost per part, easy
integration into many environments, and ability to print in a wide range of
engineering-grade thermoplastic materials. It suffers a variety of weaknesses as
well, such as performance inconsistency for parts in the Z-direction, and slow
printing speed.
In the past, this has created a conflicted competitive picture for commercial aero-
space companies. Less expensive material extrusion systems’ print quality could
leave something to be desired, and were slow, but faster print technologies could be
orders of magnitude more expensive and involved powders or resins that are not as
user-friendly.
Only a couple of years ago, Stratasys’ FDM technology—the “official” material
extrusion process—seemed on the verge of being surpassed by low-cost systems
and the faster production rates of powder bed fusion technologies. Instead, it has
made a strong comeback. Stratasys has developed a new range of solutions targeted
specifically at the aviation sector.
Stratasys’ Fortus 900 system has become the system of choice for production
of parts made in flame retardant, high performance Ultem 9085 (PEI) material,
produced by Saudi Arabia-based Sabic. In mid-2015, Airbus first announced that
as many as 1000 flight parts were 3D printed using Stratasys technology for
the A350 XWB aircraft. In 2016, the companies announced that Airbus had stan-
dardized on ULTEM 9085 for the production of flight parts for its A350 XWB
aircraft.
One very interesting new development that Stratasys is currently working on is
the industrialization of PEKK material for electrostatic discharge parts for outside
the cabin. This material has already been used as a custom developed material for
select customers and may soon become available commercially.
In early 2017, Etihad Airways Engineering received an approval from the
European Aviation Safety Agency (EASA) to design and certify 3D-printed parts
for aircraft interiors, becoming the first airline maintenance, repair, and overhaul
under EASA to hold certification approvals for 3D printed parts flying on Etihad
Airways aircraft.

15.4.4 Polymer bed fusion


While ideal for serial production of small parts, this family of technologies is lim-
ited in terms of size capabilities. Thus, the reality is that still today many polymer
powder bed fusion systems installed within the commercial aerospace industry are
utilized mostly for a variety of prototyping applications. However, this is changing
rapidly, many existing applications of these systems may transition to predomi-
nantly serving production roles for spare flight parts, and even serial production
applications. The opportunities for powder bed fusion in the aerospace industry is
set out in the Exhibit below.
Additive aerospace considered as a business 337

Opportunities for polymer powder bed fusion in commercial aerospace manufacturing


Opportunity Benefit Example
Replacement parts for Reduced need for tooling Plastic window breather pipe
older aircraft where resulting in lead time on BAE 146
previous tooling is no reduction and cost savings
longer available
Streamlining complex Reduces assembly times, ECS ducts for Boeing and
plastic assemblies number of pre-flight Northrop Grumman
checks
Viable replacement for PEEK and PEKK Structural components such
aluminum cast/milled thermoplastic powders as braces, hinges, brackets,
parts offer comparable as well as electrical boxes,
performance to aircraft housings, etc.
aluminum but with
significantly less weight
Source: SmarTech Publishing.

15.4.5 Composites
Composites are already accepted and widely utilized in the aerospace industry.
They are mostly carbon-based, glass-based, with the use of aramid and natural
fiber reinforced polymers being explored. However, the primary requirements
for composites in aerospace are for manufacturing of large parts, for which AM
processes are mainly experimental today. There is much hope for the future,
though.
Aerospace is probably the main adopter of composite materials and also one of
the primary industries for AM adoption and industrialization. These two aspects are
not necessarily related when it comes to 3D printing with composites today, as the
primary requirements for composites in aerospace are for manufacturing of very
large parts (which may be possible by AM in the long term, but is still only experi-
mental today).
The main types of composites that are used for aerospace are carbon fiber, glass,
and aramid-reinforced epoxy. But other types are also used such as boron reinforced
with a tungsten core. These materials are widely used for both structural applica-
tions and components and they are used in every kind of aircraft and spacecraft.
The benefits of using composites can be quite dramatic. For example, in an experi-
mental program, Boeing successfully used 1500 composite parts to replace 11,000
metal components in a helicopter.
Aircraft interiors are a good market for composites. While in some cases interior
parts may be subject to less exacting standards for manufacturing, they are certainly
no less important from the perspective of weight savings of aircraft. Because com-
posite manufacturing is a labor-intensive practice, several 3D printing companies—
including Stratasys, Cincinnati Incorporated, and various materials manufacturers—
have made significant investments in automating the process without sacrificing the
excellent mechanical properties of the fiber reinforced materials.
338 Additive Manufacturing for the Aerospace Industry

In traditional manufacturing methods for high-performance, fiber-reinforced


polymer matrix, composite structures require the use of hard tooling for the mold or
mandrel that dictates the internal part shape. These molds are traditionally made of
metal (aluminum, steel, or Invar alloys), although specialized composite materials
and high temperature tooling boards are also used. Regardless of material, fabrica-
tion requires significant labor and machining, leading to high costs, waste, and long
lead times consisting of weeks for relatively simple shapes and many months for
more complex tools.
Stratasys’ FDM industrial thermal extrusion technology has been successfully
used for lay-up and repair tooling applications for years, but was limited by the
lack of materials capable of withstanding the 350 F cure temperature frequently
required for aviation and aerospace structural demands. With the introduction of
Stratasys’ latest ULTEM 1010 resin, the technology has demonstrated numerous
new advantages for fabrication at process parameters in excess of 350 F and
100 psig.
FDM is thus becoming the technology of choice for rapid production of high
temperature ( . 350 F), low volume composite lay-up and repair tools. The
lay-up tools produced using FDM technology have similar design and use consid-
erations as traditional tooling, particularly those with higher coefficients of ther-
mal expansion. However, for more complex geometries where access is limited,
the part must be cured in two halves and then bonded together in a post-
processing step.
The use of Stratasys FDM technology for sacrificial composite tooling removes
many of these limitations by employing a proprietary, dissolvable thermoplastic
material called ST-130TM. FDM sacrificial tooling allows the production of a
composite part without a bonded seam. This means that it is created without any
additional support tooling and is removed hands-free, shortening lead times from
design to part.
FDM sacrificial tooling begins with the design of the tool, based on the design
of the final composite part. The sacrificial tool is then processed using Insight soft-
ware, which uses a custom fill pattern that was developed specifically for this mate-
rial to improve flow during the tool removal process. The sacrificial interior fill
pattern also provides adequate strength under autoclave temperatures and pressures
while shortening build time in the FDM system. Once the composite part is fully
formed and cured, removal of the tool is completed by submersing the part and tool
into the Stratasys support removal detergent solution.

15.5 Regulatory factors in additive manufacturing


aerospace
To date, aerospace companies, engineering associations, and government agencies
have made little progress in developing adequate industry wide accepted aerospace
standards and qualification/certification guidelines for AM materials and processes.
Additive aerospace considered as a business 339

Yet, studies have identified over 150 variables that may need to be controlled for a
given AM machine to produce stable and repeatable parts, demonstrating an
increased risk to the aerospace industry due to the lack of adequate standards.

15.5.1 Europe
EASA has released specific guidelines relative to implementation of AM in both
manufacturing and repair operations.
Under the guidelines, the applicant must demonstrate that a material is
suitable for the intended use of the part being fabricated and that the material is
being purchased per an approved material specification. Similarly, the applicant
must demonstrate, by test, the capability of the fabrication method to produce a
consistently sound structure that is performed under an approved process specifica-
tion. The applicant is also responsible for ensuring that design values used in the
evaluation of any parts produced using AM are applicable to the material and pro-
cess specifications used to fabricate the parts.

15.5.2 United States


In response to AM becoming prevalent in the aerospace industry, the Federal Aviation
Authority (FAA) has commissioned an Additive Manufacturing National Team. This
team is dedicated to applying a safety risk management philosophy for the identifica-
tion and application of AM as appropriate for high-risk products. The team also sup-
ports industry development of new standards and specifications for AM.

15.6 The geography of additive manufacturing


aerospace
North American aerospace manufacturers have led the way in purchasing and
developing solutions for AM in aerospace. This region’s association with polymer
print equipment from both 3D Systems and Stratasys seem to have given the region
a slight edge in this regard. Final part manufacturing activity seems to be more
active in North America with GE Aerospace, Pratt & Whitney, Honeywell, and
Boeing all actively pursuing AM.
Europe, led by Airbus, is catching up fast. Airbus also continues to utilize poly-
mer technologies from Stratasys for some final parts, while actively researching
industrialization of direct metal 3D printed parts through its internal “Bionic 3D
Printing” and other research projects. GKN Aerospace in the United Kingdom is
also producing DED AM parts for use in civil aircraft.
Meanwhile, Middle Eastern players, led by the “Big Three” airlines, have
recently entered the market, focusing specifically on production of flying, non-
safety-critical polymer AM parts for aircraft interiors. And, in May 2017, the first
Chinese built aircraft, the C919 from COMAC, successfully completed its maiden
flight with several non-flight-critical 3D printed metal and polymer parts.
340 Additive Manufacturing for the Aerospace Industry

15.7 Competitive implications of additive manufacturing


aerospace
In the past couple of years, as design for AM has become more widespread and
integrated into in aerospace engineering CAD software, more competitive advan-
tage won through design improvement have emerged in various aspects of the pro-
duction workflow and supply chain. It is possible that, in the long run, such
initiatives may be more sustainable than marginal weight reduction initiatives, since
they are harder and costlier to imitate.
Topology optimization has become commonplace in aerospace part design,
as have design improvements actuated through the use of highly optimized
software-generated shapes. As AM moves toward serial part production, signifi-
cant additional benefits can be derived from direct manufacturing of complex
sub-assemblies, as demonstrated by several proof-of-concept studies.
Airbus and GE have been especially influential in the AM aerospace business,
but other firms are also important. These include Stratasys, which is active in com-
mercial aviation applications with many different applications and technologies;
EOS; SLM Solutions; DMG Mori; and Trumpf. Some of Trumpf’s—and other—
metal powder or wire-fed systems are highly strategic for aerospace as they have
large chambers and very high deposition rates that can be sufficient for serial pro-
duction, meaning they can produce very large aircraft parts in little time.
Surface texture characterization
and optimization of metal 16
additive manufacturing-produced
components for aerospace
applications
Agustin Diaz
REM Surface Engineering, Brenham, TX, United States

16.1 Introduction
16.1.1 The basics of additive manufacturing surface texture
Additive manufacturing (AM) is an ideal option to produce fast and feasible proto-
type parts. Advancements in the field have allowed AM to become one of the lead-
ing technologies that can produce components that are often too difficult, if not
impossible, to obtain using classical subtractive manufacturing methods, and that
are not cost prohibitive [1,2]. The layer-by-layer addition of material to produce a
whole part, including the simultaneous assembly of multiple components, opens the
window of possibilities and innovation to design very complex, more efficient, and
lighter components. Two of the main advantages of AM technology are the consid-
erable decrease in manufacturing cost and time associated with building the parts,
advantages that are extrapolated to the applications of prototyping, quick testing,
and mass production [35].
Among the most widely used AM printing techniques is the powder bed method
[(PBM), such as electron beam melting (EBM), laser melting (LM), and laser sin-
tering (LS)], but other very popular techniques are getting traction in recent years
[6,7]. The versatility and reliability of the PBM makes it a perfect candidate to con-
struct complicated and more efficient components for the aerospace industry [7].
Nevertheless, PBM-produced components have a characteristically rich surface tex-
ture inherent of the building process, packed with many surface and near-surface
defects. Defects that can be encountered on these surfaces include: partially sin-
tered/melted powder, v-notches, surface and near-surface porosity, lack of fusion,
lack of penetration, delamination, slumping, and others that make them susceptible
to early mechanical failure and corrosion [811]. Consequently, post-processing,
and surface finishing of components built by this method are necessary in order to
obtain a functional part.

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00018-2


© 2019 Elsevier Inc. All rights reserved.
342 Additive Manufacturing for the Aerospace Industry

16.1.2 Surface anatomy of additive manufacturing components


The surface texture of a 3-D printed part using the powder bed melting/sintering
method is extremely complex (Fig. 16.1). The building process imparts a particular
fingerprint on the surface characteristic of PBM-built components that yields textures
unlike those observed on traditional subtractive metal parts, such a simple periodic
machining or honing marks. Moreover, different AM machines produce different sur-
face textures; however, there are several common surface texture features that are
present in almost all of the components produced by the PBM (vide infra). These par-
ticular surface texture features are the main components of the fingerprint, and the
degree of their presence on the surface is linked to the printing parameters, such as:
the hatch spacing, contour, powder size, source type, source power, scan time, layer
thickness, type of material, environment in the building chamber, orientation of the
component in the bed, and many others [1218]. In other words, by merely changing
one of these parameters during the PBM building process, one can obtain compo-
nents with particularly unique and varied surface textures.

Figure 16.1 Surface anatomy of a PBM-built component along the XZ, YZ (A and B), and
XY (C and D) planes, a diagram showing the different aspect of the surface anatomy features
(E) and the bottom of the component with their typical support and support-remaining
structures on the surface (F). In this example, the specimen is an EBM Ti6Al4V surface
built in an ARCAM A2X. PBM, Powder bed method; EBM, electron beam melting.
Surface texture characterization and optimization 343

Before we continue with the discussion, it is imperative that we define briefly


what surface texture is and what their constituents are (Section 16.2 will go into
deeper details on this subject). The texture of a surface is defined by the features
and irregularities that show deviations from the intended form/geometry of that sur-
face [19]. When a surface profile is collected, the obtained data is a surface texture
profile, which is a collection of these features and irregularities. The collected data
are deconvoluted using different fittings and filtering systems, which will subtract
the form/geometry of the surface and, based on surface spatial wavelength, will cal-
culate the roughness profile and the waviness profile. Details about the form fitting,
surface spatial wavelength filters, and best practices for surface profiling of AM
components will be discussed in Section 16.2. Based on these definitions, the sur-
face texture of an AM component can be dissected, and its anatomy can be exposed
and characterized.
The anatomy of the surface texture of PBM-built components shows four main
features that can be identified by taking a closer look at the morphology of the sur-
face (Fig. 16.1). There are other minor and less common artifacts, but they are not
going to be addressed in this chapter; they can be found in several reviews or books
on AM [2,11,15,2023]. The most predominant surface texture feature is located
on the XZ and YZ planes (being the build direction the Z axis) of the components
relative to the powder bed (the so-called vertical surface), while the other three are
located on planes that are nearly parallel (XY plane) to the powder bed (the so-
called horizontal surface) [2,12,24,25].
The first surface texture feature that will be described has been widely studied in
the literature and is the iconic surface that characterizes AM-built components, the
vertical surface. This feature is usually encountered in a vertically inclined plane
relative to the powder bed, and is always exposed and in contact with the powder in
the bed. Its main characteristic is a very spatial wavy component, often referred to
as the rough surface produced from the layering during the building process, and a
very rough surface composed of partially melted/sintered powder (Fig. 16.1A and B).
If there is a relatively pronounced inclination, this surface will show the so-called
staircase feature, and depending on the building orientation of the component
during the building process, the staircase feature can be encountered in two surface
regions: the upskin surface and the downskin (overhanging) surface (Fig. 16.1E).
The second surface texture feature is located at the bottom of the built compo-
nent (the very first layer of the component) that can be in direct contact with the
building plate, or in some cases is suspended by support structures (Fig. 16.1E and F).
In many occasions, this surface is cut by machining methods to retrieve the part from
the build platform, or the support structure is partially broken for the same purpose,
leaving behind remaining parts of the support structures connected to the AM compo-
nent (Fig. 16.1F). In these cases where support structures are employed, the downskin
(overhanging) surface will have specific features caused by the support structure
employed.
The third surface feature characteristic of PBM-built components is very similar
to the features already described; however, it is only present when the component is
suspended on support structures. This type of feature is usually encountered in the
344 Additive Manufacturing for the Aerospace Industry

downskin regions; however, in some cases, several parts are built on top of each
other, using the component at the bottom as the build platform. This type of feature
shows a very rough pattern, with lots of support structures remaining at the surface.
In addition, many times excess of partially melted/sintered/adhered powder is
attached to the support structures and to the surface of the component.
The fourth and last surface texture feature that characterizes PBM-built compo-
nents appears on the top surface, parallel to the bed. This feature is characterized
by the presence of the scan lines, melt pools and, in some cases, stair-case features
(Fig. 16.1C and D). The features and morphology characteristics of this top surface
will depend greatly on the printing parameters, such as source, power, hatch spac-
ing, contour, and powder size. In some occasions, some partially melted/sintered
powder can be encountered in this surface region embedded between the melted
pools, but is not frequent and it is in minimal amounts.
PBM-built surfaces show different patterns of roughness and waviness in each
one of the aforementioned surface features. The observed types of surface rough-
ness can be attributed to two different origins: (1) primary roughness, caused by the
solidification of the melt/sintering metal into pools sections (Fig. 16.1B—melting
pool); and (2) the secondary roughness, very predominant pattern, composed of par-
tially melted/sintered or trapped powder particles on the surface (Fig. 16.1B) [26].
By the same token, the waviness of AM-produced parts will vary with the direction-
ality of the building plane. A primary waviness can be identified on the top layer of
the part (XY plane) formed by the melting pool and the beam pathway (Fig. 16.1C
and D), and a secondary waviness produced in the layering-up process (Fig. 16.1A).
The former is often attributed to the layering effect in the building process. The
only problem with this assumption is that when the surface spatial wavelength is
measured, it is a complete order of magnitude larger than the layer thickness param-
eter used during the building process. The typical average layer thickness used dur-
ing the building process is around c. 70 μm for EBM and c. 30 μm for LS/LM
techniques. Nevertheless, the surface spatial wavelength of this component is
around 300500 μm (Fig. 16.1A). The origin of those waves is still not completely
understood, but it seems to be a synergistic effect between the penetration depths of
the source on the material (beam power), metal layers growth and curl, roller or
rake interaction, and machine vibrations. However, more research has to be done to
come with a final conclusion on the origin of those waves.
Due to the strong relationship between the secondary surface roughness and the
particles size, EBM-produced parts will have a rougher surface than LS/LM pro-
duced parts, as EBM-produced parts use particle sizes bigger than those used for
LS/LM. The average surface roughness (Ra) [using a contact profilometer with a
non-skidded 5 μm probe, following ISO 4288:1996 recommendation, with an evalu-
ation length (λn) of 12.5 mm and a long-wave cut-off filter (λc) of 2.5 mm, see
Section 16.2.2 for details] obtained by EBM is around 20 μm (B800 μin), while for
LS/LM is half of that. The roughness parameter obtained is proportional to the powder
particle size, which means that the secondary roughness dominates the profile in most
of the cases. In order to do a proper characterization and interpretation of the surface
texture profiles, the selection of proper cut-off filters is crucial, in order to specify the
Surface texture characterization and optimization 345

proper spatial wavelength. The proper selection of these filters will allow for the cor-
rect separation of the waviness profile from the roughness profiles, producing mean-
ingful surface roughness values. This will be the focus of the next section.

16.2 Best practices for surface texture characterization


of additive manufacturing components
16.2.1 Introduction
The surface texture of AM components is extremely rich, and it is filled with many
features that make them very challenging to characterize with the current technol-
ogy [2,27]. There is an active effort from the ASME-B.46 Project Team 53 and the
ISO/TC 261—ASTM F-42 committees to establish proper standard parameters for
surface texture characterizations of AM components. Nevertheless, despite these
efforts, the surface texture of AM components are very complex and there is a need
for new mathematical/statistical models to create appropriate fittings and filters to
analyze the collected topographical data. The main problem encountered with the
proper surface characterization of AM components is the fact that the partially
melted/sintered powder at the surface is taking over the surface profile collected,
with numerous gaps and re-entrant features.
If the surface texture of an AM-built component is observed closely (Fig. 16.1)
there are easily distinguishable features that can be used to define the surface tex-
ture components (Section 16.1). Consequently, in theory, if the surface roughness is
defined and governed by the partially melted/sintered powder, then the total height
of the surface roughness profile (ISO 4287 Rt parameter) can be defined by the
average powder particle size used to build the component, with an Ra (ISO 4287)
approximated to one-seventh of the Rt value, a very common approximation
between Rt and Ra [28]. In other words, by our initial definitions, for a component
built with Ti6Al4V powder (particle sizes in the 50100 μm range) by EBM,
the surface of which is visually full of partially melted/sintered powder, the Rt
value should be close to 100 μm and the Ra should be around 14 μm. These values
are actually very close to those obtained using a profilometer, and applying the
proper filters to deconvolute the true surface texture profile. In order to understand
the proper filters selection to separate roughness from waviness profiles, the same
examples and definitions will be used in the next sections. However, a brief review
on surface texture characterization and analysis will be explained using AM surface
features as an example to understand in more depth the best practices for cut-off fil-
ter selection, in order to specify the proper spatial wavelength.

16.2.2 Brief surface texture review


In order to understand the proper methods and best practices for surface texture
characterization of AM-built components, a brief review on surface texture
346 Additive Manufacturing for the Aerospace Industry

measurements will be discussed in this section. The surface texture is composed of


three main components: (1) form, (2) waviness, and (3) roughness. When a surface
trace profile is collected, all the above-mentioned features are embedded within the
data. Consequently, a fitting function to remove the form is applied, followed by a
filtering process to separate the roughness profile from the waviness profile
(Fig. 16.2). In a nutshell, because the surface trace profile encloses the form (geom-
etry/shape) along with the waviness and roughness, further data manipulation is
used to deconvolute each one of these surface components, which will then produce
the surface roughness profile and the ubiquitous parameter Ra.
The profile obtained from the direct measurement of the surface is called the pri-
mary profile, also known as the true profile (Fig. 16.2). The first step toward decon-
volution of the obtained data is the fitting of the primary profile; this will remove
the underlying geometry form (shapes) features, such as curves, tilting, etc. It is a
good practice to report the fitting model used on the profile analysis along with the
surface profiles. Fig. 16.2 shows the primary surface profile of an EBM-built
Ti6Al4V component, along with the optical topographical image. The obtained
profile is still complex, and it is composed of a combination of the waviness and
the roughness profiles. The waviness component of the surface texture is defined as
the long-spatial wavelength shape on the surface onto which the roughness is super-
imposed, while the roughness component is defined as the short-spatial wavelength
feature on the surface of the waves. In order to separate the roughness profile from
the waviness profile, a filtering function is applied to the primary profile
(Fig. 16.3). This filtering function is a critical part of the surface texture analysis,
and it is essential for the user to understand it in order to obtain correct surface
roughness and waviness values during the data analysis. There are many filtering
functions, but Gaussian filter is the most widely used, and is also recommended by
ASME and ISO standards (ISO 16610-21:2011). This filter will be applied using a

Figure 16.2 Typical contact surface primary profile (tip radius 5 μm, non-skidded, scan
length 17.5 mm and evaluation length 17.5 mm) of an Ti6Al4V EBM built part (left),
along with an optical image (top right) and its 3-D representation (bottom right). EBM,
Electron beam melting.
Surface texture characterization and optimization 347

Figure 16.3 Typical contact surface roughness (black) and waviness (red, marked with an  )
profiles [tip radius 5 μm, non-skidded, sampling length 0.8 mm, long-wave cut-off surface
spatial wavelength λc (Lc) 5 0.8 mm, scan length 17.5 mm and evaluation length 17.5 mm]
of an Ti-6Al-4V EBM built part (left), along with an optical image (top right) and its 3-D
representation (bottom right). EBM, Electron beam melting.

cut-off spatial wavelength (λc or Lc), which discriminates between roughness and
waviness. The λc filter is also known as the long-wave, or high pass cut-off filter,
since it filters the long surface spatial wavelength components of the profile. A
short or low-pass cut-off filter (λs) is also applied mostly to remove the electronic
noise from the instrument signal. For the sake of simplicity, this filter will not be
discussed, hence it does not have too much impact in the values that will be ana-
lyzed in our examples and analyses; however, is a best practice to report it along
with the profile and the roughness parameters values.
The correct selection of the long-wave cut-off filter is essential due to the role
this filter plays in dictating what the roughness and the waviness profiles will be;
hence, it will tremendously impact the values of the final roughness and waviness
parameters [such as Ra, Rt, Wa (average surface waviness), Wt (total height surface
waviness), etc.]. Fig. 16.4 shows the roughness and waviness profiles from the
same primary profile (Fig. 16.2) at different cut-off filters. The impact of the selec-
tion of this long-wave filter can be observed in the progression of the profile as the
cut-off filter changes. Shorter cut-off filters will have lower roughness parameter
values with higher waviness values, while longer cut-off filters will have the oppo-
site effect. The dramatic effect that the selection of the long-wave cut-off filters has
on the values for Ra, Rt, Wa, and Wt can be pictured on Table 16.1. It is important
to mention that all the values obtained in Table 16.1 belong to the same primary
profile, originating from the same trace and surface shown in Fig. 16.2. At this
point, a direct conclusion that should be drawn from this discussion is that any
roughness or waviness value reported in the literature without the specification of
the cut-off filters used is meaningless! Unfortunately, an overwhelming amount of
publications found in the literature report roughness values without specifying the
surface spatial wavelength cut-off filter.
Based on this discussion, the main question should be: what is the proper filter
for AM surface texture characterization? The answer to this question remains open,
348 Additive Manufacturing for the Aerospace Industry

Figure 16.4 Contact surface roughness (black) and waviness (red, marked with an  ) profiles
(tip radius 5 μm, non-skidded, scan length 17.5 mm and evaluation length 17.5 mm) of a Ti-
6Al-4V EBM built part at different cut-off filters (λc 5 2.5, 0.8, 0.25, 0.08 mm from top to
bottom). Scale: square is 20 m height and 1 mm wide. See Table 16.1 for the Ra, Rt, Wa,
and Wt values for each profile after filtering. EBM, Electron beam melting.

Table 16.1 Ra, Rt, Wa, and Wt values for the same surface using different cut-off (λc)
filters

λc Filter (mm)a 2.5 0.8 0.25 0.08


Ra (μm) 20 13 6 1
Rt (μm) 142 94 54 31
Wa (μm) 9 17 22 24
Wt (μm) 49 94 131 155
a
Gaussian filter.

as no measuring standards have been developed due to the difficulty associated


with characterizing non-periodical, complex, and granulated surfaces that character-
ized AM surfaces. Nevertheless, the filter to use for the surface characterization of
the component should always be provided and specified by the design engineer in
the blueprint, and should be in accordance with the functional application for the
component. However, this requirement is rarely followed and, in most cases, the
design engineer or the final user requests only an Ra value, without any type of
Surface texture characterization and optimization 349

specification. These practices make it extremely important to re-emphasize that an


Ra value without the cut-off filter used [also referred as roughness sampling length
(lr) because they typically share the same numerical value (lr 5 λc)] is meaning-
less! Nevertheless, there are some best practices that we can follow in order to
define the proper filter to fit the data, such as the assumptions that we employed in
the introduction of this section to estimate the Ra of an AM component. Based on
the aforementioned definition for our specific case, in which the surface roughness
is composed of partially melted/sintered powder and the waviness is the “layering”
feature, the total height of the roughness should be close to the average particle
size. Therefore, the proper filter to be used to analyze the surface trace of that com-
ponent should be the 0.8 mm filter according to Fig. 16.4 and Table 16.1, which
will produce an Rt and an Ra of 94 and 13 μm, respectively, in perfect agreement
with our surface roughness definition. In the next section, we will expand on the
rationale employed to characterize the surface texture of AM-built components.

16.2.3 Surface texture characterization of additive


manufacturing components
16.2.3.1 Introduction
As we mentioned before, there are no specific standards to follow in order to do a
proper surface texture characterization of AM-produced components, but there is a
vast amount of literature addressing this issue that can be used as guidance [2].
Moreover, there are some basic steps that can be followed to get the best possible
information from the obtained surface profile. The first point to address is the differ-
ent techniques that can be used to interrogate the surfaces and discuss in brief their
advantages and limitations. There are two main types of technologies available in
the market to generate a surface profile: the contact and non-contact profilometers.

16.2.3.2 Additive manufacturing surface characterization by


contact profilometry
We will begin our discussion by addressing the most basic and most widely used
profilometer in the industry, the contact profilometer [2]. This technique works by
the direct interaction (contact) of a probe tracing the surface, generating a two
dimensional (2-D) data set of heights over a certain length of the surface. In this
type of measurement, factors such as the probe size, shape, and skidded gages
(waviness suppressed) are important and need to be specified when reporting mea-
surements (best practice). Nevertheless, a considerable limitation of the contact
probe method is that the probe will not be able to capture surfaces covered by
inclined peaks (re-entrant), and the deepest features on the surface; this hampers the
proper surface interrogation of AM components (Fig. 16.6). In addition, the charac-
teristic granular surface of AM surfaces frequently causes jumps and temporary
loss of contact, and, in some cases, lateral drifting of the probe, producing
350 Additive Manufacturing for the Aerospace Industry

misleading data (Fig. 16.6) [29]. Nevertheless, contact profilometry is a very pow-
erful tool and lots of information can be extracted from a proper trace [2].
One of the best ways to characterize an AM surface using a contact profilometer
is by tracing the surface orthogonal to the build direction, so the waviness feature
of the “layering” is captured (Fig. 16.5). Nevertheless, the design engineer should
specify in which direction the tracing should be done (ISO 1302:2002).
Furthermore, the traverse length should be as long as possible for surfaces with this
rich and significant texture (ISO 4288:1996). Ideally, an evaluation length (λn) of
40 mm is recommended for AM components with roughness over 10 μm, with a
sampling length (lr) of 8 mm, when made possible by the geometry of the part and
the limitations of the instrument. Realistically, that is a very long trace length and
most instruments do not have the capacity for it. Moreover, many components will
not have an accessible surface that is long enough to allow for a 40 mm trace, or
that is within the height range of the profilometer. Consequently, an evaluation
length (λn) of 12.5 mm with a sampling length (lr) of 2.5 mm is acceptable, and
should be enough. This way most of the features from the surface can be captured
and analyzed accordingly (Fig. 16.5).

