Journal of Materials Science & Technology 35 (2019) 242–269

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Journal of Materials Science & Technology

journal homepage: www.jmst.org

Invited Review

Progress in additive manufacturing on new materials: A review

Neng Li a , Shuai Huang a , Guodong Zhang a , Renyao Qin a , Wei Liu a , Huaping Xiong a,∗ ,
Gongqi Shi b , Jon Blackburn b
a
3D Printing Research & Engineering Technology Center, Beijing Institute of Aeronautical Materials, Beijing 100095, China
b
TWI Ltd, Granta Park, Great Abington, Cambridge, CB21 6AL, UK

a r t i c l e i n f o a b s t r a c t

Article history: Recent efforts and advances in additive manufacturing (AM) on different types of new materials are
Received 3 April 2018 presented and reviewed. Special attention is paid to the material design of cladding layers, the choice of
Accepted 16 April 2018 feedstock materials, the metallurgical behavior and synthesis principle during the AM process, and the
Available online 13 September 2018
resulted microstructures and properties, as well as the relationship between these factors. Thereafter,
the trend of development in the future is forecasted, including: Effects of the particles size and size
Keywords:
distribution of powders; Approaches for producing fine microstructures; Opportunities for creating new
Additive manufacturing
materials by AM; Wide applications in reconditioning of damaged components; Challenges for deep
Feedstock material
Laser and electron beam melting
understanding and applications of the AMed new materials. The idea of “Develop Materials” or “Create
Microstructure Materials” by AM is highlighted, but a series of scientific, technological and engineering problems remain
Property to be solved in future.
© 2018 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science &
Technology.

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
2. Progress in additive manufacturing on new materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
2.1. Al and Mg alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 243
2.2. Ti alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 244
2.3. Steels . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 245
2.4. Ni or Co-based superalloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 246
2.5. Intermetallic compounds . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 247
2.6. Metal matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 250
2.6.1. Al matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 250
2.6.2. Ti matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 251
2.6.3. Ni matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 252
2.6.4. Co matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254
2.6.5. Fe matrix composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 254
2.7. Laser cladding amorphous coatings . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 256
2.8. Polymeric materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257
2.9. Ceramics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 257
2.10. Gradient materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 259
2.11. Biomaterials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 262
2.12. High entropy alloys . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 263
3. Outlook . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265
3.1. Significance of the particles size and size distribution of powders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265
3.2. Approaches for producing fine microstructures . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 265

∗ Corresponding author.
E-mail addresses: xionghuaping69@sina.cn, xionghp69@163.com (H. Xiong).

https://doi.org/10.1016/j.jmst.2018.09.002
1005-0302/© 2018 Published by Elsevier Ltd on behalf of The editorial office of Journal of Materials Science & Technology.
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269 243

3.3. Opportunities for creating new materials by additive manufacturing . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 266

3.4. Further study and wide applications in reconditioning of damaged components . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 266
3.5. Challenges for deep understanding and applications of the AMed new materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 267
Acknowledgements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 267
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 267

1. Introduction tested parallel to the layer build up orientation, had the high-
est tensile strength with over 530 MPa. The ageing treatment at
In contrast to conventional processing methods, additive 325 ◦ C for 4 h remarkably increased the hardness from the as-built
manufacturing (AM) is based on an incremental layer-by-layer specimen, indicating a distinct hardening effect due to Al3 Sc pre-
manufacturing. As such, most relevant AM technologies use pow- cipitates. The addition of element scandium led to not only high
der or wire as a feedstock which is selectively melted by a focused strength but also ductile behavior, due to grain refinement that
heat source and consolidated in subsequent cooling to form a caused high plasticity (the elongation of 14% and the reduction
part [1,2]. Today, it has become possible to reliably manufacture of area of 20%) compared to other high strength Al-alloys (e.g.
dense parts with certain AM processes for a number of materials, 7050).
including steels, aluminium and titanium alloys, superalloys, metal Surface modification of the feedstock alloy powders has been
based composites and ceramic matrix composites [3–6]. In the near examined for the control of the microstructures of the AMed com-
future, the AM material variety will most likely grow further, with ponents. In 2017, Martin et al. [13] reported an approach to change
e.g. high-performance materials such as intermetallic compounds the columnar grains to equiaxed grains for 3D printing of high-
and high entropy alloys already under investigation. strength aluminium alloys, that is, pre-alloyed gas-atomized 7075
Thus, AM transforms more and more from rapid prototyping to spherical powders with an average particle size of 45 ␮m were
rapid manufacturing applications [7], which require not only pro- coated with 1 vol.% hydrogen-stabilized zirconium nucleants using
found knowledge of the process itself, but also of the microstructure an electrostatic assembly technique to ensure uniform distribu-
resulting from the process parameters and consequently of the tion in the powder bed and avoid settling. Upon melting zirconium
properties of the manufactured parts [8]. Each AM method has nanoparticles were pulled into the melt pool and reacted with
its specific applications based on its own advantages. Powder bed aluminium alloy to form Al3 Zr. Al3 Zr has more than 20 match-
selective fusion methods are suitable to produce complex and high ing interfaces with the primary fcc aluminium phase, exhibiting
accuracy components. While wire-fed AM methods (beam/arc) less than 0.52% lattice mismatch and 1% variation in atomic den-
have the highest deposition rates due to the feedstock of wire mate- sity, providing an ideal low-energy heterogeneous nucleation site.
rials, which are commonly used to produce large scale components The large number of the nucleation sites ahead of the solidifica-
[9]. tion front induced a fine equiaxed structure under the same laser
As pointed out by Gu [10], materials are the basis of AM tech- processing conditions as for the unmodified powder, as shown in
nology and materials creation hopefully adds new dimensions to Fig. 1(a–c). Furthermore, the nucleant particles were uniformly
three-dimensional printing (3DP) and extends the connotation of incorporated into the microstructure, and they could provide addi-
this advanced technology, thereby providing new opportunities for tional strengthening and resistance to grain gro%h owing to pinning
the future development of AM/3DP. The idea of “Create Materials” effects [13]. Such kind of approach to change the grains and tailor
by AM/3DP is a step-by-step process based on the ideas of “Use the resulted properties through surface modification of the feed-
Materials” and “Develop Materials” [10]. Murr et al. stated that, stock alloy powders is greatly effective and is worth extending to
AM could fundamentally alter or extend the traditional materials other material systems.
science and engineering paradigm relating to structure-property- As one of the most promising lightweight structural materials,
processing (synthesis)–performance [3]. Multiple materials and magnesium alloys have been widely used in aeronautic industry.
multiscale structures provide a possible route to optimizing overall Pawlak et al. studied the selective laser melting (SLM) of AZ31 mag-
properties of components [11]. nesium alloy spherical powder, with the particle size of 45–100 ␮m
In this paper, the recent efforts and advances in the study of AM [14]. Porosity levels less than 0.5% were achieved. From Fig. 2 (a),
on new materials were reviewed. Special attention is paid to the it can be found that performed microstructure analysis of melted
material design of cladding layers, the choice of feedstock materi- material shows significant refinement in comparison to cast mate-
als, the metallurgical behavior and synthesis principle during the rial. Both material microstructures (cast and melted) consist of
manufacturing process, and the resulted microstructures and prop- ␣-Mg non-homogenous solid solution, and ␣ + ␥ Mg17Al12 non-
erties, as well as the relationship between these factors. Totally equilibrium eutectic colonies in degenerated form located between
12 types of new materials are discussed, and lots of encourag- grains of high aluminium content.
ing research results have been achieved. On this basis, from the SLM of AZ91D has been carried out on the rolled AZ31B sub-
authors’ viewpoint some important research directions or ideas are strate plates, in which spherical gas atomized AZ91D powders with
proposed for the future work. a mean particle size of 59 ␮m were used as the starting material in
the SLM experiment [15]. Nearly full dense AZ91D (99.52%) with the
microhardness of 100 HV, UTS of 296 MPa and ␴0.2 of 254 MPa can
2. Progress in additive manufacturing on new materials be obtained using laser volume energy density of 166.7 J/mm3 . The
SLMed AZ91D consists of equiaxed ␣-Mg matrix and fully divorced
2.1. Al and Mg alloys eutectic ␤-Mg17 Al12 [15].
According to another reference, a high power diode laser (HPDL)
Modified aluminum alloys with a scandium content beyond the has been used to selectively melt one of the phases present in
eutectic point offer great potential to become a high prioritized the microstructure of the surface of a magnesium-aluminium alloy
aerospace material. Schmidtke et al. demonstrated the prepara- (AZ91D), in which the ␤-phase (Mg17Al12 precipitates) is molten
tion of aluminum scandium alloy with the main composition of while ␣-matrix is kept solid [16].
Al-4.5Mg-0.66Sc-0.51Mn-0.37 Zr by laser AM [12]. The specimens
244 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269

Fig. 1. Additive manufacturing of 7075 Al alloy via selective laser. (a) Al7075 powder functionalized with nanoparticles. (b) Equiaxed grain growth. (c) Functionalizing the
powder feedstock with nanoparticles produces fine equiaxed grain growth and eliminates hot cracking [13].

Fig. 2. SEM images of microstructure. (a) Cast AZ31 alloy. (b) Phase microstructure analysis of AZ31 alloy processed with SLM [14].

