Superalloys 2016 proceedings of the

13th International Symposium on

Superalloys sponsored by the Seven
Springs International Symposium
Committee in cooperation with the High
Temperature Alloys Committee of the
Structural Materials Division of TMS
The 1st Edition Mark C. Hardy
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SUPEMLLOYS
2016
SUPEMLLOYS
2016
Proceedings of the

13th International Symposium

on Superalloys

Sponsored by
the Seven Springs International Symposium Committee in cooperation with the
High Temperature Alloys Committee of the Structural Materials Division of TMS
(The Minerals, Metals & Materials Society) and co-sponsored by ASM International
and IOM 3 (The Institute of Materials, Minerals and Mining)

Held
September 11-15, 2016 at the Seven Springs Mountain Resort,
Seven Springs, Pennsylvania, USA

Edited by
Mark Hardy, Eric Huron, Uwe Glatzel, Brian Griffin, Beth Lewis, Cathie Rae,
Venkat Seetharaman, and Sammy Tin

W l LEY TMS
 Copyright © 2016 by The Minerals, Metals & Materials Society.
All rights reserved.

Published by John Wiley & Sons, Inc., Hoboken, New Jersey.

Published simultaneously in Canada.

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10 9 8 7 6 5 4 3 2 1

W l LEY TIMIS
 TABLE OF CONTENTS
Superalloys 2016
Preface xiii
Dedication xv
Best Paper Award xv/'/'
Committee Members x/'x

Symposium Keynote Address

Innovation through Collaboration 3

S.J. Patel and J.J. deBarbadillo

Session 1: Alloy Development I

Alloys-by-Design: Towards Optimization of Compositions of Nickel-Based Superalloys 15

Roger C. Reed, Alessandro Mottura, and David J. Crudden

CMSX-4® Plus Single Crystal Alloy Development, Characterization and Application Development 25
Jacqueline B. Wahl and Ken Harris

Development of a Low-Density Rhenium-Free Single Crystal Nickel-Based Superalloy by Application of Numerical

Multi-Criteria Optimization Using Thermodynamic Calculations 35
RalfRettig, Kami I Matuszewski, Alexander Müller, HaraldE. Helmer, Nils C. Ritter, and Robert F. Singer

Investigation of Superalloy Composition Space Using High Throughput Thin Film Synthesis and Synchrotron X-Ray
Diffraction 45
L.D. Connor, P.M. Mignanelli, S. Guérin, J.P. Soulié, C. Mormiche, S. Frost, R. Greenhalgh, B.E. Hayden,
and H.J. Stone

Interactive Session A: Alloy Development II

Development of a Low-Cost Third Generation Single Crystal Superalloy DD9 57

J.R. Li, S.Z. Liu,X.G. Wang, Z.X. Shi, andJ.Q. Zhao

Grain Boundary Precipitation Strengthening of Phosphorus-Added Nickel-Iron Base Superalloy 65

Yusaku Hasebe, Koichi Takasawa, Takuya Ohkawa, Eiji Maeda, and Takashi Hatano

Development of New SX Superalloys - Fast Experimental Feedback Versus Thermodynamic Modeling 75

R. Võlkl, E. Fleischmann, R. Rettig, E. Affeldt, and U. Glatzel

Experimental Study of the Binary Ni-Ru-System Using Diffusion Couples Manufactured by Encapsulating Cast 83
Robert Popp, Rainer Võlkl, Thomas Gõhler, and Uwe Glatzel

The Role of Local Chemical Composition for TCP Phase Precipitation in Ni-Base and Co-Base Superalloys 89
T. Hammerschmidt, J. Kofimann, C.H. Zenk, S. Neumeier, M. Gõken, I. Lopez-Galilea, L. Mujica Roncery,
S. Huth, A. Kostka, W. Theisen, and R. Drautz

Precipitation Kinetic Modeling of the New Eta-Phase Ni6AlNb in Ni-Base Superalloys 97

Markus Rath, Erwin Povoden-Karadeniz, and Ernst Kozeschnik

Development of Ni-Cr-Fe-W-Al Superalloy for Advanced Ultra-Supercritical Fossil Power Plants 107
X. C. Hao, M. Q. Ou, T. Liang, C. Xiong, Y. C. Ma, and K. Liu

Development of Low or Zero-Rhenium High-Performance Ni-Base Single Crystal Superalloys for Jet Engine and
Power Generation Applications 115
Kyoko Kawagishi, Tadaharu Yokokawa, Toshiharu Kobayashi, Yutaka Koizumi, Masao Sakamoto,
Michinari Yuyama, Hiroshi Harada, Lkuo Okada, Masaki Taneike, and Hidetaka Oguma

ν
Design of Next Generation Ni-Base Single Crystal Superalloys Containing Ir: Towards 1150 °C Temperature
Capability 123
T. Yokokawa, H. Harada, Y. Mori, K. Kawagishi, Y. Koizumi, T. Kobayashi, M. Yuyama, and S. Suzuki

Sulfur and Minor Element Effects on the Oxidation of Bilayer γ'+ β Bond Coats for Thermal Barrier Coatings on
René N5 131
David J. Jorgensen, Akane Suzuki, Don M. Lipkin, and Tresa M. Pollock

High Temperature Creep of γ'-Containing CoNi-Based Superalloys 141

Michael S. Titus, Luke H. Rettberg, and Tresa M. Pollock

Effects of Si Addition on the High Temperature Strength and Oxidation Behavior of γ'-Bearing Co-Based
Superalloys 149
An-Chou Yeh, L-Ting Ho, Sheng-Chi Wang, and Chia-Fu Cheng

The Effect of Alloying Elements on the High Temperature Oxidation of Solid-Solution Strengthened Ni-Base
Superalloys 159
Dae Won Yun, Y.S. Yoo, H.W. Jeong, and SM. Seo

Effect of Bond Coat and Substrate Chemistry on the Interfacial Degradation of Thermal Barrier Coatings 167
L. T. Wu, R. T. Wu, T. Osada, KL. Lee, Μ. Bai, and P. Xiao

Effect of Re and Ta on Hot Corrosion Resistance of Nickel-Base Single Crystal Superalloys 177
J.X. Chang, D. Wang, G. Zhang, L.H. Lou, and J. Zhang

Session 2: Alloy Development III

Advanced Supersolvus Nickel Powder Disk Alloy DOE: Chemistry, Properties, Phase Formations and Thermal
Stability 189
Andrew Powell, Ken Bain, Andrew Wessman, Daniel Wei, Timothy Hanlon, and David Mourer

Y Phase Instabilities in High Refractory Content γ Y Ni-Base Superalloys 199

Stoichko Antonov, Dieter Lsheim, David N. Seidman, Eugene Sun, Randolph C. Helmink, and Sammy Tin

Development of Nickel-Cobalt Base P/M Superalloys for Disk Applications 209

Y.F. Gu, T. Osada, Τ. Yokokawa, Η. Harada, and J. Fujioka

Superalloys for Advanced Energy Applications: Inconel Alloy 740H - A Case Study on International
Government-Industry-University Collaboration 217
John deBarbadillo, Brian Baker, andXishan Xie

Session 3: Blade Alloy Manufacture

Application and Validation of a Directional Solidification Model and Dendrite Morphology Criterion for Complex,
Single-Crystal Castings 229
J.D. Miller, K.J. Chaput, D.S. Lee, andM.D. Uchic

Innovations in Casting Techniques for Single Crystal Turbine Blades of Superalloys 237
Dexin Ma, Fu Wang, Qiang Wu, Samuel Bogner, and Andreas Bührig-polaczek

The Distribution and Retention of Yttrium and Lanthanum in Cast Single Crystal Superalloys 247
S.P. Leyland, LMEdmonds, S. Lrwin, C.N. Jones, A. Bhowmik, D. Ford, and C.M.F. Rae

Interactive Session B: Alloy & Component Manufacture I

Multiscale Modeling of Heat Treatment Processing for Single-Crystal Ni-Base Superalloys 259
Chen Shen, Akane Suzuki, and Douglas G. Konitzer

vi
Microstructure Instability of Ni-Base Single Crystal Superalloys during Solution Heat Treatment 267
N. D 'Souza, D. Welton, J. Kelleher, G.D. West, Z.H Dong, G. Brewster, and H.B. Dong

Development of Thermal Barrier Coating System Using EQ Coating for Advanced Single Crystal Superalloys 279
Kazuhide Matsumoto, Kyoko Kawagishi, and Hiroshi Harada

Effect of Rejuvenation Heat Treatment and Aging on the Microstructural Evolution in Rene N5 Single Crystal Ni
Base Superalloy Blades 285
Joydeep Pala, Dheepa Srinivasana, and Eric Cheng

The Formation Mechanism, Influencing Factors and Processing Control of Stray Grains in Nickel-Based Single
Crystal Superalloys 293
Yafeng Li, Lin Liu, Taiwen Huang, Dejian Sun, Jun Zhang, and Hengzhi Fu

Resonant Ultrasound Spectroscopy for Defect Detection in Single Crystal Superalloy Castings 303
B.R. Goodlet, L.H. Rettberg, and T.M. Pollock

Investigation of Oxide Bifilms in Investment Cast Superalloy IN100 313

M.A. Kaplan, R.K Guarriello, and G.E. Fuchs

A New Analysis of the Microstructure of Ni-Based Single-Crystal Superalloys: Relevant Topological Parameters
for Efficient Microstructural Modeling 323
M. Degeiter, M. Perrut, B. Appolaire, Y. Le Bouar, and A. Fine I

Single-Crystal Superalloy Joining 333

Akane Suzuki, Jeffrey Schoonover, Chen Shen, and David Wark

Selective Electron Beam Melting of the Single Crystalline Nickel-Base Superalloy CMSX-4®: From Columnar
Grains to a Single Crystal 341
Markus Ramsperger and Carolin Kòrner

Defect Formation and Its Mitigation in Selective Laser Melting of High γ' Ni-Base Superalloys 351
Xiqian Wang, Noriko Read, Luke N. Carter, R. Mark Ward,Moataz andM. Attallah

Developing Processing Parameters for Nickel-Base Superalloys for the Electron Beam Melting Additive
Manufacturing Process 359
Francisco Medina, Michael Kirka, UlfAckelid, and Ryan Dehoff

Parameter Optimization for Electron Beam Melting of IN718 Based on Melt Pool Characterization 367
Xiao Ding, Yuichiro Koizumi, andAkihiko Chiba

Effect of Heat Treatments on the Microstructure and Texture of CM247LC Processed by Selective Laser Melting 375
R. Muñoz-Moreno, V.D. Divya, OM.D.M. Messé, Τ. Lllston, S. Baker, and H.J. Stone

Session 4: Blade Alloy Behavior

Thermal Cycling Creep Resistance of Ni-Based Single Crystal Superalloys 385

Jonathan Cormier

Influence of Crystal Orientation on Cyclic Sliding Friction and Fretting Fatigue Behavior of Single Crystal Ni-Base
Superalloys 395
Balavenkatesh Rengara], Sotaro Baba, andMasakazu Okazaki

Sustained Peak Low-Cycle Fatigue in Single Crystals with Equilibrium γ-γ' Coatings 405
M.A. Lafata, L.H. Rettberg, C. Mercer, and T.M. Pollock

vii
 Session 5: Disk Alloy Manufacture

Heteroepitaxial Recrystallization Observed in René 65™ and Udimet 720™: A New Recrystallization Mechanism
Possibly Occurring in All Low Lattice Mismatch γ-γ' Superalloys 417
Marie-Agathe Charpagne, Thomas Billot, Jean-Michel Franchet, and Nathalie Bozzolo

Systematic Evaluation of Microstructural and Thermo-Mechanical Effects on the As-Forged Condition of Alloy
ATI 718Plus® 427
Ana Casanova, Katja Loehnert, Daniela Huenert, Mark Hardy, and Catherine Rae

Effect of Ingot Size on Microstructure and Properties of the New Advanced AD730™ Superalloy 437
C. Croze t, A. Devaux, R. Forestier, S. Charmond, M. Hue Her, D. Helm, and W. Buchmann

Inhomogeneous Grain Coarsening Behavior in Supersolvus Heat Treated Nickel-Based Superalloy RR1000 447
IM.D. Parr, T.J. Jackson, M.C. Hardy, D.J. Child, C. Argyrakis, K. Severs, V. Saraf, andJ.M. Stumpf

Interactive Session C: Alloy & Component Manufacture II

The Influence of the Starting Grain Size during High-Temperature Grain Boundary Engineering of Ni-Base
Superalloy RR1000 459
Martin Detrois, John Rotella, Robert L. Goetz, Randolph C. Helmink, and Sammy Tin

Evaluation of AD730™ for High Temperature Fastener Applications 469

A. Devaux, W. Li, C. Crozet, and J.M. Lardón

Conventionally Forged RR1000 Billet for Forged Turbine Components 479

Kevin J. Bockenstedt, Christopher M. O 'Brien, Ramesh S. Minisandram, George J. Smith, and David J. Bryant

Deformation Mechanisms and Microstructural Evolution of γ + γ' Duplex Aggregates Generated during
Thermo mechanical Processing of Nickel-Base Superalloys 487
Beijiang Zhang, Guangpu Zhao, Wenyun Zhang, Guohua Xu, and Heyong Qin