Figure 16.5 Visual representation of the surface features captured from a cross-sectioned
EBM-built IN-625 component at different traverse lengths (evaluation lengths from top to
bottom 1.25, 4.0, and 12.5 mm). EBM, Electron beam melting.

Figure 16.6 Optical image of a transversal polished cut of an EBM-built IN-625 component
showing by the arrows the inaccessible surfaces areas to trace by contact and optical
profilometers. EBM, Electron beam melting.
Surface texture characterization and optimization 351

Fig. 16.5 shows a visual representation of the surface captured at different tra-
versal lengths, along with the evaluation lengths (λn) and possible sampling lengths
(lr) for that surface. It is evident that the longer the trace, the more features are cap-
tured and the more room to look for the proper filters (longest sampling lengths).
Note that the equivalent of 1/2 of the sampling length is usually subtracted from
each one of the extreme ends of the traverse length to avoid the distortion that
occurs when the filtering functions are applied during the data analysis process
[29]. Notice that a short tracing with an evaluation length (λn) of 1.25 mm, cannot
use certain long-wave cut-off filters (λc), such as the 2.5 mm filter. The importance
of the long tracing length on AM-built components resides not just in the capacity
to capture most of the surface features, but also in the capability to apply different
long-wave cut-off filters to evaluate the best one for a specific surface.
One of the most accurate and best methods to select the proper filters (λc and
λs) for a particular surface is the analysis of the surface spatial wavelength content
of the trace (Fig. 16.7). This very helpful tool comes with certain software packages
used for surface metrology data analysis, such as OmniSurf from Digital
Metrology. Fig. 16.7 shows the surface spatial wavelength content for the trace dis-
played in Fig. 16.3, with a 0.8 mm long-wave cut-off filter selected. The surface
spatial wavelength content graph shows the distribution of spatial features on the
trace. A periodical surface characteristic of traditional machined or honed surfaces
will show a clear bimodal distribution in the spatial wavelength content spectrum.
At the interface of the two distributions, a spatial wavelength is selected to deter-
mine the cut-off filter. It is important to emphasize that this procedure is only appli-
cable to traces obtained with a non-skidded probe. In the case of AM-built
components, the distribution is quite complex; nevertheless, a bimodal distribution
can still be identified. Based on this spatial wavelength content graph, the cut-off
filter was selected at 0.8 mm. Further analysis of the selected long-wave cut-off fil-
ter on the spatial wavelength content graph indicates this filter is reasonably suited

Figure 16.7 Surface spatial wavelength content graph from the surface trace in Fig. 16.3.
The green cut line shows the position of the cut-off filter (at 0.8 mm) delimitating the
roughness profile wavelengths (red curve, marked with an R) from the waviness profile
wavelength (blue curve, marked with W).
352 Additive Manufacturing for the Aerospace Industry

for this specific surface, since it filters out almost the entire long spatial wavelength
components of the trace. This can be seen under the blue curve, and correspond to
the waviness profile (Fig. 16.7). By the same token, all the shorter spatial wave-
length components are under the red curve, confined to the roughness profile.
Moreover, additional analysis of the long-wave cut-off filter identified by this
method showed an excellent agreement with the previously discussed methods that
also identified a long-wave cut-off filter of 0.8 mm.

16.2.3.3 Additive manufacturing surface characterization by


non-contact profilometer
The non-contact profilometer can be 2-D or 3-D; however, the 2-D non-contact pro-
filometer produces the same kind of data set as the already discussed contact profiler
(Section 16.2.3.2). Consequently, the 2-D non-contact profile can be analyzed follow-
ing the same aforementioned best practices. On the other hand, the discussion of this
section is mainly focused on the surface characterization of AM components by 3-D
areal surface metrology. The 3-D optical surface metrology is gaining fast traction on
the surface characterization and analysis of AM components [2,15,20,30]. There are
different 3-D optical surface metrology technologies on the market, including confo-
cal microscopy, coherence scanning interferometry and focus variation microscopy,
among others [2]. However, the details behind each of these technologies, their
advantages, and limitations are beyond the scope of our discussion.
The great advantage of using 3-D optical surface metrology for AM-built
components resides in the massive amount of information and high level of details
collected in the process. Nevertheless, proper selection of the evaluation area, of
the form suppression, and of the filtering operations is essential to obtain real and
meaningful information out of the surface interrogation, just as in the case of
the 2-D surface profiles. There are a vast number of publications on the use of this
technique for the characterization of AM-built components, and the reader is
encouraged to read the original work for further details [2,15,20,31,32]. However,
there are no standards established for the surface characterization of AM surfaces
using this technique. Consequently, in the case when the design engineer does not
specify the surface texture characterization parameters in the blueprint, a similar
approach to the one used before should be employed to determine surface rough-
ness parameters with meaningful values. Briefly, the form is fitted to remove the
part’s shape from the profile (a flattening operation), and then nesting indexes
filters (analogs to the long-wave and short-wave filter) are employed to separate the
roughness component from the waviness component (ISO 25178-3).
At this point, we can use the same approach previously explained for the best
practices to collect and analyze the surface profile of an AM component. The first
step to ensure proper data collection and analysis is the collection of an appropriate
evaluation area, which should be as big as possible. At least an area equal to
2.5 mm 3 2.5 mm is needed to do the correct analysis of the surface, ensuring the
collection of enough surface features and details; however, bigger evaluation areas
are highly encouraged [20]. Fig. 16.8 shows a typical non-contact 3-D optical
Surface texture characterization and optimization 353

Figure 16.8 Typical non-contact 3-D optical surface measurement of a Ti6Al4V EBM-
built component. EBM, Electron beam melting.
From suppressed.

surface profile of an EBM-built Ti6Al4V surface, with a captured area of


5.1 mm 3 5.1 mm, flattened by least-square mean plane. In this example, the eval-
uation area (4.3 mm 3 4.3 mm) was big enough to capture the wavy pattern from
the “layering,” and the rich roughness from the surface. The captured areal surface
measurement can be deconvoluted into the roughness and waviness components to
visualize each component with different long-wave and short-wave nesting indexes
filters, which are similar to the λc and λs filters explained before (Section 16.2.3.2).
The roughness and waviness surface wavelength components for this surface can be
observed in Fig. 16.9, where a 0.8 and 0.25 mm long-wave nesting indexes filters
were employed. The difference between them is very significant, and it can be appre-
ciated by comparing the waviness components obtained from two different cut-off fil-
ters. The 0.25 mm cut-off filter shows a stronger waviness component, as was the
case for the 2-D profilometer data analysis. Table 16.2 shows the areal surface rough-
ness parameter for this surface using different nesting indexes filters.
The data analysis for this 3-D surface map can be simplified by converting the
data into multiple 2-D surface profiles and applying the same filters explained
before for the 2-D primary surface profile (Section 16.2.3.2). Remember to capture
the 2-D profile from the 3-D profile in an orthogonal direction to the surface “layer-
ing” features. Now we are faced with the most challenging and confusing part of
the process, the correct filter selection. By following the logic of how the surface
was defined in principle, and given that the surface we are using as an example is
the same used for the contact profilometer measurements, we know that the Ra
value should be around 13 μm, and the Rt should be around 94 μm. Table 16.2
shows the Ra and Rt surface roughness parameters, which were extracted from the
non-contact 3-D optical surface’s measured, and compared to the previously
obtained contact profile by using different filter lengths. In addition, the surface
area roughness parameters Sa and St (counterpart to Ra and Rt for 2-D surface
354 Additive Manufacturing for the Aerospace Industry

Figure 16.9 Non-contact 3-D optical surface measurement [roughness spatial component
(left) and waviness spatial component (right)] of a Ti6Al4V EBM-built component using
two different cut-off filters. EBM, Electron beam melting.

Table 16.2 Sa, St, Ra, and Rt (from contact and non-contact profiles) values for the same
surface using different cut-off (λc) filters

λc Sa Rad Rad St Rtd Rtd


Filter (µm)b (non-contact) (contact) (µm)c (non-contact) (contact)
(mm)a (µm) (µm) (µm) (µm)
0.25 15 12 6 243 119 54
0.40 19 13 8 245 90 70
0.80 24 19 13 259 144 94
2.5 30 25 20 269 159 142
a
Gaussian filter (ISO 16610-21:2011).
b
ISO 25178-2.
c
ASME B46.1.
d
ISO 4287:1996.

analysis) are reported. It can be seen that the analysis with the previously used
0.8 mm filter did not correlate with the expected results. A shorter filter of 0.25 mm
seems to have a better correlation with the data previously analyzed by contact profi-
lometry, and with the expected results based on our initial definition of the surface.
Nevertheless, as mentioned before an analysis of the surface spatial wavelength
content is one of the best tools available to determine the best filter for this measure-
ment. The spatial wavelength content analysis shows a clear bimodal distribution
with a node at c. 0.40 mm of spatial wavelength, which is the best filter for this
Surface texture characterization and optimization 355

Figure 16.10 Surface spatial wavelength content graph from the surface profile in Fig. 16.7. The
green cut line shows the position of the cut-off filter (at 0.4 mm) delimitating the roughness profile
spatial wavelengths (red curve, marked with an R) from the waviness spatial profile wavelength
(blue curve, marked with W).

measurement (Fig. 16.10). Now the correlation of the surface roughness values
obtained from the contact and non-contact profilometers are in a notable agreement.
The use of this filtering selection exercise enables us to get a better idea of the real
conditions of the as-built surface, but it should be noted that further surface and near-
surface analyses show a more complex system that is almost impossible to measure
with the techniques discussed so far in this section (Fig. 16.6).
X-ray computer tomography scan (XRCT-scan) can be used to get a better idea
of the real conditions of the surface and the near-surface regions [2,23,27,3338].
This new trend, used to perform a complete survey of the surface and near-surface,
is gaining traction in the academic realms, where there is more budget and time-
frame flexibility. However, this technique is more expensive and time consuming
than other techniques, and needs a significant amount of data manipulation to
obtain a proper surface profile. Despite these facts, XRCT-scan has a great advan-
tage over the previously discussed techniques since it collects data from all the sur-
faces, including the internal and non-accessible surfaces (Fig. 16.6). XRCT-scan
allows for non-destructive 3-D surface measurements, but in order to be viable for
surface metrology the resolution has to be at the sub-micron level [27]. The data
analysis can be complicated, but once the data are collected, they can be analyzed
by the previously discussed 3-D non-contact surface measurement procedure.

16.3 Surface finishing of additive manufacturing


components
16.3.1 Introduction
It is of general knowledge in the aerospace community that the mechanical proper-
ties of a component will depend on their surface texture integrity. The as-built AM
356 Additive Manufacturing for the Aerospace Industry

components have too many surface defects and stress raisers to be mechanically
robust; therefore, a post-printing process, or, in many instances, processes, is
needed to make the parts functional. In order to improve the surface texture of the
components, the partially melted/sintered particles, melt pools, and surface defects
have to be removed or at least minimized. Employing a purely mechanical process,
such as machining, honing, grinding, blasting, or even tumbling, will have difficul-
ties accessing all of the surfaces and will not uniformly remove the imperfections
from the surface. Moreover, the highly complex geometries and free-form capabili-
ties of AM-built components make them very challenging to surface finish using
the classical techniques. Nonetheless, the more post-processing steps that have to
be employed to achieve a better surface, the more the process will deviate from the
AM advantages and benefits, such as short time and cost-effective processing, thus
defeating the purpose.

16.3.2 Basics of surface finishing to take into account before


printing
There are various factors that the design engineers and final users need to take into
account before printing a component to allow for a proper surface finishing. The
first and most important of these factors is the final application of that component,
and the type of surface texture needed for its functional application. It is a best
practice to include these requirements in the blueprint, specifying the required sur-
face roughness, along with the preferred surface finishing technique. In addition,
the blueprint should include the measurement indications for the surface texture
analysis with the fitting and filtering methods to be used to calculate the surface
roughness and waviness parameters (ISO 1302:2011). As a rule of thumb, the
design engineer should specify the surface texture for the specific functional appli-
cation of the designed component and the metal removal allowance for surface
finishing.
One of the most important aspects that the design engineer needs to take into
account is the amount of extra metal to be added to the surface (also referred as sac-
rificial metal or material) to compensate for the metal removal during the finishing
process. Most of the surface finishing techniques are subtractive, meaning that there
will be significant removal of the surface metal (depending on the requirements for
initial to final conditions) which could potentially throw the component out of toler-
ance. The actual amount of sacrificial metal will greatly depend on the initial condi-
tions of the surface texture, the geometry of the component, the final surface
texture needed, and the surface finishing technique of choice. Different surface fin-
ishing techniques remove different amounts of material on different areas of the
component, depending on their functional targeting mechanism (details of this
action mechanism will be discussed in Section 16.3.3). Moreover, certain surface
finishing techniques, especially the mass finishing techniques, might remove metal
from different areas of the components at different rates, creating a non-
homogenous surface metal removal throughout the component. Preferential metal
Surface texture characterization and optimization 357

removal on the edge of the components is always an issue with mass finishing tech-
niques, such as vibratory and tumbling finishing; however, fixture assistance can be
employed to protect the sensitive regions on the components, when necessary,
avoiding the rounding and edging of the components. In addition, the surface
removal rates of different surface finishing techniques are affected by the special
features on the AM-built surface because they hamper the access of the finishing
mechanism action onto those areas (e.g., abrasive media action on narrow surface
features). Some finishing techniques will have preferential surface removal of the
AM-built vertical surface (refer to the surface feature discussion in Section 16.1.2),
composed mostly of partially melted/sintered powder, while others will be more
efficient on different types of surfaces, such as the AM-built horizontal surface
(refer to the surface feature discussion in Section 16.1.2). However, all of these
issues can be taken into account, and certain iterations with the component can be
done to match the process to the surface finishing technique of choice. In other
words, the process can be optimized to add extra material to the most accessible
areas of the surface, thus allowing for the areas where the surface removal is the
slowest to get finished. This will produce a final component within tolerance and
with the desired surface texture. It is a best practice for the design engineers to get
in contact with their surface finishing suppliers or operators to discuss all of these
aspects of the design before printing the component.
The surface roughness parameter Rt (total height of the profile- vertical distance
between the highest peak height and the lowest valley depth along the profile evalu-
ation length) and the dimensions of the powder particle size can be used to deter-
mine the amount of sacrificial metal needed to achieve the desired finishing.
Fig. 16.11 shows a simplistic scenario of the relationship between the surface tex-
ture and the metal removal necessary to produce the desired surface roughness on
that surface. In this example, the Rt value is stipulated as 400 μm, meaning that
there is a maximum height of 400 μm from the top of the highest peak to the bot-
tom of the lowest valley. This implies that in order to produce a smooth surface, at
least 400 μm of metal need to be removed from the surface, and it can be compen-
sated by overgrowing the component with that amount of additional material.

Figure 16.11 Representation of the surface obtained by the metal powder melted/sintered
method and the subsequent metal removal, necessary to produce a smooth surface.
Highlighted by the dotted square is a valley full of partially melted/sintered powder covered
by a peak on the top.
358 Additive Manufacturing for the Aerospace Industry

At this point, it is imperative that we discuss very important aspects that might
have been partially discussed in previous sections. Note that removing the same
amount of metal as the Rt value from the surface will not remove the partially
melted powder and the melting pool features of the surface. First of all, assuming
that the profilometer was capable of perfectly tracing the whole surface, which is
physically impossible (Fig. 16.6), the bottom of the valley is delimited by the top of
at least one powder particle. Therefore, in order to produce a smooth and defect-
free surface, the height corresponding to the diameter of the particles embedded
into the valleys needs to be added to the total amount of metal to be removed from
the surface. These types of surface features can be observed in Fig. 16.11,
highlighted in a dotted blue square where various peaks are covering some valleys
filled with partially melted/sintered particles (see also Fig. 16.6). In summary, in
order to remove all of the partially melted/sintered powder from the surface and
from the valleys, a total surface metal removal of at least the Rt value plus 1.5 times
the average powder particle size must be achieved. For this example, a total of
500 μm (assuming an average powder particle size of 65 μm) will yield a smooth,
defect-free surface; barring any near-surface defects, such as porosity, that could
appear during the finishing process. For instance, in a study published by Sun et al.
[14], the authors concluded that 650 μm of surface removal was necessary to elimi-
nate all the detrimental surface defects for an EBM-built Ti6Al4V component.

16.3.3 Surface finishing of additive manufacturing components


For the aerospace industry, the mechanical performance of AM-built components is
of vital importance due to the critical implications of early failures. In most cases,
the culprit of all failures resides in the surface, and in the case of AM-built compo-
nents, this is not an exception. Surface defects, such as notches, partially melted/
sintered powder, microcracks, and porosity are very common on the AM-built sur-
faces, and they will prompt early mechanical failure under stress. In order for these
components to be approved for use in aerospace applications, these entire surface
defects need to be eliminated.
There are several reports in the literature addressing the surface finishing of
AM-built components by several methods. However, the discussion in this section
will be limited to surface finishing processes that have been successfully tested on
fatigue experiments, which is the main priority for the aerospace industry. This dis-
cussion will be centered on the mechanisms of surface improvement and the practi-
cality of the surface finishing techniques that can be applied in the aerospace field.
Therefore, the review of fatigue testing of machined specimens will be limited, and
used just as a reference point in this section due the impracticality of this technique
for mass production. Moreover, it is important to mention that the comparison of
fatigue data from different sources is extremely difficult, due to the countless
variety of variables that change between studies and methods. One of the most
common factors that makes this comparison so difficult is the fact that many studies
correlate their experiments and discussion of the results based on an Ra value.
These Ra values are typically reported without specifying vital information about
Surface texture characterization and optimization 359

the surface trace, such as evaluation length (λn), sample length (λc), probe size,
skidded vs non-skidded, etc. [2,39]. As mentioned before, the Ra value without this
vital information is meaningless and in many cases can be very misleading. In addi-
tion, there are several fatigue testing methods, stress ratios, specimen geometries,
and printing processes, which make the collection and classification of the data
very challenging and, to a certain extent, makes every study unique. Nevertheless,
Tong et al. [39] did an amazing data collection of most of the testing and results
reported in the literature in their review article.
One the most relevant studies addressing the effect of surface finishing on the
mechanical performance of an AM-built component was reported by Bagehorn
et al. [40] in a collaborative work between Airbus Group Innovations and the
Institut für Werkstoffkunde (Materials Science), Leibniz Universität Hannover. This
group performed a series of surface finishing techniques followed by a high cycle
fatigue testing (axial, R 5 0.1) on HIPped (hot isostatic pressure) Ti6Al4V spe-
cimens printed at 45 without support structure in an EOS M270 machine. They
tested the effectiveness of the surface finishing process [milling (machined), blast-
ing, vibratory, and a micro-machining] on the fatigue performance of the speci-
mens, compared to the as-printed specimen. They concluded that even though the
fatigue properties of all the surface finished specimens improved, there is still room
for improvement. The milled specimens outperformed all other surface finished
specimens by over 30%, and the as-built specimens by over 60%. Further surface
analysis showed that milled specimens had fewer amounts of surface defects; how-
ever, they did not report the amount of metal removed for each one of the subtrac-
tive finishing processes. Nonetheless, the use of a milling process on mass
production AM-built components is highly impractical, costly, and time consuming.
Even though the other surface finishing techniques did not perform as well as the mill-
ing process, they showed promising results, being the more practical techniques for
high throughput mass processing capabilities. Furthermore, the authors reported sig-
nificant differences between the surface roughness values (Note: the authors of this
article did not report any of the surface fitting or filtering used to produce these
values; however, the authors specified that they followed DIN EN 4287.) obtained for
the different surface finishing techniques: blasting (Ra 5 10 μm), vibratory
(Ra 5 1 μm), and a micro-machining (Ra 5 0.4 μm). As a matter of fact, this surface
roughness did not correlate with the observed fatigue testing, showing a different ten-
dency with run-outs for blasting at 525 MPa, vibratory at 575 MPa, and a micro-
machining at 500 MPa. Fracture analysis by scanning electron microscopy (SEM) of
the specimens showed surface defects as the main cause for the crack initiation sites.
It is important to mention that both micro-machining process and the vibratory process
took around 50 hours to finish, while the blasting was around 7 minutes. Nevertheless,
an advantage of the vibratory finishing process over the other three techniques studied
is its batch processing capability. Vibratory finishing is capable of accommodating
thousands of specimens in the same cycle, without the need of any fixture aids and
with minimal operator interaction, making this technique very cost effective.
The aforementioned study is a perfect example of the effect of pure mechanical
surface finishing on fatigue performance. In theory, mechanical surface finishing
360 Additive Manufacturing for the Aerospace Industry

alone targets the peaks on the surface, reducing (or smashing) the peaks until the
process reaches (or fills) the valleys. The problem with these surface techniques is
that often they miss the deepest valleys and notches on the surface, therefore leav-
ing significant stress raisers on the surface. On the other hand, surface finishing by
physicochemical and mechanical-chemical mechanisms yield better surface textures
for mechanical performance. The use of chemically-assisted surface finishing pro-
cesses has the potential to reach deeper on the surface, thus targeting more effi-
ciently the stress raisers.
Another study, from Benedetti et al. [41], investigated the effects of surface fin-
ishing by shot peening, vibratory, and electropolishing on the fatigue performance
of LM/Ti6Al4V ELI. In this study, not all the surface-finished specimens were
HIPped; hence they had mixed results. In this case, early failure due to near-surface
porosity, not corrected by the HIPing process, was observed. Nevertheless, they
were able significantly to reduce the surface roughness [Evaluation length of 4 mm
by contact profilometer, no probe details, nor cut-off filter mentioned, but by rule
of thumb, can be assumed that is a fifth of the evaluation length (by default func-
tion in the instrument), λc 5 0.8 mm.] by applying vibratory finishing followed by
electropolishing. By using a combination of these techniques, the Ra was reduced
from c. 7 μm to a remarkable Ra of 0.54 μm. The fatigue performance (high cycle
axial fatigue test R 5 21) for the vibratory finishing, followed by electropolishing
of the specimen, was 14% better than the as-built component, but it was signifi-
cantly outperformed by the specimens subjected only to vibratory finishing or shot
peening. Other than this aforementioned study, and even though there are many
publications on electropolishing of AM-built components (mostly porous struc-
tures), there is a void on reporting and studying the mechanical performance of
electropolished AM-built components [4245].
The chemical milling process (also called chemical polishing, etching, or pick-
ling) is another physicochemical surface finishing technique that has a profound
effect on the surface texture and fatigue performance on AM-built specimens. In
theory, the chemical polishing process should work similarly to the electropolishing
process, in which the electropolishing process is an electrolytic process (non-spon-
taneous, ΔG . 0) and the chemical polishing is a galvanic process (spontaneous,
ΔG , 0). The main limitations of this technique are the environmental impact,
high cost of the chemicals, danger to the operator, waste handling, and costly dis-
posal. Nonetheless, chemical milling effectively removed the excess powder from
the surface of an EMB-built Ti6Al4V tensile strength specimen, improving its
surface texture [14]. In a study performed by Sun et al. (a collaboration between
the Centre for Additive Manufacturing from the RMIT University, and the
Commonwealth Scientific and Industrial Research Organization, both in
Melbourne, Australia), a simple, but elegant, experimental design was employed to
investigate the correlation between surface texture reduction by chemical etching
and the tensile strength properties of EMB-built Ti6Al4V components. Upon
surface finishing by chemical etching with a hydrofluoric acid and nitric acid solu-
tion [3:6:100 HF(48%):HNO3(70%):H2O, Kroll reagent] for 2 hours, a significant
improvement was observed, with a doubling of the tensile ductility and an increase
Surface texture characterization and optimization 361

in the ultimate tensile strength (UTS) and yield strength (YS) of 15%. In addition,
the authors determined that 650 μm of metal removal was necessary to eliminate all
the surface and near-surface defects from the surface (see Section 16.3.2) [14].
Unfortunately, there was no fatigue testing on this study; but, based on the theory,
these components should perform very well under mechanical stress due to the
elimination of stress raisers from the surface [33,34,46,47].
The final surface finishing technique that will be addressed is the chemically
accelerated vibratory finishing (CAVF). This process was patented and developed
by REM Surface Engineering in the 1980s and it has continued to evolve since
then, gaining great acceptance in the aerospace field [4853]. This process has
been demonstrated to be one of the best approaches to employ when surface finish-
ing AM-built components, in which the surface is chemically-activated, due to a
mechanical stimulus the surface roughness and defects are removed. The CAVF is
the basic principle behind REM’s Extreme ISF Process, a proprietary process also
developed by REM Surface Engineering to improve the extreme surface textures
characteristic of AM-built parts [32,53,54]. This process targets the removal of the
loosely attached and partially melted/sintered powder particles on the surface, and
polishes the surface by removing melted pools. The process typically removes up to
seven times the average particle size from the metal on the surface (around
400 μm) in order to eliminate all the surface defects. One of the limitations of
vibratory finishing is that the media employed has to reach the surface with a cer-
tain force to create an abrasive action and eliminate the peaks. In cases where the
surfaces are inaccessible, the media cannot achieve the necessary force; thus, no
effective action occurs. However, this is not the case for the CAVF, where the
chemistry homogeneously reaches the entirety of the surface, and the media just
needs to contact the surface with a gentle rubbing action to remove the chemically-
activated metal surface. This simple, yet elegant, approach considerably reduces the
rounding, edging, and heterogeneous surface removal problems faced by the vibra-
tory and tumbling finishing processes. Furthermore, the CAVF has shown a dra-
matic effect on the mechanical performance of AM components by eliminating
surface defects and v-notches from the surface. The next section will be dedicated
to the discussion, with a case study, of these results.

16.4 Additive manufacturing-built components surface-


finished by the Extreme ISF Process
16.4.1 Introduction
As mentioned in the preview section, the Extreme ISF Process for surface finishing of
AM components is capable of significantly reducing the surface texture by targeting
it from different flanks. The combination of the chemical activation of the surface
with the mechanical action of the media in a vibratory bowl is capable of eliminating
the surface defects and stress risers associated with early mechanical failure. In this
362 Additive Manufacturing for the Aerospace Industry

section we will discuss some results and examples of the capability of this process,
and their implication on the mechanical performance of AM-built components.

16.4.2 Examples of surface treated by the Extreme ISF Process


The surface of an EBM-built Ti6Al4V component before and after the first and
final cycle of the Extreme ISF Process can be observed in Fig. 16.12. The first
cycle of the process targets all the surface roughness features associated with the
building process of the PBM, while the second cycle targets all the surface wavi-
ness components. The process uses different chemistries specially designed for each
alloy, at various concentrations under different reactions conditions, according to
the initial state of the surface. The media selection in the vibratory bowl is carefully
chosen to target the surface features that need improvement and to ensure a homog-
enous surface removal. In a certain way, the Extreme ISF Process is a mixture
between a highly technical and controlled science and the art of surface optimiza-
tion by vibratory finishing.
The surface shown in Fig. 16.12 is from a bike seatpost designed by Spencer
Wright and built in an ARCAM A2x EBM machine, in collaboration with AddAero
Mfg. (Fig. 16.13) [55,56]. A total surface removal of 300 μm (0.01 in.) was needed
to eliminate all the stress raisers from the surface. Note that the internal cavity sur-
face of the component was not the primary target of the process because this

Figure 16.12 Optical microscopy 3-D images of a Ti6Al4V surface obtained by EBM
and the subsequent surface after the first and final cycle of the Extreme ISF Process. EBM,
Electron beam melting. Note, the height scales are widely different in each image.

Figure 16.13 EBM-built Ti6Al4V bike seatpost (10 cm long) before and after the Extreme
ISF Process (left) and the SEM image of the surface before and after the Extreme ISF Process
(right). In collaboration with Spencer Wright and AddAero Mfg. EBM, Electron beam melting.
Surface texture characterization and optimization 363

surface is a functional surface that needs to be glued to a carbon fiber post and
needs the waviness surface texture to allow for the proper adherence. The Ra went
from 34 μm [λc 5 2.5 mm and λn 5 12.5 mm, as ISO 4288:1996, contact profil-
ometer and non-skidded (5 μm) probe] to 1 μm [λc 5 0.8 mm and λn 5 12.5 mm,
contact profilometer and non-skidded (5 μm) probe], for a 97% surface roughness
improvement. (Note that the λn for the surface finished surface is not following the
recommended ISO 4288:1996 guidelines, but it is a lot longer than the recommended
length. This best practice will ensure the capture of as many surface features as pos-
sible, even after the surface finishing process of the AM-built component.) The total
processing time was under 24 hours, and this technique is capable of processing as
many parts as necessary (more than 10,000 if necessary), since the process takes
places in a vibratory bowl that comes in many different sizes and configurations.
Another good example is the surface finishing by Extreme ISF of an EBM
Ti6Al4V Rocket Nozzle (ARCAM A2X) in collaboration with AddAero Mfg.
(Fig. 16.14) [54,57,58]. This project demonstrates the capabilities of the Extreme
ISF Process applied to the aerospace field. The as-built component is c. 28 cm
height, 11 mm diameter across the combustion chamber, 4 cm diameter across the
throat, and 9.6 cm diameter at the exit. The surface roughness of the component
was reduced from an Ra of 25 μm to an Ra of 0.08 μm in the exterior and an Ra of
2.2 μm in the interior, for a 99.6% improvement of surface roughness in the exterior
and a 91% in the interior. Surface traces evaluated with the following parameters
(contact profilometer and non-skidded probe):
1. Initial trace . λc 5 2.5 mm and λn 5 12.5 mm, as ISO 4288:1996
2. Final trace exterior . λc 5 0.25 mm and λn 5 12.5 mm
3. Final trace interior . λc 5 0.8 mm and λn 5 12.5 mm
The total process time was around 48 hours, with the capability of processing
several components at the same time.
The presented examples showed the potential of the Extreme ISF Process to
surface-finish AM-built components. The process is capable of significantly

Figure 16.14 AddAero Mfg. Ti6Al4V Rocket Nozzle (EBM-ARCAM A2X) surface-
finished by the Extreme ISF Process (A) and the stereolithography (STL) showing the
cooling internal channels (B), AddAero Mfg. Ti6Al4V Injector Assembly (EBM-
ARCAM Q20 1 ) (C) and computer-aided design (CAD) Model of the full Rocket Assembly
[D(a)] Injector Assembly [D(b)] Rocket Nozzle. EBM, Electron beam melting.
364 Additive Manufacturing for the Aerospace Industry

reducing the surface texture of the AM-built components with the capacity to pro-
cess several components at the same time, making the technique cost effective.
Corollary 16.6 (see Section 16.6) shows different alloys AM-built components pro-
cessed by Extreme ISF, showing the potential of the technique to process different
types of alloys from different PBM. The next section will be focused on the
improvement of the mechanical properties of the components surface-finished by
the Extreme ISF Process.