Zhang et al. used SLM to sinter a powder mixture of Mg-9%Al
[17], in which the average size of Mg powder particles with an irreg-
ular shape and Al particles with spherical feature is 42 ␮m (D50 ) and
17 ␮m (D50 ), respectively. The sintered sample mainly consisted of
Mg, intermetallic compounds Mg17 Al12 , as well as MgO and Al2 O3 .
Besides, considering the poor corrosion and wear resistance
of magnesium alloys, surface coating has been examined for sur-
face production and repair [18]. Liu et al. summarized the material
systems preplaced on magnesium alloys, including the traditional
metallic materials, novel ternary alloys, amorphous alloys and high
entropy alloys. The feasibility of depositing variable thickness of
cladding material on the magnesium alloy substrate makes it pos-
sible to repair machine parts using the laser cladding method [19].
2.2. Ti alloys
Fast progress has been made in the study of AM of Ti alloys, such
as Ti6Al4V, TC11, TC21, Ti5553 and Ti-8Al-1Er.
First of all, Ti-6Al-4 V blocks were deposited using a 3.5 kW
Nd:YAG laser and Ti-6Al-4 V wire with the diameter of 1.2mm
[20]. The as-deposited Ti-6Al-4 V can achieve strength and ductility
properties that is similar to the wrought Ti-6Al-4 V material (AMS
4928). Furthermore, the particular impurity levels of the deposited
blocks are considerably below the acceptable levels according to
aerospace material specifications (AMS 4911 L). Butler et al. [21]
evaluated the growth textures during wire-feed electron beam
directed energy deposition of Ti-6Al-4 V onto a <112>␤ -oriented
beta-single crystal Ti-6Al-4 V substrate. It was found that a portion
of the build grew epitaxially from the substrate in a single crystal
fashion (region labeled “1” in Fig. 3). In contrast, the other por-
tion of the build after two layers (∼1.1 mm in build height) showed
evidence of almost random nucleation and growth (region labeled
“2”). Equiaxed grains (region 2) gradually transitioned to conven-
tional <001 > -oriented columnar grains. In addition, as the build
height increased, region 2 grains tended to progressively consume
the region 1 until a full transition to a near <001 > -fiber texture was
attained.
Carroll et al. investigated the anisotropic mechanical properties
of a Ti6Al4V three dimensional cruciform component fabricated
using a directed energy deposition AM process. While the aver-
age ultimate tensile strength in both directions was 1060 MPa, the
achieved elongations of 11% and 14% along the longitudinal and
transverse directions, respectively [22]. The ability of attaining high
ductility was dependent on the prevention of lack-of-fusion defect,
and the anisotropy in ductility was attributed to the columnar
prior-␤ grain morphology and the presence of grain boundary ␣,
which served as a path along which damage could preferentially
accumulate, leading to fracture. Besides, the presence of additional
oxygen, of the order of 0.0125 wt%, in the Ti6Al4V component
increased both the ultimate tensile strength and yield strength,
and only slightly reduced ductility, that is, the introduced oxy-
gen contamination did not lead to embrittlement of the component
[22].
A typical ␣ + ␤ titanium alloy Ti-6.5Al-3.5Mo-1.5Zr-0.3Si
(named TC11 in China) was fabricated by laser melting deposi-
tion process [23]. The as-deposited sample exhibits a strong tensile
anisotropy due to the columnar grains morphology and the strong
texture of ␤ <001 > parallel to the deposition direction. Despite the
anisotropy, the ␣ + ␤ annealing can increase the mechanical prop-
erties in both strength and ductility to levels that are much higher
than the specification limits of the alloy.
In the meantime, the study on direct laser deposition of Ti-
6Al-2Zr-2Sn-3Mo-1.5Cr-2Nb (TC21) alloy and Ti-5Al-5Mo-5V-3Cr
(Ti5553) alloy are still in progress [24,25]. The tensile properties of
laser AMed TC21 samples show significant anisotropic under two
different heat treatment conditions. The horizontal samples exhibit
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 3. IPF maps of the ␣-phase and calculated prior-␤ phase (X dir.  ND) captured from the “cross-section” YZ plane (a), (b), respectively, and section of a [-110]-oriented
stereographic projection with relevant planes/directions identified (c)[21].
Fig. 4. Microstructure of electron beam deposited Ti-8Al-1Er (a) and Ti-6Al-4 V (b), normal to build direction [27].
stronger strength than the vertical sample, and the total elongation
of the horizontal sample is much inferior to that of the vertical ones
[26].
Besides, oxide dispersion strengthened alloys, which benefit
from rapid solidification are well suited for AM processes [27]. Of
the titanium–rare earth alloys, rapid solidification of Ti-Er received
the most attention because of the relatively large solid solubil-
ity extension of Er in titanium and the thermal stability of Er2 O3
precipitates which can refine grains and enhance the elevated tem-
perature properties. To determine the effectiveness of AM process,
a novel composition titanium alloy of Ti-8Al-1Er was fabricated by
wire feed electron beam deposition process. The microstructure
showed no evidence of columnar grain structure, but rather a more
equiaxed grain structure which is very different compared to the
Ti-6Al-4V [28,29]. The grain size appears bi-modal in nature, with a
mixture of large and small grains. The Er2 O3 dispersoid radii are less
than 0.5 ␮m within the size range required for elevated temper-
ature alloys. The dispersoids are observed along grain boundaries
and in parallel strings indicative of formation along crystallographic
planes (Fig. 4) [27].
2.3. Steels
In the study on the laser rapid forming of 34CrNiMo6 steel,
Huang et al. pointed out that cooling condition has a signifi-
cant effect on the microstructure and mechanical properties of
245
the laser rapid formed thin-wall component [30]. The component
under the metal-cooling condition has the least tensile property,
whereas that under the water-cooling condition is most brittle.
Under the air-cooling condition, the microstructure changes from
bainite + ferrite + retained austenite in the top zone to the coarse
ferrite + cementite in the bottom zone. The component exhibits
the lowest tensile strength but the best plasticity because of the
greatest tempering effect of the laser rapid forming process [30].
Work on the laser solid forming process of AISI 420 stainless
steel, indicates that the purification occurs when the oxygen partial
pressure is lower than a certain threshold [31]. The oxygen adsorp-
tion mainly takes place in the molten pool stage. The decrease of
the oxygen partial pressure and increase of the contents of ele-
ments forming volatile oxides and original oxygen in the deposited
material all promote the purification [31]. According to another
work, the decrease of the environment oxygen content resulted in
the decrease of the number density of the oxide particle within the
laser solid formed sample of AISI420 stainless steel [32].
Work in the laser solid formed 300 M steel, found out that the as-
deposited microstructure consists of martensite and coarse bainite,
and the microstructure becomes uniform after the heat treatment,
composed of tempered martensite, bainite and a small amount of
retained austenite [33]. The change of the microstructure also has
an evident effect on the fatigue crack growth rate of the materials.
Jerrard et al. [34] and Facchini et al. [35] have fabricated 17-
4PH stainless steel by SLM and they reported the occurrence of
246 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 5. 3D-optical micrograph composite section view for 17-4PH stainless steel
fabricated by SLM. The build direction is shown by arrow at lower right [3].
metastable austenite or mixtures of austenite (fcc, a = 0.357 nm)
and martensite (bcc ␣–ferrite (Fe), a = 0.286 nm) to compose the
microstructures for the fabricated products. Recently Murr et al.
reported SLM fabrication of 17-4PH stainless steel components in
an argon cover gas, with directional martensite (bcc) oriented in the
[200]␣ direction, parallel to the build direction shown by the arrow
in Fig.5, for either argon or nitrogen-atomized powder [3]. Fur-
thermore, almost in the meantime, Lin et al. even investigated the
microstructure and mechanical properties of laser solid formed and
laser forming repaired 17-4PH stainless steel [36]. The microstruc-
ture of laser deposited zone (LDZ) consisted of martensite laths and
a small amount of second strengthening phases particles, such as
M7 C3 and NbC carbides. The microstructure of HAZ consisted of the
ferrite strips and martensite laths. The comprehensive mechanical
properties of the laser solid formed and laser forming repaired 17-
4PH stainless steel were equivalent with those of the wrought. Only
their ductilities were just below those of the wrought. Additionally,
the tensile strength of the repaired sample is between those of the
laser solid formed and the wrought samples [36].
2.4. Ni or Co-based superalloys
Ni-base alloys are typically used to manufacture hot-section
components of gas turbine engines, as such alloys offer higher yield
strength with increasing operating temperatures primarily due to
the presence of the secondary ␥’ phases.
The basic research results concerning the fabrication of Inconel
625 superalloy by electron beam melting (EBM) have been carried
out [37]. The 3D-optical metallograph composite section was illus-
trated in Fig. 6(a), and the columnar precipitates, shown in the TEM
image in Fig. 6(b), have been identified as ␥”-Ni3 Nb bct platelets
coincident with the NiCr fcc matrix {111} planes. Correspondingly,
the NiCr matrix grains evident in the horizontal plane of the 3D
composite view in Fig. 6 exhibit a [200] texture in the horizon-
tal plane, and parallel to the build direction ([HKL]= [200]) and a
[220] ([110]) texture in the vertical reference plane as shown in
the vertical reference plane TEM image in Fig. 6(b).
Many researchers paid attention to the AM of Inconel 718 alloy
due to its high application potential. A regular microstructure
with good metallurgical bonding, minimal defects and fine den-
dritic grains was formed in SLMed In718 samples [38]. But after
heat treatment, the regular dendritic structure disappeared and a
needle-like ␦ phase precipitated at grain boundaries when ␥’ and
␥” phases dissolved in the matrix. As reported in literature [39],
Fig. 6. (a) 3D-optical microscopy image composite section view for alloy 625 com-
ponent fabricated by EBM. The build direction is noted by the arrow (lower right).
(b) TEM bright-field image showing Ni3 Nb bct precipitate plates coincident with
NiCr fcc {111} planes noted. The vertical reference plane view corresponds to (a)
[3,37].
Inconel 718 alloy parts were manufactured by laser solid form-
ing technology with two types of laser scanning paths, i.e., single
direction raster scanning (SDRS) and cross direction raster scanning
(CDRS). The as-deposited grains of the CDRS sample are finer than
those of the SDRS sample. The ultimate tensile strength of those
two samples is similar to each other, but the ductility of the CDRS
sample is much better than that of the SDRS one. Furthermore, the
influence of Laves phases on the high-cycle fatigue behavior of laser
AMed Inconel 718 has also been studied [40].
Tayon et al. [41] examined the evolution of microstructure,
crystallographic texture, and mechanical properties of Inconel 718
alloys fabricated via electron beam freeform fabrication (EBF3 ) pro-
cess (Fig. 7). The microstructure of as deposited (AD) condition
displays a range of strong texture components for L orientation
(deposition direction) that are largely concentrated around <001 > .
After heat treatment (HT) of solution and aging, recrystallization
occurred and the extent of texture appreciably decreased. The aver-
age UTS and YS values for the L orientation in the EBF3 block (either
in the AD or the HT condition) were greater than those for the as-
cast Inconel 718 but less than those for rolled Inconel 718. The heat
treatment significantly increased both UTS and YS compared to AD
condition and reduced the anisotropy (Table 1).
IN 718 was processed by SLM to produce columnar microstruc-
tural morphology composed of primarily <200>-textured ␥’ phase
precipitate columns [42].
In another work, IN 718 was processed using laser rapid form-
ing (LRF) and consisted of columnar dendrites that grew epitaxially
from the substrate parallel to the deposition direction, with a thin
layer at the top of the sample where the dendrites grew along
the laser scanning direction, referred to as direction-changing den-
drites [43].
In-738LC alloy as a typical cast nickel-based superalloy, was
produced by laser solid forming (LSF). Cracking was frequently
found for LSF superalloy due to the high content of Al + Ti [44,45].
It was found that the crack-free sample could be obtained for In-
738LC alloy with 1050 ◦ C preheating [46]. The In-738LC obtains its
strength primarily from the presence of a large amount of ␥’ phases
in the nickel-based fcc matrix (␥). Compared with the cast refer-
ence, reported in Rickenbacher’s work [47], the yield strength and
ultimate tensile strength of the as-deposited samples were both
14% higher while the elongation was 44% higher.
The scanning laser epitaxy (SLE) process has been investigated
for similar-chemistry powder-substrate and dissimilar-chemistry
powder substrate combinations, and the process has yielded
encouraging results in producing epitaxial microstructural deposits
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 7. Optical micrograph of the lengthwise section of the first half of a CMSX-4 sample with the starting edge on the left side of the image [48].
Table 1
Tensile YS and UTS in the (L–T) plane of the Inconel 718 EBF3 block in the AD and the HT conditions [41].
Orientation Property AD (measured) (MPa)
YS 655
L
UTS 978
YS 699
T
UTS 936
45 YS 703
deg UTS 993
even for SX alloys (Fig. 7). This should be of great significance for
turbine hot section repair [48].
Achieving epitaxy in metal AM is challenging and requires tight
control of processing parameters such as energy source power,
scanning speed, and spot diameter. Complete powder melting sys-
tems have been significantly more successful than partial powder
melting systems in the production of epitaxial microstructure. The
demonstrated potential to produce epitaxial microstructure by
using a metal AM process could open up entirely new paradigms of
manufacturing if the process is demonstrated to be repeatable and
robust in the future [49].
Rene 142, a commercial, columnar grained, gas turbine air-
foil Ni-based superalloy, has been fabricated from a pre-alloyed,
atomized powder by AM using electron beam melting. The fabri-
cated EBM product is relatively optimized with regard to potential
creeprelated behavior in turbine blade applications without any
post-fabrication heat treatment [50].
Special emphasis is also put on the specific properties and pos-
sibilities of selective electron beam melting (SEBM) for Co-Cr-Mo
alloys. During SEBM, Co–Cr–Mo alloys solidify via the fcc ␥-phase
which is not or only partially transformed into the stable ␧-phase
during the building process. The as-built samples show a pro-
nounced texture as a result of epitaxial growth with preferred
grain orientation of the ␥-phase in <001 > direction. The M23 C6
precipitates (M = Cr, Mo, Si) are aligned along the build direc-
tion with a mutual distance of about a few microns [51–53]. After
adequate heat treatment (hot isostatic pressing + homogenisation)
Co–Cr–Mo alloys built by SEBM show superior properties compared
to wrought or cast alloys [51].
2.5. Intermetallic compounds
The recent efforts and advances in AM of mainly two types of
intermetallic compounds, TiAl based alloy and NbSi based alloy, are
presented and summarized in this section.
TiAl based alloys are highly attractive for the aeronautical indus-
try as new high temperature light-weight structural materials due
to their low density (3.7–3.9 g/cm3 ), high elastic moduli, excellent
tensile strength and creep resistance at high temperature [54–56].
Therefore, TiAl alloys have shown a potential for the application
with the service temperature of 760–850 ◦ C. However, the room
temperature tensile elongation is very poor and only about 1%,
which makes the TiAl-base alloy difficult to be processed into com-
ponents especially the complex-shaped ones. Compared to the
247
HT (measured) (MPa) Cast (literature) (MPa) Wrought (literature) (MPa)
986 488 1182
1114 786 1369
998 – 1208
1162 – 1374
995 – –
1171 – –
traditional manufacturing methods such as cast, extrusion and
forging, the additive manufacture technologies, such as SEBM, SLM
and LDMD, are the emerging near-net and net forming technolo-
gies and will be applied to produce the near-net-shape or net-shape
TiAl based alloys components [57]. Li et al. even developed the
laser cladding TiAl intermetallic compound coatings on the tita-
nium alloy [58,59,60]. AM of TiAl based alloys has been a hot area
of research in recent years.
Among these metal AM technologies, laser direct metal depo-
sition(LDMD) was first used in the fabrication of TiAl based
alloys. As early as 2000, Seivastava et al. [61,62] fabricated
simple shapes of TiAl alloy material using LDMD technology
with gas atomized Ti-48Al-2Mn-2Nb powders. They demonstrated
that the microstructure of TiAl based alloy prepared by LDMD
was heterogeneous in nature and very fine, as compared to
the conventional manufacturing methods [61,62]. In addition,
the compositional heterogeneity present in the LDMD-fabricated
TiAl based alloy could be eliminated by post heat treatment.
However, the obvious grain coarsening occurred after annealing
[61,62].
Qu et al. [63,64] successfully fabricated two types of TiAl spec-
imens with size of approximately 40 mm × 40 mm × 3 mm, which
combined with preheating before LDMD process. The microstruc-
tures of the two as-deposited TiAl specimens were all fully lamellar
structure consisting of ␥-TiAl and ␣2 -Ti3 Al. Their grain size was
50–100 ␮m and the ultra-fine lamellar spacing was about 0.2 ␮m,
as shown in Fig. 8 [63,64], and their room temperature ductility
was very poor, only 0.2% for Ti-47Al-2.5V-1Cr specimen and 0.3%
for Ti-40Al-2Cr specimen, which were obviously lower than that
of cast TiAl based alloy [63]. In addition, the tensile strength and
ductility could be significantly enhanced by annealing. The tensile
strength of the two TiAl based alloy specimens was improved from
about 550 MPa to 650 MPa, and their room temperature ductility
reached 0.6% after annealing at 1125 ◦ C/30 min and followed by W.
Q. [64].
Lober et al. [65] investigated the SLM process of TiAl based
alloy, and bulk cylinders and dodecahedron unit cells of Ti-44Al-
4Nb-1Mo-0.1B alloy with a relative density of around 99% were
successfully manufactured [65]. The as-fabricated microstructure
was fine grained nearly lamellar ␤ structure, and the supplied com-
pression strength and strain were approximately 1900 MPa and
9.5%, respectively. Additionally, the compression strain could be
greatly improved to 16.5%, but its compression strength would
decrease to 1670MPa [65].
248 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 8. Microstructure of the as-deposited Ti-40Al-2Cr (a, b) and Ti-47Al-2.5V-1Cr (c, d) alloy [63,64].
Fig. 9. Microstructure of the SLM-processed Ti-45Al-2Cr-5Nb alloy [66].
Shi et al. studied the effect of laser scanning speed and energy
density input on Ti-45Al-2Cr-5Nb alloy processed by SLM [66,67].
The SLM-processed alloys were dominated by high-angle grain
boundaries (HAGBs) and the content of HAGBs increased with
increasing energy density inputs or deceasing laser scanning speed.
Moreover, the increase of laser scanning speed and the decrease
of energy density input all could lead to an obvious decrease of
average grains size. The SLM-produced TiAl alloys consisted of ␣2
matrix, ␥ and B2 phases randomly distributed in the matrix, as
shown in Fig. 9. With the increase of energy density inputs or
decrease of laser scanning speed, the content of ␣2 phase increased,
while the contents of ␥ phase and B2 phase decreased [66,67].
Although the relative density of the SLM-process Ti-45Al-2Cr-5Nb
alloy was only around 92%, the nanohardness of the TiAl alloy was
up to 9.5 GPa, which was much higher than those of the tradi-
tional casting counterparts (5.1 GPa) and traditional roll bonding
fabricated TiB2 reinforced TiAl alloy (6.73 GPa). Moreover, its com-
pression strength was approximately 1250 MPa [66].
EBM is very suitable to process high melting temperature,
refractory, and/or reactive materials [68]. Equiaxed, small-grain
(∼2 ␮m) structures with lamellar ␥/a2 -Ti3 Al colonies with average
spacing of 0.6 ␮m have been fabricated by AM using EBM of Ti-47Al-
2Cr-2Nb (at.%) titanium aluminide powder. The EBM-fabricated
titanium aluminide prototype density was ∼3.76 g/cm3 , roughly
98% of theoretical density [69]. But, during the EBM processes, due
to the vacuum environment, the preferential vaporization of high
vapor pressure elements is noticeable.
It was reported that the atomic percentage of aluminium
decreased along with the increase of energy input. Element loss
of aluminium can reach 15 at.% for Ti-47Al-2Cr-2Nb alloy [70].
By adjusting the processing parameters including layer thickness
and beam parameters and taking advantage of the short return
times, Al loss was reduced to about 0.5 at.% for this TiAl alloy
[71]. Mohammad et al. studied the effect of EBM parameters
on microstructure and mechanical properties of Ti-48Al-2Cr-2Nb
(at.%) titanium aluminide and the ultimate tensile strength of the
EBMed specimens close to wrought form (480 MPa) but superior to
castings (275–380 MPa) [72].
Todai et al. reported that Ti-48Al-2Cr-2Nb alloy fabricated
by EBM exhibited a unique layered microstructure composed of
duplex-like region and ␥ bands (Fig. 10) [73]. Duplex-like region is
predominantly composed of lamellar-structured ␥/␣2 fine grains
and fine equiaxed ␥ grains, while ␥ bands is composed of coarser
equiaxed ␥ phase grains. Regardless of ␪, the average layer thick-
ness of the duplex-like region and the ␥ band was approximately
60 ␮m and 30 ␮m, respectively. The grain size in the ␥ bands
is approximately 20 ␮m. Owing to the unique layered and finer
microstructure, the yield strength and the tensile elongation of the
specimens shows the orientation dependence. But, in general, the
room temperature yield strength is good, i.e., at ␪ = 0◦ , 45◦ and 90◦
it is ∼605 MPa, ∼556 MPa and ∼587 MPa, respectively. The yield
strength of the as-EBMed specimens at room temperature was
higher than that prepared by casting. In addition, the room tem-
perature ductility of the specimen at ␪ = 45◦ is over 2%, while the
elongation of the specimens at ␪ = 0◦ and 90◦ is about 0.5% and
2%.
Besides, Ma et al. [74,75] presented an interesting method for
fabrication of titanium aluminide components by using in-situ
alloying and layer AM based on the gas tungsten arc welding
(GTAW) process combined with separate feeding of commer-
cially pure titanium wire and pure aluminum wire. The bottom
region of the components showed a lamellar (␥/a2 ) structure and
interlocked grain boundaries, whereas the top region revealed sys-
tematic occurrence of interdendritic ␥ phase. The ultimate tensile
strength of the Y-direction and Z-direction is 549 ± 23 MPa and
488 ± 50 MPa, respectively. The specimens tested in the Y-direction
are found to have higher ultimate tensile strength (UTS) and yield
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269 249