Full Field Modeling of the Zener Pinning Phenomenon in a Level Set Framework - Discussion of Classical Limiting
Mean Grain Size Equation 497
B. Scholtes, D. Llin, A. Settefrati, N. Bozzolo, A. Agnoli, andM. Bernacki

Friction Stir Processing of Cast Alloy 718 505

Bharat K. Jasthi, Edward Chen, Brahmanandam Kaligotla, Todd Curtis, Michael West, and Christian Widener

Integrated Process Modeling for the Mechanical Properties Optimization of Direct Aged Alloy 718 Engine Disks 513
Bernd Oberwinkler, Andreas Fischersworring-Bunk, Marco Hüller, and Martin Stockinger

Influence of Carbide Distribution on Ductility of Haynes®282® Forgings 523

C. Joseph, M. Hòrnqvist, R. Brommesson, and C. Persson

An Approach to Microstructure Modelling in Nickel Based Superalloys 531

Aleksey Reshetov, Olga Bylya, Nicola Stefani, Malgorzata Rosochowska, and Paul Blackwell

Mechanical Properties of Cast & Wrought Hybrid Disks 539

Hesser Taboada Michel, Layla Sasaki Reda, Georgia Effgen Santos, Jonathan Cormier, Christian Dumont,
Patrick Villechaise, Philippe Bocher, Damien Texier, Eric Georges, Florent Bridier, Florence Hamon,
and Alexandre Devaux

viii
 Session 6: Disk Alloy Behavior I

Separating the Influence of Environment from Stress Relaxation Effects on Dwell Fatigue Crack Growth in a
Nickel-Base Disk Alloy 551
J. Telesman, T.P. Gabb, and L.J. Ghosn

Microstructural Aspects of Fatigue Crack Initiation and Short Crack Growth in René 88DT 561
Zafir Alam, David Eastman, George Weber, Somnath Ghosh, and Kevin Hemker

Statistical Assessment of Fatigue-Initiating Microstructural Features in a Polycrystalline Disk Alloy 569

William C. Lenthe, Jean-Charles Stinville, McLean P. Echlin, and Tresa M. Pollock

Determination of Orientation and Alloying Effects on Creep Response and Deformation Mechanisms in Single
Crystals of Ni-Base Disk Superalloys 579
T.M. Smith, L. V. Duchao, T. Hanlon, A. Wessman, Y. Wang, and M.J. Mills

Session 7: Alloy & Component Manufacture III

High Temperature Properties of a Single Crystal Superalloy PWA1484 Directly Recycled after Turbine Blade Use 591
Satoshi Utada, Yuichiro Joh, Makoto Osawa, Tadaharu Yokokawa, Toshiharu Kobayashi, Kyoko Kawagishi,
Shinsuke Suzuki, and Hiroshi Harada

Manufacture of Large Ni-Base Ingots and Forgings 601

Nikolaus Blaes, Bernhard Donth, Andreas Diwo, and Dieter Bokelmann

Influence of Hot Working Conditions on Grain Growth Behavior of Alloy 718 609
Chuya Aoki, Tomonori Lleno, and Takehiro Ohno

Microstructure-Sensitive Model for Predicting Surface Residual Stress Relaxation and Redistribution in a P/M
Nickel-Base Superalloy 619
M.E. Burba, D.J. Buchanan, M.J. Catón, R. John, andRA. Brockman

Interactive Session D: Alloy & Component Behavior I

Fatigue Crack Growth Rate Assessment of Superalloys by the EBSD Method 631
D. Kobayashi, T. Takeuchi, andM. Achiwa

Stage I Fatigue Crack Propagation in a Single Crystal and a Directional Solidified Ni-Base Superalloy 639
Motoki Sakaguchi, Ryota Komamura, Yuta Hosaka, and Hirotsugu Lnoue

Anisothermal High-Temperature Cyclic Behavior of a Ni-Based Single Crystal Superalloy 647

Jean-Briac le Graverend, Jonathan Cormier, Franck Gallerneau, Serge Kruch, and José Mendez

Discussing the Effect of Gamma Prime Coarsening on High Temperature Low Stress Creep Deformation with
Respect to the Role of Refractory Elements 655
T. Goehler, C. Schwalbe, J. Svoboda, E. Affeldt, andR.F. Singer

On the Development of ICME Tools for Creep and Aging of CMSX®-8 665
E.A. Estrada Rodas, S. Gorgannejad, R. W. Neu, Z. Dyer, P.M. Draa, and S.R. Shinde

Creep Deformation of a 6th Generation Ni-Base Single Crystal Superalloy at 800 °C and 735 MPa 675
Y. Yuan, K. Kawagishi, Y. Koizumi, T. Kobayashi, T. Yokokawa, and H. Harada

Effect of Hf and Β on Transverse and Longitudinal Creep of a Re-Containing Nickel-Base Bicrystal Superalloy 683
Y.S. Zhao, J. Zhang, Y.S. Luo, G. Sha, D. Ζ. Tang, and Q. Feng

ix
Mechanical Properties and Microstructure Design in Repairing Mar-M 509 Alloy Turbine Components 693
Zengmei Wang Koenigsmann, Ravi Shankar, and Richard Fenton

Evaluation of Temperature and Stress in First Stage High Pressure Turbine Blades of a Directionally-Solidified
Superalloy DZ125 after Service in Aeroengines 701
Y.D. Chen, Y.R. Zheng, C.B. Xiao, and Q. Feng

On the Temperature Dependence of Creep Behavior of Ni-Base Single Crystal Superalloys 711
P. Wollgramm, X. Wu, and G. Eggeler

Microstructure Changes and Oxidation Resistance of Aluminized Ni-Based Single Crystal Superalloys 719
Hideyuki Murakami and Kazuki Kasai

Factors Affecting TBC Furnace Cycle Lifetime: Temperature, Environment, Structure and Composition 727
B.A. Pint, J A. Haynes, M.J. Lance, H.L. Aldridge, Jr., V. Viswanathan, G. Dwivedi, and S. Sampath

Oxidation Coating Life Extension in Gas Turbine Blades during Repair 735
Dheepa Srinivasan, N. Dayananda, Neha Kondekar, Mounika Gandi, and Hariharan Sundaram

Session 8: Blade Alloy Behavior II

High Temperature Creep Damage Mechanisms in a Directionally Solidified Alloy: Impact of Crystallography and
Environment 747
L. Mataveli Suave, J. Cormier, P. Villechaise, D. Bertheau, G. Benoit, F. Mauget, G. Cailletaud, and L. Marcin

Characterization of Tilt and Twist Low Angle Grain Boundaries and Their Effects on Intermediate-Temperature
Creep Deformation Behaviour 757
Yao Wang, Dong Wang, Gong Zhang, Langhong Lou, and Jian Zhang

Crack Initiation and Propagation during Thermal-Mechanical Fatigue of IN792: Effects of Dwell Time 763
Paraskevas Kontis, DavidM. Collins, Sten Johansson, Angus J. Wilkinson, Johan J. Moverare,
and Roger C. Reed

Creep and Oxidation Behaviour of Coated and Uncoated Thin Walled Single Crystal Samples of the Alloy
PWA1484 773
Fabian Krieg, Mike Mosbacher, Markus Fried, Ernst Affeldt, and Uwe Glatzel

Session 9: Disk Alloy Behavior II

ATI718Plus® - New Nickel Based Disc Alloy and Its Capability 783
D. Huenert, M. Proebstle, A. Casanova, R. Schluetter, R. Krakow, M. Buescher, P. Randelzhofer, A. Evans,
K. Loehnert, T. Witulski, S. Neumeier, and C. Rae

Thermal Stability of Cast and Wrought Alloy Rene 65 793

Andrew Wessman, Aude Laurence, Jonathan Cormier, Patrick Villechaise, Thomas Billot,
and Jean-Michel Franchet

Novel Techniques to Assess Environmentally-Assisted Cracking in a Nickel-Based Superalloy 801

André A.N. Németh, David J. Crudden, David M. Collins, David E.J. Armstrong, and Roger C. Reed

Interactive Session E: Alloy & Component Behavior II

Benchmarking Crystal Plasticity Models with Micro tensile Evaluation and 3D Characterization of René 88DT 813
David W. Eastman, Zafir Alam, George Weber, Paul A. Shade, Michael D. Uchic, William C. Lenthe,
Tresa M. Pollock, and Kevin J. Hemker

χ
Characterization and Modeling of Deformation Mechanisms in Ni-Base Superalloy 718 821
D. McAllister, D. Lv, H. Deutchman, B. Peterson, Y. Wang, and M.J. Mills

Dislocations Nucleation and Interaction with Grain Boundaries in a Polycrystalline Nickel Base Superalloy 831
O.M.D.M. Messé and C.M.F. Rae

Effect of Large Plastic Strains and Strain Gradients on Residual Stress Relaxation in Shot Peened IN100 841
Dennis J. Buchanan and Reji John

Relationship between the Microstructure, Low Cycle Fatigue and Creep Properties of a Cast and Wrought Ni-Co
Base Superalloy TMW-4M3 Disk 849
Shinichi Kobayashi, Tomonori Lleno, Takehiro Ohno, and Hiroshi Harada

Probability of Occurrence of Life-Limiting Fatigue Mechanism in P/M Nickel-Based Superalloys 859

S.K Jha, W.J. Porter, M.J. Catón, R. John, D.J. Buchanan, A.H. Rosenberger, andJ.M. Larsen

Influence of Residual Stresses on the Fatigue Life of a Shot-Peened Nickel-Based Single Crystal Superalloy: From
Measurements to Modeling 867
Amélie Morançais, Mathieu Fèvre, Manuel François, Nicolas Guel, Serge Kruch, Pascale Kanouté,
and Arnaud Longuet

Relationships between Microstructural Parameters and Time-Dependent Mechanical Properties of a New Nickel
Based Superalloy AD730™ 877
Louis Thébaud, Patrick Villechaise, Jonathan Cormier, Florence Hamon, Coraline Crozet, Alexandre Devaux,
Jean-Michel Franchet, Anne-Laure Rouffié, andAntoine Organista

A Unified LCF Model for Conventionally Heat Treated Inconel 718 887
Michael D. Marotta and David C. Dudzinski

Effect of Non-Metallic Ceramic Inclusions on Strain Localization during Low Cycle Fatigue of a Polycrystalline
Superalloy 897
Jean-Charles Stinville, Victoria M. Miller, and Tresa M. Pollock

Effects of Oxidation on Fatigue Crack Initiation and Propagation in an Advanced Disk Alloy 907
R. Jiang, N. Gao, Μ. Ward, Ζ. Aslam, J.C. Walker, and P.A.S. Reed

Physics-Based Modeling Tools for Predicting Type II Hot Corrosion in Nickel-Based Superalloys 917
KS. Chan, M.P. Enright, J.P. Moody, and S.H.K. Fitch

Characterization of Grain Boundaries and Associated Minor Phases in Disk Alloy ME3 Exposed at 815 °C 927
Chantal K. Sudbrack, Laura J. Evans, Anita Garg, Daniel E. Perea, and Daniel K. Schreiber

Session 10: Environmental Behavior

Slip Localization and Hydrogen Embrittlement of Alloy 718 939

Zhenbo Zhang, Gideon Obasi, Roberto Morana, and Michael Preuss

Effects of Sea Salt on the Oxidation of CMSX-4® at 1100 °C 949

Η. T. Pang, F. Li, S. Pahlavanyali, L.M. Edmonds, G. Brewster, and C.M.F. Rae

Damage Evolution during Compressive Hold Sustained Peak Low Cycle Fatigue of a Ni-Based Single-Crystal
Superalloy 959
Swapnil Patil, Shenyan Huang, Mallikarjun Karadge, Doug Konitzer, and Akane Suzuki

xi
 Session 11: Co 3 AlW & High Entropy Alloys

The Role of the Base Element in γ' Strengthened Cobalt/Nickel-base Superalloys 971
C.H. Zenk, S. Neumeier, M. Kolb, N. Volz, S. G. Fries, O. Dolotko, I. Povstugar, D. Raabe, andM. Gõken

Alloying Effects on Microstructural Stability and γ' Phase Nano-Hardness in Co-Al-W-Ta-Ti-Base Superalloys 981
H.J. Zhou, W.D. Li, F. Xue, L. Zhang, X.H. Qu, and Q. Feng

Oxide Scale Formation in Novel γ-γ' Cobalt-Based Alloys 991

C.A. Stewart, R.K. Rhein, A. Suzuki, T.M. Pollock, and C.G. Levi

High Temperature Properties of Advanced Directionally-Solidified High Entropy Superalloys 1001

Te-Kang Τ sao, An-Chou Y eh, Jien-Wei Y eh, Mau-Sheng Chiou, Chen-Ming Kuo, H. Murakami,
and Koji Kakehi

Session 12: Additive Layer Manufacture

Inconel 625 by Direct Metal Laser Sintering: Effects of the Process Parameters and Heat Treatments on Microstructure
and Hardness 1013
Giulio Márchese, Massimo Lorusso, Flaviana Calignano, Elisa Paola Ambrosio, Diego Manfredi,
Matteo Pavese, Sara Biamino, Daniele Ugues, and Paolo Fino

A Multi-Scale Multi-physics Approach to Modelling of Additive Manufacturing in Nickel-Based Superalloys 1021

C. Panwisawas, Y. Sovani, M.J. Anderson, R. Turner, N.M. Palumbo, B. C. Saunders, L. Choquet, J. W. Brooks,
and H. C. Basoalto

Integrated Thermal Process Optimization of Alloy 718Plus® for Additive Manufacturing 1031
Jiadong Gong, Hallee Z. Deutchman, Alonso Peralta, Dave Snyder, Michael P. Enright, John McFarland,
James Neumann, Jason Sebastian, and Greg Olson

A Study on the Effects of Substrate Crystallographic Orientation on Microstructural Characteristics of René N5

Processed through Scanning Laser Epitaxy 1041
Amrita Basak and Suman Das

Author Index 1051

Subject Index 1055

xii
 PREFACE
The purpose of the International Symposium on Superalloys, which takes place every four years, is to provide a forum
for researchers, producers, and users to exchange recent technical information regarding the high temperature, high
performance materials that are used in gas turbine engines and related products. The principal goal of the Symposium
is to highlight new initiatives and future growth opportunities for superalloys, recent advances in the understanding
of their behavior, and progress in integrating them into new systems. The first Symposium, held in 1968, emphasized
phase instabilities in superalloys. Since then, the scope of the Symposium has expanded considerably to cover all
aspects of research, development, manufacture, and application of these materials. Over the years, the Symposium
has developed rich traditions, encompassing a high quality peer reviewed publication, which is presented before the
conference, single session presentations, and lively discussions during and after formal sessions, which are facilitated
by the Seven Springs Mountain Resort.