16.4.3 Improvement of the mechanical properties of additive


manufacturing-built components by Extreme ISF Process
Surface finishing of AM-built components can potentially improve their mechanical
performance if the stress risers are eliminated. In the previous section, this issue
was addressed using different surface finishing techniques with mixed results. In
this section we will discuss the mechanical properties of AM-built components that
were surface finished by the Extreme ISF Process. In general, the process is
designed to target the stress raisers, such as the v-notches, melt pools, partially
melted/sintered powder, and minicracks on the surface. The first step of the
Extreme ISF has demonstrated to be enough to produce significant improvement of
the mechanical performance, even though it does not significantly reduce the Ra
value. However, this first step eliminates the stress raisers, thus has a profound
impact on the mechanical properties of the component.
Diaz et al. [32] studied the tensile strength of EBM-built Ti6Al4V components,
printed in a vertical and horizontal configuration, processed by the first cycle of the
Extreme ISF. The surface roughness (Ra) of the components was reduced by 35% for
the horizontal specimens, and 62% for the vertical specimens [measured by using a
contact profilometer, non-contact probe, long cut-off filter (λc) of 2.5 mm, as recom-
mended by ISO 4288-1996 for a 12.5 mm trace]. Nevertheless, the UTS and YS of
the processed specimens improved from 1007 and 945 MPa in the as-printed horizon-
tal specimens, to 1034 and 979 MPa in the processed horizontal specimens; and from
945 and 841 MPa in the as-printed vertical specimens to 1000 and 945 MPa in the
processed vertical specimens. These results are in complete agreement with those
reported by Sun et al. [14] for the surface finishing of the same types of specimens.
The fatigue improvement of AM-built specimens surface-finished by the
Extreme ISF Process was an open secret communicated to REM Surface
Engineering by its customers, but there was no actual data sharing. There have been
a couple of presentations on the RAPID show and MS&T conferences where lim-
ited data was presented by REM’s customers, showing the significant fatigue
improvement. Witkin et al. were the first group officially to report the performance
of AM-built Ti6Al4V specimens processed by the Extreme ISF Process. The
specimens processed were selective laser melting (SLM)-built Ti6Al4V notched
fatigue specimens (Kt 5 3) and EBM-built flat dog-bone specimens [59,60]. It is
important to mention that the specimens were not overgrown to compensate for the
metal removal of the surface finishing; therefore the surface removal was limited to
Surface texture characterization and optimization 365

Figure 16.15 SEM images of the EBM fatigue specimen at the fracture and on the side,
showing the depth of the surface defect and surface morphology in the before and after
specimens. EBM, Electron beam melting.

200 μm for the EBM specimens, and 100 μm for the SLM specimens, which is far
from the 650 μm optimal metal removal recommended (Fig. 16.15) [14].
Nevertheless, even though the surface-finished EBM specimens were 400 μm thinner
(and the surface-finished SLM specimens 200 μm thinner) than the as-built counter-
parts, the results showed that they significantly outperformed the as-built specimens.
Moreover, the results showed that the SLM-notched specimens processed by the
Extreme ISF Process doubled their life and endurance limit compared to the as-built
components (high cycle axial fatigue, R 5 0.1). By the same token, the EBM speci-
mens showed a 10-fold increase in life improvement compared to the as-built speci-
mens, with a doubled endurance limit. However, fracture analysis showed that the
crack initiator comes from imperfections at the surface for all of the specimens,
which would have been significantly reduced with extra metal removal.
The Ra of the surface-finished EBM specimen was 14 μm [λc 5 2.5 mm and
λn 5 12.5 mm, as ISO 13565-1:1996, contact profilometer and non-skidded (5 μm)
probe] vs an Ra of 21 μm for the as-built specimens, for a reduction of 25%. In the
case of the SLM surface-finished specimens, the Ra was 0.5 μm [λc 5 2.5 mm and
λn 5 12.5 mm, as ISO 13565-1:1996, contact profilometer and non-skidded (5 μm)
probe] vs an Ra of 7.5 μm for the as-built specimens, for a reduction of 93%.
Interestingly, these Ra values do not correlate with the mechanical performance of
the tested specimens, especially the Ra of the surface-finished EBM specimens.
This phenomenon seems very consistent with the fatigue studies of AM-built com-
ponents, where the stress raisers from the surface cannot be easily identified due to
the complexity of their surfaces. Nevertheless, the v-notches are still the stress rai-
sers that dominate the fracture initiation and their effect is dependent of their geom-
etry (depth, radius, and the v-angle of the lower points) [33,34,47,60]. In the next
section, we will address other surface roughness parameters that better correlate
with the mechanical performance of AM-built specimens.

16.4.4 Further analysis of surface texture parameters associated


with mechanical performance
It is well known in the industry that the Ra value does not always correlate with the
mechanical performance of the components. The Ra parameter is a shapeless
366 Additive Manufacturing for the Aerospace Industry

parameter that accounts for the height of any surface feature within an spatial wave-
length bandwidth selected by a cut-off filter. Nevertheless, there is significant corre-
lation between the surface texture and the mechanical performance of the
component; it is just that the simplistic Ra parameter cannot capture the essence of
that correlation. There is an active area of research looking for a roughness parame-
ter that can prove functionality toward mechanical performance. Perhaps the surface
roughness parameter Rv (maximum profile valley depth, ISO 4287:1997) is a better
parameter to correlate with mechanical performance, since it can relate to the
notches on the surface and crack initiation [34]. However, the Rv parameter seems
to be too simplistic to encompass all the crack initiation phenomena, since it is still
a unidimensional (height) parameter that does not take into account the geometry of
the notch. Nevertheless, there are some hybrid parameters, mostly coming from the
3-D non-contact profilometer, that could help us understand and predict the
mechanical performance of a component based on its surface texture. In general,
these parameters combine the amplitude and spacing features of the surface textures
and describe the surface area.
One of these parameter is the developed interfacial area ratio (Sdr, ISO 25178-
2:2012), defined as the ratio of the increment of the interfacial area of a surface
over the sampling area [61]. This parameter basically establishes the relationship
between surface area and flatness, property reflecting the texture of the surface.
When the surface is perfectly flat, the Sdr becomes zero (0); if the spatial complex-
ity on the surface texture increases, then the Sdr value will increase. A large Sdr
value indicates the significance of either the amplitude or the spacing, or both inde-
pendent of the Sa value. For example, after surface finishing of an AM-built com-
ponent by the Extreme ISF Process, a significant reduction of Sdr of two orders of
magnitude was observed. Quantitatively, the as-built Ti6Al4V EBM compo-
nents showed a Sdr of 175% with an Sa of 24 μm and an Ra of 20 μm, while the
components processed by Extreme ISF showed a Sdr of 4.3% with an Sa of 6 μm
and an Ra of 14 μm vs a machined (from the as-built) component that showed a Sdr
of 2.4% with an Sa of 0.9 μm and an Ra of 1.2 μm [32]. This is also the case with
the root mean square surface slope (Sdq) parameter, comprising the surface evalu-
ated over all directions (ISO 25178-2:2012). This parameter also provides a very
good assessment of the conditions of the surface texture. Reduction in the Sdq value
is indicative of an improvement in the surface roughness, due the fact that Sdq is
affected by texture amplitude and spacing. However, this improvement cannot be
appreciated from the Sa value alone (see Fig. 16.16) [62]. For this parameter, the
as-built Ti6Al4V EBM components showed a Sdq of 65 with an Sa of 24 μm
and an Ra of 20 μm, while the components processed by Extreme ISF showed a
Sdq of 17 with an Sa of 6 μm and an Ra of 14 μm vs a machined (from the as-
built) specimen that showed a Sdq of 13 with an Sa of 0.9 μm and an Ra of
1.2 μm [32]. Those samples were tested for their tensile strength and the Extreme
ISF-processed specimens outperformed the as-built and the machined components,
although the Sa and Ra values did not show a change as significant as the one
observed for the machine component. Therefore, the Sdr and Sdq did show a closer
relationship with the tensile stress results [32].
Surface texture characterization and optimization 367

Figure 16.16 Surfaces with similar Sa values showing evident difference on surface
textures, easily differentiated by the Sdq parameter.
Source: Taken with permission from: Michigan Metrology, LLC, “Glossary of Texture
Parameters,” 2014.

16.5 Conclusions
AM is an ideal option for the aerospace industry to produce complex geometries,
with optimized weight reductions and cost effectiveness. However, there is a signif-
icant surface roughness associated with the printing process. These surfaces are
very difficult to characterize and to analyze. There are a series of steps that can be
followed as best practices to try properly to report surface roughness values in the
literature. Nevertheless, this surface can be optimized by different surface finishing
processes, but sacrificial metal must be added to the part to allow for surface finish-
ing. For optimal mechanical performance, a surface finishing technique capable of
removing surface stress raisers, such as notches and partially melted/sintered pow-
der, is highly desirable. Different surface finishing techniques have demonstrated to
improve the mechanical performance of additive-manufactured components.
However, the collection of studies on this matter is highly variable, using different
fatigue tests on various types of materials for different alloys with different surface
finishing processes. In addition, the measurements of the surface roughness reported
in the literature are difficult to understand due to the lack of proper information
necessary to give a meaningful value to the reported surface roughness parameter.
Moreover, there is a clear need for more standardized data showing a clearer view
of the effect of surface finishing on the mechanical performance of the components.

16.6 Corollary
This corollary section shows other alloys printed by different AM PBM and
surface-finished by the ISF Process to give the reader a more ample perspective of
the capabilities of the process (Figs. 16.1716.23).
Figure 16.17 Ti-6Al-4V DMLS-built followed by shot peening.

Figure 16.18 17-4 PH SS DMLS-built.


Figure 16.19 15-5 PH SS SLM-built (EOS M 270).

Figure 16.20 316L SS SLM-built (EOS M 270).


Figure 16.21 Maraging steel SLM-built (EOS M 270).

Figure 16.22 IN-625 SLM-built (EOS M 270).


Surface texture characterization and optimization 371

Figure 16.23 IN-718 SLM-built (EOS M 270).

Acknowledgments
The authors want to give special thanks to Dr. Donald Cohen and Michigan Metrology,
LLC, for his advice, edits, time, and for kindly performing the optical profilometer mea-
surements. Special thanks also to Bill Yost and Joyce Hyde from GelSight, for generously
generating the metrology data using their GelSight elastomeric sensor to capture high-
quality pictures of the surface. The author wants to thanks Dr. Jeniree Flores for her help
and insight on editing the chapter from a non-expert perspective. Moreover, the author is
deeply thankful to Matt Bell for his help on editing and correcting the document.

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Developing and applying ICME 1
modeling tools to predict 17
performance of additively
manufactured aerospace parts
Brain W. Martin, Thomas K. Ales, Matthew R. Rolchigo and
Peter C. Collins
Department of Materials Science and Engineering, Iowa State University, Ames, IA,
United States

17.1 Introduction
Integrated computational materials engineering (ICME) may be described as a gen-
eralized design framework that permits the prediction of relevant materials proper-
ties and performance of a given material and geometry subjected to a given set of
boundary conditions that represents either a processing route or a lifetime of ser-
vice. ICME integrates computational models and experimental data, often spanning
across length and time scales. Successful ICME efforts permit engineering decisions
to be made. Given that performance is comprised of statistical representations of
individual properties, a perfect set of models is not required. Indeed, an “80% cor-
rect” set of models may provide a sufficiently accurate measure of performance to
enable an engineering decision to be made (i.e., the goal of ICME efforts).
The adoption of additive manufacturing (AM) into systems requires an approach
for the informed qualification of processes and materials in an accelerated manner.
ICME is an appropriate strategy to pursue to achieve such informed (and acceler-
ated) qualification, as AM is a relatively new manufacturing approach, and does not
have decades of historical data that is captured in a designers knowledge base.
Notably, ICME frameworks can be quite individualized. The simulation tools and
data that may be necessary for one ICME effort may not be necessary for another.
Thus, what is presented in this chapter is an example of tools that may be integrated
into an ICME framework for AM of metallic materials. To establish an ICME
framework, it is necessary to understand the problem, and understand the key con-
nections that require the integration of models and data. Thus, we first must con-
sider the commonalities (and differences) between AM processes.
AM may be generally described as any process that consists of the computer-
controlled movement of a process zone in which new material is added volume-by-
volume until a desired net- or near-net-shape part is produced. This definition (In
principle, this definition can also accommodate emerging solid-state AM processes,
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00019-4
© 2019 Elsevier Inc. All rights reserved.
376 Additive Manufacturing for the Aerospace Industry

although that is not the subject of this chapter.) is sufficiently broad, and easily
accommodates all metal-based AM processes, which may have quite different
energy (heat) sources (e.g., lasers, plasmas, or electron beams), environments
(atmosphere, vacuums), and build rates.
Fig. 17.1 provides a simple schematic showing the interaction between three pri-
mary variables associated with fusion-based AM processes. These three variables,
along with the incoming feedstock (e.g., powder, wire) affect the physical processes
during deposition. For example, a process that occurs under vacuum is likely selec-
tively to lose certain alloying elements, depending upon their vaporization tempera-
tures/partial pressures relative to those of other alloying elements. Alternatively, it
is reasonable to expect that processes that occur under atmosphere would poten-
tially getter trace interstitial elements (e.g., oxygen, nitrogen) from the inert atmo-
sphere, depending upon the partial pressures and processing temperatures. The
thermodynamics of the incoming material has a strong effect. For example, steel
and aluminum can be processed under atmosphere or inert shield gases, whereas
titanium requires high purity inert gasses or vacuum. Consequently, these changes
in chemistry should be captured in an ICME framework for AM.
Fig. 17.2 shows a proposed ICME framework for fusion-based AM processes,
and Table 17.1 gives more details about the components that may be part of an inte-
grated set of models to predict the fusion zone. It is important to note briefly that
not all of the details, including specifically the thermophysical properties, are
known for the temperature ranges relevant to these processes, as they often exhibit
significant superheats.

Environment

Possible Possible Most AM


not process
Atmosphere process processes

Possible Possible Possible


not process process
process

Possible Possible
Arcam not process
Vaccum process
Energy source
Low (<1 lb/h) e am am m
nb be bea
tro sm
a
er
ec s
El Pl
a La
Possible Possible
Sciaky not process
High (>15 lb/h) process

Build rate

Figure 17.1 General schematic of different regimes of fusion-based AM processes. AM,


Additive manufacturing.
Developing and applying ICME 377

Probabilistic
modeling
(design allowables)

Integrated multiphysics fusion Physics-based


process model property model
Energy–material–environment–
Constitutive equations
Chemistry
interactions* CP/FEM
Input Melting:
Previous layer Shape of Defects
composition new material molten pool
S->S phase transf.
Melt pool physics
(surface tension*, microstructure
viscosity*, convection) Phase field
Rules-based
State-of-matter interactions*
Solidification
Data-based
(G–L, L–S, G–S)
(GS, texture)
Part distortion
Heat-transfer
Phase transformations

Figure 17.2 Linkages in a generalized ICME framework. ICME, Integrated computational


materials engineering.

indicates aspects of a model which are themselves dependent upon the instantaneous
condition of the simulated material state (e.g., temperature).

Given that the principal utility of an ICME framework is to enable an engineer-


ing decision to be made, it is clear that not every element of this proposed ICME
framework is necessary for every problem. For example, if the primary objective of
executing an ICME framework is to predict the residual stress of a component, it is
possible to arrive at a reasonably accurate prediction by considering the heat-
transfer and macroscale thermal fields. However, if the primary objective is to pre-
dict the end composition (One of the challenges associated with the insertion of
additively manufactured aerospace materials into applications is the fact that the
composition changes during melt processes. Interstitial content will change, and for
some processes and alloys, the fraction of primary alloying elements will also
change (e.g., Ti6Al4V processed under vacuum can lose a large amount of its
Al content due to preferential vaporization). Thus, the end fabricator may be
responsible for certifying part composition.) of a component, other models are
required in an ICME framework.
For the purposes of this chapter, we will focus on a slightly simpler ICME
framework, shown in Fig. 17.3. This framework informs the structure of this chap-
ter. Assuming an input composition, we will first describe how certain physics of
the process can be understood and modeled. These physics include: heat flow in
both the melt pool and the whole part; fluid dynamics effects; and macroscale
effects from uneven heating and cooling on the whole part. Once the process effects
are understood and simulated, it is then possible to predict both chemistry and
microstructure (influenced by both chemistry and the complex thermal history)
within the final part, including an understanding of the nature of solidification and
Table 17.1 Selected details of aspects that might be included in a fusion process model

General category of physics Details and examples


in the fusion zone
Energymaterial interactions Reflection, absorption, surface topographies where
reflected energy at point X is absorbed at point Y,
pressure/stress from income energy on liquid surfaces,
ionization of elemental species in proximity to the
interface
Materialenvironment Volatilization/absorption of certain elements and the
interactions attending changes in local stresses and temperatures at
the liquidenvironment interface when species leave/
absorb
Energyenvironment Scattering of incoming energy due to plumes and
Interactions ionized material
Melting All of the physics of melting processes, including mass
and thermal driven convection (Marangoni flow), melt
pool shape, formation and collapse of keyholes,
gravity, buoyancy, and the thermophysical properties
that influence these processes (e.g., surface tension,
viscosity, density)
Interfacial Interactions GL: volatilization/absorption, details controlled by
between states of matter spatial distributions in elemental species and
temperatures on both sides of interface, possible
quantum effects. GS: gaseous species “plating” of
atomic species as they cool and potential solid-state
absorption of interstitial elements such as oxygen and
nitrogen when the solid is at a very high temperature.
LS: solidification/melting
Heat flow Primary heat flow modes (convection, conduction,
radiation). Secondary heat flow modes due to surface-
mediated processes, such as volatilization/absorption.
Effects of heat flow on solidification and subsequent
solidsolid phase transformations; part distortion;
defect formation

Input Process Chemistry


composition model model

Physics-based
property model
Constitutive equations
Microstructure
model

Probabilistic
modeling
(design allowables)

Figure 17.3 Simplified ICME model that has been developed and applied for Ti6Al4V.
ICME, Integrated computational materials engineering.
Developing and applying ICME 379

reheating in AM builds. Once chemistry and microstructure are predicted, there


have been models developed to predict properties, and subsequently performance,
from microstructural and chemistry quantification as it varies within an AM part.
We conclude by presenting some gaps in our current understanding, and thus our
modeling capabilities.

17.2 Part 1: Process modeling


Our general understanding of the AM process, as it relates to final part properties,
can be ascribed to two main regimes. The first relates to the overall thermal history
of the final part, as well as uneven cooling rate and thermal histories resulting in
residual stresses within the part. The complex localized thermal histories are also
discussed, as a result of multiple reheats. This same regime, including the multiple
reheats, is responsible for the solid-state phase transformations that lead to complex
microstructures. The second regime includes the physics of the melt pool itself,
which involves a complex multiphysical environment where heat flow (convection,
conduction, and radiation) is coupled with fluid flow, mass transport, resulting in
such complex phenomena as Marangoni convection and PlateauRayleigh instabil-
ities that can lead to the formation of defects.
The motion of the high-energy, highly localized heat source and relatively low
heat conduction of some metals (including titanium, a critical alloy for aerospace
components), results in large thermal gradients (G 5 |rT|) during the AM process.
The motion of the highly localized heat source results in a complex thermal field
that deviates from simple, Cartesian coordinate based thermal fields. Given that
most AM processes involve multiple layers, with the heat source passing over pre-
viously solidified material, and it is clear that there is complex temporal nature to
the thermal history. The theses of Kelly [1] and Ales [2] and the seminal works of
the team of Denlinger, Martukanitz, and Michaleris [35] provide important
modeling details to capture the thermal history of additively manufacturing, and
some of the macrolevel effects (e.g., thermal cycling and thermal distortion).
Due to expansion on heating and contraction on cooling, parts produced using
AM often are affected by the creation of residual stress fields within each layer and
across the entire part. While the exact nature and scale of these residual stresses
depends on the part geometry, build rate, heat input, and thermophysical properties
of the material, it is possible to draw some conclusions. For aerospace structural
alloys, within each layer, cyclic expansion and contraction results in tensile stress
at the top of the layer and compressive stress at the bottom. Collins et al. [6] com-
piled multiple modeling efforts to quantify the residual stresses present. The trend
in terms of material type is higher stresses in Ni-based alloys (400800 MPa),
lower in Ti alloys (100200 MPa), and even lower in Al alloys (25 MPa) [7].
Consistently, the tensile stresses within each layer were found to be greater than the
corresponding compressive stresses. These macroscale residual stresses, which are
fundamentally associated with gradients in strain-accommodating defects, such as
380 Additive Manufacturing for the Aerospace Industry

dislocations, result in the large-scale distortion found in finished parts. One obser-
vation that has been made is that the size of the melt pool, which corresponds
directly to the energy density of the build, was found to correspond directly with
the residual stresses. A larger (and therefore hotter) melt pool resulting from slower
build rates and/or a larger input power leads to higher thermal gradient.
Experimental and modeling confirms that large thermal gradients result in higher
residual stress. In one example, Martukanitz et al. [3,8] used data from in situ tem-
perature measurements made during electron beam deposition of a 107 layer part.
Data from the melt pool measurements were fed into a sophisticated thermal model,
resulting in data that agrees with 3D scan distortion measurements (Fig. 17.4) [3].
In addition to the macroscopic distortion, the high levels of residual stress can
result in cracking, layer delamination, or hot tearing either during or after deposi-
tion. There are at least two possible origins for these high residual stresses. First,
the spatially varying cyclic thermal histories will result in local thermal distortion

(A) 60
Distortion (mm)

40 Experiment Simulation
20
0
–20
–40
–60
3500 3000 2500 2000 1500 1000 500 0

X-coordinate (mm)

5.00+01
(B)
4.50+01

4.00+01

3.50+01

3.00+01

2.50+01

2.00+01

1.50+01

Z 1.00+01
Y
5.00+01
X
0

Figure 17.4 (A) Experimental versus computational comparison of part distortion in a large
AM build and (B) graphical representation of computational results [3]. AM, Additive
manufacturing.
Developing and applying ICME 381

due to the coefficients of thermal expansion. Second, for materials with solidsolid
phase transformations, the repeated excursions through the solid phase transforma-
tions may lead to crystallographic strains that cannot be rapidly (and repeatedly)
accommodated by the matrix crystal phases, resulting in the formation of defects.
Interestingly, the formation of large residual stresses in a part may also have further
effects on phase transformations not only in systems with strain-induced phase
transformations (e.g., some types of martensites), but also in variant selection in
alloys such as Ti6Al4V.
For the purposes of the simplified example ICME outline shown in Fig. 17.3, we
focus on the thermal history and its influence on the resulting chemistry and micro-
structure. As noted previously, other articles and theses deal very effectively with
thermal modeling (e.g., [15,913]). Regarding the effects of the various physics
of the molten pool and solidification, some very exciting modeling results have
emerged over the past few years, and we present the generalities of this past
research briefly.
There has been a large body of work focused on the complex physics within the
melt pool, especially in recent years [1417]. Regarding these physics, the first
consideration is the distribution of the heat within the molten pool, which is often
(but not necessarily) modeled as a Gaussian distribution [1820]. This ideal input
distribution is likely rarely accurate, owing to scattering of incident photons or elec-
trons by the vapor clouds and both “static” and dynamic powder in both powder-
blown and powder bed systems [15] (Fig. 17.5A). Further complicating these
energy inputs is the fact that the absorptivity (often assumed to be an extrinsic vari-
able) does change with surface temperature and surface topography, and is another
physical factor that is considered in the modeling of this process. Knapp et al. [18]
used a model to study the effect on the final part of the input power (see
Fig. 17.5B), where the model included heat flow via radiation and conduction, mass
input, fluid flow, and a moving heat source. In this work (and reassuringly), even
excluding loss of mass via vaporization, the geometry of a single pass agrees with
experimental results of nominally identical parameters, as seen in Fig. 17.5B.
Another important physical process present in all AM systems is the Marangoni
Effect. This is a mass flow fluid mechanics effect, where a gradient in surface tem-
perature results in a force. In AM systems, this gradient in surface temperature is
due to the presence of a steep thermal gradient. Often, the Marangoni Effect is
responsible for the large amount of convection present in the melt pool and thus the
primary means of ensuring chemical homogeneity in the melt pool.
Models of powder bed fusion process have shown the effect of Marangoni con-
vection on the geometry and motion within the melt pool [16] (see Fig. 17.5C).
When the models are executed with a temperature independent, constant surface
tension, a nonphysical bulbous melt pool is generated. While this melt pool shape
can give some insight into the process [18], accounting for Marangoni allows the
modelers to move closer to the reality. Others have demonstrated that accounting
for the jet of metal vapor further changes the shape and motion of the pool. The
study of this jet of vapor can lead to interesting insights as to otherwise unpredicted
effects of the state of the build chamber environment. Matthews et al. [17] studied
(A) 0.8 (B) Temperature (K)
14.0
1000 1693 1733
0.6

Height (mm)
13.5
50 (mm/s)
α 0.4 13.0
Total
Spheres 12.5
0.2 Substrate
12.0
2.0 1.5 1.0 0.5 0
0.0 Width (mm)
0 500 1000
Temperature (K)
Distance (μm) 14.0
1000 1693 1733

Height (mm)
13.5 50 (mm/s)

13.0

12.5

12.0
2.0 1.5 1.0 0.5 0
Width (mm)

(C) Homogeneous laser Laser ray tracing 40 Constant surface tension Recoil + Marangoni
deposition 30
20
Liquid 10
0
–10
–20
–30 (ii) (iii) Marangoni effect (iv)
Solid Point contact –40
(i) Flat contact 60 80 100 120 140 160 180 200 220 240 60 80 100 120 140 160 180 200 220 240 60 80 100 120 140 160 180 200 220 240
shadow

Figure 17.5 (A) calculated absorptivity (a) for a bimodal powder bed, with the incident beam size given by the circles on the insets [15]; (B) calculated
deposit shape, size, with information regarding temperature and fluid flow also provided immediately adjacent to transverse cross sections of as-deposited
316 L stainless steels at different powers (1500 W top and 2500 W bottom) [19]; (C) incremental inclusion of additional physics, showing the increase in
model fidelity as heat transfer, melt pool depth, and fluid flow are all mediated by the additional physics that are noted in each sub-image [18].
Developing and applying ICME 383

Figure 17.6 (A) Micrographs and (B) confocal height maps with varying argon pressure
[17].

the effect of changing the argon pressure on a powder bed AM system, and found
that this had a profound effect on the melt pool and powder available to be melted
(Fig. 17.6). Larger positive argon pressure suppressed the negative pressure of the
vapor jet and contributed to more metal powder being pulled into the melt track. As
the argon pressure was taken to low values, the vapor jet was able to blow metal
powder away from the melt track, and resulted in piled-up powder along the track.
This vapor jet within the melt pool also leads to another important phenomenom
in the AM process, which is the cyclic formation and collapse of a keyhole. With
sufficient power input, the metal vapor within the melt pool can form a deep, nar-
row hole, which cyclically collapses and reforms, and can trap porosity in the build.
This is most pronounced in the extremely high input power in electron beam pro-
cesses, where the keyhole can even result in plasma jets that further complicate the
process and any associated modeling effort [21,22]. Modeling of the keyhole has
also been useful for predicting porosity in builds, with high speed camera imaging
of the keyhole collapse and reform serving to verify the process models further, in
both electron beam and laser systems [23]. Thus, porosity can result from both
incomplete melting of the feedstock (i.e., when the energy density is too low, and
insufficient for to achieve fusion) and the cyclic keyhole formation and collapse
(i.e., which the energy is too high and causes elemental vaporization/volatilization).
With respect to the subsequent solidification, generally speaking, solidification
models can be ascribed to one of four main approaches: (1) process map models;
(2) phase field models; (3) cellular automata models; and (4) kinetic Monte Carlo.
The process map models typically start with concepts of heat transport and then
384 Additive Manufacturing for the Aerospace Industry

60,000 Δt 100,000 Δt 135,000 Δt


(0.0153 s) (0.0255 s) (0.0344 s)
(A) (B) (C)
Model 15
including
fluid flow

10
20 µm

(D) (E) (F)


15
Control
runs
without
fluid flow
0

Figure 17.7 Solute profiles in a TixW system for models (A-C) including and (D-F)
excluding fluid flow under different time steps in the model (real times in parentheses) [33].

calculate values of the thermal gradient (G) and the velocity of the solidliquid
interface (R), enabling the formulation of the so-called GR plots that provide
maps of the predominate types of microstructures based upon the operating solidifi-
cation mechanisms. These approaches have been adopted for both titanium and
nickel-based alloys [12,13,2426]. Researchers pursuing phase field modeling for
solidification have often coupled the phase field method with finite element model-
ing to calculate the macroscopic temperature fields [27,28]. Cellular automata has
seen increased use (see an example showing the influence of calculated fluid flow
in Fig. 17.7), as it is based upon a relatively simple framework where rules evolve
over time, and can also capture some of the fundamental aspects of thermodynam-
ics and diffusion [2934]. The regular grid of cellular automata models is also ben-
eficial, as it enables it to be linked with finite element methods that give the
thermal gradients. Kinetic Monte Carlo [35,36] is the least well-explored method,
but seems to show some promise for accurately predicting grain boundaries in mul-
tilayered AM builds.