Fig. 10. Microstructure of the vertical cross-section of at ␪ = 0◦ (a), 45◦ (b), and 90◦ (c), at high magnification [73].

Fig. 11. BSE images of the as-deposited alloy (a), and the alloy annealed at 1500 ◦ C for 24 h in flowing argon (b). Processing parameters: laser power = 432 W, powder feed
rate = 18.1 g/min, scan speed = 400 mm/min [82].

strength (YS) than those tested in Z-direction. However, there is no

observable difference in elongation.
In the material field, much attention has been paid to another
kind of ultra-high-temperature structural materials worldwide,
Nb-Si based alloys. They have shown great potential to replace Ni-
based supreralloys due to their high melting point (>1750 ◦ C) and
low density (6.6–7.2 g/cm3 ) as well as attractive specific mechan-
ical properties at elevated temperatures of 1200–1400 ◦ C [76–78].
Over the past few years, several processing techniques includ-
ing vacuum arc melting, induction melting, investment casting,
directional solidification (DS), and powder metallurgy have been
successfully employed to fabricate Nb-Si based alloys [79–81].
Although the Nb-Si alloy prototype airfoil have been fabricated by a
hybrid arc-melting and drop-casting technique, by overcoming the
difficulties of developing the melting capability of the appropri-
ate scale and the matching ceramic mold materials, obtaining the
proper dovetail geometry of an airfoil is still a complex endeavor, Fig. 12. Schematics of LMD with dual powder feeding method [83].
and requires numerous time-consuming, post-machining opera-
tions [76]. In the light of AM technology, it could produce near solid-solution (NbSS ) phase, Nb5 Si3 intermetallic compound and
net shape components with complex shape and even with com- HfO2 particles, and is much finer than those of a cast alloy with
plex internal features. Additionally, due to the rapid melting and similar composition. No changes to the structure of phases present
solidification characteristics of AM processing, it is easy to achieve occurred during heat treatment at 1500 ◦ C for 24 h, although the
finer microstructure and to reduce composition segregation of Nb- microstructure moved towards a more stable state (as shown in
Si based alloys, which is possible to improve the overall properties. Fig. 11(b)).
Dicks et al. deposited the alloys with the composition of Liu et al. [83] fabricated Nb-17Si-23Ti (at.%) ternary alloys
Nb-22Si-26Ti-6Cr-3Hf-2Al (at.%) by laser directly forming using using in-situ reaction laser melting deposition (LMD) from Nb-28
pre-alloyed gas-atomised powder, and demonstrated that direct at.% Ti powder mixture and pure Si powder (Fig. 12). The as-
laser deposition was a suitable technique for the fabrication of deposited samples mainly consisted of NbSS , metastable Nb3 Si and
the Nb-Si based alloy, allowing samples to be produced with Ti-rich NbSS . As shown in Fig. 13, the in-situ reaction LMD pro-
high dimensional accuracy [82]. As shown in Fig. 11(a), the cessing resulted in remarkable refinement of microstructure and
microstructure of the as-deposited alloy consisted of bcc niobium the average size of NbSS was about 1–3 ␮m, which was further
250 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 13. BSE images of the as-deposited Nb-17Si-23Ti alloys fabricated by LMD with the laser power of 1 kW (a) and 2 kW (b), and BSE images of longitudinal sections (c) and
transversal sections (d) for the as-deposited Nb-17Si-23Ti alloys with DS microstructure. Inserts are enlarged images, and arrows indicate the build direction [83].
refined in comparison with that of the LMD Nb-26Ti-22Si-3Hf-
2Al (at.%) alloy from the corresponding gas-atomised alloy powder
[82]. With the increase of the laser power from 1 kW to 2 kW,
the NbSS morphology changed from discontinuous dendritic to
near equiaxed, and the microhardness increased from 822 HV
to 951 HV, meanwhile, the indentation fracture toughness was
improved from 12.3 MPa m1/2 to 14.1 MPa m1/2 . Furthermore, fine
directional solidification (DS) microstructures were achieved by
LMD as well, and presented remarkable mechanical properties. Its
micro-hardness was as high as 1075 HV and indentation fracture
toughness was up to 20.3 MPa m1/2 , where the toughening effect
was mainly attributed to the directional growth of fine NbSS and
Nb3 Si phases.
Guo et al. [84] investigated the microstructure, hardness and
oxidation behavior of Nb-18Si-24Ti-2Cr-2Al-2Hf (at.%) alloy fab-
ricated by SLM using pre-alloyed powder. Results showed that
the as-built alloy consisted of Nbss, ˛-Nb5 Si3 , ˇ-Nb5 Si3 and Nb3 Si.
Sphere shaped Nbss phases with a maximum diameter of 300 nm
were obtained. After heat treatment at 1500 ◦ C for 4 h, the Nbss
phases interconnected to form a continuous matrix with discontin-
uous ˛-Nb5 Si3 phases, and the average hardness of the SLM parts
decreased from 810 HV to 542 HV. Compared with the oxide scale
on arc-melted alloy, oxide scale formed on SLM-processed after
oxidation at 1300 ◦ C for 0.5 h was more compact with fewer holes,
combined with the formation of a more continuous SiO2 layer at
the initial oxidation stage.
To date, the related studies of Nb-Si based alloys prepared by AM
technique have been carried out and extremely finer microstruc-
ture, higher hardness, higher room temperature toughness and
better oxidation resistance at high temperature could be obtained
by AM [82–84]. However, due to the intrinsic brittleness of Nb-Si
based alloys, and the rapid melting and solidification process during
AM, micro-cracks tend to appear in the preparation of larger scale
samples. In our opinion, to realize the application of AMed Nb-Si
based alloys, further research work is highly needed for composi-
tion optimization by adjusting the level of Si and adding the alloying
elements of Ti, Hf, and etc., as well as processing optimization such
as preheating during AM.
2.6. Metal matrix composites
Lots of research work focused on AM of metal matrix compos-
ites (MMCs), including Al, Ti, Co, Fe matrix ones, and the achieved
results were fruitful, in which the in-situ reactions for the synthe-
sized products were impressive.
2.6.1. Al matrix composites
To improve the mechanical properties of aluminum matrix, the
aluminum borate whisker Al18 B4 O3 of 0.5–1 ␮m in diameter and
10–30 ␮m in length was used via laser surface melting [85]. The
results showed that microhardness of the laser layer (294 HV) was
improved 65% compared to aluminum matrix (178 HV), because
of the presence of Al2 O3 particles, solid solution hardness and
the grain refinement of the laser layer following rapid quench-
ing associated with the processes [85]. Besides, the whiskers were
decomposed and ␥-Al2 O3 appeared at the surface of the composite
after the laser surface melting. A great deal of ␥-Al2 O3 existed at
the bottom of the laser pool.
Kang et al. reported a novel Al-based composite reinforced by
nano-sized Al91 Fe4 Cr5 quasicrystal (QC) on Al substrate by SLM
[86]. This composite material was prepared from the mixture of
pure aluminum and Al65 Cu20 Fe10 Cr5 QC powders, which could pro-
duce parts with sophisticated form and fine microstructure with
near-zero material waste. Additionally, the sample obtained at rela-
tively low laser power presented a mixed microstructure including
partially melted QC, micro-QC and nano-QC. The instrumented
indentation test indicated that the partially melted QC particle pre-
sented higher hardness (8.59 GPa) than that of the other structure
in the composite (4.58 GPa or 3.37 GPa). However, due to the ultra-
low ductility of the QC alloy, SLMed QC/Al composite was easy to
crack [86]. Besides, they also studied the microstructure and wear
behavior of hypereutectic Al-Si alloy, in-situ fabricated using SLM
of a mixture of eutectic Al-12Si (wt.%) and pure Si powders, and
fairly dense hypereutectic Al-Si alloys were obtained [87].
Yang et al. studied the effect of different Si content on wear
resistance of AZ31D magnesium alloys by laser cladding with Al-Si
powders [88]. Al and Si powders were mixed with the weight ratio
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269 251

Fig. 14. Schematic reaction process that takes place in Al12Si20Ti/SiC coating. (a) An SiC particle in a molten Al-Ti matrix. (b) Reaction between SiC particle and molten Al.
(c) Reaction between molten Ti with Al4 C3 and Si. (d) Al and TiC ring formation [90].