This, the Thirteenth Symposium takes place at a time when superalloy users are striving to improve the efficiency of
power systems to reduce emissions, weight, and operating costs by using alloys that are not just capable of higher
temperatures or stresses, but are produced with lower amounts of scarce or expensive raw materials. There is also an
impetus to develop and validate alloys and products much faster than in earlier times. Increasingly, these aspirations
require computational modeling and simulations of alloy systems and manufacturing processes, and a greater depth
of understanding and modeling of material and component behaviour. Insights into the latter are often improved
substantially using observations and data from new and sophisticated experimental techniques. As demonstrated by
the examples in these proceedings, achieving incremental or step-change improvements in superalloy production,
performance, and affordability necessitates collaborative working between academia, producers, and users in the
superalloy community.

The Keynote Address of this Symposium is from Shailesh Patel and John (Jack) deBarbadillo of Special Metals
Corporation, a division of Precision Castparts Corporation (PCC). Their paper and keynote lecture provide an insight
into innovation from an alloy producer's perspective. They show examples of collaborative working at (PCC),
commenting on the successes and the challenges.

Starting with the Second Symposium in 1972, each Symposium and its corresponding published proceedings have been
dedicated to an individual as a means of honoring his or her contributions to the superalloy industry. The Thirteenth
International Symposium is dedicated to Louis Lherbier, a true pioneer and innovator in our field. Further details of
Lou's career and contributions can be found on the following pages.

Finally, it should be noted that this Symposium would not have been possible without the efforts of the current and past
members of the two committees that serve the International Symposium on Superalloys. The Program Committee for
the Thirteenth Symposium, listed below, was responsible for preparation of the technical program, including critical
review of abstracts and manuscripts for originality, technical content, and pertinence to industry. The entire Organizing
Committee, listed in the frontmatter of this book, devoted considerable effort to organizing all other aspects of the
Symposium.

We would like to also recognize the tremendous work of the TMS staff, particularly Trudi Dunlap, Louise Wallach,
Christina Raabe Eck, Jennifer Booth, and Caron Gavrish, in helping to organize a successful conference.

Mark Hardy
Eric Huron
Uwe Glatzel
Brian Griffin
Beth Lewis
Catherine Rae
Venkat Seetharaman
Sammy Tin

xiii
 DEDICATION

Louis W. Lherbier
The 13th International Symposium on Superalloys is dedicated to Louis W. Lherbier for his
substantial contributions to our field. He has been a pioneer and innovator in the development
and processing of high strength powder metallurgical and cast/wrought superalloys for gas
turbine disk applications

Lou Lherbier's career has spanned 60 years. After graduating from Carnegie Mellon University with a degree in
Metallurgical Engineering, he was initially employed by Universal Cyclops Specialty Steel Corporation (later Cytemp
Specialty Steel) for 35 years. This was followed by 5 years at Dynamet Incorporated and then approximately 20 years
at Carpenter Technology. All of that time was dedicated to specialty alloy technology, including the melting and
processing of alloys ranging from tool steels, stainless steels, and titanium to nickel and cobalt-based Superalloys.
During a large part of his career, his time was dedicated to the manufacturing of these same materials by powder
metallurgy (PM) technology.

As a young metallurgist, Lou's efforts were directed at technology issues on a wide variety of specialty alloys, none
more difficult and perplexing than the segregated structures and poor hot workability of high speed steels. When it
became apparent in the mid 1960s that powder metallurgy technology could solve the segregation and workability
problems in high speed steels, Lou recognized that the same technology could be applied to other materials including
superalloys. Universal Cyclops went on to make the first superalloy IN 100 metal powder for Pratt & Whitney, a
version of which is still used in today's jet engines.

In 1967, Lou became Manager of the R&D Laboratory at Universal Cyclops. He became involved with the development
of melting and processing procedures for manufacturing Alloy 718, to be used in General Electric's first TF39 engines.
Through melting and homogenization practices, Lou and his co-workers succeeded in eliminating black spot indications
(freckles) and Laves phase problems in this alloy. In 1976, he successfully lobbied his employer for the opportunity to
recruit a dedicated group to work exclusively on powder metallurgy technology. He also secured a number of Air Force
contracts dedicated to the development of superalloy powder metallurgy. Lou's group developed the CAP technique
(powder consolidation using atmospheric pressure in glass molds) and demonstrated the manufacture of dual-property
rotating disks by bonding a powder metallurgy hub to a cast blade ring using hot isostatic processing (HIP). The team
demonstrated that extrusion of a HIP'ed billet at an extrusion ratio of 3:1 gave equivalent results to the direct extrusion
of loose powder at an extrusion ratio of 7:1.

XV
These successes used superalloy powder metallurgy technology primarily for military engine disks. Lou saw the
potential future of PM superalloys and convinced his management to install the first large (2000 lb) vacuum melt gas
atomization facility to manufacture superalloy powders. The bright future was dramatically set back when the failure
of an as-HIP'ed disk resulted in a crash at the Farnborough Air Show in 1980. The demand for powder metallurgy
diminished temporarily, and Lou returned to being the R&D Director and later Vice President ofTechnology at Cytemp
Specialty Steel. The highlight ofthis period was the development of fine grain Alloy 718 and the understanding of the
origins of white spots. The industry did eventually develop hot working processes to produce PM components with
improved quality (in part, based on some of Lou's earlier extrude and forge window studies) and today PM parts are
extensively used across the industry in both commercial and military engines.

In 1991, Lou retired from Cytemp Specialty Steel and immediately went to work for Dynamet Incorporated, a titanium
bar and wire manufacturer. Dynamet had just purchased the powder operations from Cytemp. He became Vice President
- Technical Director and led a successful effort to develop processing technology for the alloys Beta C and Ti-6Nb,
while still maintaining a strong interest in powder metallurgy technology. Carpenter Technology purchased Dynamet
in 1997 and Lou remained as Vice President. In 2001, Lou returned full time to powder metallurgy technology as
Director ofMarket Development and Powder Commercialization for Carpenter. He has spent the last 15 years assisting
in the development ofHIP'ed near net shape parts, metal injection molding, and additive manufacturing.

Lou has given presentations throughout the world that emphasize the melting, processing, and structural characteristics
of Superalloys including those made by powder metallurgy technology. He has authored many technical articles as
well as the chapter "Melting" in the book The Superalloys (McGraw Hill, 1987). He has received a number of awards
including ASM International Fellow, the MPIF Distinguished Service Award, the ASM Pittsburgh Chapter Edgar C.
Bain Award, and an award from AVS-VMD for Technical Contributions to the Specialty Metals Industry. He was
honored by the ASM Pittsburgh Chapter by presenting the Pittsburgh Nite Lecture, and the Andrew Carnegie Lecture.
Lou has been part ofthe teams that have won three IRI00 Awards. Lou holds a number of patents involving the design
and processing of tool steels, stainless steels, and Superalloys. Last but not least, through it all, Lou has always been a
welcomed source of advice and knowledge for beginning metallurgists and his peers throughout the industry.

PAST DEDICATEES
1972 - Clarence Bieber

1976 - Falih Damara

1980 - Rudy Thielman

1984 - Gunther Mohling

1988 - Herb Eiselstein

1992 - Carl Lund

1996 - John Radavich

2000 - Wilfred "Red" Couts

2004 - Fred Pettit

2008 - Raymond Decker

2012 - Anthony Giamei

xvi
 BEST PAPER AWARD
The following paper was selected by the Awards Committee ofthe International Symposium on Superalloys
as winner ofthe Best Paper Award for the 13th symposium:

Thermal Cycling Creep Resistance of Ni-Based Single Crystal Superalloys

Jonathan Cormier, ISAE-ENSMA / Institut Pprime

The selection was based on the following criteria: originality, technical content, pertinence to the superalloys
and gas turbine industries and academic community, and clarity and style.

xvii
 Thirteenth International Symposium on Superalloys
COMMITTEE MEMBERS
General Chair Eric Huron

Secretary Tony Banik

Treasurer Gern Maurer

Program Chair Mark Hardy

Program Committee. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. Uwe Glatzel

Brian Griffin

Beth Lewis

Cathie Rae

Venkat Seetharaman

Sammy Tin

Publication Chair Venkat Seetharaman

Arrangements Chair Dave Novotnak

International Publicity Akihiro Sato

Jian Zhang

U. S. Publicity Jacqui Wahl

Student Coordination Michael Mills

Awards Committee Chair Roger Reed

Awards Committee Ken Green

Tresa Pollock

TMS Staff Liaisons Trudi Dunlap

Jennifer Booth

Caron Gavrish

Christina Raabe Eck

Louise Wallach

xix
 Superalloys 2016: Proceedings of the 13th International Symposium on Superalloys
Edited by: Mark Hardy, Eric Huron, Uwe Glatzel, Brian Griffin, Beth Lewis,
Cathie Rae, Venkat Seetharaman, and Sammy Tin
TMS (The Minerals, Metals & Materials Society), 2016