17.3 Part 2: Predicting chemistry


The composition of structural alloys has a strong influence on not only the micro-
structure, but also directly on the mechanical properties through mechanisms such
as solid-solution strengthening. Indeed, in previous work [37,38], it has been shown
that the composition can be attributed to between 70% and 90% of the strength
Developing and applying ICME 385

displayed by Ti6Al4V. As noted previously, the fact that fusion is the basis for
current AM processes, it will be necessary to understand and predict chemistry of
AM products. The final composition will likely be different from the starting com-
position, due either to interstitial pickup in atmosphere (including inert atmosphere)
or solute loss due to preferential vaporization under vacuum. In addition to these
macroscale effects, it is also necessary to consider the partitioning of solute species
during solidification. Both composition effects will be considered below.

17.3.1 Solute loss (vaporization) or pickup (gettering)


Previously, we have reviewed compositional variations found in many AM parts
[6]. Since the AM process is a melting and solidification process, certification of
the input material does not guarantee the final part will retain that chemistry. The
presence of interstitial elements (e.g., oxygen, nitrogen, hydrogen) in the atmo-
sphere, even in trace amounts (e.g., partial pressures in inert atmosphere), can have
a pronounced effect on microstructure and mechanical properties. The use of metal
powder feed, with its high surface-to-volume ratio, can exacerbate this problem as
interstitial elements often lead to nanometer scaled surface layers, such as oxides or
nitrides. Titanium, for example, is extremely susceptible to oxygen pickup, where
oxygen serves to increase strength and lower ductility of titanium alloys. The miti-
gation of these effects can manage in the process environment, where a clean build
chamber and careful control of the partial pressures of certain elements within the
atmosphere can reduce any chemistry changes due to interstitial pickup.
With regard to elemental loss during the process, it has already been established
that the melt pool sees extremely high, localized temperatures. For AM techniques
that occur under vacuum (e.g., electron-beam-based AM techniques), such high
temperatures combine with the low pressures of the build environment and results
in preferential vaporization of certain elements [6]. This evaporation of elemental
species is related to the partial vapor pressure of the individual elements. The func-
tional form of the partial vapor pressures is nonlinear with respect to temperature
(e.g., in Ti6Al4V, Ales [2] has calculated the loss of Al under vacuum using the
equation pAl(T) 5 10.91716211/T, where the partial pressure is given in Bayres
[39]). Elements with low vapor pressures and melting points relative to the other
constituent elements are even more susceptible. While the problem is exacerbated
for vacuum-based processes, similar vaporization does occur for all AM processes.
One example is electron beam melted Ti64, where aluminum levels can be
reduced up to 15% by weight [4042]. Laser systems, such as the Optomec LENS,
have also seen reduction in Al content, and feedstock must be adjusted to compen-
sate for this expected loss [43]. Thus, in addition to controlling the composition of
the input material (i.e., powder, wire), it is also necessary carefully to control the
temperature of the molten pool to achieve desired compositions of as-built parts.
Often, the loss or pickup of elements throughout the AM process is simply
reported with respect to the starting material, and few studies have tried to model
the evaporation or condensation of elements. Given that AM is a nonequilibrium
process, more complex modeling than simple partial pressure equations is needed.
386 Additive Manufacturing for the Aerospace Industry

Semiatin [44] used the Langmuir equation to predict the flux at free surface of the
melt (Js) for each element i, expressed as
rffiffiffiffiffiffiffiffiffiffiffiffi
Mi
Js 5 Xi P0i γ i
2πRT

where X is the mole fraction, P is the vapor pressure at absolute temperature T, γ is


the activity coefficient for liquid melt, M is the molar mass, and R is the gas con-
stant. Based on Semiatin’s approach, Collins [6] and Ales [2] have also applied the
original Langmuir equation [45] to elemental absorption, where the mass flux
towards the surface, m, is defined as
rffiffiffiffiffiffiffiffiffiffiffiffi
Mi
m5 pi
2πRT

where p is the partial pressure of element i. While the equations for interstitial flux
seems to indicated that increasing temperature would lead to less interstitial pickup,
increasing temperature means increasing melt pool size, and thus a greater area of
flux for the elements, and conducted a simple analysis that shows this approach can
be used to predict the gettering of interstitial elements from argon environments of
varying purity. At the time of writing this chapter, the authors do note there are
other issues that remain to be understood, including composition gradients adjacent
to the molten pool.
Thus, while there are quite possibly other factors at play, the rate of pickup and
absorption of elemental species during the AM process is determined by surface-
mediated flux. This also means that the melt pool itself is being sufficiently mixed
as to be homogenous, and solute redistribution occurs primarily during solidifica-
tion. The temperature and size of the melt pool is also an important parameter, and
efforts should be made to monitor better and control the melt pool, so that the
superheating of the melt pool is minimized [6].

17.3.2 Solidification partitioning


The high cooling rates and high velocity of the solidliquid interface in the AM
process is consistent with definitions of rapid solidification. As this is a far-from-
equilibrium process, there is the potential for significant supersaturation in the solid
solution after the liquid-to-solid phase transformation. This can result in solute trap-
ping within the final part, leading to distinctive features unique to the AM process.
Aziz [46] presents a basis to understand the conditions under which solute trapping
can occur, which can be rewritten for AM and is presented below, with respect to
the velocity of the solidification front V, equivalent to the rate of solidification R.

1 δT Dliquid
V 5R5 c i
jrTj δt a0
Developing and applying ICME 387

60
(A) (B)

Peak intensity of AI (a.u.)


55

50

45

40

35
0 50 100 150 200 250 300
Distance from top surface (µm)

Figure 17.8 Solute partitioning that leads to the so-called fish scaling and the subsequent
local ordering (A) micrograph showing composition-driven fish-scaling and (B) composition
profile across such bands [47].

In the above equation, T is the temperature, t is time, a0 is the interatomic spac-


ing during growth, and Dliquid is the diffusion coefficient of solute in liquid. When
this condition is satisfied, the liquid phase experiences solute trapping, and the solid
solubility is extended.
As the primary heat loss from the melt pool is via conduction into the as-built
part, the highest thermal gradient is usually in the z-direction. This is directly
related to the strong texture seen in AM parts, such as h0 0 1i fiber || z-direction. In
addition to promoting a strong texture in AM parts, the high thermal gradient pro-
motes solidification that initiates at the solidliquid interface and proceeds along
the maximum gradient. The solidification modeling activities, including the cellular
automata models developed by Rolchigo [33,34] for various binary titanium alloys,
show cellular structures with partitioning between the domains. The solidification
also promotes other compositional partitioning, giving rise to features including the
so-called fish scaling microstructural features [47] that correspond with geometric
aspects of the molten pool, and which are visible in cross section.
This solute trapping that can occur in additively manufactured metallic materials
has various effects on microstructure and properties, including the formation of
nonequilibrium phases. Tomus et al. [48] observed a supersaturation of the Al2Sc
system deposited with electron-beam AM process and noted that it corresponded
with much higher properties than conventionally manufactured alloys. Thijs et al.
[47] studied supersaturation and fish scaling in Ti6Al4V, and found some areas
with Al content of up to 25 wt%, resulting in the formation of Ti3Al (Fig. 17.8).

17.4 Part 3: Predicting microstructure


As with any alloy system, chemistry strongly influences the microstructures of
alloys produced using AM. However, given that one of the main benefits of AM is
388 Additive Manufacturing for the Aerospace Industry

the ability to produce net- or near-net-shape components (i.e., no subsequent defor-


mation processes to modify the microstructure), AM requires that the fundamentals
of solidification be considered to engineer and control the microstructure. As noted
previously, additively manufactured materials can exhibit a strong texture and spa-
tial variation in the composition. One such alloy where texture exhibits a pro-
nounced influence on the mechanical properties is Ti6Al4V. It has been shown
that the texture can result in differences in the yield strength by at least 5% [38].
Ti6Al4V is one of the most widely used alloys, but is particularly susceptible to
forming texture, given its very narrow freezing range. In principal, it should be pos-
sible to change chemistry and thus modify the texture by controlling the physics of
nucleation and solidification.
One such method is the growth restriction factor Q that was introduced by
Maxwell et al. [49] and which has been used to describe the effect of solute concen-
tration on the solidification and grain nucleation in cast alloys. Q is effectively a
thermodynamic metric given as

dΔTc
Q 5 mc0 ðk 2 1Þ 5
dfs

where m is the slope of the liquidus line, k is the partition coefficient, and c0 is the
solute concentration. In addition, the growth restriction factor is equivalent to the
rate of development of constitutional undercooling (Tc) relative to the rate of devel-
opment of solid (i.e., fraction solid fs). The grain refinement of cast titanium-based
alloys with addition of boron was described, using this model, by Tamirisakandala
et al. [50]. The observed effect of boron has also been exploited to refine grains
and eliminate texture in β-Ti alloys by Mantri et al. [51]. Fig. 17.9 shows electron
backscattered diffraction (EBSD) maps and pole figures of the four systems studied,
where the addition of trace boron to binary TiV and TiMo systems markedly
decreased the grain size and eliminated the texture and large columnar grains. For
the Ti12Mo wt%, the addition of 0.5 wt% B resulted in a 100-fold reduction in
grain size. In addition to the effects of the growth restriction factor, Mantri et al.
attribute the insolubility of boron in titanium as having an effect where the rejection
of boron to the solidification front resulted in a constitutionally supercooled front,
and a larger frequency of grain nucleation.
The effect of solute concentration, while a factor in some systems, does not
always provide the full picture. A model was developed by Easton and St. John to
describe, semiempirically, the effect of nucleant particles, combined with under-
cooling and the growth restriction factor, on the final average grain diameter in cast
Mg and Al alloys [52,53]. The average grain diameter d is given as

b
d5a1
Q
(A) (a) Ti–20V Build direction Ti–12Mo (b) (B) (a) 001 101 111 max = 36.280
19.940
10.959
6.023
TD TD TD 3.310
1.819
1.000
0.550
RD
Ti–20V RD RD

(b) 001 101 111 max = 1.759


1.601
Titanium-Beta 1.457
111 1.326
TD TD TD 1.207
1.099
1.000

Ti–20V–0.5B 0.910
500 μm 001 101 500 μm RD RD RD

(c) Ti–20V–0.5B Build direction Ti–12Mo–0.5B (d) (c) 001 101 111 max = 34.541
19.140
10.606
5.877
TD TD TD
3.257
1.805
1.000
0.554
RD Ti–12Mo RD RD

(d) 001 101 111 max = 1.935


1.733
1.553
1.391
TD TD TD
1.246
1.116
1.000
0.896
100 μm 100 μm RD Ti–12Mo–0.5B RD RD

Figure 17.9 (A) EBSD maps and (B) the corresponding pole figures showing considerable grain refinement and reduction of peak textures of beta
stabilized titanium alloys upon the incorporation of small amounts of boron [51].
390 Additive Manufacturing for the Aerospace Industry

where a and b are defined in terms of the density of nucleant particles ρ, fraction of
activated particles f, a constant b1, and the undercooling required for nucleation ΔTn:

1
a5
ðρf Þ1=3
b 5 b1 ΔTn

The Easton and St. John model proved useful for describing the effect of grain
refinement of silicon on as-cast pure Ti [54]. Mendoza [19] applied the Easton and
St. John model to explore the effects of tungsten on the grain refinement of binary
titaniumtungsten alloys deposited using a powder-blown, laser-based AM plat-
form. Fig. 17.10 shows the results of these studies, where increasing concentrations
of W resulted in a measurable refinement in the resulting grains. While the singular
effect of the growth restriction factor had a predominate effect on the grain refine-
ment, the full EastonSt. John model was required to describe fully the effect by
considering nucleation effects. Specifically, partially unmelted tungsten particles
served as nucleation sites for grains during the rapid cooling of the AM process.

(A) (a) Ti–5W (b) Ti–13W (c) Ti–25W

100 µm

(B)
175

150
Grain size (µm)

125

100

75

50

25
5 10 15 20 25
% wt Tungsten

Figure 17.10 (A) SEM micrographs and (B) stereo logically measured values showing the
grain refinement of a binary Ti-xW system confirming the Easton-St. John model describing
grain refinement during solidification [19].
Developing and applying ICME 391

While these are just a few ways of controlling and modeling microstructure in
AM parts via chemical additions, the application of older models developed for cast
materials to new AM parts should continue to be explored. As with any new pro-
cess, new alloy chemistries are needed fully to exploit the benefits of AM.
Beyond these solidification microstructures, it is necessary to predict the solid-
state phase transformations as well [3]. The types of modeling approaches that
might be considered in predicting the solid-state phase transformations include: (1)
classical methods, including the JohnsonMehlAvramiKolmogorov and Sestak
and Berggren equations [5565]; (2) the phase field method [6669]; (3) and
rules-based or database governed predictions that are based upon either modeling or
experimental data.

17.5 Part 4: Predicting properties and performance


One of the main the goals of an ICME framework to understanding the AM process
is to predict the mechanical properties, such as yield strength, toughness, or fatigue
of a component based upon the previous elements in the ICME framework. We
have previously accomplished this by rigorously quantifying [70] microstructural
features, and using a hybrid modeling approach that integrated two machine learn-
ing tools, namely artificial neural networks (ANNs) with genetic algorithms (GAs)
[37,38,41,71]. The ANN uses highly flexible functions (e.g., the hyperbolic tangent
function) to establish the interrelationships that exist among a set of rigorously
quantified input variables (e.g., composition, microstructure) and a set of output
variables (e.g., yield strength, fracture toughness, fatigue [7275]). Virtual experi-
ments allow the trained ANNs to be explored in systematic ways. For example, by
holding all of the input parameters except one at a single value, such as their aver-
age value for a given dataset, and then allowing that single input to vary over its
range, it is possible to see the dependency of a property on that single input. This
type of experiment is likely to be possible in a laboratory, given the complex and
interdependent ways in which composition and microstructural features influence
properties. The GA can then be exercised on the same dataset with a postulated
equation where physically relevant terms are present. The GA then optimizes the
equations, solving unknown weights and exponential powers, and once the equation
is optimized, it can be compared to the ANN through the use of the same virtual
experiments. The use of this approach has led to the deduction of a constitutive
equation to predict strength of the material.
A model that was previously developed for wrought structures was applied to
additively manufactured Ti6Al4V. Over the course of our most recent work on
large-scale AM of Ti6Al4V structures [38], we have made a few important dis-
coveries. First, texture has a pronounced influence on the mechanical properties.
Second, once texture is accounted for, the equation for wrought Ti6Al4V struc-
tures is nominally identical to additively manufactured Ti6Al4V. Third, the
equations can be applied to any AM component, independent of subsequent heat
(A) Yield strength-EBAM Ti-6AI–4v (B)
predicted vs experimental

Predicted yield strength (MPa)


1000 Pred. YS - α+β stress relief
Pred. YS - α+β HIP

Fvα·89 + Fvβ·45+
Pred. YS - β anneal
950 0%
+5%

Fαv ·(149·xAI + 759·xo0.667) + Fvβ·((22·x0.7


–5% 0.667 0.5 0.7 0.5 2
v ) + (235·xFe ) ) +
900
Fcol
v ·150·(tα–lath)
–0.5
·(tβ–nb)0.5+
σys =
850 Fcol
v ·125·(tcolony)
–0.5
+
800 (–1)·(AxisDebit) +
v ·αMGb ρ
FBW
750

700
700 750 800 850 900 950 1000
Measured yield strength (MPa)
0.999
0.990
(C) 0.900
0.750
Probability 0.500
0.250
0.100
0.050 σYS, yield stress
Phenomenological model
0.010 Monte Carlo simulation
0.005 +/–σMSE
+/–2σMSE
0.001
650 700 750 800 850 900 950 1000

Stress σ(MPa)

Figure 17.11 (A) Prediction of the properties of as-deposited Ti6Al4V subjected to three heat treatments [38]; (B) the equation
corresponding equation [38]; and (C) a representation of a similar equation for the cumulative probability distribution of Ti6Al4V [76].
Developing and applying ICME 393

treatments, as long as the composition and microstructure can be measured or pre-


dicted accurately. Finally (and importantly), there is an unexpectedly large disloca-
tion density in certain heat treatments (i.e., those that keep most of the as-deposited
material state). The demonstration of a single equation to predict the strength of
additively manufactured Ti6Al4V subjected to three different heat treatments is
shown in Fig. 17.11A and B, with the predicted versus experimental data shown in
Fig. 17.11A, and the equation presented in Fig. 17.11B, where the volume fractions
of phases, size of features, and chemistry are included [38].
Continuing this demonstration of the ICME framework for additively manufac-
tured Ti6Al4V, it is necessary to transition the prediction of properties to the
prediction of performance. One way to interpret performance is through the use of
cumulative probability distribution functions (pdfs), where the probability of
achieving any given value of a property (e.g., yield strength) is plotted (see
Fig. 17.11C; [76]). If the models described previously were to describe perfectly
the properties of the material, the cumulative pdfs of the predicted data would over-
lap perfectly with experimentally measured data. However, even for good models,
when looking at the data on a probability plot in which the tails of the data are
emphasized, it may be that the model does not accurately predict the experimentally
observed data. Thus, we have successfully turned to using a “distributiontransla-
tionrotation” approach to shift and skew the models as necessary to represent the
physical data. This statistical refinement of the model can occur in statistical space,
and does not change the model. This approach has been previously reported in the
literature [76], and additional publications will be forthcoming in the near future.

17.6 Limitations
Throughout the remainder of this chapter, we have referred to successful demon-
strations of modeling activities, and/or have provided some important fundamental
details to enable others to develop modules to an ICME approach. However, despite
the successful outcomes that these activities have demonstrated, there are still lim-
itations that need to be considered. Arguably, the most important limitations are
associated with what we either do not know or have difficulty measuring/comput-
ing. Three limitations will be discussed briefly.
The first limitation is associated with the fact that the process is quite complex,
and multiple physics are active, potentially “erased” in the previous layer, and reac-
tivated. In addition, many of the important physics associated with phase transfor-
mations, defect formation, chemistry, or texture formation occurs at different
regions (e.g., solid-state phase transformations occur below the molten pool; nucle-
ation events, convection, conduction, and instabilities occur within or at the surface
of the molten pool; chemistry changes at the surface and above the molten pool;
and solidification/solid-state phase transformations occur behind the molten pool)
are characterized by details that are at either the nanosecond or nanometer scales.
Currently, the AM community lacks the tools that may permit the investigation of
3400 –60
(C) –55
–100 (A) (B)
–50
3300 –45
–80
–40
–35
–60 3200
–30
–25
–40
3100 –20

–20 –15
–10
10 20 30 40 50 60
0 3000
(D)

20
2900

40

60 2800

80
2700

100
2600
–30 –20 –10 0 10 20 30

Figure 17.12 (A) One direction SAW velocity map of electron-beam as-deposited Ti6Al4V; (B) the orientation map deduced from multiple
SAW velocity maps; (C) the high resolution inset from (B); and (D) a tiled, mosaic optical image from the same region as (C). All units in (A) and
(C) are in millimeters.
Developing and applying ICME 395

these physics at the appropriate length and time scales to understand what is hap-
pening. However, very recent investments in programs to develop in situ AM cells
in synchrotron beamlines should allow the community to discover new science to
understand better AM processes.
The second limitation is associated exclusively with defects. In some systems,
including titanium-based alloys, inspectability of additively manufactured compo-
nents is a challenge. Spatial variation in the anisotropy of the as-deposited micro-
structures can interact with nondestructive evaluation techniques, providing new
challenges when identifying defects, and potentially influencing the probability of
detection (i.e., pod). The companion chapter in this volume speaks specifically to
the challenges associated with nondestructive evaluation of additively manufactured
articles. Interestingly, while there are challenges, the line-by-line, layer-by-layer of
AM may permit the measurement of local microstructural state (including defects),
and allow the so-called digital twins to be created for each component built.
The third limitation that we will discuss briefly is the variation in scale of micro-
structural inhomogeneity. In traditional processing, the multistep forging sequences
can chemically homogenize the material, and predictably produce texture that is rel-
atively spatially consistent throughout a part. While texture can be controlled in
AM [77], most AM processes have relatively small melt pools (e.g., ,1 mm).
There are large-scale AM processes where the size of the molten pool permits heat-
transport mechanisms to compete and produce spatially varying microstructures,
including texture (Fig. 17.12). As is apparent in the figure, the scales of these
microstructural domains are much greater than what the materials scientist would
typically measure. To measure the texture of these domains, the authors have turned
to adopting a new technique (spatially resolved acoustic spectroscopy, or SRAS) to
analyze the local orientation. During SRAS, a laser passes through a grating and
sets up a surface acoustic wave (SAW), the velocity of which can be accurately
determined. The velocity of the SAW is related to the elastic stiffness tensor (cij). If
the SAW velocity and elastic stiffness tensor are known, the orientation can be cal-
culated [7881]. This method is especially exciting as it permits the measurement
of texture and local orientation over areas that far exceed what is typically mea-
sured using other techniques. The limitation is the spatial resolution, which is cur-
rently B25 μm.

17.7 Summary
It is possible to develop and execute an ICME framework for structural metallic
materials for aerospace applications. Any ICME framework is based upon a series
of decisions that depend upon the overall objective. There are some exciting model-
ing activities that can be integrated into an ICME framework, including activities
that predict distortion and solidification microstructures based upon a thermal his-
tory. One of the important aspects of any ICME framework is the ability to predict
the composition of the as-deposited material, as it will invariably deviate from the
396 Additive Manufacturing for the Aerospace Industry

precursor powder or wire. The Langmuir equation has been used to predict elemen-
tal loss under vacuum and solute pickup under atmosphere. However, there are still
unknown details of both the molten pool shape and the material transfer physics
that will influence the successful implementation of the Langmuir (or similar)
approach. Once chemistry is known, it is possible to couple chemistry with cooling
rate and predict microstructure.
Given a specific microstructure and composition, it is currently possible to pre-
dict the yield strength of the widely used aerospace alloy Ti6Al4V. Given the
knowledge base that exists for certain aluminum-based alloys and nickel-based
superalloys, it should be possible to integrate that knowledge into an ICME frame-
work and make preliminary predications regarding their properties. Once a constitu-
tive equation for properties is known, it is possible to predict the performance of
the material, as represented by design allowables and the cumulative probability
distribution function.
While such modeling capabilities have been demonstrated, there are still gaps in
the AM knowledge base. These gaps will be reflected in any ICME framework.
However, there is extensive work underway to fill these knowledge gaps, and over
the next decade, significant progress is expected.

References
[1] S.M. Kelly, Thermal and Microstructure Modeling of Metal Deposition Processes With
Application to Ti6Al4V (Doctoral dissertation), Virginia Tech, 2004.
[2] T.K. Ales, An Integrated Model for the Probabilistic Prediction of Yield Strength in
Electron-Beam Additively Manufactured Ti6Al4V (Masters dissertation), Iowa State
University, 2018.
[3] R. Martukanitz, P. Michaleris, T. Palmer, T. DebRoy, Z.-K. Liu, R. Otis, et al., Toward
an integrated computational system for describing the additive manufacturing process
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Developing and applying ICME 397

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Nondestructive evaluation of
additively manufactured metallic 18
parts: in situ and post deposition
Lucas W. Koester1, Leonard J. Bond1,2,3, Hossein Taheri1,2 and Peter
C. Collins4
1
Center for Nondestructive Evaluation, Applied Sciences Complex II, Iowa State
University, Ames, IA, United States, 2Department of Mechanical Engineering,
Iowa State University, Ames, IA, United States, 3Department of Aerospace Engineering,
Iowa State University, Ames, IA, United States, 4Department of Materials Science and
Engineering, Iowa State University, Ames, IA, United States

18.1 Introduction
Additive manufacturing (AM) is a rapidly emerging technology consisting of the join-
ing of materials to make parts from 3D model data, usually layer upon layer, as
opposed to subtractive and formative manufacturing methodologies [1]. The ability to
construct complex components rapidly with little material waste is poised to have
transformative effects on many industries. However, qualification of novel
manufacturing processes and methodologies is a common slowing point before wider
application can be realized. AM methods in the aerospace industry have been used for
production of less-than-critical components, including cockpit and fuselage interiors
for a number of years. The flexibility and enabling design capability are, however,
driving wider application to critical structures for repair, replacement, and new part
production.

18.1.1 Additive manufacturing components in service


A number of components have now been produced by AM and flown by various aero-
space entities. The first Federal Aviation Administration (FAA)-approved engine com-
ponent to fly in commercial jets was in 2015 with the T25 housing for a sensor to
monitor compressor inlet pressure and temperature [2]. The FAA approved the use of
the housing in the GE90 engine after identification of the opportunity to utilize AM
based on value. A process from proper material and machine identification to compo-
nent and subsequently engine level certification was then formulated. Since then, the
framework has been followed for the use of various AM components in a number of
engines, including a novel fuel nozzle that enabled weight savings of 25% and reduced
the number of brazes and welds from 25 to 5 in the Leap engine [3].
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00020-0
© 2019 Elsevier Inc. All rights reserved.
402 Additive Manufacturing for the Aerospace Industry

Predating the applications for aviation systems, several space applications had
driven the development of AM for some critical applications. Lockheed Martin uti-
lized AM for fabrication of titanium waveguide brackets that have now traveled bil-
lions of miles and currently reside on the Juno spacecraft as they orbit Jupiter.
Since the maiden spaceflight of an AM component, Lockheed Martin has
announced its redesigned A2100 geosynchronous satellite launched in 2017 utilized
AM for 10% of its components. The National Aeronautics and Space
Administration (NASA) has also identified the potential for a diverse range of AM
parts for use in space systems. In looking further to the future, the capability to pro-
duce reliable, complex components in space on demand has obvious implications
for manned space travel. NASA recently produced the first fused deposition model-
ing 3D-printed part in the microgravity environment of the International Space
Station as a proof of concept [4].
While the applications and design freedom enabled by AM are exciting, particu-
larly for the aerospace community, companies and agencies are proceeding with cau-
tion in deploying AM components for mission-critical applications. In looking back
at the history of the development of traditional manufacturing methods, the building
of a sound experience and knowledge base developed with time. Such a process of
gradual incremental change and maturation is being accelerated with AM and pre-
sents some significant challenges. That said, the development and deployment of
AM-fabricated parts is continuing to proceed at an unprecedented pace.
Furthermore, the complexity of AM processes and the dependence of the perfor-
mance of the resulting material on process conditions have yet to be fully under-
stood, which introduces the potential for significant variation in performance for
AM components.
Quantitative characterization techniques are required for finished components to
comply with existing inspection standards and procedures for identifying defects, veri-
fying microstructure, determining final part geometry, and assessing material property
variation in critical components. The potential variability and flexibility in process
conditions motivates development and deployment of rapid, quantitative process mon-
itoring and characterization in situ to fully realize the capability of AM systems and
the parts that they can produce. Whether post-production or during fabrication, AM is
a challenging area for both process monitoring and nondestructive testing.

18.1.2 Regulatory actions and standardization


The FAA has submitted an AM Strategic Roadmap to establish plans and practices
for businesses dealing with the development and application of AM technologies as
of September 2017 [5]. The document will likely follow the examples set by other
organizations, such as the Department of Defense (DOD) and the Additive
Manufacturing Standardization Committee (AMSC), in which the American
Society for Testing and Materials (ASTM) has a lead role [6,7]. Both have estab-
lished roadmaps to accelerate standards and specifications for the rapid develop-
ment in the AM industry. The roadmaps examine the state of the industry, identify
existing standards in development, and make recommendations for priority areas
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 403

where gaps have been identified. A general structure has been produced that
acknowledges commonality among AM methods, but realizes the need for specific
standards and test methods based on raw materials, process, and end applications
considered (Fig. 18.1).
ASTM established Committee F42 on AM Technologies in 2009 [8]. The
International Organization for Standardization (ISO) formed ISO/TC 261 for similar
purposes in 2011 [9]. After a meeting in 2013, the two groups formed a Joint Plan
for Additive Manufacturing Standards Development to expedite standards develop-
ment across the two organizations and avoid duplication of effort. The group has
since produced and adopted several joint standards, including AM terminology and
standard guides. Numerous Work Items are underway to address specific AM meth-
ods and materials including metals and polymers [8].
Areas of concern identified by these working groups and agencies include pro-
cess monitoring to enable closed-loop feedback and control, reliable nondestructive
evaluation (NDE), and quality control, among others. The design of the standardiza-
tion structure surrounding a process or material can take several forms. For exam-
ple, Metallic Material Properties Development and Standardization, often used to

Additive manufacturing standards structure


Qualification System performance Round robin
Terminology Data formats
General AM guidance and reliability test protocols General top-level
standards AM standards
Design guides Test methods Test artifacts Safety Inspection methods etc.
• General concepts
• Common requirements
• Generally applicable
Feedstock materials Process / Equipment Finished parts
Material category-specific Process category-specific All finished parts

Metal powders Ceramic powders Material Powder bed fusion Mechanical test methods
jetting Category AM
Directed energy NDE/NDT Post-processing
Photopolymer
Polymer powders Binder jetting methods methods
standards
resins deposition
Metal Polymer Material Bio-compatibility test methods Specific to material
etc. Sheet lamination category or process
rods filaments extrusion
Chemical test
Vat photopolymerization methods
etc. category

Material-specific Process-material-specific Material-specific

Titanium Powder Material Titanium alloy Paper Sand


Steel rods bed fusion extrusion
alloy powders
with nylon with ABS Nylon ABS Aluminum alloy
Nickel-based Specialized AM
Nylon powder Powder bed
alloy powders Directed energy
deposition with fusion with steel Nickel-based alloy etc. standards
ABS filament etc. titanium alloy etc. Specific to material,
process, or application
Application-process-
Application-material-specific material-specific Application-material-specific

Aerospace Medical Aerospace Medical Aerospace Medical

Automotive etc. Automotive etc. Automotive etc.