Fig. 15. EBSD maps of AA6061/TiC in situ composite containing TiC. (a) 0; (b) 2.5%; (c) 5% [91].

of Si 8.0 wt.%, 12.5 wt.% and 60 wt.%, and mixed with resin PVA,
and then placed on the substrate surface with a thickness of about
0.5 mm. The clad layer with the Si content of 12.5% exhibited the
optimum wear resistance. The major reinforcing phase Mg2 Si par-
ticulate with eutectic Mg17 Al12 phase was found in the clad layer,
and the micro-hardness increased 4.85 times due to the presence
of this intermetallic phase [88].
Anandkumar et al. fabricated the coating composite consisting
of an Al-Si matrix reinforced with SiC particles by laser cladding on
UNS A03560 cast Al-alloy substrates from the mixture of powders
of Al-12 wt% Si alloy and SiC [89]. The undissolved SiC particles were
mainly found at the bottom of the clad tracks, where the maximum
temperature reached during the processing was lower, and Al4 SiC4
and Si particles dispersed in a matrix of ␣-Al + Si eutectic. These
results show that Al4 SiC4 and Si increase the hardness from 90 HV to
250 HV of the material by dispersion hardening but not contribute
to its abrasive wear resistance, because they are softer than the
abrasive particles [89].
Moreover, Riquelme et al. reported the deposition of Al/SiCp
coatings on AA6082 aluminum alloy using laser cladding [90]. The
employed method consists of the addition of different alloying ele-
ments (Si or Ti) to the composite matrix powder to modify the
equilibrium of the detrimental Al4 C3 formation reaction. Al40Si/SiC
is the hardest coating because of the higher percentage of SiC and
primary and partially dissolved Si than the others. Fig. 14 shows
a schematic figure that explains the reaction process, in which SiC
particles are completely dissolved and it only can be seen that a ring
of TiC forms in the surroundings of a smaller SiC particle. Besides,
the molten Ti reacts with the Si and forms TiSi2 . The formation of
these products decreases the reinforcement amount [90].
Lijay et al. synthesized aluminum alloys AA6061 reinforced with
various amounts (0, 2.5% and 5%, mass fraction) of TiC particles by
in situ reaction of inorganic salt K2 TiF6 and ceramic particle SiC
with molten aluminum [91]. The in-situ formed TiC particles act
as effective grain refiner and refine the grains of cast aluminum
matrix from ∼90 ␮m to ∼30 ␮m (Fig. 15), and they completely
change the dendritic structure of as-cast AA6061 [91]. This may
be due to that TiC particles acted as grain nucleation sites and
refined the grains of aluminum matrix effectively. Besides, possible
intermetallic compounds including Al3 Ti and Al4 C3 were detected
in significant quantity.
2.6.2. Ti matrix composites
Discontinuously reinforced Ti6Al4V/TiB composites were fab-
ricated using direct laser deposition by injection of premixed
powders of TiB2 and Ti6Al4V [92]. Additionally, (TiB + TiC) rein-
forced Ti matrix composites were prepared by SLM using spherical
commercially pure titanium (CP-Ti) powder with the particle size
distribution of 15–45 ␮m and polyhedron-shaped reinforcing B4 C
particles with a mean particle size of 5 ␮m [93]. The TiC and TiB
252 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 16. Evolution mechanism of SLM-processed B4 C/Ti composite parts at variable
laser power: (a) 125 W, 800 mm/s, (b) 200 W, 800 mm/s [93].
phases were formed by in situ reaction in a route of 5Ti + B4 C →
4TiB + TiC. Moreover, the in-situ whisker-like TiB and granular TiC
phases significantly grew and coarsened with the increase of the
laser power (Fig. 16), and this would result in the decrease of the
composite hardness [93].
A compositionally graded TiC/Ti6Al4V material was successfully
fabricated by direct laser fabrication with TiC powder with particle
size ranging from 100 to 200 ␮m and Ti6Al4V wire with a diameter
of 0.45mm [94]. This design of the feedstock material combination
of TiC powder and Ti6Al4V wire is interesting. After the laser pro-
cessing, the TiC particles are distributed uniformly in the Ti6Al4V
matrix, and along most of the length of the compositionally graded
sample TiC was completely melted and formed primary TiC, eutec-
tic TiC and secondary TiC. When the volume fraction of TiC particles
reached 74%, some unmelted TiC was retained. The sliding wear test
showed that the sample with 24 vol.% TiC exhibited the optimum
balance of the tribological properties [94].
Surface modification of Ti6Al4V alloy was conducted by AM
using ball milling treated mixtures of Ti and SiC powder parti-
cles. Two laser cladded layers of 90%Ti+10%SiC and 80%Ti+20%SiC
were deposited onto the Ti6Al4V substrate. Chemical reactions took
place between the Ti and SiC particles in the composite layers,
and the reaction products consisted of TiC and Ti5 Si3 . The formed
Ti5 Si3 particles present an average size of about 200 nm and TiC
ones about 1 ␮m. The 80%Ti+20%SiC cladded layer increased the
hardness of the Ti6Al4V matrix from 339.1 HV to 932.2 HV, and this
was mainly attributed to the high hardness of the TiC and Ti5 Si3. In
particular, the hardness of TiC is high up to 2856HV-3060HV [95].
A novel oxide dispersion strengthened (ODS) titanium alu-
minide alloy (Ti-45Al-3Nb-0.2Y2 O3 at.%) was developed for
powder-based processing technologies with a focus on spark
plasma sintering and AM [96]. The ODS particles were homoge-
neously distributed in the alloy matrix after processing in the liquid
state. A significantly reduced texture formation was observed with
this novel alloy.
Ti-Co elemental powder blends in nominal chemical composi-
tions of 60Ti-40Co (wt.%) with a particle size of 140–320 mesh were
Fig. 17. Bright-field TEM micrograph of micro-morphology of TiC in eutectic austenite (a) and HREM image of TiC-␥-Ni interface (b) [98].
selected as raw material, and TiCo/Ti2 Co dual-phase intermetallic
coatings consisting of TiCo block primary phase and Ti2 Co continu-
ous matrix were fabricated by laser cladding on a commercial ␣ + ␤
titanium alloy BT9 [97]. The coatings exhibited an average hardness
of about 720 HV and excellent wear resistance under dry sliding
wear test conditions.
2.6.3. Ni matrix composites
Concerning the AM of Ni matrix composites, series of material
reaction systems were used for different purposes, including Ni-Ti-
C, Inconel 690-TiC, Ni-TiC, NiCr-Cr2 O3 -La2 O3 , Ni60-BN, Ni-Mn-Si,
WC-NiBSi, etc.
Ni alloy composite coating reinforced by in situ reacted TiC parti-
cles with a gradient distribution was prepared using one-step laser
cladding with a pre-placed mixture on a 5CrMnMo steel substrate
[98]. Titanium and graphite particles were used as raw reaction
material, with the average size of 2 ␮m and 4 ␮m respectively. They
were mixed with Ni alloy powder, in which the titanium graphite
powder was 30 vol.%. The mixed powders were painted on the
substrate to give a thickness of about 0.8 mm. Laser cladding was
carried out with a 3 kW continuous wave CO2 laser to produce a
series of single clad tracks without overlap. The phases of the laser
cladded coating consist of ␥-Ni, TiC, Cr23 (C, B)6 , Ni5 Si2 and Cr2 B,
without the presence of Ni-Ti binary compounds. A large number
of formed TiC particles are uniformly distributed in the interden-
dritic regions, which means that TiC particles have been trapped by
the rapid advancing solid-liquid interface. The size distribution of
the TiC particle is of the order of nanometers, as shown in Fig. 17(a).
It is also noticeable that the interface between the TiC and the ␥-Ni
austenite remains clean and free from any deleterious phase due
to interface reactions (Fig. 17(b)). Because of the high solidification
speed the interface reaction between the particle and the molten
alloy is completely restrained.
An interesting phenomenon was observed that, the volume frac-
tion of TiC particles exhibited a smooth gradient distribution as a
function of the coating depth, that is, the volume fraction of TiC
particle changed from 1.86% at the bottom to 38.4% at the top
surface layer. This gradient distribution of TiC particles should be
attributed to the relative lower density of TiC compared with the
Ni alloy. In other words, it is understandable that the TiC particles
tend to segregate to the upper regions in the particle-reinforced
MMC layer. Fig.18 shows that, the volume fraction of TiC particles
and the microhardness of the coating varied gradually with the
coating depth, and the highest value of the microhardness reached
1250 HV0.2 [98].
Titanium carbide (TiC) reinforcement particles were incorpo-
rated into Inconel 690 alloy with laser direct deposition to build
functionally gradient MMCs [99]. The used raw materials included
the Inconel 690 spherical particles of diameter 44 ␮m to 149 ␮m
with a typical alloy composition of 27.0 Cr, 8.0 Fe, 0.05 C, 0.50
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 18. Gradient distribution of TiC particles and Microhardness variation with the
coating depth [98].
Si, 0.50 Mn, 0.50 Cu, bal. Ni, and the irregularly shaped TiC parti-
cles of the similar size. The composition varied from 100% Inconel
690 at layers 1 and 2 to increasing concentrations of TiC for the
subsequent 18 layers. High temperature dissolution of TiC was not
detected under the processing conditions including the laser power
of 350 W, laser scanning speed of 17 mm/s and layer thickness of
0.254 mm. It was found that increasing the amount of TiC parti-
cles altered the microstructure of the Inconel 690 matrix (Fig. 19).
The microstructure became more refined as the amount of TiC
increased, and the predominant grain shape shifted from colum-
nar to equiaxed. Furthermore, a finely dispersed dendritic TiC phase
appeared when TiC above 30.0% by volume was present. Wear test
results showed an average of 42% decreased in volume loss on the
disk by increasing content to 40 vol.% TiC.
Concerning the refining effect of the microstructures in the laser
cladded layers, presently it is well known that the addition of
rare earth elements is an effective approach, for example, evident
refinement and spheroidzation of the primary phase of the laser
Fig. 19. Microstructure of Inconel 690/TiC samples. (a) Equiaxed grains found in 8.7 vol.% TiC. (b) Groups of columnar dendrites in 15.3 vol.% TiC layer. (c) Dendritic TiC phase
(43 vol.% TiC) [99].
Fig. 20. Transmission electron microscopic images of TiC particles in primary dendrites of ␥-Ni (a) and dislocation (b) [101].
253
clad composite coatings was reported by addition of La2 O3 in the
NiCr-Cr2 C3 precursor mixed powders, and in this case the volume
fraction of primary blocky Cr7 C3 and Cr7 C3 /␥ eulectics was also rel-
atively decreased [100]. Besides, Liu et al. investigated the effects of
La2 O3 addition on the microstructure and wear properties of laser
clad ␥/Cr7 C3 /TiC composite coatings on ␥-TiAl intermetallics alloy
substrate with NiCr-Cr3 C2 precursor mixed powders [100]. The
addition of rare-earth oxide La2 O3 led to obvious refinement and
spheroidization of the primary phase of the laser clad composite
coatings and relative decrease in volume fraction of primary blocky
Cr7 C3 to Cr7 C3 /␥ eutectics, as well as increase of the coating micro-
hardness. When the addition of La2 O3 was approximately 4 wt.%
the laser clad composite coating possessed the highest hardness,
and toughness and thus the best enhancement of wear resistance
of about 30% [100].
The refinement phenomenon was also observed in the laser
cladded Ni-TiC coating deposited on AISI 4140 steel [101]. There
was an improvement in 15%–20% of relative wear resistance for
the claddeed coating compared with the bare steel substrate. TEM
results in Fig. 20 revealed deformation twinning in ␥-Ni and the
presence of high dislocation density. In addition to TiC phase, spher-
ical multiphase nano-crystalline area was detected in the vicinity
of interdendritic regions. The formation of the greater number of
nuclei and a reduction in nuclei growth was attributed to lan-
thanum ion, which partially dissolved in the nuclei and reduced
crystal growth velocity. Furthermore, larger numbers of defects
were generated at the interface of TiC and ␥-nickel. La atoms were
captured by these defects causing an increase in the nucleation rate
and decrease in surface energy of crystallization.
With regard to Ni-based composite coatings, Luo et al. fabri-
cated the 30 wt% WC/70 wt% (Ni-NiCrBSi) coating on the Ti-6Al-4 V
substrate by laser cladding [102]. The content of the NiCrBSi had
a remarkable influence on the phase constituents and the micro-
hardness as well as the fracture toughness of the coatings.
For laser cladding of the Ni60-hBN coating on a medium carbon
steel, the high-energy ball milling of nano-Ni onto nano-h-BN was
conducted with the aim to enhance the compatibility between the
254 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 21. Microstructure of as-fabricated WCp/NiBSi MMC (a) and higher magnifica-
tion (b) [106].
h-BN and the Ni-based alloy (Ni60) matrix during laser cladding
processing [103]. The main phases in the laser clad coating were
composed of hard precipitates CrB, Ni3 B, Cr7 C3 , and nickel based
solid solution (␥), which were mostly distributed in the upper layer
of laser cladding zone, and greatly increased the microhardness of
the coatings [103].
Zhang et al. synthesized three Ni-Mn-Si coatings on a copper
substrate by laser cladding [104]. The highest hardness of about
1100 HV occurred in the clad layer of coating Ni (40 at.%)-Mn (20
at.%)-Si (40 at.%), and Ni-and-Mn silicides were the major factors
in increasing the hardness of the coatings, in which Ni-Si phases
played a more important role than Mn-Si in increasing the hardness
and decreasing the friction coefficient of coatings [104].
Wang et al. reported the design and fabrication of
Ni60.16 Zr33.84 Al6 alloy coating on a AZ91HP magnesium sur-
face by laser cladding [105]. The coating layer mainly consists of
amorphous, two ternary intermetallic phases with Ni10 Zr7 and
Ni21 Zr8 type structure. These phases make the coating exhibit high
hardness (930 HV), good wear resistance and corrosion resistance.
Another important research result should be mentioned here.
Benefited from the unique preheating process, dense and crack-free
WCp/NiBSi metal matrix composite MMC samples were obtained
successfully by EBM [106]. The WC reinforcements in the EBM
specimens were evenly distributed in both the vertical and hori-
zontal planes. Although dissolution occurred at different degrees,
the reinforcements still maintained spherical morphology under
a thermal shock by an electron beam radiation. The typical thick-
ness of the dissolution band was about 5 ␮m (Fig. 21). The average
macro-hardness of the MMC reached 58HRC in both the horizon-
tal and vertical directions. The measured flexural strength, impact
toughness and compressive strength were 930 MPa, 3.6 J/cm2 and
1850 MPa, respectively.
2.6.4. Co matrix composites
Weng et al. produced MMC coatings on Ti-6Al-4 V titanium alloy
by laser cladding with the pre-placed powders of Co42 Co-based
self-fluxing alloy, B4 C, SiC and Y2 O3 [107]. The composite laser
cladding coatings were mainly reinforced by CoTi, CoTi2 , NiTi, TiC,
TiB2 , TiB, Cr7 C3 , and Ti5 Si3 , resulting from the in-situ reactions in
the molten pool. The average micro-hardness of the cladding zone
was even high up to 1134 HV0.2 , and thus the wear resistance was
enhanced by over 10 times compared with the substrate. How-
ever, it was also pointed out that too much SiC (14 wt.%) would
lead to coarse microstructure and a rise in brittleness, and was not
propitious to the wear resistance [107]. Ti5 Si3 /TiC reinforced Co-
based composite coatings were also fabricated on Ti-6Al-4 V alloy
by laser cladding with Co42 and SiC mixture [108]. In this case the
microhardness of the coatings was enhanced to over 3 times the
substrate. Similarly, too much SiC (20%) addition led to cracks in the
cladding layer, and they were detrimental to further improvement
of the wear property.
Besides, composite coatings on titanium alloy were attempted
by laser cladding with Co42+TiN mixed powders [109]. The coatings
were comprised ␥-Co/Ni, CoTi, CoTi2 , Co3 Ti, NiTi, TiN, CrB, Cr7 C3 ,
TiC, TiB, and TiC0.3 N0.7 phases. The dissolution and re-precipitation
of TiN occurred during the laser cladding process. The in-situ
formed TiC tended to grow on the surface of the undissolved TiN,
and TiCo0.3 N0.7 was produced from the reaction between TiC and
TiN with the addition of 30 wt.% TiN. The wear resistance of the
cladding coating under dry sliding wear test was increased to 18.2
times the Ti-6Al-4 V substrate.
Although Stellite 6 with the unique chemical composition
(29%Cr, 4.5%W, 1.5%Mo,1.2%C, Co balance, in weight), is the most
popular Stellite alloy employed in various field of industry, it was
found deficient due to insufficient hardness and wear resistance
especially in some applications where metal-to-metal sealing hard-
facing was subjected to high loading and high-cycle operating.
Therefore, to enhance the hardness and wear resistance of Stel-
lite 6, a Stellite alloy mixture hardfacing consisting of 70% Stellite 3
and 30% Stellite 21was created via laser cladding for control value
seat sealing surface [110]. The microstructure of the Stellite alloy
mixture hardfacing was composed of fcc Co solid solution, M7 C3
carbide, (W, Co)6 C and (Co, Mo)3 C carbides, indicating a hyper-
eutectic microstructure with the carbides as the primary phase.
Furthermore, the volume fraction of total carbides in this alloy was
estimated 40%. This mixture hardfacing surpassed Stellite 6 and
Stellite 3 in combined properties of hardness, wear resistance and
laser processing, and according to the test result of the industry
application, no leakage was found on the corresponding sealing
surface under the specified duration of 30,000 cycles [110].
Ding et al. studied the effect of aging treatment on the
microstructure and wear resistance of VN alloy reinforced Co-based
laser cladding composite coatings with the ageing temperature
ranging from 550 ◦ C to 750 ◦ C [111]. The phase constituents of the
composite coatings after aging treatment at 550 ◦ C and 650 ◦ C were
not changed and mainly composed of ␥-Co, Cr23 C6 , Co5.47 N, ␴-FeV
and VN phase, but ␴-FeV phase disappeared after the ageing treat-
ment at 750 ◦ C. The volume fraction of Cr23 C6 and VN was gradually
increased as aging treatment temperature increased, resulting in
about 10% improvement in both the microhardness and the wear
resistance [111].
To improve the wear resistance of clad material Co-based alloy,
VN alloy/Co-based composite coatings modified by Ti was pre-
pared on a mild steel using laser cladding. The mixed powders used
were 5.0 wt.% VN alloy powders (2.5–7.5 ␮m), Ti powders (1.2 wt.%-
9.6 wt.%, 2–10 ␮m) and balance of Co-based powders (53–120 ␮m).
The VN/Co-based coatings were mainly composed of ␥-Co, Cr23 C6 ,
Co5.47 N, ␴-FeV and VN phases, and new TiN and VC phases as the
reaction products: TiC + VN = TiN + VC, were detected in the com-
posite coatings after adding Ti [112]. The formation of TiN, VC
and other intermetallic compounds in the composite coatings after
adding Ti retarded the growth of dendrites, promoted the trans-
formation of long rod-like dendrites into short rod-like dendrites
and the formation of fine grains and a large number of equiaxed
grains, and hindered the formation of cross-slip and jog of the dis-
locations. The action mechanism of Ti on the microstructure and
VN/Co-based composite coatings was illustrated in Fig. 22.
2.6.5. Fe matrix composites
Qin et al. fabricated high Co-Ni secondary hardening steel coat-
ing (mainly containing about 13 wt.% Co, 10 wt.% Ni and 2 wt.% Cr)
on the 18Cr2Ni4WA steel (low alloy hardened steel) by laser depo-
sition method to improve the wear resistance of substrate surface
[113]. The microstructure of high Co-Ni secondary hardening steel
coating was displayed in Fig. 23, mainly consisting of martensite,
lath retained austenite, Fe(Cr, Co, Ni)3 C cementite and fine-scale
(less than 0.1 ␮m in length) M2 C carbides. It was believed that the
enhanced hardness of the laser cladded coating was attributed to
the strong secondary hardening of fine M2 C carbides, solid-solution
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269 255