Symposium Keynote Address

 Superalloys 2016: Proceedings of the 13th International Symposium on Superalloys
INNOVATION THROUGH COLLABORATION
S J. Patel and J.J. deBarbadillo
Special Metals Corporation
3200 Riverside Drive, Huntington, WV 25705
Keywords: Superalloys, Gas Turbines, Collaborative R&D
Abstract
The history of superalloys and their enabling role in aircraft
propulsion has been a remarkable saga of technical innovation and
collaboration in a never ending quest for improved performance
and economy. This has been achieved in an environment of fierce
competition between Original Equipment Manufacturers (OEM's)
and between their material suppliers. Through the years, notable
collaborative activities have occurred involving companies,
government laboratories and agencies and universities. The
industrial and political environment and its influence on
collaboration have evolved from the inception of the technology
in WW II through the cold war era to the current era with the
spread of technology throughout the world. This paper reviews
this history through a modern perspective and uses examples to
point to the future of collaborative innovation.
Introduction
The conception of age-hardened nickel-chromium alloys is
attributed to Merica in the US and Chevenard in France in the late
1920's, but a strong commercial need for the materials did not
exist at that time. The real start of the superalloy age began in the
UK with the Whittle gas turbine engine. Sir Frank Whittle, shown
with his demonstration WU engine in Figure 1, realized that the
stainless steel blades that he initially employed were not
sufficiently durable to sustain practical flight missions.
Figure 1. Sir Frank Whittle with a bench scale model of his gas
turbine engine (Google Images).
In 1940 Whittle wrote to Leonard Pfeil, Research Director at the
Mond Nickel Company (later Inco), requesting that he develop a
superior alloy meeting 800°C tensile and creep requirements. Pfeil
improved the creep strength of an existing Ni-Cr alloy by adding
sufficient Al and Ti to enable γ' formation. He thereby created the
first superalloy, later designated NIMONIC® alloy 80 [1, 2], This
alloy was used in Whittle's second flying engine in 1942.
©NIMONIC and INCONEL are trademarks of Special Metals.
3
Edited by: Mark Hardy, Eric Huron, Uwe Glatzel, Brian Griffin, Beth Lewis,
Cathie Rae, Venkat Seetharaman, and Sammy Tin
TMS (The Minerals, Metals & Materials Society), 2016
The Whittle engine and the Gloster Meteor aircraft it flew on did
not win the war for the Allied Forces, but they sparked the
incredible co-development of superalloys and aircraft turbine
technology for military and later commercial aircraft. The early
history of superalloy development is described in detail by
Betteridge [3] and Sims [4],
The WW II era was a period when technology was shared freely
between companies and especially between the US and UK. A
duplicate of the Whittle W.1X engine was delivered to the GE
plant in Lynn, Massachusetts where it was further developed into
the GE I-A engine that flew on the Bell P-59 in 1942 [5],
Pioneering alloy developers such as Clarence Bieber, Gunter
Moehling, Rudy Thielemann as well as Leonard Pfeil and his co-
workers developed many of the iconic superalloys using largely
empirical methods. In an interesting (and rare) paper, presented to
the Philadelphia ASM chapter, Bieber describes his innovative
alloy development techniques [6].
This open era changed in the late 1940's as the world transitioned
to a Cold War mentality. Military aircraft performance continued
to drive superalloy technology which developed rapidly in the US,
UK, France and Russia. Much of the development in the US was
sponsored or inspired by the Department of Defense (DOD) and
later National Aeronautics & Space Administration (NASA), both
of which built extensive research facilities. International Nickel
Ltd. also built large research centers in the US at Sterling Forest,
New York and in the UK in Birmingham. Inco's goal was to
develop markets for nickel, and in the process, broadly shared
technology. With a need to understand the basic science of
superalloys, universities began to make important contributions.
The work of Decker and Freeman at University of Michigan that
demonstrated the value of Β and Zr as grain boundary
strengtheners is an example [7]. The Seven Springs conference
came into being in 1968 as an industry forum to discuss phase
stability in superalloys [8], This was the "golden age" of
superalloy technology innovation. All of the major alloy
paradigms and process innovations germinated or were adopted
between 1950 and 1970. These include vacuum melting,
remelting, powder atomization, directional solidification,
isothermal processing, mechanical alloying, electron beam
welding, coating, internal cooling and even the additive
manufacturing concept.
In this period, more formal collaborations were developed, often
led by US DOD or NASA and aimed at furthering aircraft
performance, but occasionally dealing with issues such as raw
material shortages. In this pre-internet world, intellectual property
(IP) security was primarily a matter of controlling the movement
of people and paper. DOD and NASA projects had various levels
of security, but control via ITAR was relatively straight forward
(but not leak-proofl). Technical papers by industry technologists
were common as companies endeavored to publicize their
developments and government technical reports were relatively
accessible. A strong collegial environment developed among
technologists in the industry despite the fact that they worked for
competing companies. A large number of patents were filed
during this era, and with rapid adoption of new technology at the
time, there was the expectation that by the time they had expired,
technology would have moved on. In this time computer
technology was in its infancy and process sensing and data
collection was almost non-existent. The transaction between
supplier and purchaser was based entirely on testing a product to
verify that it met specification.
The transition to the current state was gradual and it had many
facets. Some obvious ones are the rise and eventual dominance of
commercial aviation as a consumer for new engine technology.
This introduced a strong cost saving mentality to an industry that
previously was primarily motivated by performance. Another
factor was the maturation of the technology, as the melting point
of nickel defined a tangible limit. The end of the cold war and
globalization of the aircraft industry and its suppliers also had an
influence. Economic nationalism on the one hand and
proliferation of offsets and sponsored low cost suppliers created a
tension that did not exist previously. During this transition many
of the corporate research labs such as Inco and Climax were
down-sized or closed, thus eliminating key facilitators of
collaborative efforts. Research at Air Force Research Lab
(AFRL), NASA, and the Defense Advanced Research Projects
Agency (DARPA) shifted from superalloys to "advanced
materials" and university research dependent on NSF funding
followed this trend. Chet Sims addressed this issue in his invited
paper at Seven Springs in 1988 [9],
Another powerful driver of cultural change was the computer and
computer enabled technology. Now, vast amounts of data could
be collected, stored, analyzed and instantly transmitted to
collaborators, customers or competitors anywhere in the world.
Heavy investments by DARPA and DOD agencies in process
modeling began to bear fruit as computer memory and speed
made modeling of complex systems practical. With the maturation
of technology, the focus became more and more on process
control, resulting in highly controlled fixed practices that have
become the foundation of Integrated Computational Materials
Engineering (ICME). Concern in the US about proliferation of
technology briefly relaxed with the end of the cold war only to
strongly re-emerge after Sept 11, 2001 in the guise of preventing
proliferation to so-called rogue states and terrorist organizations.
Computer security measures implemented to combat industrial
technology espionage have become a significant constraint to the
flow of information and to industrial collaboration.
All of these factors, acting synergistically, have combined to
change the nature of technical collaboration. The progressive
decline in the number of technical papers presented by industry
representatives as prime authors at this conference is a direct
result of this changing environment. Whether it is because the
new technical developments are considered not to be of sufficient
academic value, or engineers are too busy to communicate or
there is fear of internal IP leakage or ITAR violations, all have
their influence. But that does not mean that collaboration has
ceased, nor does it mean that it is no longer relevant to the goals
of the industry. Collaborations now occur in different, more
constrained, ways and the results may not be reported in the open
literature. The following discussion is based on some recent
examples that show how collaboration is occurring and how it can
4
be enhanced. The examples are by no means exhaustive; they
were selected to illustrate different forms of successful
collaboration.
Examples
A new supply-chain paradigm - Intra-company Collaboration
Precision Castparts Corporation (PCC) was founded in Portland in
1949 as the Oregon Saw Chain Company. Its small steel
investment casting foundry was spun off as PCC in 1957. Its
General Manager Ed Cooley based his business model on being
able to make the largest and most complex castings in the
industry. Cooley entered the aircraft casting business in 1965. He
aggressively honed his capabilities for making complex nickel and
titanium investment cast parts. In doing this he built a highly
successful business that generated a significant return on
investment [10], In 1986 PCC began to diversify when it
purchased the TRW airfoils business in Cleveland Ohio. Later
PCC redefined itself as a parts supplier to the aircraft engine and
then to the entire aircraft. PCC successively acquired Wyman-
Gordon (forgings), SPS (fasteners), Special Metals (nickel-base
alloys), Timet (titanium alloys), and Primus (airframe structural
components). Wyman-Gordon and Special Metals were also
participants in the oil and gas, fossil and nuclear energy markets,
so this sector became a prominent part of PCC's core businesses.
To complement the capabilities of already large companies, PCC
purchased several smaller, but well-known companies, such as
Carlton Forge, McWilliams Forge, Rollmet and Rath-Gibson.
PCC is now organized with three divisions (Castings,
Aero structures and Forged Products and Metals) with 162
separate business units and 30,500 employees. The overall
structure of PCC is illustrated in Figure 2.
Figure 2. General organization of PCC businesses.
In 2016 PCC was itself purchased by the Berkshire-Hathaway
Group, under whose direction it will maintain its focus on
providing increasing value to its customers.
While the PCC business model does not directly foster external
collaborative policy or projects, it does create an internal
environment for collaborative innovation across company
boundaries not previously possible. PCC does not have a
corporate R&D facility or function. However, it does actively
promote an internal virtual technical environment that develops
and shares best practices and creates multi-function teams to work
on common problems or opportunities. To this end there have
been several corporate and divisional technical conferences
organized around a central theme with strict presentation and
format requirements. This has provided a forum for young
engineers to be recognized and to develop their network among
their peers in other related companies. In addition, more
technology specific meetings are held on a regular basis. These
include such varied topics as vacuum melting, raw materials
utilization, computer simulation and process automation. A
corporation-wide technology development program also
encourages peer interchange among young engineers.
Intercompany Collaboration With No Formal Agreement -
Large Gas Turbine Wheels. Successful multi-company
collaborations do not always require elaborate formal agreements.
An example is the adaptation of INCONEL® alloy 706 for
wheels, spacers and shafts for large frame gas turbines. This
development was carried out entirely between the OEM (General
Electric Power) and its supply chain (melters and forgers) with
nothing more than simple bi-lateral non-disclosure agreements.
Alloy 706 was developed by Eiselstein and Clatworthy in 1970 as
a low-cost derivative of alloy 718 [11, 12]. The inventors
envisioned it as a general purpose alloy; however, they were
aware that the alloy was less prone than alloy 718 to solidification
segregation. This concept was further developed by Suarez et al;
however, they were unable to identify process conditions that
prevented both segregation and ingot cracking [13]. The
possibility of using a large diameter age-hardened nickel-base
alloy for a gas turbine wheel was explored by GE at that time. The
properties of alloy 706 were considered attractive [14]. However,
for various reasons, the time was not ripe for a transition from
steel to nickel turbine rotors. Over the succeeding 20 years, the
Inco patent expired without there being a significant application.
By the late 1980's GE's gas turbine designers had pushed
operating temperatures to the limit of steel capability. GE then
initiated work with its supply chain to develop a 706 rotor
capability. Gas turbine rotors are an order of magnitude larger
than aircraft turbine rotors and the high forging loads required to
forge these disks could only be delivered by three 50 KT+ forging
presses at Alcoa, Wyman-Gordon and at Issoire in France.
Similarly, only four nickel alloy melt shops (Allvac, Aubert &
Duval, Carpenter, and Inco Alloys International) had the melting
and remelting capability to produce cropped and conditioned
ingots as heavy as 15 T. While the basic equipment existed within
these companies, there were significant differences that precluded
a universal practice. Accordingly GE defined a set of product
criteria and then worked with the supply chain to develop multiple
process pathways. The introduction of this product was described
by Schilke et al [15],
Figure 3. Wyman-Gordon 50 KT forging press in Grafton, MA.
5
This was not an easy scale-up of an established material. Alloy
706 is resistant but not immune to solidification segregation. The
alloy also forms a significant amount of Laves phase during
solidification that results in very low as-cast ductility. The high
level of residual stress in large ingots makes the alloy sensitive to
cracking. The initial practice was Vacuum Induction Melting
(VIM) and Electro-slag Remelting (ESR) which produced suitable
forged structure and properties, but was unreliable due to
remelting instabilities. GE then specified triple melt (VIM-ESR-
VAR) on the belief that the shallower melt pool in Vacuum Arc
Remelting (VAR) and the improved stability provided by a sound
electrode would minimize the possibility of a segregation anomaly
that would be impossible to detect. That change did not solve the
cracking problem which is illustrated by an example from Special
Metals (Figure 4) and described by Minisandram [16]. Each of the
melt shops developed solutions to the problem for their own
unique processes using thermal stress modeling to define process
windows. In this respect each melter worked independently with
minimal input from GE.
Figure 4. Catastrophic longitudinal cracking of a 706 ESR Ingot.
Similar development was required for ingot conversion
(billetizing) and closed die forging. Along the way composition
and heat treatment criticalities and ultra-sonic inspection
techniques were developed. The final result was a fixed practice
specification that promoted a uniform product made by multiple
suppliers with different equipment. Throughout this development
there was communication between GE and its suppliers that
preserved the confidential information of each supplier. For a
project of this nature to succeed, there must be a clear and
narrowly defined product goal with a credible revenue potential
and trust that confidentiality will be maintained. The 706
development left a legacy of "big ingot" technology that provided
a basis for the adaptation of superalloys for a new generation of
energy systems described in the next example [17, 18].
AUSC - Industry Consortium with Very Long Term Goals.
Historically, the primary materials of construction for coal-fired
steam boilers and coupled steam turbines which generate more
than half of the world's electricity were heat-resisting ferritic steel
grades. In the 1990's it was recognized that the operating
temperatures had reached the limit where ferritic steels could no
longer be used. The next generation of power plants that was
designed to operate at or above 700 °C would require super-
austenitic steels or possibly nickel-base alloys. Consortia were
launched in Europe (1998) and the US (2001) to develop the
material technology with the expectation that the first
demonstration plants could be built in about 2010 [19]. This
became known as Advanced- Ultrasupercritical steam technology
(AUSC). The problem of developing the technology and financing
of such plants proved much more difficult than initially thought.
In the early work alloy 617, a weldable solid-solution and carbide
strengthened nickel-base alloy with a prior history of use for
chemical process vessels and gas turbine transition ducts, was