Figure 18.1 Standards Structure approved by ASTM F42 and ISO TC261. [2017 American
National Standards Institute/National Center for Defense Manufacturing and Machining,
operating America Makes—the National Additive Manufacturing Innovation Institute
(America Makes)]. ASTM, American Society for Testing and Materials; ISO, International
Organization for Standardization.
404 Additive Manufacturing for the Aerospace Industry

derive design allowables statistically from experimentally determined statistical dis-


tributions of material properties, is not straightforward to apply to AM materials
due to the breadth of processes and materials that AM encompasses. Thus, the focus
is placed on characterizing and “freezing” a process in an acceptable state, followed
by validation using “witness” specimens produced under identical conditions for
validation. This is evidenced by recent guidance produced by NASA for metallic
spaceflight hardware produced by laser powder bed fusion (LPBF) [10].
A key component of this quality control strategy is quantitative nondestructive
evaluation of critical components for build errors that may induce defects detrimen-
tal to material performance. Thus, application of existing nondestructive evaluation
techniques or modification to address issues specific to AM components is a neces-
sary and likely part specific for critical applications. Part geometric complexity,
microstructure, and surface condition all impact nondestructive evaluation techni-
ques and need to be addressed to ensure reliable defect detection.

18.1.3 Material properties and defects in additive manufacturing


Applications of AM that seek to supplant traditional manufacturing methods due to
advantages in cost, performance, or lead-time must still meet material property and
characterization requirements for the end application, regardless of the manufactur-
ing method. For aerospace components, attempts at weight reduction can lead to
complex internal and external geometries that complicate inspection. Defects tend
to form between layers and generally do not propagate far in the build direction
leading to crack-like defects perpendicular to the build direction. Furthermore, sur-
face roughness tends to be high (on the order of or larger than casting processes)
due to a weld like material consolidation process. A coverage map of NDE methods
over the spatial resolutions and target depths within the material is given in
Fig. 18.2.
Complex external/internal geometry and roughness have compelled the use of
penetrating radiation as the most likely method for successful inspection. However,
internal defects may or may not be void, which negatively impact contrast in x-ray
and ultrasonic methods [11]. For large components, penetration issues can limit the
inspectable volume of the material quickly with radiographic and ultrasonic techni-
ques. Surface roughness affects the reconstruction process in x-ray computed
tomography, particularly for near-surface defects that are of particular concern for
fatigue considerations. Roughness also negatively impacts defect detection capabili-
ties in ultrasonic inspection in most cases [12]. Multiple layers of internal structures
or internal lattice structures are not inspectable with ultrasonic techniques. Post-
production surface finishing can help mitigate the effects of roughness on inspect-
ability, but can induce compressive surface residual stresses that may make inspec-
tion for surface breaking defects more difficult [13].
The resulting, as-built microstructure in metal AM also tends to follow the melt
pool solidification path and thermal gradients [14]. Seeding from powder particles
and previous melted layers can cause complex microstructure that complicates
ultrasonic inspections for defects. Post-processing of materials by heat treatment
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 405

St
an
X- da
ra rd
y ,m
in CT ini
ith
w e ,m
Location of interest

ep um icr
o-
De vol Co ,n
m an
Si p o-
Ult m lex fo
ras ple ge cus
ou ge om
nd om etr
Th et y Volumetric
erm ry
al defects
e Volume/surface
r th Eddy defects
a c e
Ne urfa current
s
Non-interferometric White light
At ce optics Optical interferometry
rfa surface breaking very near surface
su
mm μm nm
Resolution

Figure 18.2 Resolution coverage map for various NDE techniques with applicability to AM
for geometric defects. NDE penetration limits the application of techniques that are diffusive
and optical methods are limited to surface interrogation. AM, Additive manufacturing; CT,
Computed tomography.

can form microstructures more amenable to inspection, but removes the capability
for tailoring of local material properties during building that may be achieved by
additives to feedstock powder that has been demonstrated for certain materials
[15,16]. Such post-processing also adds cost to components that may or may not
meet the criteria for deployment.
A number of geometric internal defects may also form during fabrication. Micro-
porosity is linked primarily with porosity entrapped in starting-powders. These
defects are generally higher contrast, but can be small (necessarily smaller than start-
ing powder diameters), and thus difficult to detect. Larger scale porosity tends to be
formed by improper heat source characteristics that lead to entrapped gasses due to
melt pool dynamics or keyhole collapse. Post-processing with hot isostatic pressing
has shown some capability to consolidate these defects below a certain size, though
the defects may reemerge after additional heat treatment, particularly for materials
deposited in inert as opposed to vacuum environments [17].
Lack of fusion (LOF) type defects are unique to AM and are primarily caused
by poor processing parameter selection. The defects may be filled with unconsoli-
dated powder that reduces x-ray CT contrast in post-production inspections with
large voxel sizes. The presence of unmelted powders may be resolved if sufficient
resolution can be achieved by using μ-CT techniques [18]. Resonance type testing
can be a method of detecting LOF defects, but is binary in its decision and
406 Additive Manufacturing for the Aerospace Industry

nonspecific, relying on a statistical basis for rejection of a component based on


shifts in resonant frequencies [19]. Balling is a phenomenon that causes powder
particles to become entrapped within the melt pool, leading to the formation of
small spheres on the order of the heat source spatial extent. These unstable melt
pool dynamics can lead to higher roughness, which negatively impacts fatigue and
inspectability. These balled regions may also be removed during powder spreading,
increasing the chance of producing LOF and layer defects [20].

18.2 State of the art


Nondestructive evaluation plays a key role in AM for the aerospace industry. The
production of components with AM is often most attractive for low-production runs
and high-value alloy materials. Qualification strategies primarily consist of deter-
mining an operating window, “freezing” the process to produce components and
witness test pieces, and post-production inspection. Establishing process windows
for new AM methods or materials could prove costly and time consuming, how-
ever. Thus, numerous agencies have identified the need for enhanced in situ sensing
and characterization techniques.
The DOD AM Roadmap identified the need for development in NDE and pro-
cess control technologies to enable consistent processing and verification of part
quality [6]. Monitoring and in situ characterization for closed-loop control is predi-
cated on the existence of nondestructive techniques that are reliable, rapid, and
quantitative. Similar views were expressed by the AMSC, acknowledging the low
technology readiness level of in situ process monitoring for machine state and mate-
rial condition [7].

18.2.1 Optical and thermal monitoring


Optical and thermal emissions monitoring have received much attention due to the
relative ease with which they can be applied. Line-of-sight access is available in
most commercially available machines on which most research has been performed.
Methods to monitor optical emissions can include the use of photodiodes, high-
resolution cameras, and high-speed cameras. Point-based measurement systems,
such as photodiodes and pyrometers, often require system integration to track the
melt pool during deposition. In contrast, full-field techniques monitor optical and
thermal emissions for a large area, potentially continuously during a build. The
accumulation of this data in a tomographic assembly over the entirety of the build
after processing can then be likened to a quality map, as shown in Fig. 18.3.
Optical monitoring of melt pool spatter has shown to be linked to different
energy density conditions of the heat source for 18Ni (300) maraging steel powder
[22]. Monitoring of balling in the melt pool has also been linked with energy den-
sity in fabrication of stainless steel [23]. Photodiode and camera optical signatures
can also be spatially correlated to establish process maps of thermal accumulation
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 407

Figure 18.3 Beginning with (A) CAD geometry, the model is (B) discretized according to
the spatial resolution of the inspection method. Layer-by-layer inspection data is (C) post-
processed and stored according to position and (D) assembled upon build completion to
produce a tomographic image [21], CC BY 4.0. CAD, Comparison to design.

due to geometry effects [24]. A photodiode-high speed camera hybrid system that
monitored melt pool dimensions and average thermal emission from the melt pool
has been shown to be effective in reducing over-melting and gas porosity. The
method was patented and licensed to Concept Laser, but requires integration with
the system optics [25]. In summary, the majority of optically based techniques infer
part quality from optical emissions and melt pool stability and dynamics. Direct
measurement of defects using optical methods must be at or very near the surface
[using optical coherence tomography (OCT)]. Imaging of surface breaking defects
is difficult due to low contrast between consolidated and unconsolidated regions,
but has shown some promise with multiple viewing angles and lighting conditions
[26]. Optical determination of geometric accuracy would involve high-resolution
optical imaging at each layer and comparison to design files (or other) for geomet-
ric accuracy.
Thermal monitoring allows for a means to monitor heat accumulation within the
component, potentially over the entire build area when using thermal cameras.
However, obtaining absolute temperatures is difficult due to varying emissivity
values at the surface, depending upon the state of the material (e.g., molten, solidi-
fied, or powder). Thus, early investigations examined variation in thermal charac-
teristics qualitatively. Pavlov et al. varied hatch spacing (distance between
subsequent material deposition passes) and layer height, utilizing a two-wavelength
pyrometer to examine variations in pyrometer signal levels on in a selective laser-
melting process. Small hatch spacing that allowed sufficient contact between laser
passes showed heat accumulation with subsequent passes and higher pyrometer sig-
nal levels. As hatch spacing increased, a transition region was observed between
complete contact and no contact between deposited lines. Varying the height of the
deposition also showed increasing pyrometer signal levels caused by eventual loss
of contact with the substrate. They also observed drops in pyrometer signal level
where powder spreading was insufficient and proposed the instrument as a process
monitoring tool. In a similar manner, balling was monitored optically and linked
with pyrometer signal analysis for variations of energy density in two laser-based
AM systems, and an operating window that minimized balling was identified [23].
In an effort to quantify thermographic measurements, Rodriguez et al. [27] pro-
posed additional calibration and instrumentation to account for variables that affect
408 Additive Manufacturing for the Aerospace Industry

the thermographic imaging process, including the effect of the viewing window,
mean radiant temperature within the environment, and surface emissivity. Their
results showed that thermocouples and algorithms to predict surface temperature (a
parameter used to adjust beam current to mitigate thermal accumulation) likely
underestimate surface temperature when compared with corrected thermal imaging
data. As mentioned previously, quantitative data such as temperature evolution dur-
ing manufacturing can be related to microstructural evolution and resulting part
material properties, eventually leading to microstructural control. This potential was
partially demonstrated by Raplee et al. with thermographic data corrected for sur-
face emissivity. The resulting thermal gradients and estimated solidliquid inter-
face velocity could aid in predicting areas with equiaxed or columnar type grain
regions and (Fig. 18.4), varying melting strategies [28].
Given the influence of melt pool dynamics, thermal history, and dimensions on
resulting part geometry and microstructure, melt pool monitoring in fine detail has
also been investigated as a monitor and potential control on the resulting part prop-
erties. Fox et al. investigated coaxially aligned near infrared imaging of a novel,

(A)

Layer temperature
1200

50 1150

1100

Temperature (ºC)
100
20 μm 1050
Y (pixels)

150
1000
200
950
250 900

300 850

800
350
750
50 100 150 200 250 300 350 400 450
X (pixels)
20 μm

New temperature data @ 70 mm New temperature data @ 70 mm


(B) build height pixel x = 200, y = 150 point melt (C) build height pixel x = 200, y = 200 line melt
1200 1200
Apparent temperature (ºC)

Apparent temperature (ºC)

1150 1150

1100 1100

1050 1050

1000 1000

950 950
0 5 10 15 20 25 30 35 40 45 50 0 5 10 15 20 25 30 35 40 45 50
Time (s) Time (s)

Figure 18.4 The relationship of (A) corrected thermal imaging and (B and C) thermal
history and resulting microstructure in Inconel 718 fabricated with electron beam additive
manufacturing with different melt strategies [28], CC BY 4.0.
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 409

instrumented laser-based AM test bed (Additive Manufacturing Metrology


Testbed). Infrared image collection at 30,000 frames per second can be used to
extract melt pool dimensions with image analysis [29]. However, even with such
acquisition rates, blurring, high dynamic temperature ranges, and relatively low res-
olution of the detector (12 μm/pixel) remain obstacles and significant work remains
in this promising area.

18.2.2 Post-production inspection


Geometric and material aspects of AM components pose challenges for reliable
NDE. These challenges include roughness, anisotropy of material properties, com-
plex internal and external geometry, and the nature of the defects encountered. The
surface condition of as-built components most closely resembles castings, Surface-
based inspection techniques, primarily optical and penetrant methods, are nega-
tively impacted by surface roughness [13]. Existing standards for inspection of
rough casting components will likely be applicable with some modification to AM
components [30]. Similar concerns exist for surface condition improvement and the
effects on defect detection, including inducing compressive residual stresses caused
by peening (commonly used to remove loosely attached surface powder particles)
that may close surface cracks, or the masking of defects by smeared material after
subtractive machining. Many of the aspects of inspection have been addressed by
other works and a complete discussion is outside the scope of this article [13,31].

18.2.3 Emerging methods


Due to the limitations of surface-based inspection techniques, volumetric techniques
are being investigated for in situ characterization and inspection. Volumetric techni-
ques may afford the capability to inspect at less frequent intervals by interrogating
multiple layers at a time. Furthermore, defects that may not be surface breaking may
also be indicated. These techniques include primarily ultrasonic and acoustic methods
as well as novel, system-integrated melt pool imaging, as discussed previously [32].
Laser ultrasonics has been identified as a potential method to monitor AM builds
for surface breaking defects, sub-surface defects, and microstructure by a number
of authors [33]. The method has been shown to be capable of identifying larger arti-
ficial defects (produced via electrical discharge machining) in a direct energy depo-
sition (DED)-produced Inconel alloy [34,35]. The investigation of porosity in situ is
also under investigation by incorporating laser ultrasonic excitation and detection
into LPBF optics [36]. The mapping of surfacewave acoustic velocity can also be
used for determining information about microstructure and defects [37]. Spatially
resolved acoustic spectroscopy (SRAS) has been demonstrated ex situ for AM
metals, mapping acoustic wave speeds with resolutions as low as 20 μm can infer
grain structure by abrupt changes in wave speed associated with neighboring crys-
tallites with different crystallographic orientations [38]. The experimental configu-
ration and an example result are shown in Fig. 18.5, comparing optical
metallography with the wave-speed mapping result. Wave-speed values for pores
410 Additive Manufacturing for the Aerospace Industry

Generation Detection (A)


laser laser 1
(1064 nm) (532 nm)
0.8

0.6

0.4
Optical
train Detector
0.2

Generation Optical Surface (B) ms–1


patch spot acoustic 2950
wave

2900
∅p
οs

2850

2800

Figure 18.5 SRAS experimental configuration (left) showing the generation patch and
resulting surface acoustic wave. Correlation between images (right) produced by (A) optical
imaging and (B) the acoustic wave speed map can been seen for pores [dark in (A)] and
additional wave-speed variations caused by microstructural crystallite orientations [39], CC
BY 4.0, assembled from two figures. SRAS, Spatially resolved acoustic spectroscopy.

are missing due to the absence of waves for detection in the voids [39]. Scanning in
multiple directions can then determine crystallographic orientation. The detection
capability for defects has also been recently demonstrated ex situ, to inform a
rework or repair strategy demonstrated on polished samples [40].
A major impediment to laser ultrasonic investigation of AM materials in situ is
surface roughness and condition. Surface roughness highly attenuates surface waves
and complicates reliable detection of surface displacements. Methods to ameliorate
this restriction include development of new sensors and detectors that can correct
for the effects of surface roughness with relative ease. Speckled knife edge detec-
tors have been developed that utilize an array of sensors to determine corrections to
speckle introduced by surface roughness using a sensor array and comparing the
data from adjacent sensors [41]. While capable, laser ultrasonics hardware tends to
be relatively expensive when compared with full-field visualization techniques.
Thus, incorporation of such equipment into commercial machines will need to dem-
onstrate value added, potentially through in situ repair or enabling customizable
spatial microstructures.
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 411

Acoustic monitoring has also garnered consideration given that stress waves
propagate through the bulk of the material and can be used to infer or measure
directly material properties and defects [42]. Gaja and Liou [43] observed good cor-
relations between high energy acoustic events collected with an acoustic emissions
transducer attached directly to the build plate and defect formation including cracks
and porosity. Acoustic monitoring can also detect signatures that are potentially
characteristic to the fabrication process, such as powder impacts during DED, laser
generated ultrasound near/inside the melt pool, and machine vibrations and noises.
Wasmer et al. [44] monitored acoustic noise in a noncontact manner with a fiber
Bragg grating and, based on wavelet analysis and a trained convolution neural net-
work, were able to classify build condition based on acoustic noise in powder bed
fusion AM.
Acoustic methods collect information nonselectively provided there is sufficient
acoustic power in the bandwidth of the transducers used. Acoustic monitoring
metrics can be separated to allow independent examination of indications from
crack-like events and characteristic process noise, given the relatively short duration
of such high-energy events. An example of this method is given in Fig. 18.6, in
which acoustic metrics can be used as indicators of damage and process state in
directed energy deposition of titanium 6Al-4V on tool steel. Root-mean-squared
(RMS) noise levels vary dramatically during the build as well as a sharp decrease
in noise levels after build completion seen in Fig. 18.6A. Also depicted is the total
count of high amplitude events (referred to as “Hits”) that may be used as a defect
density indicator. After eliminating high-amplitude events often associated with
defect formation, including cracks and porosity, isolation of low-amplitude noise
results in a noise level that has been shown to be unique for this process under vari-
ous build conditions (Fig. 18.7). Contact acoustic emissions sensors were attached

Figure 18.6 Acoustic monitoring of a directed energy deposition system can be (A) an
indicator of material damage from tracking high-amplitude events associated with defects
and (B) a passive process monitor by measuring RMS noise levels and comparing with
known “good” levels [45]. RMS, Root-mean-squared.
412 Additive Manufacturing for the Aerospace Industry

(A) × 10–5
6
Baseline
Powder only
5 Normal
Low laser power
Normal standard dev. (σ)

Low powder feed


4

0
0 0.5 1 1.5 2 2.5
Normal mean (μ) × 10–4
(B)
Clustering all data and silhouette mean values using spectral features Cf, CA, and PA
in one experiment for each build condition–high frequency band

BL: Base Line


C1: Optimum settings
C2: Low power
C3: Low powder feed
CO: Powder feed only

20
Peak amplitude of Fourier

15
transform (PA)

10 1400
f)
(C
m

1350
or

5
sf
n
ra

1300
rt

0
ie
ur

2.5 1250
fo

2
of
z)
cy

Centro 1.5 1200


(k

id amp
en

litude 1
qu

of Fou 0.5
rier tra
fre

nsform 0 1150
id

(CA)
tro
en
C

Figure 18.7 Clustering of acoustic metrics derived from temporal samples of process noise
can be used to classify machine states (varied around normal with baseline tests) in (A) the
temporal metrics including RMS noise level central tendencies and deviations and (B)
spectral characteristics, including centroid locations and amplitudes [4547]. RMS, Root-
mean-squared.

to the build plate and noise levels (RMS) were recorded during deposition under
different build conditions, including Normal (100% Laser Power, 100% Powder
Feed), Low Laser Power (78% Laser Power), Low Powder feed (50% Powder
Feed), and Powder Only (No Laser Power). Baseline conditions were recorded
when the machine was prepared for deposition, but otherwise at rest to determine a
lower noise threshold.
Nondestructive evaluation of additively manufactured metallic parts: in situ and post deposition 413

Apart from the potential capability as a process monitor for AM equipment


including pumps, motors, heat sources, and material condition, others have
raised concern that such a monitoring technique is a bridge between physical
and cyber systems that may enable bad actors to do harm by intellectual prop-
erty theft [48]. The potential of acoustic monitoring has been identified by
General Electric evidenced by patents of acoustic monitoring methods [42,49].
Work remains to be done to provide quantitative, physics-based predictions of
noise levels from machine/material sources and the direct relationship between
noise levels or high amplitude events and the resulting material state need to be
further elucidated.

18.3 Practical considerations


The drive to monitor and characterize AM materials in situ has led to great techni-
cal achievements toward this end. However, once the measurement science has
matured to identify and characterize the material properties and defects of interest,
the implication on added cost and inspection time must also be addressed. This
added cost is illustrated in Fig. 18.8 for two schemes of NDE data collection during
building for LPBF [21].
Hirsch et al. investigated the applicability of two NDE techniques: SRAS and
OCT, a method requiring translucency/transparency primarily applicable to poly-
mers, based on implications of added build time and potential spatial resolution of
the methods. The method provided a penalty factor on the build time that quantifies
the estimated added time required for inspection at every layer. SRAS was found to
have a temporal penalty of 59 and 1442 for coarse and fine scans (50 and 20 μm
minimum detectable defect), respectively. Thus, optimization, inspection at inter-
vals greater than one layer, or other means likely need to be formulated to make the
inspections palatable to end-users. OCT systems simulated had a temporal penalty
of 2.4 and 5.4 for a 30 μm minimum detectable defect [21].

(A) In-situ
Energy beam NDE scan NDE latency Recoating/Resetting for
interaction time, tbuild time, tscan time, tlatency next ALM layer, treset

Total time per layer


(B) Online
Energy beam Recoating/Resetting for
interaction time, tbuild next ALM layer, treset

NDE scan NDE latency Total time per layer


time, tscan time, tlatency

Figure 18.8 Potential inspection schemes for layer additive manufacturing (A) in situ and
(B) online, suggesting that parallel material consolidation and NDE inspection can enable
inspection at every layer [21], CC BY 4.0.
414 Additive Manufacturing for the Aerospace Industry

The added cost of these inspections is reflected in machine productivity, addi-


tional hardware associated with the inspections, and calibration, upkeep, and valida-
tion of the inspection systems. For well controlled and calibrated AM processes and
materials, it is anticipated that the approach of “freezing” a process and the produc-
tion of “witness” coupons on validated systems will remain the favorable method.
However, the production of prototype components and multiple design iteration
processes, particularly with experimental alloys or processes that are not thoroughly
well characterized, could benefit greatly from layer-by-layer inspection, but will be
slow to be adopted until inspection times are reduced to a minimum.

Acknowledgments
This article was funded as part of an Industry-University Core Project by the Center for NDE
(CNDE), Iowa State University. Thanks go to Quad City Manufacturing Lab (QCML) which
has provided access to and operation of the Direct Energy Deposition (DED) system for gen-
eration of the experimental data used in Figs. 18.6 and 18.7.

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[44] K. Wasmer, C. Kenel, C. Leinenbach, S.A. Shevchik, In situ and real-time monitoring
of powder-bed AM by combining acoustic emission and artificial intelligence, in:
Industrializing Additive Manufacturing—Proceedings of Additive Manufacturing in
Products and Applications—AMPA2017, Springer International Publishing, Cham,
2018, pp. 200209.
[45] L.W. Koester, H. Taheri, L.J. Bond, T.A. Bigelow, E. Faierson, Acoustic emissions
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[46] H. Taheri, L.W. Koester, T.A. Bigelow, E. Faierson, L.J. Bond, In-situ process monitor-
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[47] H. Taheri, L.W. Koester, T.A. Bigelow, E. Faierson, L.J. Bond, In-situ additive
manufacturing process monitoring with an acoustic technique: clustering performance
evaluation using K-means algorithm, J. Manuf. Sci. Eng (2018). Submitted.
[48] M.A. Al Faruque, S.R. Chhetri, A. Canedo, J. Wan, Acoustic side-channel attacks on
additive manufacturing systems, in: Proceedings of the 7th International Conference on
Cyber-Physical Systems, 2016, pp. 19:119:10.
[49] S.A. Gold, T.G. Spears, Acoustic monitoring method for additive manufacturing pro-
cesses. US Patent Application US20170146488, 2017.
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Combining additive
manufacturing with conventional 19
casting and reduced density
materials to greatly reduce the
weight of airplane components
such as passenger seat frames
Francis Froes
Light Metals Industry, Tacoma, WA, United States

Autodesk research scientist Andreas Bastian, at the company’s Pier 9 technology


center in San Francisco has “bridged the gap” between 3D printing and conven-
tional metal casting [1], he has created a lightweight frame for an airplane seat
(Fig. 19.1A), which could not only reduce carbon emissions, but also save airlines a
lot of component weight and money through the associated fuel saving
(Fig. 19.1B).
The mass distribution in Seats is shown in Fig. 19.2 [2]. Autodesk has used additive
manufacturing (AM) and generative design to help airliners reduce carbon emissions,
fuel consumption, and weight before: In 2015, the company collaborated with Airbus
to create a 3D printed airplane cabin structural component. Once the dividing bionic
partition, currently undergoing Federal Aviation Administration (FAA) testing, is
deployed across the production backlog of Airbus A320 jets, it’s estimated to reduce
carbon emissions drastically: equal to removing 96,000 cars from the road.
An algorithm in Autodesk’s Netfabb software was used to produce the geometry
for Bastian’s aircraft seat frame, which would work in any standard commercial jet.
The goal was to keep the frame as strong as the original, but make it much more
lightweight; using lattice and surface optimization, the software was able to design
a complex structure that will make the aircraft seats so lightweight that the need for
jet fuel is significantly reduced. However, conventional manufacturing methods
would not be able to create the complex geometries that are often used with 3D
printing technology, and the cost of 3D printing at scale is not yet at a point where
it is competitive with traditional production methods, such as casting.
While there are several metals used for 3D printing, the casting process can be
completed with thousands of metals and composites. Also, even using Autodesk
Project Escher technology [1], 3D printing volumes are typically just a few cubic
feet, while casting can work with huge objects. So Bastian combined the two
Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00021-2
© 2019 Elsevier Inc. All rights reserved.
420 Additive Manufacturing for the Aerospace Industry

Figure 19.1 (A) Airline passenger seats. (B) Andreas Bastian with airplane seat frame.

technologies: positive molds for the seat frames, containing the lattice geometry,
were 3D printed in plastic in order to save money and time, and were next used to
make affordable, ceramic casting molds (Fig. 19.3) by basically using the “lost
wax” process (Fig. 19.4). Examples of the final complex seat assembles are shown
in Figs. 19.1, 19.5 and 19.6.

“While additive manufacturing holds great promise for the future of


manufacturing, it’s still very new for many product developers,” said Bastian [1].
“Casting, by contrast, has been around for millennia and is incredibly well
understood. There are hundreds of thousands of engineers, foundries, and factories
with deep expertise in it. That’s one of the reasons I am looking for a bridge
between the two.”
Combining additive manufacturing with conventional casting 421

Actuation system; 0,860


kg; 2%
PU-foam; 0,823 kg; 1%

Fabric/Leather; 2,027 kg;


4% Steel; 5,808 kg; 10%

Foam; 4,626 kg; 8%


Cable; 1,954 kg; 3%

LRU (IFE); 6,792 kg; 12%

Aluminium; 24,776 kg;


43%
Seat Belts; 0,832 kg; 1%

Plastics; 9,248 kg; 16%

Figure 19.2 Mass distribution in conventional airline seats.

Figure 19.3 Since Pier 9 is not equipped with molten metal investment casting capabilities,
Bastian worked with Michigan-based foundry Aristo Cast.
422 Additive Manufacturing for the Aerospace Industry

Figure 19.4 The basic steps in the conventional investment casting “lost wax” Process. In
the fabrication process used in the present work, the wax injection is replaced by the
construction of a complex plastic assembly using AM. This assembly is coated with a
ceramic shell and the plastic is melted out in the dewaxing step. The molten metal is then
poured into the complex ceramic cavity and the final metal (aluminum or magnesium) part is
formed as one monolithic piece (rather than the separate castings shown above) as shown in
Figs. 19.1, 19.5 and 19.6. AM, Additive manufacturing.

Figure 19.5 Close-up view of the complex, almost organic, lattice structure resulting from
the design optimization software.

Andy Harris, part of Autodesk’s advanced consulting group, worked with


Bastian on the seat frame project.

“We can generate these incredible high-performance designs, but we had to look
beyond direct metal additive manufacturing for this project,” Harris explained.
“The size and cost just wouldn’t work for fabricating this part.”
Combining additive manufacturing with conventional casting 423

Figure 19.6 Bastian shows off how lightweight the new seat frame really is.

“We’ve seen a lot foundries in our region shutter their doors in recent years as
manufacturing moves overseas,” said Aristo Cast CEO Jack Ziemba. “We see
adopting new techniques, like additive manufacturing, even when blended with our
expertise in casting, as a way forward—not just for our company but for lots of
other foundries in the Midwest” [1].

Aristo Cast realized that the weight of the airplane seat frame could be reduced even
more if it were cast in magnesium, which is 35% lighter than the typical aluminum.

“We leapt at the opportunity to work with Andreas and Autodesk,” said Aristo
Cast Vice President Paul Leonard. “It’s an exciting project and allowed us to
pioneer some new techniques for magnesium casting. It also gave us a chance to
learn more about advanced design and optimization techniques. That’s still quite
new in our industry” [1].