Fig. 22. Diagram illustration for the action mechanism of Ti on the microstructure of VN alloy/Co-based composite coatings [112].

Fig. 23. Laser cladding high Co-Ni steel coating on 18Cr2Ni4WA steel: (a) cross-section morphology of coating and substrate; (b) and (c) SEM micrograph of coating and
substrate, 1- martensite, 2- retained austenite, 3- M3 C cementite, 4- M2 C carbides; (d) locating pins in airplane repaired using laser cladding technology [113].

strengthening of Co and Ni additions, precipitation hardening of
M3 C cementite, and transformation strengthening of martensite
[113]. Currently, this laser repair technology has been used to the
maintenance of the aircraft parts, as shown in Fig. 1(d).
SLM was used to fabricated 316 L stainless steel (SS) and hydrox-
yapatite (HA) powders mixture with an objective to develop
load-bearing and bioactive implants [114]. To produce the com-
posite, the 316 L SS powders (50 ␮m) were mixed with 5 vol.% HA
particles (5 ␮m) using a bespoke made blender. The microhardness
of 316 L SS/HA composite fabricated using SLM is 241.4 HV, higher
than that of the SS (212.1 HV), and this was due to that 316 L SS/HA
has a finer grain size than that of 316 L SS. Here, the grain refine-
ment was attributed to the role of HA particles as nuclei to facilitate
heterogeneous nucleation (Fig. 24). Besides, the SS/HA composite
fabricated using SLM exhibited a tensile strength of 95 MPa which
is adequate for load-bearing application and also is not too stiff to
prevent stress shielding [114].
Guan et al. [115] reported the 316 L matrix composite produced
using the polycarbosilane (PCS) -316 L. The sintered grains and
pores of the pure 316 L was presented in Fig. 25 (a). In Fig. 25(b)
and (c), a typical structure with steel matrix grains surrounded
by a network of white precipitates was observed, with various
PCS contents. The microstructure of the composite material is uni-
form, with homogeneously distributed reinforcements of M7 C3
and iron silicides phase, which was generated by in situ reaction
of the metal alloy elements with PCS-derived SiC. The maximum
yield strength (YS), ultimate tensile strength (UTS) values about
526 MPa and 898 MPa are achieved with the addition of 3 wt.% PCS,
which is due to a multiple strengthening effect including solid
solution strengthening, load transfer between matrix and rein-
256 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 24. Typical SEM view of (a) SS/HA and (b) 316 L SS microstructure [114].
Fig. 25. SEM images of the microstructure of (a) 316 L alloy and composites reinforced with (b) 3 wt% PCS. (c) 7 wt% PCS[115].
forcement, grain refinement and grain boundary strengthening
[115].
Some researchers investigated the AM of ceramic-reinforced Fe-
based matrix composites, for example, gas atomized powder blends
of AISI 316 L stainless steel (particle size of 45–60 ␮m) and SiC (par-
ticle size: 25–40 ␮m) in the weight ratio of 95:5 and 80:20 were
used as feedstock material. A defect free and homogeneous com-
posite layer was formed under optimum processing condition. The
microhardness of the clad layer increases to 340 VHN (for 5% SiC
dispersed) and 800 VHN (for 20% SiC dispersed) as compared to
150 VHN of commercially available AISI stainless steel [116]. The
improved hardness and wear resistance are attributed to dispersion
of SiC and precipitations of Cr2 C3 and Fe2 Si in the microstructure.
Furthermore, Li et al. [117] investigated the effect of NbC content
on the microstructure and wear resistance of Fe-based composite
coatings. It was found that ␣-(Fe, Cr), (Fe, Cr)7 C3 , NbC existed in all
coatings. NbC particles formed by the chemical reaction of Nb and C
dissolved in the molten pool. With the increase of NbC content, both
the size and the amount of NbC increased obviously, and the particle
morphology transformed from quadrangle to the petaloid shape
gradually. Moreover, with the increase of NbC content, the average
micro-hardness increased from 819.3 HV0.2 (5 wt.%) to 900.5 HV0.2
(20 wt.%).
Multiple carbides reinforced Fe-based surface composite coat-
ings were fabricated successfully by laser cladding a precursor
mixture of graphite, ferrotitanium (Fe-Ti30) and ferromolybdenum
(Fe-Mo70) powders [118]. (Ti, Mo) C multiple carbides showing
an fcc crystalline structure, were in situ formed in the coating
with flower-like dendrites or cubic shape, and they were homo-
geneously distributed in the matrix. Furthermore, the fabrication
of nanometer Al2 O3 dispersion strengthened Fe-Cr-Mo composite
coatings by crosscurrent CO2 laser on 316 L steel was also reported
[119].
Besides, a novel Fe85Cr4Mo8V2C1 (wt%) wire material was suc-
cessfully applied on a carbon-rich 1.2379 tool steel by a manual
laser cladding process [120]. A fine, homogeneous microstructure
composed of martensite, austenite as well as VC- and Mo2 C-type
carbides was formed. The generated FeCrMoVC coatings were uni-
form and crack-free exhibiting an increased microhardness (from
627 HV0.1–829 HV0.1) and an enhanced abrasive wear resistance
compared to the substrate material.
The surfaces of AISI 5115 steel samples were successfully alloyed
using FeCrC powder and the plasma transferred arc (PTA) cladding
method [121]. The highest hardness was ∼886 HV in the alloying
zone, compared to the hardness in substrate material (192 HV). The
increase in hardness was explained by the presence of hard phases,
such as the martensitic phase, Cr7 C3 , Fe23 C6 and iron carbides in
the microstructure.
In short conclusion, for AM of Fe matrix composites, a great deal
of research work focused on how to design the feedstock materials
and choose a suitable processing method, in order to promote the
formation of high-hardness carbides within the Fe-matrix compos-
ite coatings.
2.7. Laser cladding amorphous coatings
Amorphous materials have been a hot topic owing to the excel-
lent mechanical, electrical and magnetic properties. It is propitious
to the formation of amorphous phases due to the high heating and
cooling rates during laser cladding. With regard to some certain
cladding materials with better glass forming ability (GFA), amor-
phous phases are easier to form in the cladding coatings [122]. Up
to now, amorphous alloys such as Ni-Fe-B-Si-Nb, Fe-Co-B-Si-Nb,
Fe-Cr-Mo-Y-B-C and Co-Fe-based amorphous phases, have been
obtained in laser cladding coatings on steels [123–125]. Al-Ni-Y
and Fe-Si-B amorphous alloys were also fabricated by laser cladding
on Ti-6Al-4 V alloy for the improvement in wear resistance of the
coatings [126,127].
Iron-based amorphous materials, owing to their high hardness,
elastic modulus, wear resistance, and corrosion resistance, can be
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
potential materials for surface modification and engineering of
many structural alloys. A novel functional coating was synthe-
sized via laser cladding of an iron-based (Fe48 Cr15 Mo14 Y2 C15 B)
amorphous precursor powder on AISI 4130 steel substrate. The
formed composite coating consisted of Fe-based nano-crystalline
dendrites and amorphous matrix [128]. The formation of the
amorphous/nanocrystalline phases were due to the action of the
sufficiently rapid heating and cooling of the laser technique and a
number of elements with short atomic radius, such as B, C and N
[128]. Additionally, Fe-Co-B-Si-Nb amorphous composite coating
was fabricated by high power diode laser cladding, and both dilu-
tion ratio and scanning speed are the two decisive factors for the
fabrication of amorphous coatings [129].
Shu et al. successfully synthesized an amorphous coating on
Q235 steel (low carbon steel) by laser cladding Co-based self-fluxed
alloy powder [130]. The size of the preplaced alloy powder was
100–250 ␮m. Near the interface a dendrite zone was formed, with
the thickness of only 10 ␮m, and an amorphous layer with the thick-
ness of approximately 400 ␮m appeared over the distance of 10 ␮m
from the interface. In this coating layer, though the XRD peaks
associated with (Co, Fe) solid solution was identified, the volume
fraction of amorphous phase was up to 85.1%.
Amorphous-nanocrystals reinforced coating could be formed on
TA2 alloy by laser cladding of Fe3 Al-B4 C-TiN mixed powders. The
TiB2 nanocrystals were produced through the in situ metallurgi-
cal reaction, which blocked the motion of dislocation [131]. In the
meantime, the Al3 Ti + TiB2 /(Ni coated WC) laser clad coating on the
Ti-6Al-4 V alloy can increase microhardness and wear resistance of
the substrate. With addition of Al2 O3 /nano-Y2 O3 , the SiO2 -Al2 O3 -
Y2 O3 system and the Al-Ni-Y amorphous alloys were produced,
which were beneficial to the wear resistance. Furthermore, the
M6 C (Ni2 W4 C) content in the coating decreased due to the action of
Al2 O3 /nano-Y2 O3 , and the finer microstructure was obtained [126].
The corresponding microhardness of the Al2 O3 /nano-Y2 O3 added
coating was increased to 1300–1400 HV0.2 . It will be a trend for
laser cladding amorphous coatings on titanium alloys.
Zhang et al. reported the preparation of Zr55 Cu30 Al10 Ni5 bulk
metallic glasses (BMGs) using laser solid forming (LSF) process
from the plasma rotating electrode process (PREP) powder [132].
The as-prepared powders were composed of amorphous phase and
Al5 Ni3 Zr2 -type phase. The Zr55 Cu30 Al10 Ni5 deposit with five layers
fabricated by the finest powder with the size range of 53–75 ␮m
exhibited a large volume fraction of amorphous phase (78.7 vol.%).
The residual Al5 Ni3 Zr2 type phase could be observed in remelted
zone only if the powder size was larger than 106 ␮m. The volume
fraction of crystallization in the deposit increased with the increase
in powder size.
2.8. Polymeric materials
Polymers and reinforced plastics are used in a variety of load
bearing applications, from household goods to aerospace products.
These materials are lightweight, strong and relatively inexpensive,
but difficult to create intricate geometries. However, the develop-
ment of AM has made it easier to produce reinforced plastics in
complex geometries.
Pure polymers are no longer able to meet the increasing strength
requirements, so additives are incorporated into the polymer to
enhance the strength of the polymer. For example, the use of poly
vinyl alcohol (PVA) and exploded nanodiamond (DND) dispersions
as a new type of ink for 3D printing was reported [133]. Poly
vinyl alcohol (PVA) solution was added to detonation nanodiamond
(DND) dispersions in order to obtain aqueous PVA-DND dispersions
with a final concentration of 10%w/w of PVA and of 0.1, 0.5, 1 and 5%
w/w of DND with respect to PVA. The results showed that the mean
indentation modulus was improved by 22%, 44% and 200%, respec-
257
Fig. 26. Scheme of the printing process for carbon fiber reinforced PLA composites
[135,136].
tively. The melting temperature (Tm ) and degree of the crystallinity
(␹c ) changed with the DND concentration, and the addiction of
DND in PVA matrix produced an enhancement of the structural
and thermal properties [133].
Besides, Torrado et al. evaluated the effect of additives on
the anisotropy observed in the mechanical properties of tensile
test specimens printed from acrylonitrile butadiene styrene (ABS)
based material systems [134]. In this study, a total of six ABS-based
polymer matrix composites and four polymer blends were cre-
ated and evaluated. The maximum ultimate tensile stress (UTS),
32.9 MPa, corresponded to the ABS/TiO2 composite. Additionally,
a ternary blend of ABS combined with styrene ethylene butadi-
ene styrene and ultra high molecular weight polyethylene lowered
the mechanical property anisotropy in terms of relative UTS to a
difference of 22 as compared to 47 for samples printed from ABS
[134].
Carbon fiber-reinforced polymer has been studied systemati-
cally [135-137]. Rapid fabrication of carbon fiber reinforced PLA
composites has been realized by using continuous carbon fiber
as reinforcement phase and plastics as matrix (Fig. 26). Temper-
ature and pressure are critical parameters to the forming process.
Impregnation of plastics into the fiber bundle could be achieved
when the temperature of liquefier was in the range of 200–240 ◦ C.
With the optimized process parameters, 3D printed composites
with a fiber content of 27% could achieve the maximum flexu-
ral strength of 335 MPa and flexural modulus of 30 GPa, and they
should have further potential application as light structures in the
fields of aviation and aerospace [135].
An important part of modern established implants and stem
cell-based tissue is the generation of feature that has a close
naturalness. Based on Danilevicius’s report, the pre-polymer
were photosensitized by adding 1–3 wt.% of thioxanthen-9-one
or 2-Benzyl-dimethylamino-1-butanone-1 photoinitiators. Poly
DiMethyl Siloxane thermo elastomer was used for producing trans-
parent mask for UV micromolding, in which it was mixed with
matched curing agent using weight ratio 10:1. As shown in Fig. 27,
An example could be a chain-mail structure consisting of inter-
twined rings which are not directly connected to each other. Such
a scaffold could be used for skin tissue engineering, providing great
flexibility and mechanical strength [138].
2.9. Ceramics
AM of ceramic components was widely investigated in the
past decade due to the requirement of high-performance ceramic
258 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 27. Chain-mail structure consisting of joint rings hanging on supporting walls,
showing possibility to fabricate flexible scaffolds [138].
components with complex structure, which is difficult and even
impossible to produce by traditional methods. The main challenge
in the laser fabrication of ceramic parts is the intrinsic brittleness
of ceramic during the process. So unlike laser metal deposition,
suitable processing parameters for direct ceramic fabrication are
extremely limited [139].
Concerning the AM of ceramics, a great deal of research work
focused on Al2 O3 or Al2 O3 -ZrO2 system ceramics. Yves-Christian
et al. [140] investigated the processing parameters for forming
Al2 O3 –ZrO2 by SLM. Dry mixed ceramic powder ratio of 58.5 wt.%
Al2 O3 and 41.5 wt.% ZrO2 was selected as the raw material. The
ZrO2 includes 6 wt.% Y2 O3 for partly stabilization of the ZrO2 at
room temperature. But it was difficult to find the optimal process-
ing parameters to eliminate cracks under general conditions, and
therefore the preheating of the ceramic to a temperature of at least
1600 ◦ C was needed during the fabricating process. Shishkovsky
et al. [141] synthesized ceramics by SLM with another composition
of ZrO2 and Al2 O3 powders. The powder mixture was prepared from
YSZ (ZrO2 90 wt.%, Y2 O3 10 wt.%) and Al2 O3 in the ratio of 4:1. In
order to minimize shrinkage and eliminate cracking and delaminat-
ing, a narrow process parameter window was merely determined
for layer-by-layer laser melting.
An approach by Wilkes et al. [142] produced net-shaped parts
with flexural strengths of above 500 MPa. They used a eutectic mix-
ture of pure alumina (Al2 O3 ) and zirconia (ZrO2 ) with the ratio of
58.5 wt.% Al2 O3 and 41.5 wt.% ZrO2 (Stabilized by 3 mol% of Y2 O3 ),
which were completely molten, while crack formation was pre-
vented by high temperature (1715 ◦ C) CO2 laser preheating. The
Fig. 28. (a) FESEM image of the dry mixed alumina/zirconia powder. (b) Phase diagram of the alumina and zirconia system [142].
Fig. 29. SEM micrographs showing the dispersion of CaF2 spheres in the inter-plate
regions of the laser clad Al2 O3 –30%CaF2 ceramic matrix composite coating [145].
eutectic material ratio exhibits a rather lower melting temperature
of 1860 ◦ C, compared to the single phases (Fig. 28). Applications of
this technology comprise high-tech engineering ceramics, exploit-
ing the possibilities of fabricating complex geometries for the
medical, automotive or aerospace sectors [143].
Liu et al. [144] manufactured Al2 O3 /ZrO2 eutectic ceramic sam-
ples with suppressed cracks by adopting assistant heating laser 3D
printing. The powders of 58.5 wt.% Al2 O3 and 41.5 wt.% ZrO2 (Sta-
bilized by 8 wt.% of Y2 O3 ) compositions with the sizes of 150 ␮m
and spherical shapes were used as raw materials. The laser power
was 200 W to 500 W with a scanning velocity of 50–300 ␮m/s. Once
again, the preheating temperature of 1000 ◦ C was needed to pre-
vent the cracks. The laser beam was directed to the substrate to
create a molten pool into which the eutectic powders were injected