considered a prime candidate for boiler tube and steam pipe. As a
higher strength alternative, Special Metals proposed age-hardened
alloy 740, that is a modification of aerospace sheet alloy 263, with
improved oxidation and coal ash corrosion resistance [20],
The US AUSC Consortium is a public/private venture comprised
of the US Department of Energy (DOE), Ohio Coal Development
Office (OCDO), Electric Power Research Institute (EPRI), and
major US boiler and turbine manufacturers. Oak Ridge National
Lab (ORNL) and the National Energy Technology Lab (NETL) in
Albany Oregon provided key material evaluation capabilities. The
US consortium evaluated many commercial and developmental
alloys for the various components in the boiler and turbine. Alloy
740 was selected for further evaluation as tube and pipe. This
alloy was later modified to improve its γ' stability and heavy
section weldability and renamed alloy 740H [21], Reviews of the
consortium activity were presented by Viswanathan et al. [22] and
Shingledecker et al. [23].
Special Metals (and other alloy producers) were not members of
the consortium, but they worked closely with members and Labs,
initially to supply material for testing and later for demonstration
of component manufacturing capability and to supply material for
boiler test loops. Two key properties on which material selection
was based were minimum creep-rupture strength in 100,000 h at
760 °C and 100 MPa, and oxidation and coal ash corrosion
penetration of less than 2 mm in 200,000 h. The creep testing of
base metal and weldments was done at ORNL while oxidation and
hot corrosion testing was done at ORNL, NETL, Babcock &
Wilcox and Foster Wheeler. The creep test data formed a key part
of a data package that the consortium presented to ASME for code
approval. Formal code approval of the alloy in Code Case 2702
was gained in 2011 [24], Alloy 740H is the first age-hardened
alloy to be approved by ASME for use in welded pressure pipe for
creep-limited service. The design stress allowables, compared
with those of solid solution strengthened boiler alloys are shown
in Figure 5.
ASME Section It - A l l o w a b l e Stresses
300 - of its programs, the Industry/University Collaborative Research
500 600 700 800 900
Temperature (*C)
-*-Gr. 91 -*-347H i 617 —230 - tnconel 740H
(CC2702)
Figure 5. ASME design allowable stress for 740H compared with
other widely used boiler alloys.
The materials characterization and qualification phase of the US
AUSC project is complete. Recent focus has been on
demonstration of capability of manufacturing components on the
6
scale needed for the plant. Special Metals and Wyman Gordon
have been involved in a number of these activities in close
collaboration with the OEMs. These include extrusion of large
diameter pipe and forging of steam turbine disks of alloy 282®.
Considerable work has also been done on manufacture of pipe
bends and fittings with Chicago Bridge & Iron Alloy Piping
Products, and Maass Flange. These activities are described in
more detail in another paper in this conference [25].
(® 282 is a registered trademark of Haynes International).
mm
ÉKíwLka-
Figure 6. Mock-up segment of header pipe that demonstrates
technical capabilities needed for AUSC power plant such as
production of large diameter ingot and pipe and welding of heavy
section and complex geometry.
The AUSC consortium collaboration has been successful in a
number of ways. Not only have the materials been developed and
qualified to enable construction of an AUSC demonstration power
plant, but it has made these materials available to the power
industry throughout the world. In addition the technology is
essential for other advanced power generation applications. In
particular supercritical C0 2 has been identified as a highly
efficient working fluid to drive compact turbines in fossil, solar
and nuclear power systems. Pilot plants designed to prove these
concepts are now under construction. This initiative that began
rather modestly 18 years ago will make a major contribution to
the world's energy future. But from an alloy developer/producer
perspective, developing alloys for an application that will take a
generation reach maturity is a very big risk.
Ma2JIC - Industry/University Center for Joining Technology
The National Science Foundation (NSF) has been a major
supporter of basic science research in the US for many years. One
Centers (I/UCRC), provides a framework for centers in a wide
range of technologies. The Materials and Manufacturing Joining
Innovation Center (Ma2JIC, formerly CIMJSEA) was launched in
2010 and is now in its second NSF award phase. This center is
anchored at Ohio State University with partners at Lehigh
University, Colorado School of Mines and University of
Tennessee. NSF centers require company membership fees and an
industrial advisory board to control selection of projects that must
be collaborative and pre-competitive in nature.
Metal joining is highly diversified in both technology and the
industries that utilize it. These joining processes include
traditional arc, laser and electron beam welding as well as brazing,
friction welding and additive manufacturing. The forty members
of the Ma2JIC center include welding products suppliers, welding
services companies, fabricators, users and institutions. Process
modeling is a key part of this program. The center supports a wide
range of projects involving superalloys including aerospace, gas
turbine, power and oil and gas applications.
One project addresses the problem of stress-relief/stress-relaxation
cracking. This mode of cracking is seen in a wide range of alloys
in aircraft, power generation, petro-chemical, and chemical
process industries. Aircraft industry readers will appreciate the
often cited weldability advantage of alloy 718 versus Waspaloy.
In power and chemical plants this mode of cracking is especially
insidious because it is driven by relaxation of residual welding
stress in large highly restrained structures by a creep rupture
mechanism. Cracking may not become evident until after years of
service. For example, a stress relaxation crack in alloy 617 in a
main steam pipe of a power plant experimental test loop was not
seen until after 10,000 h of operation [26]. It has been shown that
this kind of cracking can be prevented through joint design,
welding process control and post-weld stress-relief heat-
treatments.
Research at Lehigh and Ohio State Universities is focused on
developing predictive tests and characterizing relative
performance of commercial alloys. Many of these tests are
Gleeble-based and seek to reproduce the complex thermal and
stress cycles that accompany a multi-pass weld cycle. Analysis is
complicated by the problem of long time microstructure stability
of weldments that contain severe microstructure, composition and
stress gradients. An example of a unique microstructure that has
been observed in a weld in alloy 740H is shown in Figure 7 [27].
Figure 7. Grain boundary γ' denuded zone in alloy 740H cross-
weld creep specimen. This feature is caused by an interaction of
residual stress and a discontinuous γ' coarsening reaction [27].
A goal of this research is to develop a comprehensive model to
predict life performance of a weldment in service. Such a model
must consider multiple interacting forces as illustrated in Figure 8.
Note that many of the processes are time dependent and non-
equilibrium and must contend with steep structure and property
gradients.
The development of a holistic life model will be difficult and will
take several years to complete. One of the major gaps is the lack
of material property data to characterize the different structural
zones in a weldment such as coarse grain heat affected zone, or
across a dendrite in an un-homogenized structure. An NSF funded
basic research project at Ohio State University is addressing this
problem using a variety of novel micro-mechanical techniques.
7
Development of the model for nickel-base alloys is now
proceeding with DOE funding at Idaho National Lab (INL).
Solidification
Mif rostnifture Structure
Evolution Thru Fracture
Thermal Cycles Modes
>4
Integrated
Long Time Methodology Environmental
Microstructure for Weld Life Effects
Stability Prediction
Time Dependent Macro
Mechanical Properties Service
of Composites Residual Stress
Stress
Evolution
Figure 8. Structure for a model of weld behavior in power plant.
From an industry perspective, university based collaborative
research has a number of short-comings, not least of which is the
difficulty of finding common ground among participating
companies for a sufficiently targeted research program. Individual
membership funding tends to be limited, so external funding can
be critical. The success of a center often depends on the
commitment of the industrial advisory board and its understanding
of the open publication needs of the university partners and a
project timeline closely tied to the student graduation cycle.
Nevertheless, a strong I/UCRC can be a fruitful employee
recruiting mechanism as members can become familiar with the
capabilities of students in a variety of settings.
Metals Affordability Initiative - Industry/DOD Partnership
The Metals Affordability Initiative (MAI) is an industry/Air Force
partnership that is dedicated to development of metals technology
for military aircraft. US companies representing four tiers of the
supply chain (airframe and systems, engines, parts suppliers and
metals producers) are members. Funding is provided through
annual appropriations by the US Congress to the USAF,
designated for industry led materials technology development. A
significant industry cost share is required to supplement federal
funding for projects. Projects are selected by a Technical
Oversight Committee (TOC) where each member company,
regardless of its size, has one vote. The TOC also monitors the
technical progress of the projects and controls continued project
funding through task gate reviews. Generally, work is done at
project member companies and subcontractors that often include
small businesses and universities. A wide range of projects have
been completed since the MAI was started in 1999. Many of these
projects have resulted in early insertion for supply chain
manufacturing efficiency or products used on aircraft platforms
that support enhanced mission capability or operating cost
reduction. Much of the technical work is subject to ITAR
restrictions and may only be reported in closed forums. Highlights
of the program for 2015 have been reported [28].
One of the most successful MAI projects resulted in the adoption
of digital radiography for final part acceptance of aerospace
castings. Most aerospace structural castings require radiographic
inspection to confirm internal quality. In the late 1990s the
adoption of digital radiographic imaging transformed the medical
industry. As personal and industrial photography followed suit,
film became scarce and expensive. Other reasons for interest in
digital records are portability and permanence.
Although there was widespread interest in the casting industry in
making the conversion from film to digital, there were major
barriers that could not be overcome by one company acting
independently. PCC and Howmet made an initial start under the
Next Generation Manufacturing Technology Initiative (NGMTI),
but funding from that source was insufficient. PCC then put
together a team and proposal to MAI that was approved and got
underway in 2008. The project was also supported by DoD
Manufacturing Technology Program (ManTech). The PCC-led
team included all of the stakeholders among the casting suppliers,
OEMs and key film and equipment suppliers. Among the
problems to be overcome were 1) lack of digital reference images,
2) lack of ASTM and company specifications, 3) competing
commercial image systems and 4) need for NDT inspector
training from shooter level all the way through Level III. In many
cases this involved decades of experience with film and lack of
familiarity with computers. Another barrier was the high cost of
acquiring digital radiographic equipment that was sufficiently
robust for foundry use.
FOREIGN MATERIAL LESS DENSE 1 / 8 in. (3.2 mm|
Figure 9. X-ray radiographic image reference standards for
aerospace parts.
The project was completed in 2011, culminating with the issuance
of ASTM E2033 (Standard Practice for Computed Radiology). A
30 page procedure document for managing the differences
between the two major systems for capturing images was agreed
and implemented by each member. Training classes were
developed and delivered to all levels of NDT operator.
Comparative images were made of parts for each customer. After
completion of the work, the project received the Defense
Manufacturing Technology Achievement Award in 2011.
Foundry conversion to digital radiography at PCC Structural
Castings Division is well underway, with some locations having
completely removed film processors. The project was reviewed by
Brayshaw and Barrett [29]. The same project team is now
working on the next step in digital radiography, Assisted Defect
Recognition (ADR). To date several software companies have
demonstrated algorithms that meet the ability of a human operator
to detect discontinuities in digital x-ray images. The ability to
share digital defect maps is a critical link in ICME for aerospace
castings.
8
ICME has profound implications for the way industries
collaborate. The concept involves linking process models to
reduce variability of material properties, reduce rejections and
improve the accuracy of life prediction. While process modeling
is now strongly embedded in superalloy production technology
the incentive to link models to achieve a holistic predictive ability
has been lacking. The Air Force has invested heavily in ICME
following a National Academy of Science Report in 2008 [30].
The ICME work builds on the long history of Air Force support
for finite element modeling that accelerated the development of a
robust simulation industry in the US. Many projects within the
MAI portfolio now address some aspect of ICME including the
one just described. Projects under the MAI mantle include
prediction and measurement of residual stress caused by forging,
heat treatment and joining, its effect on part distortion during final
machining, and its effect on fatigue properties. More fundamental
programs are considering the evolution of microstructure and its
effect on the properties in forged parts. These models have been
validated and the uncertainly quantified. Work is now underway
to determine the sensitivity to process variables and to develop a
platform, data format and security controls that will enable
establishment of a digital data thread. This exposes an unresolved
point of contention between oversight agencies, system owners,
OEMs and parts/material suppliers regarding collection and
handling of proprietary process data in a digital world.
The MAI concept has been very productive. The most recent
assessment of Return on Investment (ROI) to DoD is $1.18 billion
for a government investment of $160 million [31]. Executive and
technical meetings are held quarterly with strong membership
participation. This is in part the result of the required financial
participation of the members, an obligation to involve a broad
cross-section of the supply chain in each project and a strong
business case. The active role of AFRL technical personnel is also
beneficial. The principal problems have been a primary funding
source subject to political uncertainties and the complexities
associated with management of multi-participant government
funded contracts.
SMPC - An Industrial Consortium for Remelting Research
Collaboration in process research is less common and what work
is done is less well known because of the specialized nature of the
technologies and a reluctance to publish results. A program that
has been underway in the US for twenty-five years is the
Specialty Metals Processing Consortium (SMPC). Frank Zanner,
working at Sandia National Lab (SNL), approached the US
specialty alloy melters with the notion of creating a consortium
that would focus on advanced melting technologies. Sandia hosted
a liquid metals laboratory with extensive experience in remelting
of specialty alloys for the nuclear weapons industry. DOE funding
for enhancing domestic manufacturing technology was available
at that time. Bob Torcolini of Carpenter Technology led the
difficult task of creating a consortium of highly competitive
companies. Ultimately a Delaware Membership Corporation of 13
companies was founded. This corporation executed a Cooperative
Research and Development Agreement (CRADA) with Sandia
(and later with NETL) to create a framework for projects to be
carried out by Sandia, Los Alamos and university subcontractors.
Funding was by membership fees, in-kind support and
Department of Energy (DoE) and later Federal Aviation
Administration (FAA), United States Air Force (USAF) and
United States Navy (USN). A broadly based research program in
ESR, VAR and EB hearth melting processes was developed that
used the resources of the national labs with critical validation on
industrial equipment. An example of this work is a unique
experiment on a specially built hearth window installed in a VAR
furnace shown in Figure 10. Classic images of VAR cathode spots
and drip shorts were obtained that fundamentally changed the way
the process was viewed [32].
the current generation of sub-sonic commercial aircraft engines.
This project also exemplifies many other ambitious US aerospace
projects that, while not always accomplishing their platform goal,
never-the-less made important contributions to superalloy
technology.