Harris re-ran the part simulations in Netfabb for magnesium to confirm its prop-
erties, and Bastian sent the updated 3D model to Aristo Cast. It was 3D printed in
plastic resin first, and then coated in ceramic to make a negative mold; the plastic
was later heated and vaporized off after the ceramic shell had hardened. Using the
mold, the foundry cast small quantities of the parts, but was able to prove that the
process could actually be used to scale up to 160 seats every 2 days (Table 19.1).
Bastian and Pier 9 resident Rhet McNeal determined that each seat frame,
weighing in at 766 g, is 56% lighter than the aluminum seats currently in use: the
424 Additive Manufacturing for the Aerospace Industry

Table 19.1 Characteristics of airbus 320 and 380 with modified seat frames

A321 A380
236 seats 615 seats
Weight savings 214 kg 557 kg
Annual fuel savings per aircraft 9.6 tons 63 tons
Annual carbon emission reduction per aircraft 28.9 tons 190.1 tons
Annual fleet savings (assuming fleet of 100 $1,569,365 $10,332,446
aircraft)
Lifetime fleet savings (100 aircraft over 20 $31,387,300 $206,648,920
years)
Fleet lifetime reduction in carbon (100 57,800 tons/ 126,000 tons/
aircraft over 20 years) 12,298 cars 80,894 cars

magnesium accounts for 24% of this weight reduction, while the design optimiza-
tion is responsible for the other 32%. So, if Airbus, for example, replaced the 615
seats on 100 A380 jets, which have a typical 20-year lifespan, with Bastian’s light-
weight frames, the airline could save over $205,000 (this is based on 2015 average
jet fuel costs). Going back to eco-friendly matters, this translates into a reduction of
126,000 tons of carbon emissions.
Autodesk and Aristo Cast were recently honored by the American Foundry
Society with its Casting of the Year award for the lightweight seat frame, which
Bastian is quick to note is still just a research project, but one with “clear commer-
cial applicability.”

Bastian said, “The purpose of this project was never to sell seat frames. The intent
is to show the power of combining Autodesk’s advanced technologies in generative
design and AM with a much more widely-used fabrication process: casting. Yes,
there are great applications for aerospace, but this combination can also be used
in automotive, medical devices, industrial equipment, and many other fields [1].

A concern with magnesium alloys is their flammability. However, Magnesium


Elektron has recently developed rare earth containing alloys that are not susceptible
to this problem [2]. Both Elektron 21 (also known as ASTM EV31A), a sand cast-
ing, and Elektron 43 (Mg-4.0Y-2.9RE-0.2Zr) (also known as ASTM WE43C), a
wrought plate or extrusion alloy, have undergone extensive flammability testing by
the FAA, which has shown that the use of these Elektron 21 and Elektron 43 alloys
in aircraft interior components (such as seat frames) does not reduce the level of
safety of the aircraft when compared to heavier aluminum seat components. This is
a very significant and major breakthrough for Mg alloys. The technology being
used produces a cast structure and so the integrity of the investment casting is
Combining additive manufacturing with conventional casting 425

critical, also the ability to scale up to the necessary volumes while maintaining the
quality. There are at least 400,000 seats being made annually. All the work
Magnesium Elektron has done to date involves both high-strain-rate impact testing
to meet the various loading criteria, most extreme of which is the 16 g forward load
requirement, and fatigue; although 20,000 cycles is the minimum specified the seat
producers and airlines generally work to a much higher standard [2].

Conclusions
Key to the technology described in this paper is the utilization of AM to fabricate a
complex plastic precursor that is then used to produce the mold for a metal casting.
As there are a lot of areas in an aircraft seat where moderate tensile strength in
conjunction with moderate ductility is best practice, magnesium now has a chance
for introduction into the aircraft seat business. The aircraft seat industry has been
eager to get clearance for takeoff and landing with magnesium alloys for a long
time, and now has this approval.

References
[1] Autodesk web site, accessed 5-12-17.
[2] M. Alderman, Magnesium Elektron, Private Communication, May 15, 2017.
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Synergetic technologies of direct
layer deposition in aerospace 20
additive manufacturing
Petr A. Vityaz1,2, Mikhail L. Kheifetz1,3 and Sergei A. Chizhik1,4
1
Presidium of the National Academy of Sciences of Belarus, Minsk, Republic of Belarus,
2
Joint Institute of Mechanical Engineering of the National Academy of Sciences of
Belarus, Minsk, Republic of Belarus, 3State Scientific and Production Association
hhCenterii of the National Academy of Sciences of Belarus, Minsk, Republic of Belarus,
4
A.V. Lykov Heat and Mass Transfer Institute of the National Academy of Sciences of
Belarus, Minsk, Republic of Belarus

20.1 Introduction
The aerospace industrial products are typically characterized by a complex shape
and, very so often, are made from materials that feature poor machinability. Surface
engineering of parts formed from such materials necessitates the use of concen-
trated energy fluxes to make processing more intense and ensure high product qual-
ity in additive manufacturing [13].
Therefore, when designing aerospace industrial processes, of primary importance
is the system analysis of processing methods that use the concentrated energy fluxes
in additive manufacturing in order to deposit functional layers and to shape surfaces
and edges of articles [46].
The energy fluxes cannot only shape the product, but also create a composite
material with a gradient of properties. Therefore, layer-by-layer synthesis of the
product shape should be considered as closely related to the synthesis of composite
materials in additive technologies [79].
Additive synergetic technologies of the layer-by-layer synthesis, which are based
on the surface self-organization phenomena, can stabilize the material’s properties
and the thickness of a directly deposited layer, smooth out the topography of com-
plex surfaces, and ultimately fuse into a gradient composite material formed as a
result of the layers interpenetration [10,11].

Additive Manufacturing for the Aerospace Industry. DOI: https://doi.org/10.1016/B978-0-12-814062-8.00022-4


© 2019 Elsevier Inc. All rights reserved.
428 Additive Manufacturing for the Aerospace Industry

20.2 System analysis of the processing methods using


the concentrated energy fluxes
At present, the scientific and technological requirements toward the surface
strength, hardness, toughness, and wear resistance turn out to be much more strin-
gent than those imposed upon traditional processing methods, which, in some cases,
appear inefficient in ensuring the necessary quality parameters of the product func-
tional layers. So, the aerospace enterprises often apply processing methods con-
nected with the use of plasma, electric arc, laser, electron beam, ion, and other
high-energy-density sources.
Due to the processing complexities that are connected with the use of various energy
fluxes, either sequentially or in parallel order, for forming various surface layers, a
rational layer design for the composite-material product should be considered.
Classification of technological processes (Table 20.1) includes the following
generalized groups: (1) separation (e.g., by cutting) of a blank material into work-
pieces with volume V1 and manufacturing of a part with volume V2; (2) deposition
of a surface layer, i.e., coating; in this case V2 . V1, (3) thermal or other treatment
by energy fluxes (V2  V1); (4) removal of excess material by cutting (V2 , V1); (5)
deformation, compaction, and smoothing of the material (V2  V1) [10,12]. This
classification enables one to formulate appropriate boundary conditions to an open
technological system (here term “open” is used in the synergetic meaning).
Additional degrees of freedom of boundaries in the open system, such as move-
ments or changes of external influences, enable one to control the nonequilibrium
state of the system, while additional energy fluxes at the initial moment may pro-
vide stabilization of a nonequilibrium technological process [5,11].
Fig. 20.1 summarizes the analysis of efficient processing technologies that employ
concentrated energy fluxes [4,5], which combine several methods: (1) those that
change the boundary conditions by introducing additional degrees of freedom for the
motion of a working medium (e.g., tool, technological medium, machining allowances,
formed surface, etc.), and (2) those that change the initial conditions through additional
energy sources having different concentration levels. The latter are conventionally sub-
divided according to the mode of energy distribution, or localization, over the surface
of a part: uniformly surface-distributed (I), multiply localized (II), and focused (III). In
fact, most of the combined methods can be implemented in manufacturing and only
some of them are virtually impossible at present. But, at the same time, such synergetic
effects may also occur as side effects and incidental phenomena in surfacing. The per-
formance analysis demonstrates the feasibility of processing methods that combine
both mechanical and thermal effects [10,11].
Distribution analysis of the processing methods, with regard to the accuracy of
surface formation, was performed according to the classification scheme shown in
Table 20.1 depending on the energy concentration level (I, II and III) for a variety
of typical energy sources (Fig. 20.1). For deformation and machining, the accuracy
of the surface treatment was assessed by deviations in size and shape, waviness,
and roughness; for thermal treatment, it was judged by the irregularities in the depth
of thermal hardening or softening zones and by the thickness of a defective surface
Table 20.1 Combined physicochemical methods of surface formation: effective in industry ( 3 ), of low effectiveness (2) and unfeasible (0)

I0 . Material removal II0 . Surface engineering III0 . Heat treatments IV0 . Machining V0 . Deformation using
different tools

of energy and their


Heat release zones

Thermal splitting

Tool with forced

Self-moving tool
Surface alloying

Edge tool/cutter
Amorphization/
power q, W/cm2

Thermal shock
Typical sources

Spray coating

displacement
Melt blowing
Melt outflow

Evaporation

Tempering
Quenching

Annealing
Cladding

Abrasive
melting

Striker

Roller
Plate

Ball
I. Bulk 1. IH (102). . .   0 0 3 3 3   3 3 3 3 3 3  3 3 3 3
103. . .104
2. GF  3 3  3 3 3   3 3 3 3 3 3  3 3 3 3
102. . .103. . .
(3 3 103)
3. PA 3 3 3  3 3 3   3 3 3 3 3 3  3 3 3 3
5 3 102. . .
3 3 104
II. Multiple 4. EH 103. . .   0 0 3        3 3 3 3  3 3 3
localized 5 3 104
5. WA   3 3 3 3 3   3 3 3 3 3 3 3  3 3 3
103. . .105. . .
(106)
6. SD     3 3 3 3            
5 3 106. . .
8 3 108
III. Single 7. EB (103). . . 3 3 3 3 3 3 3 3 3 3 3 3        
focused 106. . .
8 3 108
8. CW laser 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  3 3 3 3
(5 3 103). . .
106. . .109
9. PL (107). . . 3 3 3 3 3 3 3 3 3 3 3 3 3 3 3  3 3 3 3
1010. . .1014

IH, Induction heating; GF, Gas flame; PA, Plasma arc; EH, Electrocontact heating; WA, Welding arc; SD, Spark discharge; EB, Electron or ion beam; CW, Continuous wave; PL, Pulse laser.
430 Additive Manufacturing for the Aerospace Industry

Figure 20.1 The distribution of the components’ surface forming operations according to the
surface treatment accuracy and quality δ (μm), depending on the power density q (W/cm2) of
standard sources with various levels of energy concentration (The legend is in Table 20.1).
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 431

layer; for cutting into pieces and coating deposition, all the aforesaid indicators
were taken into account.
Analysis of the surface accuracy formation shows (Fig. 20.1) that the power den-
sity increases from the first to the third level of energy concentration (I ! II !
III), which, in turn, results in a reduced size of the energy distribution zones. On
the other hand, reducing the size of heat distribution zones (from I0 to V0 ) increases
stress concentration, which affects the shape and accuracy of the formed surface.
It is obvious that on level I, the accuracy does not increase. This is connected
not with a higher energy concentration, but primarily with a wider heat distribution
zone. At level II, the accuracy is minimal. This is because of formation of a large
number of stress concentrators due to the existence of numerous localized heat con-
centration zones. At level III, the accuracy does not decrease and, then, with raising
the energy density, it substantially increases due to heat focusing into narrow zones,
which is accompanied with a rapid increase in stress concentration.
From the above analysis, it follows that optimal initial conditions for different
technological operations of surface formation can be provided by a proper
choice of a concentrated energy source under given boundary conditions.
Typical sources of level I can be most efficiently used for deformation of large-
size parts, machining in the conditions when a large volume of material has to
be removed, for coating deposition and bulk heat treatment/hardening. Sources
of level II significantly decrease the surfacing accuracy, so they should be com-
bined with cutting and deforming tools, in particular in the coating deposition
and heat treatment processes. The best results in all technological surfacing
operations are obtained with the sources of level III. The data presented in
Table 20.1 support this conclusion, and the surfacing accuracy analysis proves
that the proposed classification of processing methods, which employ concen-
trated energy fluxes, is valid [4,5].
The above analysis outlines promising ways to advance surface engineering that
will provide specified accuracy and other quality factors.
A technological system for high-energy-density processing is open (in the syner-
getic sense) primarily to thermal and mechanical energy fluxes, which determine
the change of initial and boundary conditions for surfacing with an accuracy of the
order of microns. The energy that exceeds a certain level, below which the system
maintains dynamic equilibrium, should have conditions to dissipate or be adsorbed
by additional degrees of freedom of the system. In a thermomechanical system,
additional degrees of freedom are provided by the movements of a working medium
(tool, technological media, and environments) as well as by additional structures,
phases, and increased number of interfaces that adsorb excess energy and maintain
the shaping process in one or more particular states.
Thus, increased surfacing efficiency is ensured both by additional energy
fluxes and the degrees of freedom of the system’s elements. With increasing
energy concentration, the zone, where the incoming energy flux interacts with
surface, undergoes spontaneous evolution: from a wide, surface-distributed zone
it disintegrates into multiply localized zones and then they focus into a single
spot. Additional degrees of freedom of the system’s elements allow modification
432 Additive Manufacturing for the Aerospace Industry

of the surfaces, phases, and structures and thus permit maintaining the energy
fluxes and interaction processes in certain states through certain surface self-
organization phenomena.

20.3 Additive synergetic technologies of layer by layer


synthesis
Advanced technologies, along with the new hardware and software, equipment, and
outfit, are based on layer-by layer growing of surfaces and self-organization of
structures of the composite material [7,9]. Thus, when defining the basics of
advanced nanotechnologies, Alferov [13], in addition to atom probe microscopy,
mentioned the epitaxial growth of films on a surface and processes of self-assembly
of the material heterostructures.
Moreover, according to the synergetic concept, there is a limited number of states
and transition rules in a technological system [4]. The dominant processes of struc-
ture formation under intensive influences can be defined with the notion of mode,
which is used when describing distributions of continuous random variations of a
control parameter [10]. The notion of mode signifies such a parameter value when
its distribution density has a maximum.
According to the synergetic concept, stable modes adjust to the dominant
unstable ones and, thus, can be ignored. This results in a sharp reduction of the
number of control parameters, and the remaining unstable modes can serve as order
parameters determining the processes of structure formation [7].
So, particularly promising is an approach that considers additive methods as syn-
ergetic technologies that enable surface self-organization phenomena to occur in the
layer-by-layer synthesis of different materials and provide control of their properties
under various physical influences [14,15].
The surface self-organization brings about stable layer formation of a certain
thickness when the distance from the energy source or a feed material to the form-
ing surface changes significantly and thus allows to join successive layers as a
result of interpenetration [4].
The distance to the surface is a very sensitive factor in the layer formation
mechanisms that operate in the direct deposition (DD) technique while a change in
the distance is especially important for the layer-thickness stabilization in the bed
deposition (BD) technologies.
From the above, it can be concluded that the choice of an energy source and/or
feed material in additive manufacturing determines not only the technological route
but also surface phenomena that provide the self-organization processes to occur in
synergetic technologies [4].
Direct growth of parts during the layer-by-layer synthesis is possible in different
phase states, such as solid, liquid, or gaseous, and can be implemented in a variety
of high-energy processes [6,7] with surface-distributed, multiply localized, and
single-focused energy adsorption zones [16,17] depending on the power density in
the energy flux (Table 20.2).
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 433

Table 20.2 High-energy processes of layer-by-layer synthesis of parts

Cutting and deposition Phase state Energy adsorption Thickness of the


processes of the zones and energy formed or
deposited flux density, W/cm2 removed layer,
material mm
Plasma cutting, spray Solid Surface-distributed, 0.110.0 [18]
powder deposition, (powder) 5 3 102105
and hard-facing
Electroerosion treatment Hard- Multiply localized, 0.050.50 [19]
and electromagnetic surfacing 103105
hard-facing of powder (powder)
Ion implantation and Gaseous Multiply localized, 0.0020.200 [5]
deposition 103105
Electron-beam and laser Liquid (melt) Single focused, 110 (in thermo-
cutting, surface 5 3 103107 electric
melting, and alloying convection
0.11.0) [20]

Surface-distributed energy adsorption zone is formed in plasma-base processes,


such as plasma cutting, deposition, and hard-facing using metal powders [18]. The
thickness of the formed layer is determined jointly by kinetic and thermodynamic
factors, such as the velocity of powder particles and the thermodynamic potential of
the plasma flux, while the layer formation process is characterized by a ratio
between the kinetic and Joule energy of the flux.
Multiply localized energy adsorption zones are formed in the course of surface
electroerosion processing and electromagnetic powder deposition. In electromag-
netic deposition, the thickness of a quality coating is restricted: above a certain
thickness the layer loses stability, surface peaks appear, and grow. Then the apexes
of these peaks melt and evaporate so that craters are formed on their summits [19].
The electromagnetic flux allows controlling the surfacing process. Thus, motion of
the ferromagnetic powder particles and fixation of the latter to the surface is deter-
mined by the induction of the magnetic field while the heat release intensity in the
formed surface joints and powder melting are determined by the electric field
strength. The synergetic effect of the aforementioned factors brings about stabiliza-
tion of the layer thickness [4]. The process of electromagnetic surfacing is deter-
mined by electromagnetic and inertial forces and proceeds through electromagnetic
interaction of particles with the electric field in the working zone.
In the ion implantation and gas-phase deposition, the unfocused ion beam is dis-
tributed over the surface of the part, forming multiply localized energy adsorption
zones. The thickness of the produced coating is determined mainly by the thickness
of the layer where the electric potential applied to the part effectively influences the
ions [19]. This layer is determined by a relation among the electric field potential,
the plasma ion flux density, and the charge and mass of ions. Due to a joint effect
of the potential energy of ions in the electric field and thermal energy of the plasma
434 Additive Manufacturing for the Aerospace Industry

flux, the ions become spatially distributed according to the exponential law thereby
determining the thickness of deposited coating [5].
In the electron-beam and laser cutting, surface melting, and alloying, a single-
focused energy adsorption zone scanning over the entire formed surface should be
considered [4]. In electron beam processing, dissipative vortex structures are
formed as a result of convective instability in a thin surface layer of a melt. At rapid
cooling, a cellular structure is formed along the crystallization front. The thickness of
the modified layer is described by the material properties such as the surface tension
and volume expansion coefficients and the density in molten state [20]. The forma-
tion of dissipative structure in the melt is determined by thermocapillary phenomena
and is related to the buoyancy force and energy dissipation in the melt [5,20].
The considered high-energy processes permit performing layer-by-layer deposi-
tion of materials with special properties on a complex-shape surface. This, in turn,
enables engineers purposefully to modify the physical and mechanical properties of
a surface, tailoring them to the working requirements imposed on a particular
machine part [4,5,21].
The layer deposition conditions in high-intensity processes should be related to
the design features of a target product. The plasma spraying and surfacing processes
involve edge rounding [18]. The thickness of a deposited layer decreases on the
most protruding sections in electromagnetic surfacing [19]. In ion deposition of
coatings, the layer grows most intensively on the peaks with a small radius at the
vertex due to the increase of the electric potential [5]. In electron-beam or laser
melting, the thickness of the modified layer is nonuniform and depends on the
alloying elements (if any) because of the segregation of elements in the melt due to
the formation of vortices [20].
Finally, the conditions of layer deposition in high-energy processes should be
related to the design features of the target product. For layers of a prescribed thick-
ness, which are formed in physical fields, the stability of a technological system
should be ensured in the induction, plasma, electromagnetic, laser, electron, and ion
beam surface treatment.
The system analysis of the concentrated energy fluxes used in additive
manufacturing of aerospace products from poor machinable materials and the sur-
face self-organization phenomena that occur in layer-by-layer synthesis reveal that
ion and electron-beam treatment of aviation materials in a vacuum should be con-
sidered as very promising.

20.4 Ion implantation and ion deposition of coatings


Combined ion modification or ion implantation followed by ion deposition of coat-
ings is a method for improving the quality parameters both in the process of ion
modification of a surface and in the subsequent service of the latter [6,11].
As a result of high-energy surface processing, alloying atoms can be implanted
at a rather high concentration into a material to form a modified transition layer.
The implanted ions experience numerous elastic collisions with atoms of the crystal
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 435

lattice, and radiation defects, whose number by two or three orders of magnitude
exceeds the number of implanted atoms, are produced in this layer. These two pro-
cesses have a substantial effect on physical, mechanical, and physicochemical prop-
erties of the surface, which sometimes brings about structural and phase
transformations. When such a composite layer works in the condition of friction, a
specific self-organization process occurs within the layer, which involves interac-
tion of dislocations with grain and phase boundaries and slows down the develop-
ment of microplasticity [6,11]. Initial conditions for the formation and
reorganization of ion-modified layers are determined by chemical, phase, and struc-
tural composition of the substrate, type of the ions and base atoms, and the implan-
tation energy. The structural self-organization of such a layer during friction
depends on the energy of frictional interaction of the surfaces. The boundary condi-
tions in this system depend on design of modified layers and relative displacement
of the surfaces during service.
To reveal the mechanism of energy dissipation and the behavior of atoms in an
ion-modified layer, molecular dynamic simulation was performed for the case of
chromium-implanted heat treated R6M5 high-speed tool steel (0.82%0.9% C,
5.5%6.5% W, 4.8%5.3% Mo, 3.8%4.4% Cr, 1.7%2.1% V and up to 0.6%
Ni according to Russian standard GOST 19265-73) [6,11]. In the as-implanted state,
Cr atoms were considered as either located in interstitial sites (tetrahedral or octahe-
dral) of the martensite lattice or forming asymmetric dumbbell-shaped pairs with
host atoms (the so-called interstitialcy defects).
Such configurations of chromium atoms are nonequilibrium due to a substantial
elastic distortion of the lattice around them. Meanwhile, atoms in these configura-
tions are known to be highly mobile. As the implanted atoms migrate, they may
1. interact with vacancies and form stable substitutional configurations,
2. interact with each other or with other impurities in solid solution (for example, with car-
bon) to form clusters, and
3. escape into sinks (dislocations, grain, and phase boundaries).

As mentioned above, during implantation, the vacancy concentration in the mod-


ified surface layer substantially increases because of the radiation damage.
Therefore, one of the most probable diffusion-controlled reactions is the relocation
of implanted chromium atoms into substitutional positions.
Analysis of the Auger spectra confirmed the presence of a modified transition sur-
face layer with a thickness of about 1 μm (Fig. 20.2A). In this domain, the microhard-
ness, which was measured using a 10 g load on the indenter, was found to increase
from 5000 MPa in the initial state to 20,000 MPa after modification (Fig. 20.2B).
X-ray diffraction analysis has revealed a substantial increase in the martensite
lattice parameter in the modified layer, from 0.2879 to 0.2883 nm. At the same
time, a shift of the (1 1 0) and (2 0 0) martensite reflections toward smaller diffrac-
tion angles was observed or a slight decrease in the half-widths of the martensite
reflection lines. All these observations confirm our previous calculations performed
for the layer modified with chromium ions and testify to an increase of compressive
stresses. Moreover, the obtained results reject the idea that the martensite lattice
parameter changes due to distortion and different kinds of lattice strain and suggest
436 Additive Manufacturing for the Aerospace Industry

Figure 20.2 Distribution of chemical elements over depth H (μm) in R6M5 high-speed steel
(6% W, 5% Mo) after combined vacuum-ion surface modification (A); plot of surface
microhardness Hμ (MPa) versus load P (N) on the indenter (B) in the initial state (1) and
after modification (2) of R6M5 steel.

that only one explanation appears to be valid: iron atoms are substituted by chro-
mium atoms on the lattice sites, i.e., solid solution hardening occurs.
Microstructural analysis has shown that after vacuum-ion modification, the num-
ber of microcracks in the surface layer decreases without a notable change in the
phase distribution pattern. In general, the type of microstructure does not change.
The transition zone becomes a barrier for microdefects emerging on the surface,
thus increasing wear resistance of the high-speed steel.
So, combined vacuum-ion modification of the surface of the high-speed tool
steel with chromium atoms brings about substantial strengthening, which was pre-
dicted by the energy-dissipation simulation of ion-beam processing and subsequent
operation of the material. The predicted formation and growth of chromium clusters
in the martensite lattice is energetically favorable, and they can serve as sites for
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 437

Figure 20.3 The model of the formed multicomponent coating on the peaks (A) and
macropeaks (B) of the surface asperity: 1—heavy ions; 2—light ions; 3—self-spraying
zones.

further precipitation of intermetallic phases that improve the service tribological


properties of the surface.
The deposition of coatings or structure modification of surface layers by energy
fluxes results in layered structure of the processed material. Transition zones are
formed between the layers and their dimensions have a significant effect on physi-
cal and mechanical properties. The study of surfacing mechanisms combined with
modeling of the coating structure and, particularly, formation of boundaries
between the deposited layers, enables one to select optimal modes of deposition
and control the quality of surface treatment and hence working properties of the
material [3,7,8].
When considering the mechanism of deposition of multicomponent ion-vacuum
coatings, a smooth surface with peaks was taken as a basis (Fig. 20.3).
A negative accelerating potential is applied to the surface. The ion beam directed
to the substrate consists of singly charged ions of several elements, which signifi-
cantly differ by mass. Far from the solid material, the ion velocity vector is directed
perpendicular to the surface. When ions approach the peaks, the direction of their
flight changes because of a significant change in the electric field strength. Due to
a difference in ion masses, deviations will be different for unlike species. The tra-
jectory of ions with a smaller mass has a larger curvature, and they are deposited
mostly near the peak’s top. Ions with a larger mass, as well as an electrically neutral
phase (vapor, liquid droplets, fragments), are deposited more uniformly [7,8].
Due to inhomogeneity of the electric field strength, separation of the ion beam
by mass is observed near the surface of the material, while, in reality, the same is
observed with respect to the charge as well. Such separation of the ion flux at the
initial stage of coating formation will result in rapid growth of the coating at the
top of the peak (Fig. 20.3A). However, as it grows, the corner radius will decrease.
438 Additive Manufacturing for the Aerospace Industry

As a result, at a certain instant of time, the corner radius and thus the electric field
intensity will reach the values when the sputtering rate and the condensation rate
become equal, and the growth of the surface peak terminates. At the same time, the
process of coating formation in between the asperities will still continue, mostly
due to deposition of heavy ions and the neutral phase. As a result, the space
between them becomes so filled that it itself will become a site for the growth of a
new peak (see Fig. 20.3A). In the considered model, separation of the ion flux by
the mass of atoms occurs. However, in reality, the beam includes differently
charged ions, which will lead to ion separation by charge.
In ion-vacuum processing, condensation is accompanied by ion sputtering
(Fig. 20.3B). Moreover, if the condensation surface features macropeaks that
increase the electric field strength, a more intense self-sputtering process can be
expected.
As a result of the multicomponent ion condensation, zones with increased con-
centration of light and multiply charged ions will appear, where the self-sputtering
process is more intense than in other regions (see Fig. 20.3B). Consequently, the
concentration of light elements and those forming multiply charged ions in the coat-
ing will decrease due to self-sputtering.
Thus, modeling of the multicomponent ion-vacuum coating formation should
take into account ion separation by mass and charge in asperity zones, which occurs
as a result of increased electric field strength. Also, it is necessary to consider the
scale factor of surface irregularities and their shape [3,7,8].

20.5 Electron-beam heating of a coated surface


Electron-beam heating (EBH) of a surface with a preliminary deposited galvanic,
chemical. or detonation coating is a technological process that combines melting of
the coating and the substrate, with subsequent formation of a transition layer with a
large thickness [6,11].
Depending on the conditions of thermal processing and the coating thickness and
composition, the melted and then crystallized layer may have either equiaxial fine-
grained or cellular structure [4,22]. Structure formation is determined by the initial
conditions, i.e., melting and rapid chilling of a molten layer, as well as by the
boundary conditions, such as trajectory and rate of the electron beam scanning.
Billets of titanium alloys VT6 (Ti 1 3.5%5.3% Al 1 0.3% Zr) and VT9 (Ti 1
5.8%7.0% Al 1 2.8%3.8% Mo 1 1.0%2.0% Zr) were subjected to case hard-
ening in order to obtain a hardened layer with a thickness of up to 1.3 mm and then
processed by EBH [6,11]. It has been revealed that after EBH, the size of
β-converted grains near the surface increases substantially, up to 150 μm, from the
initial size of about 15 μm. In this case, the size of martensite plates is determined
not only by the grain diameter but also by structural microinhomogeneity caused by
enhancement of diffusion processes during EBH and arresting of the formed con-
centration distribution by rapid chilling. Near the surface of the specimen, the phase
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 439

composition includes two types of martensite, α0 and αv, with different concentra-
tion of β stabilizing alloying elements. This is connected with the fact that α phase,
which experiences the α-to-β transformation at rapid heating, features nonuniform
composition. The hardness gradually decreases over the cross-section from HRC
4345 on the surface to HRC 2437 in the bulk.
Studying the distribution of aluminum and titanium over a cross section enables
one to differentiate two surface layers. The first (outer) layer with the thickness of
140160 μm features almost constant content of these elements throughout the
depth, aluminum concentration being almost two times lower than in the initial
alloy. In the second layer, increased concentration of aluminum and decreased con-
centration of titanium are observed. At a larger distance from the surface, the alloy
structure features a large amount of retained α phase and grains of β solid solution
with a lower concentration of molybdenum, which were formed during the dissolu-
tion of α phase particles at rapid heating.
So, the concentration drop of alloying elements on a microlevel increases when
moving away from the surface. Taking into account that α phase, as well as grains
of β phase with reduced content of molybdenum, have an increased concentration
of aluminum, the process of EBH causes directed motion of aluminum atoms into
zones with the lowest concentration. They correlate with the domains of β phase
that border undissolved particles and molybdenum-depleted zones, which are
located at a larger distance from the surface. With increasing the heating tempera-
ture, the surface areas of β solid solution tend to an equilibrium state while the
domains of undissolved α phase and the zone with a noticeable concentration drop
displace farther off the surface, and so the concentration distribution changes.
When the titanium surface experiences melting during EBH, thermocapillary
convection develops in the molten layer. This phenomenon is caused by the temper-
ature dependence of surface tension. In such situation, the so-called Benard convec-
tion cells are formed in the melt layer [6,22]. The microstructure of titanium alloys
VT6 and VT20 (Ti 1 5.5%7.0% Al 1 0.8%2.5% V 1 0.5%2.0% Mo 1
1.5%2.5% Zr), which forms after quenching from a liquid state due to fast heat
removal to the interior, features closely packed hexagonal-cylindrical cells with a
diameter of 57 μm. Microvoids that are observed at grain boundary junctions
have a size of up to 1 μm. In the transition zone from cellular to β-transformed
structure, the amount and size of cells steadily decrease, the grain size being
100200 μm. In the interior, the maximum size of martensite-type needles corre-
sponds to the cell diameter (Fig. 20.4).
In the process of dissipative structure formation, intensive redistribution of alloy-
ing elements occurs in liquid phase; the elements that reduce surface tension are
accumulated near the walls and at corners of the cells. Substantial segregation of
elements in β phase results in the formation of alloyed αv martensite in the VT20
single-phase pseudo-α alloy in zones with cellular structure. The αv phase lattice
parameters change from a 5 0.2922 nm and с 5 0.4667 nm in the initial state to
a 5 0.2923 nm and c 5 0.4729 nm for cellular structure, i.e., the tetragonality of α0
martensite increases. The α0 martensite lattice parameters are the following:
a 5 0.2952, b 5 0.5294, с 5 0.4691 nm. As the martensite-type αv phase is formed
in the structure of VT20 alloy, the thermostability of the latter may increase.
440 Additive Manufacturing for the Aerospace Industry

Figure 20.4 Cellular structures ( 3 3000) of titanium alloys VT20 (a) and VT6 (b) with
unetched surfaces after electron-beam heating for 1 s with power density of 3 kW/cm2.