through the powder feed nozzle. The eutectic microstructure of
the clad layer exhibits complex regular characteristics. The aver-
age hardness and fracture toughness are 16.7 GPa and 4.5 MPa m1/2 ,
respectively. Formation of the typical solidification defect, shrink-
age porosity, can be significantly suppressed by adopting a scanning
rate smaller than 100 ␮m s−1 and a laser power larger than 400 W.
Wang et al. [145] fabricated self-lubrication wear-resistant
ceramic matrix composite coatings on substrates of Al2 O3 by laser
cladding CaF2 –30%Al2 O3 mixed powder blends. The laser clad
CaF2 /Al2 O3 composite coatings have a unique microstructure con-
sisting of plate-like framework of Al2 O3 primary phase and isolated
spherical CaF2 solid lubrication particles uniformly dispersed in
the inter-framework regions (Fig. 29). Compared with laser clad
monolithic Al2 O3 coatings, the CaF2 /Al2 O3 coating exhibits much
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 30. BEIs of different gradient layers. (a) 40% SiC; (b) 60% SiC; (c) 70% SiC [146].
superior wear resistance and noticeably lower friction coefficient
under dry sliding wear test conditions.
Recently an attempt was also made to fabricate Ti3 SiC2 -or-SiC-
containing ceramic matrix composites by in-situ reaction laser
cladding technique using Ti and SiC powders [146]. The parti-
cle size of spherical Ti powder and irregular SiC powder was
approximately 50–100 ␮m and 30–60 ␮m, respectively. When
the SiC volume was 40%, the microstructure (Fig. 30 (a)) of
the deposited layer was mainly composed of Ti5 Si4 , TiSi2 and
Ti3 SiC2 phases as well as Ti5 Si3 Cx . The main reaction products
in those gradient layers from 50%SiC to 80%SiC are almost iden-
tical, composed of TiC, TiSi2 and Ti3 SiC2 and SiC (Fig. 30 (b)
and (c)). From the thermodynamical viewpoint the following
chemical reactions can occur spontaneously, with the forma-
tion of TiC and titanium silicides: Ti(l)+SiC(s) = TiC(s)+Si(s);
5/3Ti(l)+Si(s) = 1/3Ti5 Si3 ; 1/2Ti(l)+Si(s) = 1/2TiSi2 (s). Additionally,
the reaction product of Ti3 SiC2 can also be achieved by the fol-
lowing reaction: Ti + Si+2TiC = Ti3 SiC2 [147]. It should be pointed
out that the ternary Ti3 SiC2 phase, due to its hexagonal crystal
structure which is formed by Si atom layer linked to octahedral
TiC, exhibits a Young’s modulus of 326 GPa and a low Vickers
hardness of 4–6 GPa [148,149], and it shows fracture toughness of
6.0–7.9 MPa m1/2 [150,151]. The mechanical properties of Ti3 SiC2
are somewhat similar to those of ductile metals and therefore it is
thought as a damage-tolerant material or “ductile” ceramic. Fur-
thermore, when the added SiC volume was increased from 50% to
80%, the volume content of the residual SiC within the clad lay-
ers was increased from 7.4% to 24.8%. The residual SiC, and all of
these reaction products exhibit high melting point, and they can be
thought as refractory ceramic matrix composites.
The in-situ reactions not only caused fine grains of the reac-
tion products, but also improved the fluidility of ceramic particles
during the laser cladding process [146]. Additionally, fine reaction
products by the laser cladding were also observed in the Nb-SiC
reaction system [152].
Fig. 31. Microstructure of SiC + Si laser clad coating. (a) Cross-section of a strip obtained by using SiC + Si powder mixture as raw material. (b) Detail of the SiC/Si composite
coating (the circle is a SiC grain) [153].
259
Lusquiños et al. [153] explored the potential of laser cladding
to repair silicon infiltrated silicon carbide ceramics by applying a
layer of SiC particles reinforced Si composite. The SiC + Si mixture
caused the formation of sound coatings without substrate dam-
age. The coatings showed homogeneous and continuous interfaces
without defects of cracks, porosities or inclusions. In the coatings,
the production of silicon carbides was surrounded by a metallic
silicon matrix (Fig. 31). According to the nanoidentation tests, the
Young Modulus (480 GPa) and the hardness (42 GPa) of SiC grains
obtained are slightly higher than the values reported in the hand-
book, and this is due to the rapid solidification of the laser assisted
process. But the mechanical properties of the laser cladded SiC + Si
composite coating are not reported in this reference.
2.10. Gradient materials
The concept of functionally graded materials (FGMs) was first
proposed in 1987 to develop heat-resistant materials for the
propulsion system and airframe of space planes [154]. Since then,
lots of research has been conducted to develop FGMs for various
applications by using gradients in physical, chemical, biochemical,
and mechanical properties [155,156]. Furthermore, much attention
has been paid to the fabrication of FGMs by AM technology due to
its series of advantages, and the AMed FGM systems include Ti-Co,
different Ti alloys, Ti-TiAl, Ti-TiC, Ni-TiC, Ti-SiC, etc.
Attempts have been made to fabricate Co layers on the surface
of Ti-6Al-4 V substrate with a compositionally graded interface by
direct laser cladding [157]. Elemental powders of Ti (particle size
2–5 ␮m) and Co (particle size 5–8 ␮m) at different weight ratio
were mixed in a ball mill to form precursors. The powder blend was
prepared by dispersing the powder mixture in alcohol with organic
binder, and it was pre-placed on the substrate by spraying with a
thickness of 250 ␮m. The precursors powder composition of the 5
gradient layers varied from 90 wt.% Ti + 10 wt.% Co (on Ti-6Al-4 V
substrate) to 10 wt.% Ti + 90 wt.% Co prior to the final layer of 100%
260 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 32. Optical micrograph of the compositionally Ti-Co system graded interface
[157].
Co. The interfaces between the successive layers are well adherent
and continuous in nature (Fig. 32). Furthermore, the microstructure
is highly refined and they grow in columnar and dendritic fashion
in the direction opposite to the direction of heat flow. The XRD
analysis results identified the formation of Ti2 Co, CoTi and Co2 Ti
Fig. 33. Macro-surface of the LMD Ti/TiAl SGM component (a). Microstructure of the as-deposited Ti-43Al-1.8V-0.8Cr (b). TEM BF of Ti-43Al-1.8V-0.8Cr (c). Ti-30Al-1.4V-0.5Cr
(d). Ti-17Al-V-1.8Zr-Mo (e), and Ti-6.5Al-V-2Zr-Mo (f) [159].
intermetallics, and the volume fraction of individual phase varied
with the depth from the Co-clad zone. A significant improvement
in microhardness (600–900 VHN) was achieved at the interfacial
region, and the graded interface possessed a superior biocompati-
bility to that of Ti-6Al-4 V sample [157].
Graded structural material of Ti-6Al-4 V/Ti-6.5Al-3.5Mo-1.5Zr-
0.3Si was designed and fabricated by laser melting deposition
method, and it exhibited good tensile properties and good metallur-
gical bonding in the gradient zone [158]. But in this graded structure
the compositions of the two titanium alloys are close to each other.
Further, Ti/TiAl structural gradient material was studied by LMD
manufacturing process from the raw materials of spherical pow-
ders of Ti-47Al-2.5V-Cr and Ti-6Al-2Zr-Mo-1V [159]. The purpose
of this research was to provide new candidate aero-engine turbine
blades and turbine disc materials. But in this material combination a
great difference existed in the compositions and mechanical prop-
erties. Fully lamellar (FL) microstructure consisted of ␥-TiAl and
␣2 –Ti3 Al was formed on the Ti-47Al-2.5V-Cr side, while coarse bas-
ket weave microstructure on the Ti-6Al-2Zr-Mo-1 V side (Fig. 33).
No cracking was found in the gradient zone after aging at 800 ◦ C
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 34. Gradient composite coating of cross section (a). Morphology of WC particles in wear-resisting layer (b), and interlayer II (c) [160].
for 48 h. The room temperature tensile strength of the Ti/TiAl FGM
specimen is up to approximately 1198.8 MPa in the longitudinal
direction, but the fracture surface exhibits brittle characteristics
and the ultimate tensile elongation on both directions is only 0.4%.
To improve the wear resistance and hardness of the 20CrMnTi
low carbon alloy steel, a gradient composite coating was manu-
factured by laser cladding Co50 alloy with addition of different
percents of Ni/WC powders (0 wt.%, 3 wt.%, 5 wt.%, and 10 wt.%)
from bonding layer to wear resistance layer [160], as shown in
Fig. 34. The gradient composite coatings mainly consist of ␥-Co,
M23 C6 and Co3 B. The interlayer and wear resistance layer also con-
tain the WC and W2 C phases. As shown in Fig. 34(b, c), WC particles
are embedded in the Co50 matrix. It is clear that the edges of the
WC particles have been molten partially during the laser cladding.
The epitaxial growth of needle-like dendrites can realize disper-
sion strengthening of the coating on the edge of the WC particles,
and they also reveal a gradient transition from the Co50 matrix to
the WC particles. It is believed that this structure is favorable to
inhibiting the formation of the cracks within the coatings. In fact,
the hardness of gradient composites coating is about 3 times as
much as that of the 20CrMnTi substrate, and the wear resistance of
the gradient composite coating has been enhanced by 36.4 times
as compared with that of 20CrMnTi [160].
Liu et al. fabricated the defect-free functionally graded Ti6Al4V-
TiC composites with 0 to 40 vol.% TiC via laser direct deposition
using the raw materials of spherical Ti64 powders and irregularly
shaped TiC particles [161]. Furthermore, in this work, the melt-
ing degree of TiC reinforcements could be controlled by properly
adjusting the deposition conditions and the particle size of the TiC
reinforcements. That is, 90–150 ␮m TiC particulates were used for
the least melting control of embedded TiC, while 45 ␮m TiC par-
ticles were used for the most melting control of TiC. The results
showed that, it was difficult to avoid the formation of dendritic
carbides when the premixed TiC is larger than 15 vol.%. By proper
controlling the input laser energy density, the Ti6Al4V-TiC com-
posites with 5–15% vol.% TiC were free from dendritic carbides. The
primary strengthening mechanism for composites with the most
control of TiC was the solid solution strengthening induced by car-
261
bon, while that for the least melting control was dominated by the
unmelted TiC particulates and the refined microstructure resulting
from the resolidified carbides [161].
Crack-free functionally graded TiC/Ti composite materials were
fabricated by laser engineered net shaping using TiC and Ti powder,
with compositions changing from pure Ti to approximately 95 vol.%
TiC [162]. In comparison to homogeneous composite deposits of
high TiC contents, the FGM fabrication effectively prevented the
crack formation.
Direct laser fabrication (DLF) has been used to deposit Ni/TiC
FGMs with compositions changing from pure Ni to Ni plus TiC
90 vol.% on a low carbon steel substrate. Nickel, titanium and car-
bon powders with the size from 74 ␮m to 178 ␮m in diameter
were used as deposition reactants. TiC particles were produced by
in-situ reaction of titanium and graphite during the laser deposi-
tion, rather than TiC particles being directly injected into the laser
melted pool. Naturally the micro-hardness exhibited a gradient,
with the maximum value of 2350 HV0.3 [163,164].
Ti/SiC system gradient materials were designed and a FGM sam-
ple with the composition changing from TC4 substrate to 90%SiC,
was successfully fabricated by in-situ reaction laser cladding tech-
nique using Ti and SiC powder [146], with a planar size of
18 mm × 10 mm and the total thickness of 1.5 mm (Fig. 35). The par-
ticle size of the used powders was 50–100 ␮m for Ti and 30–60 ␮m
for SiC. It was noticeable that some residual SiC particles were
remained in the gradient layers with SiC volume of no less than 50%
(Fig. 35), and the volume content of the residual SiC within the clad
layers was increased from 7.4% to 24.8% when the added SiC volume
was increased from 50% to 80%. The in-situ reactions also improved
the fluidility of ceramic particles during the laser cladding process.
This work verified the feasibility of fabricating light-weight heat-
resistant metal/ceramic gradient materials by in-situ reaction laser
cladding technique.
In Chung’s report, selective laser sintering technique was inves-
tigated on blends of Nylon-11 with different volume fractions
of silica nanoparticles (2%–10%). Finally, two component designs
exhibiting a one-dimensional polymer nanocomposite material
gradient were fabricated (Fig. 36) [165].
262 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 35. Cross-section gradient microstructure of Ti/SiC bulk FGM sample [146].
Fig. 36. Schematic description, and fabricated part of rotator cuff scaffold [165].
2.11. Biomaterials
SLM allows production complex 3D component directly from
CAD data by selectively melting successive layers of metal powder
on top of the previous one, using thermal energy supplied by a
laser beam [166,167], and this technology could be very suitable
for biomedical applications due to its ability to fabricate complex
shapes of custom-designed functional implants or prostheses made
from biocompatible metals [168,169].
The as-built Ti-6Al-7Nb (wt.%) alloy by SLM has layered
microstructure with thin plates of ␣’ martensite hardened by
evenly distributed dispersive phase, likely ␤-AlNbTi2 , which results
in higher tensile and compressive strengths, but lower ducility in
comparison to those of an alloy manufactured by conventional
methods [170]. Furthermore, the layered microstructure of the
material gives it a significant anisotropy of Young’s modulus, mod-
erate anisotropy of mechanical properties, but strong anisotropy of
sensitivity to the build porosity.
Zhang et al. [171] manufactured components using SLM from
a novel biomedical beta Ti-24Nb-4Zr-8Sn alloy [172,173]. Near
full density parts (> 99%) have been obtained at a laser power
of 200 W and with a scan speed range of 300–600 mm s−1 . Com-
pared with material prepared by conventional processing routes,
SLM processing produces samples with similar mechanical proper-
ties but without pronounced super elastic deformation due to the
high oxygen of the starting powder. For the near fully dense sam-
ple at 550 mms−1 the powders have completely melted/resolidified
and there is no apparent porosity in the microstructure (Fig. 37 (a)),
and elongated dimple features are clearly visible on the fracture
surface (Fig. 37 (b)). Furthermore, an example of an acetabular hip
cup complete with complex outer scaffold has been manufactured
(Fig. 37(c)).
Porous titanium scaffolds for biomedical application could be
fabricated with TiH2 -Ti blended powder system by SLM. It is
believed that, porous Ti scaffolds could circumvent the issue of
mechanical mismatch between the bulk titanium implants (espe-
cially, stiffness and elastic modulus) and natural bones, and the
pores could offer a preferable environment for bone ingrowth and
thus achieve a tight fixation between the implant and surround-
ing bone [174–176]. A high porosity of ∼70% with pore size in a
range from 200 ␮m to 500 ␮m was obtained at a laser power of
1000 W and a scan speed of 0.02 m/s with 40 wt.% Ti [177]. Further-
more, the strong diffraction peaks of Ti and weak diffraction peaks
of TiO2 were detected in the XRD spectrum of the porous struc-
ture. The generation of TiO2 result from oxidation of a minority of
Ti [177]. However, the TiH2 peaks were absent, indicating that TiH2
had been completely decomposed.
Some attempts have also been made for the AM of Co-Cr-Mo bio-
materials [178–181], for example, Sun et al. [178] studied the phase
and grain size inhomogeneity and their influence on creep behav-
ior of Co-Cr-Mo alloy manufactured by EBM. The results showed
that although constituent phase varied along the build direction
in the as-EBM-built rod (Fig. 38), from a single ␧-hcp phase in the
bottom to a single ␥-fcc phase in the top, the ␥-fcc phase could be
obtained in a wide range of build height, i.e. ∼40 mm from the top
finishing plane. In the as-EBM-built rod, the ␧-hcp phase in the bot-
tom (i.e. early-built part) exhibited weak texture, while that in the
latter-built part (far from bottom of the rod) tended to exhibit ran-
dom orientation. This can be attributed to the increase of post-build
heating temperature along the build height.
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269 263