Figure 10. View through hearth window of the arc in VAR.

Tungsten reference post in the foreground [32],

Throughout its history, SMPC has generated many patents,

publications, process tools and process understanding for its
Figure 11. NASA artist concept drawing of the HSCT; a plane
members. These include defect characterization [33], VAR
that never was paved the way for a new generation of powder disk
process models [34], advanced controllers [35], process monitors
alloys (NASA Website).
[36], instrumentation and visualization and statistical analysis
tools. Although the grand objective of commercializing new
The NASA mission requirements included a long liftoff stage to
remelting processes or controllers has yet to be achieved, SMPC
achieve cruising altitude with sustained operation at 650°C.
research has had a significant impact. There has been a
Existing powder disk alloys could not meet the dwell-fatigue or
progressive reduction in the number of anomalies that have been
creep properties needed for service. ME3 (Ni-20.6Co-13Cr-3.4Al-
detected by ultra-sonic testing in rotor quality alloy 718 and
3.7TÍ-2,4Ta-0.9Nb-2.1W-3.8Mo) [37] was the resultant alloy
Waspaloy bar produced in US melt shops since data collection
designed in the NASA/General Electric/Pratt & Whitney High
began in 2002. Data reported on a confidential basis to FAA and
Speed Research/ Enabling Propulsion Materials (HSR/EPM) [38]
provided to the Aerospace Industries Association, Rotor Integrity
program for extended use up to 600°C to 700°C allowing for
Sub-Committee (RISC) shows 40-75% reduction in reportable
increased fuel efficiency, lower fuel burn and reduced emissions.
indications in each of the four product categories. This
The alloy was designed using statistical methods [39] and
improvement is due to many factors, but the shared technology
contains a high γ' content to produce balanced monotonic, cyclic
generated by SMPC is certainly one of them.
and time dependent mechanical properties [40] while still able to
be forged and heat treated. PCC has participated in this program
Melting process research poses difficult problems for
from the exploration of the thermo-mechanical and
collaboration. To begin with, process research is very costly and
microstructural properties to the development of full scale
time consuming. Consequently, with a few notable exceptions,
forgings. Applications for both sub-solvus and super-solvus heat
universities have neglected this field. Definitive validation via
treatment have been developed and are in production.
industrial experiments is critical, but sharing of the results is
awkward and constrained. Breaking into an industrial production
NASA has supported and published extensively on ME3.
schedule with risk of equipment damage is always difficult.
Resulting data available has also provided a platform for MAI
Another significant constraint is that the cost of qualifying a major
collaboration to explore and validate ICME techniques and
process change for aero-engine bar production is almost
supports efforts to characterize how variability effects the
prohibitively expensive. Hence, process data analytical tools such
predicative capabilities of these techniques.
as the SMPC VAR process monitor can be readily applied by
member companies, while more disruptive process changes such
as its novel pool depth controller are difficult to justify. Blade Cooling - A Continuing OEM/supplier Collaboration.
Modern aircraft turbine airfoils are precisely engineered to
provide optimum performance in a challenging environment. In
HSCT - ME3, a Legacy of a NASA Project. The High Speed
addition to an oriented single crystal structure with up to 75% γ'
Civil Transport (HSCT) project was conceived as the next step in
content, they contain intricate cooling channels and thermal
commercial supersonic flight beyond Concorde. The project that
barrier coatings and operate in a combustion gas well above the
began in 1990 and ended in 1999 was managed by NASA
alloy melting point. This was not always so. The first NIMONIC
Langley. It had truly lofty goals, a 300 passenger plane that would
alloy 80 blades were machined from solid forged bar. Wrought
fly at Mach 3 at 70,000 ft. for 6000 miles. In addition the engine
blade alloy technology developed rapidly: γ' content increased
would be required to have low NOX emissions and be fuel
progressively and cobalt and refractory metals were introduced.
efficient. The engine used standard turbofan technology and hence
By the time NIMONIC alloy 115 entered the market, blade alloys
had to run very hot to achieve those specifications. GE and Pratt
could no longer be cogged from ingot. Henry Wiggin Co. (Inco)
& Whitney collaborated with NASA on engine technology. While
introduced extruded blade bar and as a weight reduction measure
the project goal of commercial service by 2020 was not realized,
produced blade forging stock with leachable iron cores as early as
critical technologies were developed that are being employed in
1953 [3]. Rolls-Royce quickly recognized the value of using these

9
channels for internal air cooling and the patterns became
increasingly complex. In 1970 John Benjamin at Inco's Sterling
Forest Research Center developed the Mechanical Alloying
process as a solid state powder processing method for making an
oxide dispersion strengthened superalloy [41]. The application
goal was an aircraft turbine blade where the oxide dispersion
would supplement γ' to provide creep strength up to the melting
point of the alloy. Over the next twenty years Inco invested
heavily in this technology. A significant application developed for
non-age hardened alloy MA754 in turbine vanes and bands. But
the alloy never succeeded for the blade application despite steady
advancements in composition, directional recrystallization and
forging [42, 43], Despite diffusion bonded wafer blade and
lamiloy technologies, the cooling barrier could not be
economically overcome in wrought alloys.
The early cast blades were also solid, but the foundry industry was
very familiar with sacrificial metal and ceramic cores. By the time
that directional and then single crystal casting processes were
developed, internal cooling patterns too complex for wrought
blades were already in widespread use. A relatively simple non-
proprietary ceramic core is shown in Figure 12.
Figure 12. Complex, durable and removable ceramic cores are the
key to success of cast blade technology.
The progression from the earliest castings with a single central
cooling passage to today's complex serpentine channels with cast
wall sections as thin as 0.015 in. was continuous. The impact of
blade cooling on turbine inlet temperature is often overlooked by
metallurgists, but Metham [44] and Goulette [45] attributed about
half of the advancement to cooling. Airfoil design is a closely
held technology of the OEMs while the technology to
manufacture them is closely held by the suppliers. This includes
alloy chemistry control, casting conditions, and ceramic shell and
core design. Initially, cores were made at the foundry, but the
manufacture of precision ceramic cores is a specialty in itself, so
today many cores are manufactured to specification by
independent suppliers.
In the 1960s airfoil designs were done as conventional
engineering drawings that could be passed through the supply
chain with appropriate confidentiality markings. In the modern
digital world CAD dimensional drawings become integrated with
data management systems at the core maker and foundry. Casting
and core making processes are designed by computer simulation,
dimensions are checked and recorded with white light systems
and defect data collected from X-ray image recognition systems.
New methods of core-making such as additive manufacturing are
10
adding new partners to the mix. All of this data can in principle be
shared throughout the supply chain almost instantaneously. This
brings us back to the question of IP integrity of the OEMs and
supply chain. Several groups are working to develop data sharing
technologies, but this remains a high level concern for suppliers.
Discussion
Clearly innovation and collaboration has driven the superalloy
industry over the past seventy-five years. This was particularly
true of the early years, when the pioneers of gas turbine
technology and nickel alloy development fed off each other's
successes (and failures) to innovate and challenge the status quo.
The various examples cited in this paper show the importance of
this symbiotic relationship between the end user and the supplier
to solve critical problems of enabling technologies as well as cost
reduction initiatives to take the industry forward. Of course the
role of government is often vital, not only for the purposes of
funding, but also to provide national mandates and a pre-
competitive framework for collaboration. If we refer to the Chet
Sims illustration of the key periods of Superalloy evolution shown
in Figure 13, the first fifty years were, in many ways, simpler
times when collaboration was often informal and exchanging
ideas and data was a matter of course, and trust.
/ ICME I
The Major Eras Process Control I =•
I I Processing
I I Al loving
I I \focuum Melting
I I The Jet Engine
11 Ί Conception ,
V- * » ' ' ' ' ' '
1940 1950 19» 19™ 1*80 1990 2000 2010
Figure 13. Update of the Chet Sims "The Major Eras" plot.
As we enter the era of predictive computer modeling and ICME to
better understand our processes, improve quality, yields and lower
costs even further, this is no longer the current paradigm. The
early days of innovating alloys and processes just to enable
engines to fly have been replaced by developing competitive
advantages through tightening process controls and proprietary
data which are treated as family jewels by companies. This is
further complicated by an evolving supplier base which is
consolidating and narrowing on the one hand in the US, but
expanding on the other in terms of potential new suppliers from
overseas. In the case of China and Japan, governments are leading
the charge and funding massive investments and consortia to
develop national capabilities in critical industries, reminiscent of
post-WW II US projects. This complex landscape is encouraging
a certain conservatism and in some cases, frankly, a paranoia in
many companies when it comes to IP protection. This is one of
the biggest barriers to successful collaborative programs in the
coming years.
The pros and cons of industry consolidation can be debated, but
from the perspective of an insider in the largest of these
conglomerates, PCC, it is clear that the intra-collaboration
throughout the supply chain from raw materials, through melting,
casting, forging to final machined components is currently driving
rapid innovation without the constraints of formal agreements and
IP sharing concerns. PCC's key role in the supply chain is to
convert novel ideas for products and processing concepts into
actual components at an acceptable cost and quality. This would
be much more difficult, if not impossible, in a world where
Special Metals, Timet, Wyman Gordon and Carlton, for example,
were all independent companies. The dynamic of internal
customers and suppliers working together to provide solutions for
the external market is extremely potent.
This relationship between cost and quality is often a controversial
one. On the one hand, cost reduction initiatives are critical to
maintain a competitive edge for both supplier and OEM. On the
other hand, too often the relentless pressures on the supply chain
to reduce costs can lead to bad decisions and a direct effect on the
quality of the final product. In fact, in many cases the primary
collaborative programs between suppliers and OEM's are focused
solely on cost reduction "pipelines", rather than innovative
technology ideas. This relationship needs to be rebalanced for the
ongoing technical health of the industry.
Finally, the current age of electronics and computers is enabling
materials technology advancements in potentially exciting new
areas, such as Additive Manufacturing. Whereas a great deal of
fundamental work is already under way at research labs and
Universities, ultimately the success or failure of this technology
will depend on key collaborations and technology transfers
between these institutes, materials companies, component
manufacturers and OEM's. In that sense, whilst so much has
changed since the early days of superalloy development, much
remains the same.
Conclusions
Whereas the need for continued collaboration across the
Superalloy world is clear, many challenges need to be faced and
addressed. The issue of Intellectual Property protection is one of
the most critical of them. This is a core concern of many in the
industry, and it may be driving behaviors within companies. This
concern is real and needs to be addressed if meaningful
collaboration is to continue between competitive companies. On
the other hand, supply-base consolidation has removed these
barriers within companies under the same parent and so
innovation is alive and well!
Acknowledgements
The authors acknowledge the contributions of Jim Barrett (PCC
Structural Castings), Larry Graham (PCC Airfoils), Beth Lewis
and Noshir Bhathena (Wyman-Gordon) in the planning and
writing of this manuscript.
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Superalloys 1988, ed. S. Reichman et al., (Warrendale, PA: TMS,
1988), 131-140.
43. R.C. Benn, and P.K. Mirchandani, "Dispersion Strengthening
by Mechanical Alloying," New Materials by Mechanical Alloying
Techniques, ed. Arzt and Schultz, (Oberusel, GR, DSM, 1988),
19-38.
44. G.W. Meetham, The Development of Gas Turbine Materials,
(New York, NY: Halsted Press Division of John Wiley & Sons, k,
1981), 13.
45. M.J. Goulette, "The Future Costs Less - High Temperature
Materials From an Aero-engine Perspective", Superalloys 1996,
ed Kissinger, et al., (Warrendale, PA: TMS, 1996), 3-6.
 Superalloys 2016: Proceedings of the 13th International Symposium on Superalloys
Edited by: Mark Hardy, Eric Huron, Uwe Glatzel, Brian Griffin, Beth Lewis,
Cathie Rae, Venkat Seetharaman, and Sammy Tin
TMS (The Minerals, Metals & Materials Society), 2016