EBH of titanium alloys VT6 and VT23 (Ti 1 4.4%5.7% Al 1 4.0%5.5% V


1 4.0%5.5% Mo 1 0.5%1.5% Cr 1 about 0.3% Zr) with a preliminary oxi-
dized surface permits increasing the microhardness both in the surface layer and
beneath it, which testifies to the diffusion of oxygen to deeper layers. The α-phase
layer becomes four times thicker. EBH of VT6 and VT23 alloys after preliminary
siliconizing causes redistribution of aluminum farther from the surface. The thick-
ness of the α-phase layer increases twice, the layer becomes more porous and par-
tially undergoes martensitic transformation. The total thickness and porosity of the
silicide layer, which was formed on the surface by the preliminary siliconizing
treatment, also increase [6,22].
When VT20 alloy with a galvanic chromium coating is heated by an electron
beam, the structure with grain diameter of 1020 μm is formed. The thickness of
diffusion layer and that of residual chromium coating are 1012 and 56 μm,
respectively [6,22]. As the heating temperature increases, the continuity of the outer
chromium coating is destroyed. Due to a higher rate of grain boundary diffusion,
chromium diffuses along the β titanium grain boundaries into the titanium matrix of
VT20 alloy. In this case, the grain size in the bulk is 80120 μm. At further heating
to a higher temperature, TiCr2 intermetallic starts melting. This brings about a char-
acteristic fine-grained structure that is formed after crystallization. The grain size is
about 210 μm and the thickness of the diffusion layer is about 30 μm.
When for EBH processing is performed with the goal of diffusion saturation of
the aforesaid titanium alloys with chromium, the heating regime is adjusted so as to
avoid surface melting. Then, solid solution of alloying elements in the surface
layers of α-titanium is formed along with compound TiCr2. The presence of α
phase throughout the entire diffusion layer indicates that the content of titanium is
larger than of chromium in the layer because Cr reacts with Ti to form intermetallic
compound TiCr2. Deeper into the material, where the concentration of chromium is
insufficient to produce TiCr2, chromium dissolves in titanium to form β solid
solution.
After EBH of alloy VT20 with a preliminarily deposited Ni coating, the grain
structure of the nickel layer becomes distorted. With increasing the heating
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 441

temperature, recrystallization of the surface zone occurs and the resulting structure
consists of equiaxed grains having 1030 μm in diameter with a pronounced mar-
tensitic intragranular structure. Solid solutions with martensitic structure, as well as
β solid solution of nickel in titanium, are formed in more distant layers. The Ni-
enriched grain boundaries are formed due to dominating nickel diffusion along the
boundaries of β-grains in VT20 alloy, which is accompanied by the intermetallic
compound formation [6,22].
At the EBH of chromium coating with a nickel sublayer, which were preliminar-
ily deposited on the surface of titanium alloy VT20, interdiffusion the TiNiCr
system occurs, which results in the formation of multicomponent solid solutions
and phase Ti2Ni (see Fig. 20.5AG). At the boundary between the nickel sublayer
and titanium substrate, eutectic reaction between Ti and compound Ti2Ni occurs.
Then the eutectic-melt layer crystallizes in the form of dendrites with a length of
812 μm in the direction normal to the outer surface. With a further rise in temper-
ature, the diffusion layer thickness reaches 300 μm. As the eutectic reaction pro-
ceeds, convection flows appear in the melt pool, thus enhancing the exchange of
elements between the coating and substrate, which results in the growth of strength-
ening layers and homogenization of the diffusion zone.

Figure 20.5 The microstructures of the surface layer ( 3 300) of the VT20 alloy with NiCr
coating after electron-beam heating to 700 C (A), 800 C (B), 900 C (C), 1000 C (D),
1100 C (E), 1200 C (F), and 1300 C (G).
442 Additive Manufacturing for the Aerospace Industry

Figure 20.6 The microstructures of the surface layer ( 3 500) of the VT9 alloy coated with
WC-15% Ni in the initial state (A) and after electron-beam heating to 1100 C (B), 1300 C
(C), and 1400 C (D).

Experimental study of surface engineering by EBH was performed for titanium


alloy VT9 with a hard-alloy WC-15% Ni coating, which was earlier deposited by
detonation spraying. EBH results in partitioning of the coating and underlying sub-
surface layers into a number of characteristic zones (Fig. 20.6AD). Due to diffu-
sion of nickel from the coating into titanium substrate, a zone of Ti-base solid
solution is formed at the former Ni/VT9 interface. Closer to the outer surface, a
zone of the β 1 Ti2Ni eutectic appears, and intermetallic compound Ti2Ni is
formed on the outside. The total thickness of these zones is about 20 μm. Together
with nickel, up to 5 wt.% of the tungsten initially contained in WC diffuses into the
titanium substrate, thus forming a Ti-base solid solution. Titanium concentration
decreases smoothly in the direction to the surface while the content of nickel
remains approximately the same throughout the formed solid solution layer. In the
course of heating, aluminum actively diffuses across the coating from the VT9 sub-
strate to the outer surface [6,22]. An increase in heating temperature causes a trans-
formation of the complex structure of the whole coating into a eutectic mixture
containing round-shaped particles of tungsten carbide. The coating processed by
EBH acquires a fine-grained structure with a grain size not exceeding 1 μm.
Also, experimental study of EBH of the VT9 alloy with a hard-alloy WC-25%
Co coating, which, as in the previous system, was preliminarily deposited by deto-
nation spraying. In this case, intermetallic compounds of titanium with Co (the
binding metal in the initial hard-alloy coating) are formed at the coating/substrate
interface (Fig. 20.7AD). Liquid phase that forms during heating substantially
intensifies the diffusion processes. The thickness of the modified layer as a whole
exceeds the thickness of intermetallic-compound layers in the titanium substrate by
a factor of 15. This is associated with a higher rate of titanium diffusion in the
metal binder, and may partly be attributed to the enhancement of diffusion in the
field of temperature gradient [6,22]. In the outer layer, the TiCo2-base eutectic acts
as a binder that provides strong adhesion of hard tungsten carbide particles to the
alloy thus imparting high wear resistance to the article.
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 443

Figure 20.7 The microstructures of the surface layer ( 3 500) of the VT9 alloy coated with
WC-25% Co in the initial state (A) and after electron-beam heating at 1100 C (B), 1300 C
(C), and 1400 C (D).

The microhardness distribution over the cross-section of the resulting coating


features a gradual decrease from the initial hard alloy coating to the titanium sub-
strate. After EBH, microhardness of the 0.10.15 mm thick outer layer is close to
that of the initial tungsten carbide-cobalt hard alloy coating. Deeper into the mate-
rial, microhardness decreases and in the bulk it corresponds to a value typical of the
titanium alloy [6,22].
Thus, during EBH of a titanium alloy with a hard-alloy detonation coating, the
nature of phase and structural transformations and the resulting composition are
mainly determined by diffusion processes at the initial coating/substrate interface.
Unlike EBH of electrolytic coatings on titanium alloy, in the case of detonation
coatings, the lamellar structure, which features different content of elements in the
layers, is preserved to temperatures up to 15001600 C. The refractory tungsten
carbide particles, which are present in the outer layer, hinder the development of
convective flows in the melt that forms at heating, and hence prevent homogeniza-
tion of the microstructure and composition in the outer layers.
In electron-beam surface engineering, the value of a quality parameter, e.g.,
hardness (Fig. 20.8A) should be compared with a structural parameter of the sur-
face. The latter can be characterized by a relative area of a modified surface, i.e., a
ratio of the surface area with modified structure to the total surface area
(Fig. 20.8B) [4,5,11].
Thus, formation of cellular structure on the EBH-modified surface of a single-
phase pseudo α titanium alloy (Fig. 20.4) occurs through the formation of dissipa-
tive vortex structures in the molten state. In this situation, a change in the state of
the thermodynamic system under consideration is determined by a prevailing con-
vection mechanism. At the onset of melting, narrow cells that are formed due to
thermocapillary force, which is described by Marangoni number, first originate and
then displace to the periphery of the heated spot. These cells consist of dissipative
vortices. With increasing the power density of an electron beam, natural convection,
which is characterized by Grashof number, develops in the central part of the
heated zone and blurs the aforesaid vortex dissipative structures. Wide toroidal
444 Additive Manufacturing for the Aerospace Industry

Figure 20.8 The distribution of the microhardness Hμ (GPa) over the depth H (μm) of the
surface layer of a titanium alloy with a chromium-nickel coating (A) with a temperature
change T(K) and the relative surface area S(%) with a modified structure as a function of the
specific power q (kW/cm2) and the duration τ (C) of electron-beam heating (B), the visible
boundary of the modified layer (I) and the melting point (II) are indicated by dashed lines.

vortices generated by the buoyancy force, which is described by Rayleigh number,


in the conditions of EBH are observed only when deep melting occurs [4,5,11].
Studying the ratio of the surface area with a cellular structure to the total surface
area (parameter S), which depends on power density q and heating time τ, has
shown that the largest area with regular structure, S 5 40%, is formed in a narrow
range of heating intensity (see Fig. 20.8B) [4,5].
From the viewpoint of the optimal control theory and nonequilibrium thermody-
namics, the above described situation can be considered as a controlled two-
parameter system. Then the cellular structure formed over a maximum surface area
(with S  40%) is characterized by a special state of the system, which is named the
unstable node, and with time the latter evolves to a limit cycle. This cycle is limited
by the solid-to-liquid phase transformation of the material. Within the frame of
these theories, formation of the solid/liquid interface during melting is described as
the unstable saddle mode. Heat/mass transfer from/to the solid/liquid interface
occurs by thermal conduction and convection, which stabilizes the state of the sys-
tem [6,7].
Synergetic technologies of direct layer deposition in aerospace additive manufacturing 445

The microhardness distribution (see Fig. 20.8A) depends on structural changes


in the system, which are connected with complex physicochemical transformations
that occur in the surface layer of titanium alloys with preliminarily deposited coat-
ings under the action of EBH. This distribution may be correlated to the pattern of
cellular structure formation (see Fig. 20.8B). Fig. 20.8A refers to electron-beam
processing of a titanium alloy with a chromium-nickel coating [4,5]. The aforemen-
tioned transformations include chemical reactions, solid-state diffusion of elements
form the coating into substrate, melting and eutectic reactions at the coating/sub-
strate interface, propagation of the melting front into the solid substrate, develop-
ment of convection in the melt pool, and subsequent solidification of the
multicomponent melt in the field of temperature gradient. In general, the pattern of
these complex processes strongly depends on the nonsteady-state temperature field
in the material, which, in turn, is eventually connected with the electron-beam pro-
cessing regime.
Thus, in order to attain a high coating-to-substrate bonding strength and improve
physicochemical parameters of the obtained surface structures, it appears necessary
rigorously to control the range of electron-beam power density and scanning
regime, which should be linked to the chemical composition of the system and the
coating thickness.

20.6 Conclusion
Additive processes of direct growth, or layer-by layer synthesis, which are selected
in accordance with the design features of the formed layers (BD-technologies) and
shells (DD-technologies) offer new opportunities for customized design and rapid
prototyping of machine parts. The surface self-organization phenomena that occur
in metals/alloys under the action of high energy density fluxes enable an engineer
to form outer layers of required thickness over a complex-shape surface. Moreover,
these technologies open up novel, very so often unique opportunities for synthesiz-
ing surface layers with phase composition, structure, and hence properties tailored
to the target function of an article. In other words, synergetic processes that are
intrinsic in the additive manufacturing technologies employing high-energy density
fluxes, e.g., ion and electron beams, present substantial interest not only for
mechanical engineering but for materials science as well.
The synergetic processes that occur in these technologies include, first of all,
self-organization of the energy adsorption zones on the material’s surface: from
surface-distributed to multiply localized and to single-focused. Second, self-
organization reveals itself in the formation of dynamic dissipative vortex structures
in the melt pool that forms on the metal surface at fast heating by an energy flux.
This has a profound effect on the spatial distribution of alloying elements, micro-
structure, and phase composition of the final solid product. In particular, formation
of regular cellular structures that are observed in the as-solidified state occurs
namely due to the aforesaid synergetic phenomena.
446 Additive Manufacturing for the Aerospace Industry

A deeper insight into the underlying physical and physicochemical mechanisms


that, in their synergism, produce the final structure of materials/coatings, necessi-
tates complex cross-disciplinary research that should employ experts in mechanical
engineering and in materials science. Such research will contribute to further devel-
opment of additive manufacturing using high-energy density fluxes and to the crea-
tion of both novel advanced materials and coatings for complex-shape articles.

Acknowledgments
The authors wish to thank Professor Anatoliy I. Gordienko for a helpful discussion and
Professor Boris B. Khina for numerous discussions and invaluable help in improving the
English language and presentation style of the paper.

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[16] M.L. Kheifetz, Analiz algoritmov proizvodstva izdeliy po modelyam samovosproizve-
deniya von Neumann [The analysis of product manufacturing algorithms according to
von Neumann’s self-reproduction models], Doklady Natsional’noi akademii nauk
Belarusi [Rep. Natl. Acad. Sci. Belarus] 45 (5) (2001) 119122 (In Russian).
[17] M.L. Kheifetz, Modeli i algoritmy proizvodstva izdeliy bez ispol’zovaniya formoobra-
zuyushchey osnastki [Models and algorithms for the production of articles without the
use of forming equipment], Vestsi Natsyanal’nai akademii navuk Belarusi. Seryya
fizika-technichnych navuk [Proc. Natl. Acad. Sci. Belarus. Physicotechnical series] (2)
(2001) 5962 (In Russian).
[18] P.A. Vityaz, V.S. Ivashko, E.D. Manoilo, Teoriya i praktika gazoplamennogo napyle-
niya [Theory and Practice of Gas Flame Spraying], Nauka i technika Publ, Minsk,
1993. 296 pp. (In Russian).
[19] M.L. Kheifetz, L.M. Akulovich, Zh.A. Mrochek, E.Z. Zeveleva, Elektrofizicheskie i
elektrokhimicheskie metody obrabotki materialov [Electrophysical and Electrochemical
Methods of Materials Processing], The Polotsk State University Publ., Novopolotsk,
2012. 292 pp. (In Russian).
[20] E.D. Eidel’man, Excitation of electric instability by heating, PhysicsUspekhi 38 (11)
(1995) 12311246.
[21] P.A. Vityaz, A.F. Ilyushchenko, M.L. Kheifetz, Operativnoe maketirovanie i proiz-
vodstvo izdeliy slozhnoy formy iz kompozitsionnykh materialov [Rapid prototyping
and manufacture of complex-shape articles from composite materials], Naukoyomkie
tekhnologii v mashinostroenii [Adv. Technol. Mech. Eng.] (2) (2011) 38 (In
Russian).
[22] A.A. Shipko, I.L. Pobol, I.G. Urban, Uprochnenie staley i splavov s ispol’zovaniem
elektronno-luchevogo nagreva [Strengthening of Steels and Alloys With the Use of
Electron Beam Heating], Nauka i technika Publ, Minsk, 1995. 280 pp. (In Russian).
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Index

Note: Page numbers followed by “f ” and “t” refer to figures and tables, respectively.

A AM-built components surface-finished by


A20X in aerospace casting industry. Extreme ISF Process, 361366
See AluminumCopper (AlCu) AMT, 1214
based casting alloy A205 applications, 1721
ABS. See Acrylonitrile butadiene styrene direct digital manufacturing, 1819
(ABS) rapid prototyping, 1920
Acoustic monitoring, 411412, 411f rapid tooling, 19
Acoustical sensors, 181 repair, 2021
Acrylonitrile butadiene styrene (ABS), 6, challenges, 169170
1617 manufacturing limitations, 22
Addaero Manufacturing, 328 postprocessing realities, 2223
Additive aerospace, 327 specification and standard development,
AM improving supply chain aerospace 23
industry, 330331 components in service, 401402
competitive implications of AM design requirements, 810
aerospace, 340 functional complexity, 9
factors driving AM in aerospace industry, property requirements, 10
328329 structural design, 9
geography of AM aerospace, 339 DMD technology, 3f
materials for AM, 331338 fabrication of various material
regulatory factors in AM aerospace, types, 36
338339 and improved aircraft design, 329
Europe, 339 improving supply chain aerospace
United States, 339 industry, 330331
3D printing technologies for tooling and manufacturing capabilities and benefits,
prototyping, 328 1012
Additive Factory concept, 327328 material economy, 11
Additive manufacturing (AM), 13, 67, 9, part consolidation, 1011
1217, 3334, 6768, 8889, 99, small production runs and turnaround
187, 213, 237, 240, 283, 301, 327, time, 12
341, 375376, 376f, 385, 387388, material properties and
401, 419, 427, 436f. See also defects, 404406
Aerospace additive manufacturing; potential future applications, 2324
Fusion additive manufacturing powder, 121
(Fusion AM) quality control for, 4043
additive nonmetal technologies, 1417 risk, 54
aerospace requirements and opportunities, software
712 design software, 83
450 Index

Additive manufacturing (AM) (Continued) SLA, 1516


as limiting factor on AM aerospace, SLS, 14
329 Additive synergetic technologies of layer by
process software, 8384 layer synthesis, 432434
specifications released and in-work, 2t Additive technologies (AT), 266, 427
surface determination of changes in structure
anatomy, 342345 using samples, 9395
finishing, 355361 economic effect of application of, 88
texture, 341 MMCs fabrication via, 266268
texture characterization, 345355 Advanced metallographic techniques,
system resolution, 79 113140
technology, 176 background, 114117
of TiAl chemical analysis, 136140
applications, 235 light optical microscopy, 122124
EBM, 248256, 248f, 252f, 253f metallographic sample preparation,
fundamentals, 235237 117121
laser metal deposition, 240245 microstructural analysis, 135136
processings, 237240, 237f shape and texture analysis, 124135
SEM, 245248 Aerospace
topological optimization for, 6871, 68f alloy, 311
Additive Manufacturing Control Plan enterprises, 428
(AMCP), 5254 industrial products, 427
Additive Manufacturing Requirements materials and requirements, 1
(AMRs), 5859 sector, 7
Additive Manufacturing Standardization Aerospace additive manufacturing. See also
Collaborative (AMSC), 39, 402403 Additive manufacturing (AM)
Additive Manufacturing Standardization additive synergetic technologies, 432434
Committee. See Additive EBH of coated surface, 438445
Manufacturing Standardization ion implantation and ion deposition of
Collaborative (AMSC) coatings, 434438
Additive materials system analysis of processing methods,
certification of, 4748 427432
qualification, 4447 Aerospace applications, 302. See also
quality control in, 4849 Selective laser melting (SLM)
Additive metal technologies (AMT), 10, gradient 3D cubes, 271f
1214. See also Additive nonmetal methods and materials, 269270
technologies MMCs
in aerospace industry, 13t fabrication via AT, 266268
DED, 1213 on nickel alloy based, 268269
PBF, 13 3D NiCrBSi nickel alloy cubes, 271f
for repair, 1718, 2021 Aging of powders, 176
geometry restoration, 21 AIA. See Automated image analysis (AIA)
structural integrity restoration, 21 Airbus, 12, 336, 340
Additive nonmetal technologies, 1417. Airbus 320 characteristics, 424t
See also Additive metal technologies Airbus 380 characteristics, 424t
(AMT) Airbus Defence and Space, 331
in aerospace industry, 15t Airbus Group, 329
FDM, 1617 Aircraft, 14
PolyJet, 16 interiors, 337
Index 451

Airline passenger seats, 420f Arcam AB, 327


Airplane seat, 419 Arcam Q10 Plus EBM system, 13
Altair, 329 ArianeGroup, 168
Aluminum, 439 Aristo Cast, 424
Aluminum alloys, 11. See also Selective Artificial neural networks (ANNs), 391
laser melting (SLM) ASME. See American Society of Mechanical
alloy and process design, 310320, 310f Engineers (ASME)
adaptation of existing high strength ASTM. See American Society of Testing
alloys, 316319 and Materials (ASTM)
design of new alloys, 311316 AT. See Additive technologies (AT)
development of composite materials, Atomization process, 250
319320 Autodesk, 329, 424
processingmicrostructureproperty Netfabb software, 419
considerations, 302309 Autodesk Project Escher technology,
AluminumCopper (AlCu) based casting 419422
alloy A205, 318319 Automated image analysis (AIA), 108,
Aluminumsilicon (AlSi) based alloy 122124
system, 306307 testing programs, 113114
AM. See Additive manufacturing (AM) Automated repair process, 23
AMCP. See Additive Manufacturing Control AWS. See American Welding Society
Plan (AMCP) (AWS)
American National Standards Institute
(ANSI), 39 B
American Society of Mechanical Engineers Backscattered electron images, 294f
(ASME), 39 Backscattered electron imaging (BEI), 117,
American Society of Testing and Materials 137, 138f
(ASTM), 3637, 402403 Balling, 405406
B417 Standard, 104105 BCC structure. See Body-centered cubic
EV31A. See Elektron 21 alloys structure (BCC structure)
International, 39 BD technologies. See Bed
WE43C. See Elektron 43 alloys deposition technologies (BD
American Welding Society (AWS), 39 technologies)
AmpliFORGE, 77 Bed deposition technologies (BD
AMRs. See Additive Manufacturing technologies), 432
Requirements (AMRs) BEI. See Backscattered electron imaging
AMSC. See Additive Manufacturing (BEI)
Standardization Collaborative Belgium-based additive factory, 335
(AMSC) Benard convection cells, 439
AMT. See Additive metal technologies Binder jetting, 36, 1314
(AMT) Body-centered cubic structure (BCC
Annealing heat treatment, 286 structure), 163
ANNs. See Artificial neural networks Boeing, 7
(ANNs) 787 Dreamliner, 18
ANSI. See American National Standards Boron, 170171
Institute (ANSI) Brittle temperature range
Apparent density, 175176 (BTR), 170171
and flow, 101105 BTR. See Brittle temperature range (BTR)
of metal powder, 104 Buoyancy force, 443444
APWorks, 331 Buy-to-fly ratios, 11
452 Index

C state graph of technological medium cell


CAD. See Computer-aided design (CAD) automaton, 441f
Camera-based process monitoring, 180181 Coatings, ion implantation and ion
Canfield analysis, 190 deposition of, 434438, 437f
Carbides of chromium (CrxCy), 265 Code of Federal Regulations (CFR), 4748
Carbon, 170171 Cold shuts, 97
emissions, 419 Cold spray. See Supersonic particle
nanotubes, 320 deposition (SPD)
Carney test for flow, 101103 Cold-cracking. See Strain-age cracking
Casting process, 237238, 419422 (SAC)
CAVF. See Chemically accelerated vibratory COMAC, 334
finishing (CAVF) Combustion chamber, 165166
Cell culture medium machine, 439, 440f Commercial aviation gas turbine engines,
Cellular automata, 383384 3334
Cellular structure, 438 Commercially pure titanium (CP titanium),
Center for Innovative Materials and 139
Processing-3D (CIMP-3D), 39 Compact preform, 93
Centrifugal casting process, 237238 Compactness, 130
Certification, 4344. See also Qualification Composites, 337338
and certification (Q&C) materials development for
of additive materials, 4748 SLM, 319320
CFR. See Code of Federal Regulations Computed tomography (CT), 3637, 108,
(CFR) 136
Chemical Computer-aided design (CAD), 83, 187188
analysis, 136140 Concept Laser, 327
composition, 174175, 265266 Consumable material, 217218
etchants, 135t Contact acoustic emissions sensors,
etching. See Chemical milling process 411412
pickling. See Chemical milling process Contact profilometry, AM surface
polishing. See Chemical milling process characterization by, 349352
Chemical milling process, 360361 Continuous DLP (CLIP), 328
Chemically accelerated vibratory finishing Continuous inkjet (CIJ), 16
(CAVF), 361 Contour scan effect on surface texture,
Chromium atoms, 435 290293
Chromium carbide (Cr3C2), 268 Contour zone, 250
CIJ. See Continuous inkjet (CIJ) Conventional crystallographic fatigue crack
CIMP-3D. See Center for Innovative initiation mechanisms, 38
Materials and Processing-3D (CIMP- Conventional manufacturing, 3336, 4445
3D) Conventional methods, 67
Circularity, 130 Conventional processing methods, 283
CLIP. See Continuous DLP (CLIP) Cooling technologies, 165166
“Co-Design to Target” industry solution, CP titanium. See Commercially pure
329, 331 titanium (CP titanium)
Coated surface, EBH of, 438445 Crack modeling, 189190
cellular structures, 443444 Crack susceptibility of high strength nickel
configurations of cellular machines, 442f superalloys, 169
distribution of microhardness, 444f Cracking mechanisms, 169
model of formed multicomponent coating Crystallographic texture, 304
on peaks, 443f CT. See Computed tomography (CT)
Index 453

D Direct metal laser sintering (DMLS), 12


D&DT community. See Durability and Direct metal part fabrication, 1819
damage tolerance community Direct rapid tooling, 1718
(D&DT community) Directed energy deposition (DED), 13, 3f,
D10 particles, 175 10, 1213, 52, 99, 214, 266267,
D50 particles, 175 333334, 409410
D90 particles, 175 Dispersion-hardened alloys (DHA),
Dassault Systèmes’ 3DEXPERIENCE 265266
platform, 329 Dissipative structure formation, 439
DD technique. See Direct deposition Distortion in fusion AM, 189190
technique (DD technique) Distribution analysis of processing methods,
DDC. See Ductility dip cracking (DDC) 428431
DDM. See Direct digital manufacturing DMDs. See Direct metal depositions
(DDM) (DMDs)
DDT&E. See Design, development, test and DMLS. See Direct metal laser sintering
evaluation (DDT&E) (DMLS)
DED. See Directed energy deposition (DED) “Do no harm” Class C designation, 56
Defect data correlation automated, future DoD. See Department of Defense (DoD)
closed-loop control possibilities, DOD. See Drop on demand (DOD)
182184 Down-skin surfaces, 284285
Dendritic cell boundaries, 90 Dreamcatcher generative design tools, 329
Dendritic structure of nickel matrix, 275 Drop on demand (DOD), 16
Density optimization, 145149 Ductility dip cracking (DDC), 173
Department of Defense (DoD), 38, 402403 powder material properties, 174177
AM Roadmap, 406 Durability and damage tolerance community
Deposition process, 217f, 230 (D&DT community), 5960
Design, development, test and evaluation Dynamic image analysis (DIA), 110111
(DDT&E), 3334
Design for additive manufacturing (DFAM), E
67 EASA. See European Aviation Safety
Detonation coating process, 438 Agency (EASA)
DFAM. See Design for additive Easton and St. John model, 390
manufacturing (DFAM) EBAM. See Electron beam additive
DHA. See Dispersion-hardened alloys manufacturing (EBAM)
(DHA) EBF3. See Electron beam free-form
DIA. See Dynamic image analysis (DIA) fabrication (EBF3)
Diffusion processes, 442 EBH. See Electron-beam heating (EBH)
Direct deposition technique (DD technique), EBM. See Electron beam melting (EBM)
432 EBSD maps, 388, 389f
Direct digital manufacturing (DDM), 14, EBW. See Electron beam welding (EBW)
1718 Eddy current (ET), 3637
direct metal part fabrication, 1819 EDM. See Electrical discharge machining
fixtures and accessories, 19 (EDM)
Direct metal depositions (DMDs), 88, 95, EDS. See Energy dispersive spectroscopy
266267 (EDS)
processes, 22 EDX. See Energy dispersive analysis (EDX)
systems, 18 EIGA. See Electrode induction melting GA
testing of mechanical properties of (EIGA)
samples of parts, 9597 ELB-Schliff’s millGrind, 19
454 Index

Electrical discharge machining (EDM), 81 ET. See Eddy current (ET)