Fig. 37. (a) Microstructures of the parts manufactured at laser scan speeds of 550 mm s−1 . (b) The fracture surface of the samples. (c) An example of precise acetabular cup
produced by SLM [171].

Fig. 38. EBSD phase maps (a, c, e) and IPF maps (b, d, f) on longitudinal cross-section of different height of as-EBM-built rod. (a, b) top part. (c, d) center part and (e, f) bottom
part [178].

Additionally, it was reported that microscale poly (␧-
caprolactone) (PCL) and hydroxyapatite nanoparticles (nHA)
composite scaffolds were even fabricated with the average fiber
diameter of 8.85 ␮m by melt electrohydrodynamic printing to
mimic collagen fibers and HA crystals in natural bone [182]. The
microscale composite scaffolds exhibited good biocompatibility
and facilitated cellular proliferation and alignment in vitro.
2.12. High entropy alloys
High entropy alloys (HEAs) were first reported by Yeh et al.
[183]. HEAs are defined as alloys that have at least five principal
elements in equimolar/equiatomic or near equimolar/equiatomic
compositions and the concentration of each element is between
5% and 35%. Due to the unique alloy design, the formation of inter-
metallics or ordered phases is suppressed and solid solution phases
are easily obtained [184–186]. HEAs have superior properties such
as high strength, excellent high-temperature strength, good corro-
sion resistance and good wear resistance. However, it is difficult
to overcome the inherent complexity and high levels of control
required to produce homogeneous bulk alloys industrially using a
conventional casting method. AM which facilitates a high level of
local process control, generates rapid solidification cooling rates,
and enables the production of complex geometries, may be a suit-
able way of utilizing HEAs as engineering materials [187]. The study
on AM of HEAs just began several years ago.
Fujieda et al. [187] first demonstrated the feasibility
to process HEAs by SEBM. Cube-shaped SEBM specimens
(20 mm × 20 mm × 16 mm) were manufactured from gas-atomized
AlCoCrFeNi powders. The SEBM specimens exhibit superior ductil-
ity and lower yield strength than the as-cast specimens, as shown
in Table 2.
Further, IPF maps and phase maps of the cast and the SEBM spec-
imens indicated that the cast specimens showed almost exclusively
B2/BCC phases and nearly no FCC phase (Fig. 39). However the SEBM
specimens exhibited the FCC phase precipitation at grain bound-
aries of the B2/BCC grains. The average grain sizes of the B2/BCC
phases of the cast and SEBM specimens are approximately 300 ␮m
264 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269

Fig. 39. IPF maps and phase maps of the cast and the SEBM specimens of the equiatomic AlCoCrFeNi HEA obtained at the cross-section perpendicular to the build direction
at the top and bottom sections [188].

Fig. 40. EBSD phase map of (a) Al-0.4. (b) Al-0.7, and (c) Al-1.0 arc-melted samples showing fcc (red) and bcc (green) phases. (d) Grain size distributions of the fcc and bcc
phases of the arc-melted samples [189].