Session 1:
Alloy Development I
 Superalloys 2016: Proceedings of the 13th International Symposium on Superalloys
ALLOYS-BY-DESIGN: TOWARDS O P T I M I Z A T I O N O F C O M P O S I T I O N S
O F NICKEL-BASED SUPERALLOYS
Roger C. Reed 1 , Alessandra Mottura2, David J. Crudden1
'Department of Materials, University of Oxford, Parks Road, Oxford, OX1 3PJ, UK
2
School of Metallurgy and Materials, University of Birmingham, Edgbaston, Birmingham B15 2TT, UK
Keywords: alloy development, nickel-superalloy, materials genome
Abstract
The composition of a range of different nickel-based superalloys
are isolated using theory-based computational modeling, termed
'Alloys-by-Design' methods. Each alloy has been designed with
different applications in mind. A polycrystalline alloy is designed
for turbine disc applications, here emphasis is placed on the
composition dependence of strength. Examples of the design trade-
offs faced when increasing alloy strength are presented. Three new
single crystal alloy compositions are designed. They are (i) a
second generation type alloy with a reduced level of rhenium, (ii) a
creep resistant alloy designed for high performance jet applications
and (iii) a low cost corrosion resistant alloy designed specifically
for industrial gas turbine applications. In each case the newly
designed alloys have been manufactured. Design critical properties
are measured and compared with modeling predictions to test the
accuracy of this alloy design approach.
Introduction
Traditionally, our industry has relied upon a relatively small
number of superalloy compositions. Why? Due to an emphasis on
trial-and-error procedures it has been usual to proceed via
campaigns involving the melting of between 10 and 100 heats,
followed by their ranking using experimental testing. Rules-of-
thumb and prior experience have been fed in at an early stage, to
decide upon the compositions to be tested. This implies an
empirical approach, necessitated by the relative immaturity of alloy
theory and modeling capability.
Today the situation is different. Alloy theory is rather more
advanced; modeling methods are available on different
lengthscales: the electronic, atomistic, microscopic and
mesoscopic. Databases of critical parameters are widely available,
for example based upon CALPHAD techniques, which whilst not
yet totally accurate are becoming of increasing usefulness.
Computational resources are rather cheap and plentiful. But the
above does not necessarily mean that modeling approaches have as
yet superceded the empirical route, or that they ever will
completely.
In this paper, a modeling-based approach termed 'Alloys-by-
Design' (ABD) [1] is proposed for the isolation of new grades of
nickel-based superalloys, circumventing the traditional empiricism.
The method combines computational thermodynamics with sub-
models which estimate design relevant material properties. The
sub-models - referred to as merit indices - are physically based and
include properties such as creep resistance [1] and yield stress [2],
see [1-3] for a more detailed description of the merit indices
included. The ABD approach has been used to isolate compositions
15
Edited by: Mark Hardy, Eric Huron, Uwe Glatzel, Brian Griffin, Beth Lewis,
Cathie Rae, Venkat Seetharaman, and Sammy Tin
TMS (The Minerals, Metals & Materials Society), 2016
of both single crystal and polycrystalline nickel-based superalloys
for turbine blade and disc applications respectively.
Description of Alloys-By-Design Method
Typically, superalloys contain as many as ten different alloying
elements, to confer the desired combination of properties [4],
Commonly Cr, Co, Al, Ta, Ti, Nb, Mo, W are present; sometimes
Re and Ru are also present in the case of single crystal alloys. To
provide grain boundary strengthening C, Β and Zr are added in the
case of polycrystalline alloys.
The large number of possible alloying elements and their
considerable solubility in nickel mean that the extent of the possible
alloy design space is very considerable. Moreover, the
contributions made by each element to the microstructure and
properties are not independent of each other, so that alloying alters
the balance of properties in a subtle way which is difficult - maybe
impossible - to judge by rules-of-thumb. This situation has
contributed to the present state-of-the-art in which existing alloy
compositions have been chosen empirically, for example using
statistical analysis of experimental data. Thus considerable use has
been made of trial-and-error based testing, and ranking of alloy
performance on the basis of measured rather than predicted
behavior. The ABD approach - involving large-scale
computational calculations to systematically search a broad
compositional range - provides a potential solution to this problem.
Description of Alloy Isolation Procedure: The algorithm used is
illustrated schematically in Figure 1. It relies upon a series of
procedural steps represented by the boxes linked by arrows. The
important, overarching strategy is to estimate the composition-
dependence of the mechanical behavior and environmental
performance. In this sense it relies upon brute, computational-force.
Required in practice - at minimum - are many tens of thousands of
calculations.
The first step therefore - see Figure 1 - is the definition of an
elemental list and associated upper and lower compositional limits
for each one, for example Table I. The second step makes use of
thermodynamic calculations made using the CALPHAD method,
specifically using the Thermo-Calc software package and an
associated database of thermodynamic parameters, in this case the
Thermotech TTNÍ8 database. For each trial composition, an
estimate is made of the fraction and composition of the
strengthening γ' phase at equilibrium, and the associated
composition of the matrix phase. Other thermodynamic quantities
such as chemical potentials - which are needed for estimation of
the susceptibility to oxidation - are determined and stored at this
point. It is also convenient to estimate kinetic parameters such as
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commencement de l'année suivante. Quelques
auteurs prétendent que Salia alors consul avec Idat. chron.
Philippe, est le même que ce Salianus[153]. Mais la
dignité consulaire ne paraît guère s'accorder avec Till. art. 11.
cette députation. Philippe, l'autre consul, était
d'une famille très-obscure. Un génie souple et
intrigant l'avait élevé jusqu'à la charge de préfet An 348.
d'Orient, qu'il posséda pendant plusieurs années. Il
était vendu aux Ariens, et nous le verrons bientôt signaler son zèle
en leur faveur par des crimes dont il fut mal récompensé.
Constance, naturellement timide, ne reçut pas sans inquiétude les
lettres menaçantes de son frère. Mais les Perses lui donnaient alors
de plus vives alarmes.
[152] Constance était dans cette ville le 8 mars 347.—S.-M.
[153] Cette opinion est celle de Henri Valois dans une note sur Théodoret, l. 2, c.
8.—S.-M.
Après le siége de Nisibe, ils étaient convenus
d'une trève avec les Romains. Cependant Sapor, xlix. Guerre de
dont l'humeur guerrière n'était gênée par aucun Perse.
scrupule, employait ce temps à faire de nouveaux
efforts. Il enrôle tout ce qu'il a de sujets propres à Liban. Basil, t.
porter les armes; les plus jeunes, pour peu qu'ils 2, p. 123 et 128-
paraissent vigoureux, n'en sont pas dispensés. Les 133.
villes restent presque désertes. Il n'épargne pas
même les femmes, qu'il oblige de suivre l'armée, Amm. l. 18, c. 9.
et de porter le bagage. Il épuise de soldats les
nations voisines, qu'il engage par prières, par argent, par force. Tout
l'Orient s'ébranle et marche vers le Tigre. Constance de son côté
rassemble les forces romaines, se met à leur tête et s'avance pour
arrêter ce torrent. Il campe à six lieues[154] du fleuve, et porte des
corps de troupes jusque sur les rives. Bientôt la poussière qui
s'élève au-delà annonce l'approche des Perses; on entend le bruit
des armes et le hennissement des chevaux. Constance, averti par
ses coureurs, va lui-même reconnaître l'ennemi; il ordonne aux
postes avancés de se replier, et de laisser le passage libre:
N'empêchez pas même les Perses, leur dit-il, de prendre un terrain
avantageux et de s'y retrancher: tout ce que je souhaite, c'est de les
attirer au combat; et tout ce que je crains, c'est qu'ils ne prennent la
fuite avant que d'en venir aux mains. Les Perses profitent de cette
confiance; ils jettent trois ponts; ils mettent plusieurs jours et
plusieurs nuits à passer le fleuve sans aucune inquiétude; et se
retranchent près de Singara[155]. Dans cette ville se trouvait alors un
officier de la garde nommé Elien; il n'avait avec lui qu'une troupe de
nouvelles milices. Mais il sut leur inspirer tant de courage, qu'étant
sortis pendant la nuit ils osèrent sous sa conduite pénétrer jusque
dans le camp des Perses; ils les surprirent endormis sous leurs
tentes, en égorgèrent un grand nombre, et se retirèrent sans perte
avant que d'être reconnus. Cette action rendit ces soldats célèbres;
on en composa deux cohortes sous les noms de Superventores et
de Prœventores, qui rappelaient leur hardiesse. Elien fut honoré du
titre de comte.
[154] A 150 stades selon Libanius, or. 3, t. 2, p. 131. ed. Morel.—S.-M.
[155] Ville au milieu de la Mésopotamie sur les bords du Chaboras, actuellement
le Khabour. On la nomme à présent Sindjar.—S.-M.
Les deux armées se rangèrent en bataille: celle
des Perses paraissait innombrable. Elle était l. Bataille de
composée de soldats de toute espèce; archers à Singara.
pied et à cheval, frondeurs, fantassins et cavaliers
armés de toutes pièces. Les rives, la plaine, la Liban. Basil. t.
pente des montagnes n'offraient aux yeux qu'une 2, p. 130-134.
forêt de lances et de javelots. Les gens de trait
couvraient les coteaux et bordaient le
Jul. or. 1, p. 23
retranchement: au-devant était rangée la cavalerie; et 24. ed.
l'infanterie formait l'avant-garde; elle se mit en Spanch.
marche et fit halte hors de la portée du trait; les
deux armées restèrent long-temps en présence.
Eutr. l. 10.
On était déja à l'heure de midi, dans les plus
grandes chaleurs du mois d'août; et les Romains,
sous les armes dès le point du jour, n'étaient pas Rufus.
accoutumés comme les Perses au soleil brûlant de
ces climats. Enfin Sapor, s'étant fait élever sur un Hier. Chron.
bouclier pour considérer l'armée ennemie, fut
frappé du bel ordre de leur bataille; elle lui parut
invincible. C'était un reste de cette ancienne Amm. l. 25, c. 9.
tactique, qui jointe à la sévérité de la discipline
avait rendu les Romains maîtres du monde. Sapor Oros. l. 7, c. 29.
savait assez la guerre pour admirer leur
ordonnance; mais non pas pour la rompre de vive
force, ni pour la rendre inutile par la disposition de [Socr. l. 2, c.
ses troupes. Soit crainte, soit stratagème, il fait 25.]
sonner la retraite, et fuyant lui-même à toute bride
avec un gros de cavalerie, il repasse le Tigre et laisse la conduite de
l'armée à son fils Narsès, et au plus habile de ses généraux. Les
Perses prennent la fuite vers leur camp, pour attirer l'ennemi à la
portée des traits prêts à partir de dessus la muraille et les coteaux.
Les Romains, au désespoir de les voir échapper, demandent à
grands cris le signal du combat. En vain Constance veut les arrêter;
ils n'estimaient ni sa capacité ni sa valeur; et malgré ses ordres, ils
courent de toutes leurs forces, et arrivent au camp sur le soir,
lorsque les Perses y rentraient en désordre. Constance voyant les
siens fatigués d'une course de quatre lieues, épuisés par la chaleur
et par la soif, fait de nouveaux efforts pour les retenir. La nuit
approchait; les archers sur les éminences d'alentour, les cavaliers au
pied de la muraille faisaient bonne contenance. Rien n'arrête la
fougue du soldat romain; il fond sur cette cavalerie, renverse
hommes et chevaux, les assomme à coups de masses d'armes. En
un moment le fossé est comblé, les palissades sont arrachées. Ils
s'attachent ensuite à la muraille; elle s'écroule jusqu'aux
fondements. Les uns pillent les tentes et massacrent tous ceux qui
ne peuvent fuir; Narsès est fait prisonnier: les autres courent vers les
hauteurs; mais à découvert de toutes parts, ils sont accablés d'une
grêle de traits; l'obscurité fait égarer leurs coups; leurs épées déja
rompues dans les corps des ennemis refusent de les servir: après
avoir perdu leurs meilleurs soldats ils se rejettent dans le camp; là se
croyant victorieux, ils allument des feux; et accablés de fatigue,
brûlants de soif, ils cherchent de l'eau et ne songent qu'à se
désaltérer. Les vaincus, profitant du désordre et favorisés des
ténèbres de la nuit, fondent sur eux; ils les percent de traits à la
lueur de leurs feux, et les chassent de leur camp. Dans cette
affreuse confusion, quelques soldats furieux se jettent sur Narsès; il
est fouetté, percé d'aiguillons, et coupé en pièces. Constance, fuyant
avec quelques cavaliers, arriva à une méchante bourgade nommée
Hibite ou Thébite, à six lieues de Nisibe, où mourant de faim il fut
trop heureux de se rassasier d'un morceau de pain qu'il reçut d'une
pauvre femme. Le lendemain les Perses, ne sentant que leur perte,
repassent le fleuve et rompent les ponts. Sapor, saisi de douleur et
de rage, quitta les bords du Tigre, s'arrachant les cheveux, se
frappant la tête et pleurant amèrement son fils. Dans l'excès de son
désespoir, il fit trancher la tête à plusieurs seigneurs qui lui avaient
conseillé la guerre. Telle fut la bataille de Singara, où les rives du
Tigre furent tour à tour abreuvées du sang des Perses et des