Electrode induction melting GA (EIGA), 99 Etihad Airways Engineering, 336
Electromagnetic surfacing, 434 European Aviation Safety Agency (EASA),
Electromagnetic surfacing process, 433 34, 336
Electron beam, 215217 Extreme ISF Process
Electron beam additive manufacturing AM-built components surface-finished by,
(EBAM), 4950, 7576 361362
Ti6Al4V macrostructure, 76, 77f analysis of surface texture parameters,
Electron beam free-form fabrication (EBF3), 365366
12 examples of surface treated
Electron beam melting (EBM), 12, 99, 341. by, 362364
See also Selective laser melting improvement of mechanical properties,
(SLM) 364365
technology, 240, 241f
Ti48Al2Cr2Nb honeycomb, 257f F
of TiAl, 248256, 248f, 252f, 253f FAA. See Federal Aviation Administration
creep properties, 255t (FAA)
element mappings by microprobe FAA Q&C approach. See Federal aviation
measurements, 249f administration Q&C approach
fatigue crack initiating from ceramic (FAA Q&C approach)
particle, 256f Fabrication processes, 60, 82, 411
Haigh diagram, 256 Face-centered cubic structure (FCC
physical effects during selective structure), 163
melting, 250f Fasteners, 10
room temperature tensile properties of Fatigue
EBM TiAl-4822, 254t crack initiation, 286
tensile properties vs. temperature, 255f performance, 307308
Electron beam power, 215216 of selective laser melted Ti6AL4V,
Electron beam welding (EBW), 12 286
Electron-beam heating (EBH), 438445 properties, 293296, 295f, 296f, 297f
Electropolishing, 360361 testing, 288, 288f
Elektron 21 alloys, 424425 FCC structure. See Face-centered cubic
Elektron 43 alloys, 424425 structure (FCC structure)
Energy FDM. See Fused deposition modeling
density function, 144 (FDM)
energy-dissipation simulation, 436437 FE model. See Finite element model
fluxes, 427 (FE model)
system analysis of processing methods, Feature cross sections, 127
427432, 429t, 430f Federal Aviation Administration (FAA), 34,
source for AM, 301 401403, 419
Energy dispersive analysis (EDX), 270 Advisory Circular 25.5711D, 60
Energy dispersive spectroscopy (EDS), 110 Advisory Circular 33.701, 6061
Entrained gas, 143 Federal aviation administration Q&C
EOS approach (FAA Q&C approach),
additive manufacturing technology, 169 6061. See also General electric
M 290 DMLS system, 18 Q&C approach
EOSTATE Feedstock attributes, 36
Exposure OT, 180181 FG structures. See Functional-gradient
MeltPool, 180, 181f, 182 structures (FG structures)
Index 455

FGMs. See Functionally graded materials large columnar microstructure in, 189f
(FGMs) Mg-B4C cermet microstructures, 205f
Filtering function, 346347 surface at high build rates, 200f
Finite element model (FE model), 69 tensile values of samples extracted from
Fitting function, 345346 joint regions, 199t
Flammability, 424425 TiB2/Ti cermet armor after hit by APM2
Flowability of powder, 103 muzzle velocity, 206f
Fortus 450 system, 335 TiB2/Ti composite integrally built on
Fortus 900mc system, 335 Ti6Al4V base, 206f
Four-dimension (4D) printing, 23 Fusion AM. See Fusion additive
Fractography, 7778, 151152, 156 manufacturing (Fusion AM)
Fracture-critical hardware, special
considerations for, 3738 G
Free-form design, 6869, 83 G/R ratio. See Thermal gradient/
Friction stir additive manufacturing (FSAM), solidification rate ratio (G/R ratio)
191192, 192f GA. See Gas atomization (GA)
laser preheating, 197f Gamma phase, 163
mechanical properties, 196t Gap analysis, 3943
of P92 steel, 194f Gas
Friction stir processing (FSP), 191192 atomized powder, 116
aluminum deck lid FSP joined to gas-discharge electron beam guns, 216
galvanized steel, 199f gas-phase deposition, 433434
damage repair, 200f materials in gas turbines, 164169
FSP/FSAM cladding, 196f pores, 303
key benefits, 193t GAs. See Genetic algorithms (GAs)
PTA in hybrid couple with, 197f Gas atomization (GA), 99, 256
Friction stir welding (FSW), 191192 Gaussian filter, 346347
FSAM. See Friction stir additive GE. See General Electric (GE)
manufacturing (FSAM) GE Avio Aero, 11, 327328
FSP. See Friction stir processing (FSP) GE90 jet engines, 34
FSW. See Friction stir welding (FSW) Geared-Turbofan engine (GTF engine), 235
Functional complexity, 9 General Electric (GE), 34, 327, 340
Functional-gradient structures (FG Aviation, 1011
structures), 268269 General electric Q&C approach, 4349
Functionally graded materials (FGMs), 10, certification of additive materials, 4748
267 qualification of additive materials, 4447
Fused deposition modeling (FDM), 14, quality control in additive materials,
1617, 330, 336 4849
Fusion, 384385 Generalities superalloys, 163, 164f
Fusion additive manufacturing (Fusion AM), defect data correlation automated, future
187188. See also Additive closed-loop control possibilities,
manufacturing (AM) 182184
cylindrical bar preform in custom titanium material challenges processing
alloy, 205f perspectives, 169173
defects, 189f challenges with additive manufacturing,
experimental examples, 198210 169170
foams produced from fusion PTA AM DDC, 173
processing, 207f liquation cracking, 171172
friction stir machine in operation, 192f SAC, 172173
456 Index

Generalities superalloys (Continued) High-intensity processes, 434


solidification cracking, 170171 High-strength thermoplastics, 1617
materials in gas turbines, 164169 HIP. See Hot isostatic pressing (HIP)
process monitoring, 177179 HIPed. See Hot isostatically pressed (HIPed)
challenges with tradition postprocess HIPing. See Hot isostatic pressing (HIPing)
inspection techniques, 179 Hollow conical electron beam, 216, 217f
novel QA approaches, 179 on consumable wire, 218f
quality assurance in AM, 177178 Hot corrosion, 163
quality assurance tie-in, 181182 Hot isostatic pressing (HIP), 36, 7778, 81,
sensor types for in situ process 266, 304
monitoring, 179181 Hot isostatic pressing (HIPing), 9596, 286,
Genesis, 9 360
Genetic algorithms (GAs), 391 Hot isostatically pressed (HIPed), 239, 288
Geometry restoration, 21 Hybrid dissimilar titanium alloy
Gesellschaft für Elektrometallurgie mbH combinations, 198199
(GfE), 238239 Hybrid manufacturing systems, 19
Gettering, 385386 Hydroflouric acid, 136
GfE. See Gesellschaft für Elektrometallurgie Hydrogen, 143
mbH (GfE) pores, 303
Glass-filled nylon, 14 Hypereutectic composition, 311312
Government agency approaches, 5161
GR plots, 383384 I
Grade 5 alloy parts, 93, 97 ICME. See Integrated computational
Grinding, 120121 materials engineering (ICME)
GTF engine. See Geared-Turbofan engine ICP-OES, 177
(GTF engine) IGF. See Inert gas fusion (IGF)
Image acquisition and processing, 129
H Image analysis method, 145
Hall flowmeter and cup, 103f, 104105 In situ characterization, 406
Hall-Petch effect, 76 In-process, 177
“Hard-to-weld” alloys, 170 In-situ process, 7980
Hastelloy X, 168 Inclination angle and processing parameters,
Hatch distance, 144, 147148 289290
Hatch zone, 250 Inclusion analysis, 108110
Hausner ratio, 105106 Inconel 718 alloy, 73f
HCF. See High-cycle fatigue (HCF) INCONEL 718, 168
Healing effect, 182184 Indirect rapid tooling, 1719
Heat Industrial 3D printing, 213
accumulation effect, 283284 Industry Q&C approaches
diffusion phenomena, 251 general electric Q&C approach, 4349
heat-resistant nickel alloys, 87 government agency approaches, 5161
heat/mass transfer, 444 Lockheed martin Q&C approach, 4951
transfer, 284285 Inert gas fusion (IGF), 177
treatment, 286 Inspection processes, 37
Heat affected zone (HAZ). See Liquation Integrated computational materials
cracking engineering (ICME), 37, 207210,
High strength alloys, 310 375, 377f, 378f
High-cycle fatigue (HCF), 286 fusion process model, 378t
High-energy-density processing, 431 limitations, 393395
Index 457

predicting microstructure, 387391 selection of optimized heat treatment


predicting properties and performance, parameters, 153
391393 selection of optimized laser parameters,
process modeling, 379384 153154
solute profiles in TixW system, 384f tensile properties, 155
solidification partitioning, 386387 Laser melting parameters (LMPs), 153154
solute loss or pickup, 385386 Laser metal deposition (LMD), 12, 240, 244t
Integrated structural integrity rationale, of TiAl, 240245, 241f, 243f
5657 Laser powder bed fusion (LPBF), 403404
Interfacial area ratio, 366 Laser sintering (LS), 341
“Intermediate” parameter set, 286287 Laser-Powder Bed Fusion (L-PBF), 3637,
Intermetallic compounds, 442 45, 52
International Organization for AM process, 5254
Standardization (ISO), 39, 403 Lattice Boltzmann method, 249
Interstitialcy defects, 435 Layer-by-layer
Ion deposition of coatings, 434438 building principles, 304
Ion implantation, 433438 synthesis, 432434, 433t
Ion-vacuum processing, 438 LC. See Laser cladding (LC)
ISO. See International Organization for LENS. See Laser engineering net-shaping
Standardization (ISO) (LENS)
LENS Blisk Repair Solution system, 21
J Life-Limited Parts (LLPs), 60
Japanese Space Exploration Agency Light optical microscopy (LOM), 108,
(JAXA), 51, 56 122124
Jet engine components and materials, 166f Light-emitting device, 1516
Joint effect, 433434 Liquation cracking, 171172, 301302
Liquid
K bath dimensions, 89, 90f
Karl Fischer Titration, 107 epoxies, 118119
Kinetic Monte Carlo, 383384 phase, 442
photopolymer resin, 1516
L LLPs. See Life-Limited Parts (LLPs)
L-PBF. See Laser-Powder Bed Fusion (L- LM. See Laser melting (LM)
PBF) LMCO. See Lockheed Martin Company
Lack of fusion (LOF), 405406 (LMCO)
Lamellar structure, 443 LMD. See Laser metal deposition (LMD)
Langmuir equation, 385386 LMPs. See Laser melting parameters (LMPs)
Laser Lockheed Martin Company (LMCO), 4951
diffraction, 175 Lockheed Martin Q&C approach, 4951
laser-material interaction, 303 LOD. See Loss on drying (LOD)
polishing/remelting technology, 285 LOF. See Lack of fusion (LOF)
power, 144, 147148 LOM. See Light optical microscopy (LOM)
systems, 385 Long-wave
ultrasonics, 409410 high pass cut-off filter, 346347
Laser cladding (LC), 266267 nesting index filters, 352353
Laser engineering net-shaping (LENS), 12 Loss on drying (LOD), 107, 177
Laser melting (LM), 267, 341 device for measuring moisture content of
refinement, 153156 metal powders, 108f
fractography, 156 Low pressure turbine (LPT), 235
458 Index

LPBF. See Laser powder bed fusion (LPBF) current Q&C state-of-the-art and gap
LPT. See Low pressure turbine (LPT) analysis, 3943
LS. See Laser sintering (LS) FAA-approved T25 compressor inlet
temperature sensor and fuel nozzle,
M 35f
Machine learning, 182 guidance in process qualification or
Magnesium, 423 feedstock specification
alloys, 424425 FAA Q&C approach, 6061
Marangoni Effect, 381 warnings, 5960
Marshall Space Flight Center (MSFC), 43 industry Q&C approaches, 4351
MSFC-STD-3716, 52 special considerations for fracture-critical
additive manufactured part hardware, 3738
classification system, 55f Metal injection molding (MIM), 99
Technical Standard and Specification, Metal matrix composites (MMCs), 265,
5254 270f, 318319
Mass fabrication via AT, 266268
distribution in Seats, 419, 421f on nickel alloy, 268269
finishing techniques, 356357 Metal powder bed
Material AM systems, 329
choice, 166 fusion technology, 331, 333
ductility, 173 Metal Powder Industries Federation, 39
economy, 11 Metal(s), 11, 331333
engineering, 1 sintering processes, 22
extrusion. See Fused deposition modeling 3D printers, 218219
(FDM) Metallic Materials Properties Development
jetting. See PolyJet and Standardization (MMPDS), 43,
properties and defects in AM, 404406 403404
Materialisation, 9 Metallographic sample preparation,
MATLAB, 145 117121
Mechanical anisotropy, 309 grinding and polishing, 120121
Mechanical polishing methods, 285 mounting, 117119
Meshify, 9 sampling, 117
MET. See Metrology (MET) Metallographic studies, 93
Metal additive manufacturing design. Metrology (MET), 3637
See also Additive manufacturing Microhardness distribution, 444f, 445
(AM) Microstructure
cost considerations, 8182 analysis, 135136, 436
design software, 83 coarsening, 150
methods and approaches, 6874 dependence of powder particles, 92
part consolidation, 7172 prediction, 387391
part integration and repair, 7273 MIM. See Metal injection molding (MIM)
topological optimization, 6871, 68f MMCs. See Metal matrix composites
process aspects of design, 7481 (MMCs)
part performance, 7478 MMPDS. See Metallic Materials Properties
process software, 8384 Development and Standardization
product and process design tools, 8284 (MMPDS)
Metal additive manufacturing processes, 17t, Moisture analysis, 106108
33, 187188. See also Additive Mold pattern fabrication, 16
manufacturing (AM) Molybdenum-depleted zones, 439
Index 459

Mounting, 117119 Netfabb software, 9, 419


MPIF Standard 03, 101103 Next generation generative software, 329
MPIF Standard 04, 104105 Nickel alloy
MPIF Standard 05, 100101 MMCs on, 268269
MPIF Standard 28, 101105 powders, 89
MPIF Standard 32, 100 surface structure, 91f
MPIF Standard 46, 105 Nickel sublayer, 441
MPS, 5254 Nickel superalloys, 163, 166167
MSFC. See Marshall Space Flight Center Nickel-based super alloys, 11
(MSFC) disc, 235
Multifunctional structures, 23 Niobium, 170171
Multilayer deposition process, 240241 alloys, 224
Multimaterial DED processes, 23 NIST. See National Institute of Standards
Multiply localized energy adsorption zones, and Technology (NIST)
433 Nitinol, 174175
Nitrogen-based SPD, 14
N Non-hardening phases, 314315
NADCAP. See National Aerospace and Nonconsumable FSAM tool, 191192, 191f
Defense Contractors Accreditation Noncontact profilometer, 352355
Program (NADCAP) Nondestructive evaluation (NDE), 3637,
Nanoparticles, 266 413
Nanoscale inclusions, 266 AM components in service, 401402
NASA. See National Aeronautics and Space clustering of acoustic metrics, 412f
Administration (NASA) emerging methods, 409413
NASA Procedural Requirement (NPR), material properties and defects in AM,
5758 404406
National Aeronautics and Space optical and thermal monitoring, 406409
Administration (NASA), 3334, 402 post-production inspection, 409
Q&C approach, 3637, 5160 practical considerations, 413414
qualification requirements regulatory actions and standardization,
additional guidance, 59 402404
additive manufactured part categories, Nondestructive inspection, 7980
5456 Nonequilibrium technological
general requirements, 5657 process, 428
industry standards, 59 Nonmetal additive manufacturing
influence of mission classification, technologies, 17t
5758 Nonoptical sensor technologies, 181
integrated structural integrity rationale, Nonspherical particles, 176
5657 Nonsteady-state temperature field, 445
process specifications, 59 Nonweldable alloys, 170
procurement specifications, 59 Novel QA approaches, 179
tailoring approach, 5758 NPR. See NASA Procedural Requirement
National Aerospace and Defense Contractors (NPR)
Accreditation Program (NADCAP), Numerical algorithms, 70
4043 Nylon 12, 6, 14
National Institute of Standards and
Technology (NIST), 3637 O
NDE. See Nondestructive evaluation (NDE) OCT. See Optical coherence tomography
Near-net-shape PM method, 239 (OCT)
460 Index

OEM. See Original equipment manufacturer Personal protection equipment (PPE), 136
(OEM) PF. See Powder forging (PF)
OffAxis sensors, 179 Phase field modeling, 383384
OM. See Optical metallography (OM) Phosphorus, 170171
OmniSurf from Digital Metrology, 351352 Photodiode-based process monitoring, 180
OnAxis sensors, 179 Photodiode-high speed camera hybrid
Open atmosphere systems, 79 system, 406407
Operating gas, 215216 Photopolymer resins, 1516
Optical coherence tomography (OCT), Photopolymerization based
406407, 413 stereolithography, 328
Optical in situ process monitoring systems Plasma beam, 200201
for AM, 179181 Plasma rotating electrode process (PREP),
camera-based process monitoring, 99, 111112
180181 Plasma transferred arc (PTA), 200201
photodiode-based process monitoring, 180 AM system, 202f
Optical metallography (OM), 272, 272f, 273f large vertical and robotic PTA system,
Optical monitoring, 406409 203f
Optimum linear energy density, 283284 plasma beam in AM build, 201f
OptiStruct, 9 PM. See Powder metallurgy (PM)
Optomec LENS, 385 Point-based measurement systems, 406
Original equipment manufacturer (OEM), 37 Polished cross saections, 135, 135f
Overhanging surfaces. See Down-skin Polishing, 120121
surfaces Polycarbonate, 1617
Oxidation resistance, 163 PolyJet, 14, 16, 20, 23, 328
Polylactic acid, 1617
P Polymerization, 36
Packing characteristics, 101 Polymers, 334336
Part categories, 51 AM, 7
Part consolidation in AM, 7172 bed fusion, 336337
Part integration and repair, 7273 Polyphenylsulfone, 1617
Part performance in AM, 7478 Porosity, 111112, 383
defects, 77 Post processing, 8081
mechanical properties, 7778 Post selective laser melting heat treatment,
microstructure, 7477 150152
part evaluation, 7980 fractography, 151152
part quality, 7879 optimized HTPs applied on tensile
post processing, 8081 samples, 150t
Part production controls, 54 tensile properties, 150151
Part production plan (PPP), 54 Post-production inspection, 409
Particle size and distribution, 99101 Postprocessing, 19, 36, 177178
Particle size distribution (PSD), 175 NDE, 80
PBF. See Powder bed fusion (PBF) parameter refinement, 153156
PBM. See Powder bed method (PBM) realities, 2223
PCRT. See Process compensated resonance techniques, 38, 150
testing (PCRT) Postselective laser melting
pdfs. See Probability distribution functions heat treatment of fatigue samples, 288
(pdfs) surface treatment, 285
Penetrant testing (PT), 3637 Powder
“Performance” parameter set, 286287 characteristics, 303304
Index 461

flow, 101 macrostructure of thick wall, 228f


flowability, 175 results of mechanical testing of
layer thickness, 144 Ti6Al4V, 229t
packing, 104 scheme of system for running of invented
powder-based laser AM, 301 process, 214f
structure evaluation of powder particles of spreading of liquid metal, 219f
different sizes, 8992 Ti6Al4V specimen structure, 226f,
Powder bed fusion (PBF), 13, 10, 1213, 227f
266267, 301 wire as substrate for deposition, 222f
process models, 381383 PSD. See Particle size distribution (PSD)
Powder bed method (PBM), 341 PSEs. See Principal structural elements
Powder forging (PF), 113 (PSEs)
Powder metallurgy (PM), 38, 87, 113, 235, PT. See Penetrant testing (PT)
239, 240f PTA. See Plasma transferred arc (PTA)
PM-PF water atomized powders, 115
PPE. See Personal protection equipment Q
(PPE) Q&C. See Qualification and certification
PPP. See Part production plan (PPP) (Q&C)
Precipitation hardening alloys, 316 QMP. See Qualification metallurgical
Premium Aerotech, 327328 process (QMP)
PREP. See Plasma rotating electrode process QMS. See Quality management system
(PREP) (QMS)
Preprocess, 177 Qualification
Primary profile, 346347 of additive materials, 4447
Primary roughness, 344 processes, 4344
Principal structural elements (PSEs), 60 Qualification and certification (Q&C),
Print services providers, 330 3334, 39, 4546
Probability distribution functions (pdfs), 393 state-of-the-art and gap analysis, 3943
Process directions, and quality control for
control methodologies, 3436 additive manufacturing, 4043
map models, 383384 standardization gaps, 3940, 41t
monitoring, 182 Qualification metallurgical process (QMP),
specifications, 59 5254
Process compensated resonance testing Quality assurance
(PCRT), 3637 in AM, 177178
Processingmicrostructureproperty tie-in, 181182
considerations, 302309, 306f Quality control
Procurement specifications, 59 for additive manufacturing, 4043
Profile electron beam 3D metal printing, in additive materials, 4849
215f measurements, 99112
cup made from CP Ti Grade 4 wire, 225f apparent density and flow, 101105
deposited bead depending on deposition inclusion analysis, 108110
parameters, 224f moisture analysis, 106108
deposited layers formed from wire, 225f particle size and distribution, 99101
deposition process, 217f porosity, 111112
formation of walls of different shape factor, 110111
thicknesses, 227f tap density, 105106, 106f
gap Z between wire exit hole and Quality management system (QMS), 40, 54
substrate, 223f Quantitative characterization techniques, 402
462 Index

R density optimization, 145149


R&D. See Research and development optimized laser processing parameters,
(R&D) 149t
Ra value, 289290, 289f process control, 143144
of top surface of SLMed cubic samples, relative vs. energy density, 148f
283284 3D plots and 2D processing windows,
Radiographic testing, 3637 147f
Radius function evaluation, 131, 132f Selective laser melted metallic components,
Rapid prototyping, 1720 283285
Rapid tooling, 1719 Selective laser melted Ti6Al4V alloy
Rare earth (RE), 302 experimental procedure
Reconfigurable tooling, 19 fatigue testing, 288
Regulatory actions and standardization, material, 286
402404 postselective laser melting heat
RepAIR project, 23 treatment of fatigue samples, 288
Research and development (R&D), 39 specimens, 286287, 287f, 287t, 288t
Resonance type testing, 405406 surface roughness measurements, 288
RMS. See Root-mean-squared (RMS) fatigue performance, 286
Root-mean-squared (RMS), 411412 fatigue properties, 293296
Rough surface, 343 postselective laser melting surface
Roughness. See also Surface roughness treatment, 285
component, 346347 surface roughness, 289293
sampling length, 347349 of SLM metallic components, 283285
Selective laser melting (SLM), 12, 88, 95,
S 99, 143, 240, 266267, 283, 284f,
SAC. See Strain-age cracking (SAC) 301. See also Aerospace applications;
Sacrificial metal or material, 356357 Electron beam melting (EBM)
SAE. See Society for Automotive Engineers adaptation of existing high strength alloys,
(SAE) 316319, 316f, 317f
Sampling, 117, 174 alloys in, 302309
SAP, 331 composite materials development for,
SAW. See Surface acoustic wave (SAW) 319320
Scan speed, 144, 147148 design of new alloys, 311316, 314f
Scandium (Sc), 311 SLM-processing parameters, 145
Scanning electron microscope (SEM), 110, SLMed aluminum samples, 143
270, 275f, 290, 291f, 292f, 293f testing of mechanical properties of
SDOs. See Standards development samples of parts, 9597
organizations (SDOs) of TiAl, 245248
Secondary dendrite arm spacing (SDAS), produced TNM-B1 3D-dodecahedron
312 structures, 246f
Secondary electron images (SEI), 116 SEM pictures of SLM producing TNM
SEI. See Secondary electron images (SEI) sample, 246f
Selective laser melted Al-7Si-0.6Mg alloy typical microstructures SEM of
post selective laser melting heat treatment, samples, 247f
150152 Selective laser sintering (SLS), 36, 14, 19
refinement of laser melting and Self-organization, 432, 434435
postprocessing parameters, 153156 SEM. See Scanning electron microscope
selective laser melted Al alloy A357, (SEM)
143149 Semiatin’s approach, 385386
Index 463

Sensor SR. See Stress-relief (SR)


acoustical, 181 SRAS. See Spatially resolved acoustic
contact acoustic emissions, 411412 spectroscopy (SRAS)
OffAxis, 179 ST-130TM material, 338
types for in situ process monitoring, Stainless steel, 99
179181 Staircase effect, 284
optical in situ process monitoring Staircase feature, 343
systems for AM, 179181 Standardization
Service providers, 330 gaps, 3940, 41t
SHAIK, 166167, 167f regulatory actions and, 402404
Shape analysis, 124135 standards structure approved by ASTM
Shape factor, 110111 F42 and ISO TC261, 403f
Short or low-pass cut-off filter, 346347 Standards development organizations
Short-wave nesting indexes filters, 352353 (SDOs), 39
SHT. See Solution heat treatment (SHT) Statistical process control (SPC), 5254
Siemens, 330331 Stereolithography (SLA), 1416
Sieve analysis, 100101, 175 Strain hardening effects, 307
for AM techniques, 102t Strain-age cracking (SAC), 172173
Signal processing methods, 184 Stratasys
Silicon (SiC), 265 FDM technology, 336
Simpleware, 9 industrial thermal extrusion technology,
Single “deposition engine tool”, 333334 338
Single-focused energy adsorption zones, 432 for sacrificial composite tooling, 338
Sintavia, 328 Fortus 900 system, 336
SLA. See Stereolithography (SLA) ULTEM 1010 resin, 338
SLM. See Selective laser melting (SLM) Stress concentration, 431
SLS. See Selective laser sintering (SLS) Stress-relief (SR), 150
Slurry ball milling method, 320 Stress-rupture strength of different alloys,
Society for Automotive Engineers (SAE), 39 164, 165f
Solid alloys, 265266 Structural integrity restoration, 21
Solid-solution strengthening, 164 Structure formation in AM
Solid-state cracking. See Strain-age cracking determination of changes in structure,
(SAC) 9395
Solid/liquid interface, 444 microstructure dependence of powder
Solidification, 311 particles, 92
cracking, 170171 structure evaluation of powder particles of
partitioning, 386387 different sizes, 8992
solute partitioning, 387f testing of mechanical properties of
Solute loss or pickup, 385386 samples of parts, 9597
Solution heat treatment (SHT), 143 Substantial effect, 434435
Spaceflight rocket engines, 3334 Substrate temperature, 144
Spatially resolved acoustic spectroscopy Sulfur, 170171
(SRAS), 395, 409410, 410f, 413 Superalloys, 7273, 99
SPC. See Statistical process control (SPC) Supersonic particle deposition (SPD), 12, 14,
SPD. See Supersonic particle deposition 21
(SPD) Supersonic particle deposition (SPD), 14
Specialized service bureaus, 328 Surface accuracy formation, 431
“Speed” parameter set, 286287 Surface acoustic wave (SAW), 395
Spherical particles, 176 Surface defects, 358
464 Index

Surface finishing of AM components, TiC. See Titanium carbides (TiC)


355361 Titanium, 89, 99, 164, 224, 385, 439
basics, 356358 surface structure, 91f
Surface oxidation induced phenomenon, 255 Titanium alloy (Ti6Al4V), 11, 13, 443,
Surface roughness, 303, 344 445
effect of contour scan on surface texture, effects in, 87
290293 Titanium aluminide (TiAl), 11, 235
measurements, 288 applications, 235
parameter, 357 EBM, 248256
Ra vs. inclination angle and processing fundamentals, 235237
parameters, 289290 laser metal deposition, 240245
of selective laser melted metallic processings, 237240, 237f
components, 283285 AM, 240
Surface self-organization phenomena, 427 casting, 237238
Surface texture characterization of AM PM, 239
components, 349355 wrought processing, 238239
best practices for, 345355 SEM, 245248
contact profilometry, 349352 Titanium carbides (TiC), 265, 268
noncontact profilometer, 352355 Titanium diboride (TiB2), 268
surface texture review, 345349 TM. See Transition metal (TM)
Surface-distributed energy adsorption zone, TNM. See TiAl alloy (TNM)
433 Tool steel powders, 99
Surface-sensitive NDE techniques, 38 Topology optimization, 340
Synergetic concept, 432 for AM, 6871, 68f
FE topological optimization of bracket,
T 70f
Tailoring approach, 5758 methods, 23
Tap density, 105106, 106f, 175176 tools, 9
Texture analysis, 124135 Tradition postprocess inspection techniques,
Thermal gradient/solidification rate ratio (G/ challenges with, 179
R ratio), 305 Traditional subtractive manufacturing, 19
Thermal monitoring, 406409 Transformation behavior, 236
Thermal warping effect, 284285 Transition metal (TM), 302
Thermocapillary force, 443444 Transmitted light technique, 117
Thermographic imaging process, 407408 True profile. See Primary profile
Thermogravimetric analysis, 107 Tungsten (WC), 265
Three-dimension (3D) Turbine blades, 165
CAD digital model, 8081 Two-dimension (2D)
LC, 266267 non-contact profile, 352
model, 213 surfaces, 113114
objects, 187188
optical surface metrology, 352 U
particle, 116 ULTEM, 1617
printers, 8788 Ultimate tensile strength (UTS), 244,
printing, 8081 360361
technologies for tooling and Ultrafine structures, 267268
prototyping, 328 Ultrasonic testing (UT), 3637
TiAl alloy (TNM), 235 Unmanned aerial vehicle (UAV), 1617
TiB2. See Titanium diboride (TiB2) Up-skin surfaces, 284
Index 465

US Food and Drug Administration Federal Weld-centerline cracking. See Solidification


Food, Drug, and Cosmetic Act, cracking
4748 Weldability issues, 169170
Welding, 200201
V Wire arc AM (WAAM), 12
Vacuum-ion modification, 436437 Work hardening alloys, 316
Vaporization, 385386 Wrought processing of TiAl, 238239, 238f
Vat photopolymerization.
See Stereolithography (SLA) X
Volumetric techniques, 409 X-ray computer tomography scan (XRCT-
Voluntary consensus standards scan), 355
(VSC), 39 X-ray diffraction (XRD), 270, 274f,
VT20 single-phase pseudo-α alloy, 439 435436
VT22 alloy, 92 X-ray fluoroscopy (XRF), 177
xBeam 3D Metal Printing, 214, 217218,
W 220221, 223, 225226, 228
WAAM. See Wire arc AM (WAAM) xBeam-01 pilot installation, 230, 230f, 231t
Warping effect, 284285
Waviness component of surface texture, Y
346347 Yield strength (YS), 360361
WC. See Tungsten (WC)
Weight loss on drying, 107 Z
Weight reduction, 328329 Zero gravity, 218
Weld cracking, 170 Zirconium, 170171

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