Table 2 ent amounts of fcc and bcc phase present in arc-melted samples.
Room temperature compressive properties of the equiatomic AlCoCrFeNi HEA pro-
Al-0.4 contains 99.9%, Al-0.7 97.0%, and Al-1.0 65.3% of fcc phase,
duced by SEBM and casting [187].
respectively. The grain size for Al0.4 CoCrFeNi is larger than 500 ␮m
␧f (%) ␴0.2 (MPa) ␴max (MPa) in diameter, while in Al0.7 CoCrFeNi small equiaxed grains of bcc
Casting 5.6 ± 1.9 1308.3 ± 77.3 1425.0 ± 127.5 appear surrounded by much bigger equiaxed fcc grains (Fig. 39(d)).
SSEBM (0◦ ) 26.4 ± 6.7 1015.0 ± 52.5 1668.3 ± 71.5 The hardness is almost doubled going from Al-0.4 (148 HV) to Al-1.0
SSEBM (90◦ ) 14.5 ± 5.3 944.0 ± 55.4 1447.0 ± 135.8 (278 HV), which is due to the increase of the fraction of bcc phase
in the alloy.
Besides, Chao et al. produced AlxCoCrFeNi (x = 0.3, 0.6 and 0.85)
and 10 ␮m, respectively. The grain refinement by SEBM is assumed HEA claddings by coaxial direct laser deposition (DLD) on a 253 MA
to be related to the rapid solidification cooling rates during the austenitic steel substrate using a mixture of blended elemental
SEBM process. The fraction of the FCC phase in the bottom part powders [190]. The variation of Al content (i.e. x = 0.3, 0.6 and 0.85)
(29.7%) is significantly higher than that of the top part (7.1%). The resulted in different phase constitutions in the HEA claddings, prin-
bottom part of the SEBM specimens was maintained at 950 ◦ C for cipally FCC phase for x = 0.3, mixed FCC + BCC phases for x = 0.6 and
about 13 h during fabrication which promoted the formation of the BCC phase for x = 0.85. The cladding cross-section was composed of
precipitation of the FCC phase at grain boundaries. The hardness coarse columnar grains, mostly enclosed by high angle grain bound-
of the FCC phase is much lower than that of the B2/BCC mixture. aries (HAGBs), and the mean grain size was ∼40.9 ± 3.7, 38.2 ± 3.1
The finer grains and larger amount of FCC phases of the SEBM spec- (FCC grain size) and 32.5 ± 1.5 ␮m for the Al0.3 , Al0.6 and Al0.85
imens contribute to the better ductility and lower yield strength HEA claddings, respectively [190]. Shon et al. also fabricated HEA
compared to the cast specimens [188]. coatings on aluminum substrate for the improvement in corrosion
Ocelik et al. concentrate on the possibilities of AM of high- resistance by laser additive manufacturing [191], using Al, Fe, Co,
entropy clad layers by laser processing [189]. The specimens were Cr, and Ni elemental powders.
designed with the chemical compositions of Alx CoCrFeNi (x values Furthermore, Joseph et al. deeply studied the HEA [192]. This
in molar ratios, x = 0.4, 0.7, and 1.0). In Fig. 40, there are differ- alloy was fabricated by direct laser fabrication and it exhibited
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
Fig. 41. Tensile strength and pitting potential of SEBM specimens under different conditions. (a) Tensile engineering stress-engineering strain curves; (b) Potentiodynamic
polarization curves [193].
significant tension/compression asymmetry in its work harden-
ing rate and ductility. The exceptionally high work hardening in
compression was attributed to profuse mechanical twinning, which
had been exacerbated by a strong texture in the as-cast material.
The crystallographic texture in the build direction shows a strong
<001 > alignment.
Fujieda et al. [193] fabricated Co1.5CrFeNi1.5Ti0.5Mo0.1 HEA
specimens and studied the effect of solution treatment (ST) on
the tensile properties and corrosion resistance (Fig. 41). The SEBM
specimens exhibited superior tensile properties to those of the
corresponding casting specimen. The solution-treated SEBM speci-
mens exhibited both high strength and high pitting potential, which
in combination were superior to the conventional alloys used in
severe corrosion environments. The strength of the SEBM spec-
imens air-cooled (A.C.) by ST was higher than that of the SEBM
specimens water-quenched (W.Q.) by ST. On the other hand, the
elongation was lower than that of the SEBM specimens W.Q. by ST.
It was believed that the finer (10 nm in diameter) ordering phase
(Ni3 Ti) of W.Q. specimen acted as a weaker obstacle to dislocation
motion and stronger resistance to pitting corrosion.
3. Outlook
3.1. Significance of the particles size and size distribution of
powders
A wide range of materials and alloys are considered as “pro-
cessable” for AM [194–196]. The term “processability”, however,
contains several parameters, which affect the additive build pro-
cesses, and the final product properties. Scanning speed, laser
power, powder feed rate are the major parameters used for laser
cladded coating technique, but there are some other parameters
which will affect the quality of clad, i.e. clad direction, preheating,
laser spot dimension, injection angle nozzle distance and percent-
age of clad overlap [197–199].
As a powder-bed AM process, the shape and size of particles
are two crucial factors for the printing process and performance of
the resulting 3DP part [200]. According to Yang et al. [201], irreg-
ular morphology and large particle size range may significantly
reduce the powder’s flowability during the 3D printing process.
Sometimes, finer powders are required to achieve finer microscale
features, better surface finishes, thinner layers and to promote
printability, especially for powder bed printing. However, fine pow-
ders may exhibit a significant aggregation which is principally
determined by van der Waals forces. In a recent review by Vorndran
265
et al. [202], it was found that the smaller-sized particles of ceramic
powders, with dimensions smaller than 5 ␮m, are prone to agglom-
erate, thus forming defects and craters on the surface of the powder
during layer preparation. However, large particles (>90 ␮m) reduce
the maximum layer packing density available in SLM. Furthermore,
it has been realized that the particle size distribution of the powders
has an important effect on their flowability and thermal behavior
as well as the mechanical properties of the manufactured product
[197,200]. Therefore the forming quality in AM can be determined
by particle size, size distribution, surface roughness, and shape
[203]. For example, in the reference [204] particle size gradation
was optimized to obtain both acceptable flowability of the pow-
der material and high-strength 3D-printed glass-ceramic products,
that is, the powder mixed by 60 wt.%, 45–100 ␮m and 40 wt.%,
0–25 ␮m particles presented the satisfactory effect. The flowability
decreased with an increasing proportion of fine particles. Addition-
ally, irregular shapes of single and agglomerated particles naturally
induce poor flowability [205,206].
3.2. Approaches for producing fine microstructures
Generally, the laser 3-D printing often produces fine microstruc-
tures in the laser cladded layer due to the high solidification rate. In
the meantime it has been realized that in-situ reaction during the
laser cladding process [207], addition of refractory particles and
addition of rare earth elements into the raw materials are three
important factors for favoring the formation of finer microstruc-
tures in the resulted parts. In the work of Gu et al. [208], the mixed
titanium and SiC powder particles were also used as raw mate-
rials for SLM, and the as-milled powder also favored the in-situ
formation of TiC/Ti5 Si3 composites. Furthermore, the low energy
from 75 W to 120 W in the SLM process caused the formation of TiC
particles with the size of 500 nm. Additionally, as described previ-
ously, when titanium and graphite particles with the average size
of 2–4 ␮m were mixed with Ni alloy powder, with the process-
ing parameters of 4-15 mms−1 beam scanning speed, 3 mm beam
diameter and 2 kW laser power, Ni alloy composite coating was pro-
duced on a 5CrMnMo steel substrate, in which TiC particles with
nanometer size was formed by in-situ reaction as the reinforcement
[98].
Another research result is noticeable concerning the fabrica-
tion of TiNi/Ti2 Ni matrix composite coatings on Ti6Al4V by laser
cladding the mixtures of NiCrBSi and different contents of TaC
(0–40 wt.%) [209]. The coating without TaC addition was mainly
composed of TiNi/Ti2 Ni as the matrix and TiC/TiB2 /TiB as the rein-
266 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
forcement. The added TaC particles with the uniform size of about
0.5 ␮m was dissolved completely during laser cladding due to the
very high processing temperature, and TaC was in-situ systhesized
again during the subsequent solidification. TaC nucleated first in the
molten pool due to its very higher melting point of about 3880 ◦ C
than those of the three reinforcements. Then TiC, TiB2 and TiB pref-
erentially nucleated and grew on the surfaces of TaC particles. In
this way, the microstructures of the coatings were refined [209].
Incorporation of an appropriate amount of rare earth (RE) in
laser claddings can remarkably prevent those defects of cracks,
pores and inclusions within the coatings by traditional coating
techniques, and the presence of rare earth in laser claddings can
notably enhance tribo-mechanical properties [210–213]. Further-
more, RE atoms with the surface activity, tend to distribute at grain
boundaries and cause a dragging effect on the movement of the
grain boundaries. Besides, the unmelted RE oxides will act as nuclei
and promote the nucleation rate [122,214].
It should be pointed out that the application of electromagnetic
field and vibration in different material preparation process, such
as casting of different metals or alloys, is effective in reforming
the fabricating process and refining the microstructure [215–217].
Besides, there have been some references about applications of
electromagnetic field and vibration in laser treatment of different
materials [218–223]. In general, the external electromagnetic field,
vibration or the two together have an agitation effect on the mate-
rials of molten state so that the diffusion and other physical and
chemical reactions will be abundant. Moreover, the electromag-
netic field can also act as a heat producer (i.e. induction heating),
which is demonstrated beneficial to the wettability between liq-
uid titanium and calcia-stabilized zirconia ceramic [224]. Vibration
is valid in the modification of solidification structure, since when
vibration is applied, heat flow is disturbed and the alignment of
grains is randomized. In addition, growing dendrites may break up,
and the pieces serve as seeds for new grains [225].
Then, incorporating electromagnetic field, vibration or other
assisted measures into laser cladding process should have a high
potential for the improvement in microstructures and properties.
Therefore, some great and even amazing results are expectant
if several factors previously mentioned are together taken into
account in the AM process, and this may directly develop some
new materials with outstanding properties and performance.
3.3. Opportunities for creating new materials by additive
manufacturing
The design of the coatings for metal substrate is important for
different working environment, including high-temperature oxida-
tion [146], wear condition, marine environment [226,227], medical
implant [228], etc. On one hand, undoubtedly, the investigation of
new cladding materials is still highly needed; on the other hand, it
is important to notice that by using gradient coatings, a composi-
tionally graded interface can be obtained with a gradual change in
microstructure instead of sudden change, which is beneficial to the
combination between the coatings and substrate and reduces the
residual stress to some extent due to the buffer effect of the multi-
ple layers [122]. Additionally, up to date, only several examples of
gradient materials as structural component by AM have appeared
[158,159,162]. Therefore, in future not only functional materials
but also structural ones are important developing direction in the
field of FGM AM.
Cooper et al. studied the additive layer manufacture of Inconel
625 metal matrix composites and demonstrated that TiC was the
most promising reinforcement particulate among Al2 O3 , SiC and
TiC ceramics. On this basis the possibility of producing “nano
reinforced composite” using micro-sized TiC particulates as the
reinforcement material was proposed, that is, under the suit-
able processing parameters the ceramic constituents would be
completely dissolved and during the cooling process they would
re-precipitate at a smaller scale [229]. Furthermore, if particulate
reinforcements on such a sufficiently small scale can be achieved,
on the one hand, the interface cracking will be substantially
restricted, and more important, the strengthening effect will be
more significant, because Orowan strengthening should be remark-
ably enhanced, and this may be beneficial to the material properties
[230]. In short, the study and development of ceramic-reinforced
metal matrix composites should be an attractive research direction
in future.
In fact, due to the requirement of high-performance ceramic
components with complex structure, and the fact that the main
difficulty in the laser fabrication of ceramic parts is the intrin-
sic brittleness of ceramic during the process, the study on the
laser fabrication of ceramics especially the ultra-high-temperature
ceramics or ceramic matrix composites is also highly needed in
future.
Besides, as we know, high entropy alloys have superior prop-
erties such as high strength, excellent high-temperature strength,
good corrosion resistance and good wear resistance. Therfore it is
also necessary to deeply study such kind of new materials in near
future [231].
As pointed out by Murr, the concept of AM could be expanded
for fabricating a variety of functional material systems and com-
ponents [232]. Such systems may require several more decades
to fully develop and optimize, but the outcomes could be truly
revolutionary in a manufacturing contex. AM opens completely
new possibilities to design novel classes of materials (architectured
materials, metamaterials) with designed or novel properties and
which cannot be realised with conventional processes [233].
3.4. Further study and wide applications in reconditioning of
damaged components
AM technology can be applied to not only the production of the
material blocks but also the reconditioning of worn components
[234]. The reconditioning of expensive or complicated components
is relatively time-consuming and if the reconditioning components
are selected taking into account their price, specific features of
service environment and also specific features of reconditioning
technology, it is often possible to obtain significant gains in time
and cost and also the quality of the bond [235–237].
So far, it has been recognized that laser cladding should have a
great potential for the repair of damaged components with a num-
ber of materials and thus, meet a great market including airplane
and submarine components, aircraft engines, equipment compo-
nents in oil and gas industry, and even for medicine and health
care [19,238,239]. For example, it is assumed that laser cladding is
a highly promising technology for the reconditioning of damaged
blades of titanium turbines. Qin et al. have fabricated high Co-Ni
secondary hardening steel coating on the low alloy hardened steel
by laser deposition method for the repair of locating pins in airplane
[113]. Reconditioning of damaged high-strength steel landing gear
actuators for aircraft and Ni-based superalloy cases for aero-engine
has been conducted by laser deposition method. The application of
AM in reconditioning of damaged components will be expanded in
future.
The epitaxial growth of single crystal microstructure (CMSX-4)
by laser cladding is undoubtedly an encouraging result [48], and
once again, this should be of great significance for turbine hot sec-
tion repair [240]. Furthermore, as described previously, the laser
cladding of SiC particles reinforced Si composite was successfully
carried out on the silicon-infiltrated SiC ceramics without substrate
damage [153], inferring the great potential of repairing ceramic
components in future. But, on the one hand, how to repair large-
 N. Li et al. / Journal of Materials Science & Technology 35 (2019) 242–269
area defects is still a great challenge. On the other hand, to a certain
ceramic or ceramic composite component to be repaired, it is not
easy to design and fabricated suitable ceramic constituents at the
surface to ensure good metallurgical bonding with the original
ceramic substrate [153,241–247] and better service performance
during the second life period.
3.5. Challenges for deep understanding and applications of the
AMed new materials
The main challenges for material AM in future include the design
of raw materials in order to obtain the desired properties for the
AMed components, the control of the stresses and distortion during
the forming process, the deep understanding of the forming process
and synthesis principle, the reproducibility of the microstructures
and properties of the manufactured materials, the need for decreas-
ing the anisotropy extent [23,24,26,170,248], the prevention of
the defects within the manufactured components as well as the
non-destructive testing for the components and the standard estab-
lishment for the preparation of the AMed materials or the relevant
AMed components. In particular, in the case of non-destructive
testing for the AMed components, in-situ sensors to provide non-
destructive evaluation during the AM process and thus allow for
early detection of flaws/defects, need to be deeply explored.
Considering the possibility of some abnormal phenomena in
metallurgical reactions and the resulted micro-scale and even
nano-scale phase constituents in the AMed new materials using
raw multi-component particles, the computer simulation and pre-
cise prediction of the particle size of the reaction products and the
detailed phase constituents, will become very difficult but in the
meantime extremely necessary. Maybe it will cost long time to
solve this complex problem. But, once this difficulty is overcome
gradually, it will in turn greatly promote the advance of the design
science of AMed materials and even new science in the materials
field.
Finally, with the continuous development and increasing
applications of AMed materials, the database of comprehensive
mechanical properties of the AMed materials and components
should be built [106,110,113,249], and the failure analysis and
prediction of lifecycles for the AMed components will become
extremely important. In conclusion, a series of scientific, techno-
logical and engineering problems remain to be solved in future.
Acknowledgements
This work was financially supported by the National Natural
Science Foundation of China (Grant Nos. 51775525, 51605456 and
51701198).
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