Romains, et où la mauvaise discipline fit perdre aux vainqueurs tout
l'avantage que leur avait procuré une bravoure téméraire.
En Occident, les Francs étaient tranquilles; et
Constant profitait du calme de ses états, pour li. Nouveaux
travailler à rendre la paix à l'église. Étant allé de troubles des
Milan[156] à Aquilée, il y manda Athanase, et Donatistes
apaisés en
l'engagea ensuite à passer à Trèves. Gratus Afrique.
évêque de Carthage, en allant au concile de
Sardique, avait représenté à l'empereur les
violences que les Circoncellions ne cessaient de Optat. l. 3. de
commettre en Afrique. Le prince y envoya deux schis. 3-9.
Donat. c.
personnages considérables, nommés Paul et
Macarius. Ils étaient chargés de distribuer des
aumônes, et de donner leurs soins à ramener les [Athan. apol. ad
esprits. Donat, faux évêque de Carthage, les Const. t. i, p.
rebuta avec insolence, et défendit à ceux de sa 297.]
communion de recevoir leurs aumônes. Un autre
Donat, évêque de Bagaï en Numidie, assembla les Baronius.
Circoncellions; les envoyés de l'empereur, pour se
mettre à couvert de leurs insultes, furent obligés Till. Hist. des
de se faire escorter par des soldats que leur donna Donat. art. 46 et
le comte Silvestre. Quelques-uns de ces soldats suiv.
ayant été maltraités, leurs camarades malgré les
commandants en tirèrent vengeance: ils tuèrent plusieurs
Donatistes, entre autres Donat de Bagaï. On employa contre ces
sectaires des rigueurs qui furent blâmées des évêques catholiques.
Cette conduite trop dure de Paul et de Macarius donna occasion à la
secte de les rendre odieux comme persécuteurs, et d'honorer
comme martyrs ceux qui perdirent la vie. Mais les commissaires
n'excédèrent pas les bornes d'une sévérité légitime en chassant de
Carthage le faux évêque Donat, et en traitant de même plusieurs
autres évêques obstinés. Une grande partie du peuple rentra dans la
communion catholique. Gratus cimenta cette heureuse union par un
concile tenu à Carthage; et la tranquillité rétablie dans l'église
d'Afrique subsista jusqu'à la mort de Constance.
[156] Il était en cette ville le 17 juin 348.—S.-M.
Il était temps que les menaces de Constant
arrêtassent en Orient la persécution qui avait lii. Violences
redoublé de violence après le concile de Sardique. des Ariens.
Les Ariens de Philippopolis, irrités contre les
habitants d'Andrinople qui rejetaient leur Ath. ad monach.
communion, s'en étaient plaints à Constance; et t. i, p. 354.
par les ordres de ce prince le comte Philagrius
avait fait trancher la tête à dix laïcs des plus considérables de la
ville. L'évêque Lucius fut de nouveau chargé de chaînes, et envoyé
en exil, où il mourut. Des diacres, des prêtres, des évêques avaient
été les uns proscrits, les autres rélégués dans les montagnes de
l'Arménie, ou dans les déserts de la Libye. On gardait les portes des
villes, pour en interdire l'entrée aux prélats rétablis par le vrai
concile. On envoya de la part de l'empereur aux magistrats
d'Alexandrie un ordre de faire mourir Athanase, s'il osait se
présenter pour rentrer en possession de son siége. On redoublait les
fouets, les chaînes, les tortures. Les catholiques fuyaient au désert;
quelques-uns feignaient d'apostasier. Ce fut au milieu de ce
désordre, que les lettres de Constant vinrent suspendre les coups
que son frère portait à l'église.
Constance ne se rendit pas d'abord. Son
incertitude lui attira une seconde lettre plus forte liii. Lettre de
que la précédente. Il connaissait le caractère vif et Constance à S.
bouillant de son frère; il ne doutait pas que ces Athanase.
menaces réitérées ne fussent bientôt suivies de
l'exécution. Dans cet embarras, il assemble Socr. l. 2, c. 23.
plusieurs évêques du parti, et leur demande
conseil. Ils sont d'avis de céder, plutôt que de Soz. l. 3, c. 20.
courir les risques d'une guerre civile. L'empereur
feint de s'adoucir. Il permet à Paul de retourner à
Constantinople. Il invite par lettre Athanase à le Philost. l. 3, c.
venir trouver, lui promettant non-seulement une 12.
sûreté entière et le rétablissement dans son église,
mais encore les effets les plus réels de sa bienveillance. Il lui
témoigne beaucoup de compassion sur ses malheurs, et lui fait des
reproches de ce qu'il n'a pas préféré de recourir à lui pour obtenir
justice. Cette feinte douceur n'était capable que d'inspirer de
nouveaux soupçons. Aussi Athanase ne se pressa pas d'y répondre.
Dans ces circonstances on découvrit un horrible complot qui
déshonora les Ariens, et qui fit pour quelques moments ouvrir les
yeux à leur aveugle protecteur.
Les deux évêques envoyés avec Salianus à
Constance, étaient Vincent de Capoue et liv. Insigne
Euphratas de Cologne. Étienne évêque d'Antioche fourberie
résolut de leur ôter tout crédit auprès de d'Étienne,
l'empereur, et de les perdre d'honneur à la face de évêque
d'Antioche.
toute la terre. Dans ce dessein il trama l'intrigue la
plus noire et la plus honteuse. Il avait à ses ordres
un jeune homme de la ville, dont il se servait pour Ath. ad monach.
maltraiter les catholiques. C'était un scélérat sans t. i, p. 355 et
pitié et sans pudeur. On lui avait donné le surnom 356.
d'Onagre, mot qui signifie âne sauvage, à cause
de sa pétulante férocité. L'évêque lui fait part de Theod. l. 2, c. 9-
son dessein, et n'a pas besoin de l'exciter à le 10.
remplir. Onagre va trouver une femme publique; il
lui dit qu'il est arrivé deux étrangers qui veulent passer la nuit avec
elle. Il convient avec quinze brigands semblables à lui, qu'ils se
placeront en embuscade autour de la maison où logeaient les deux
évêques. La nuit suivante Onagre conduit la courtisane: un
domestique qu'il avait corrompu par argent, tenait la porte ouverte.
Cette femme se glisse dans la chambre d'Euphratas: c'était un
vieillard vénérable; il s'éveille au bruit; et ayant demandé qui c'était,
comme il entend la voix d'une femme, il ne doute pas que ce ne soit
une illusion du diable, et se recommande à J.-C. Aussitôt Onagre
entre avec des flambeaux à la tête de sa troupe. La courtisane,
frappée de la vue d'un homme si respectable, et qu'elle reconnaît
pour un évêque, s'écrie qu'elle est trompée: on veut lui imposer
silence; elle crie plus fort: tous les valets accourent; Vincent qui
couchait dans une chambre voisine vient au secours de son
collègue: on ferme les portes; on arrête sept de ces misérables:
Onagre s'échappe avec les autres. Dès le point du jour les évêques
instruisent Salianus de cet attentat; ils vont ensemble au palais; les
prélats requièrent un jugement ecclésiastique: Salianus soutient
qu'un fait de cette nature est du ressort des tribunaux séculiers; il
demande une information juridique: il offre les domestiques des deux
évêques pour être appliqués à la question; et comme tout le
soupçon tombait sur Étienne dont Onagre était le ministre ordinaire,
il exige qu'Étienne représente aussi les siens. Celui-ci le refuse,
sous prétexte que ses domestiques étant clercs ne peuvent être mis
à la question. L'empereur est d'avis que l'information se fasse dans
l'intérieur du palais. On interroge d'abord la courtisane, qui déclare la
vérité: on s'adresse ensuite au plus jeune de ceux qui avaient été
arrêtés, il découvre tout le complot: Onagre est amené, et proteste
qu'il n'a rien fait que par les ordres d'Étienne: cet indigne prélat est
aussitôt déposé par les évêques qui se trouvent à Antioche.
L'empereur, irrité d'une si affreuse imposture,
rappelle d'exil les prêtres et les diacres lv. Constance
d'Alexandrie; il défend d'inquiéter ni les clercs ni invite de
les laïcs attachés à l'évêque Athanase. La guerre nouveau
Athanase.
des Perses qui commença alors à l'occuper tout
entier, ne lui fit pas perdre de vue le retour du
prélat. Dans sa marche même, étant à Edesse, il [Athan. apol.
lui écrivit une seconde lettre[157], dont il chargea cont. Arian. t. i,
p. 170.]
un prêtre d'Alexandrie: c'était apparemment un des
exilés qui revenait d'Arménie, et qui s'était
présenté à l'empereur. Constance pressait de Socr. l. 2, c. 23.
nouveau le saint évêque; il lui permettait de
prendre des voitures publiques pour se faire
conduire à la cour. Mais il était de retour à Theod. l. 2, c.
Antioche avant qu'Athanase se fût déterminé à le 10, 11.
venir trouver.
[157] Selon Socrate (l. 2, c. 23), Athanase était alors à Soz. l. 3, c. 19.
Aquilée.—S.-M.
Grégoire était mort à Alexandrie, et l'empereur
n'avait pas permis aux Ariens de lui nommer un An 349.
successeur. Enfin l'année suivante, sous le
consulat de Liménius et de Catulinus, Athanase, lvi. Athanase à
pressé par une troisième lettre de Constance, et Antioche.
par celles de plusieurs comtes, dont la bonne foi
lui était moins suspecte, se rend à tant de
sollicitations. Il va d'abord à Rome trouver le pape Idat. Chron.
Jules qui, transporté d'une sainte joie, écrit à
l'église d'Alexandrie pour la féliciter du retour de Ath. ad.
son évêque. De là il prend la route d'Antioche, où monach. t. i, p.
l'empereur affecta de réparer ses injustices 356 et 357. et
passées par l'accueil le plus honorable. La seule apol. contr.
Arian. t. i, p.
grace qui lui fut refusée, ce fut celle de confondre 171-174.
en face ses calomniateurs qui étaient à la cour.
Mais le prince lui promit avec serment de ne les
plus écouter en son absence. Constance écrit aux Socr. l. 2, c. 23.
Alexandrins, pour les exhorter à la concorde; il leur
recommande l'obéissance à leur évêque; il Theod. l. 2, c.
ordonne aux magistrats de punir les réfractaires; il 12.
déclare que l'union avec Athanase sera à ses yeux
le caractère du bon parti; il enjoint, par un ordre Soz. l. 3, c. 20
exprès, aux commandants de la ville et de la et 21.
province, d'annuler et d'effacer des registres
publics tous les actes et toutes les procédures
faites contre l'évêque et contre ceux de sa Phot. vit. Ath.
communion, et de rétablir le clergé d'Athanase cod. 257.
dans tous ses priviléges. On ne peut concevoir comment Constance
a pu sans rougir donner à la doctrine et aux mœurs du saint prélat
les éloges dont ces lettres sont remplies. Il entrait dans cette
conduite plus de crainte de Constant, que de sincérité et de véritable
repentir. Aussi voit-on ici ce prince se démentir lui-même. Il était
alors, autant que jamais, le jouet des Ariens, qui l'avaient tant de fois
trompé. Ce fut à leurs instances qu'ayant un jour fait appeler
Athanase: Vous voyez, lui dit-il, tout ce que je fais pour vous; faites à
votre tour quelque chose pour moi; je l'attends de votre
reconnaissance: de toutes les églises d'Alexandrie, je vous en
demande une pour ceux qui ne sont pas de votre communion.
Prince, lui répond Athanase sans se déconcerter, vous avez le
pouvoir d'exécuter ce que vous désirez; mais accordez-moi aussi
une grace. Je vous l'accorde, lui dit aussitôt Constance. Il y a ici à
Antioche, répliqua Athanase, beaucoup d'habitants séparés de la
communion de l'évêque; il est de votre justice que tout soit égal:
donnez-leur une église, comme vous en demandez une pour ceux
d'Alexandrie. Depuis la déposition d'Étienne, l'église d'Antioche était
gouvernée par Léonce, qui n'était pas moins livré à l'arianisme; et
les catholiques, appelés Eustathiens, étaient en grand nombre.
Constance, frappé de la présence d'esprit d'Athanase, ne put lui
répondre sans avoir consulté ses oracles ordinaires. Ceux-ci
jugèrent que par cette concession mutuelle leur parti perdrait
beaucoup plus à Antioche, qu'il ne gagnerait à Alexandrie, tant que
leur doctrine y trouverait un si puissant adversaire; et l'empereur se
désista de sa demande.
Dans le voyage d'Antioche à Alexandrie, Athanase
fut partout reçu avec honneur. Les évêques, lvii. Retour
excepté quelques Ariens, s'empressaient à lui d'Athanase à
témoigner leur respect. La plupart même de ceux Alexandrie.
qui l'avaient auparavant condamné ou abandonné,
revenaient à sa communion. Les prélats de Ath. apol. contr.
Palestine s'assemblèrent à Jérusalem; ils écrivirent Arian. t. i, p.
une lettre aux églises d'Égypte, de Libye, 175-177. ad
d'Alexandrie, pour les assurer qu'ils partageaient monach. p. 357-
359.
leur joie. A son arrivée ce fut une fête par toute
l'Égypte, mais une fête vraiment chrétienne. C'était
par l'imitation d'Athanase qu'on solennisait son Socr. l. 2, c. 24.
retour. On versait des aumônes abondantes dans
le sein des pauvres; les ennemis se réconciliaient; chaque maison
semblait une église; Alexandrie tout entière était
devenue un temple consacré aux actions de Soz. l. 3, c. 20
graces, et à la pratique des vertus. Tous les et seq.
évêques catholiques envoyaient à Athanase et
recevaient de lui des lettres de paix. Ursacius et Phot. vit. Ath.
Valens eux-mêmes lui écrivirent d'Aquilée, et lui cod. 257.
demandèrent sa communion. Ils venaient de
confirmer à Rome, en présence de Jules et de
plusieurs évêques, par une nouvelle protestation Pagi, ad Baron.
signée de leur main, l'anathème qu'ils avaient prononcé à Milan
contre la doctrine d'Arius; ils avaient de plus, par ce même acte,
déclaré fausses et calomnieuses toutes les accusations formées
contre Athanase: c'était confesser leur propre crime. L'Église
respirait après un orage de plus de sept années. Les évêques exilés
étaient rétablis; les Ariens quittaient en tumulte les siéges usurpés;
Macédonius, obligé de céder à Paul, ne conserva dans
Constantinople qu'une seule église. Cette paix qui était l'ouvrage de
Constant, fut bientôt troublée. Elle ne survécut pas à ce prince, dont
la mort fut l'effet d'une révolution soudaine, et la cause des plus
violentes agitations.

FIN DU LIVRE SIXIÈME ET DU TOME PREMIER.

 TABLE DES MATIÈRES CONTENUES
DANS LE TOME PREMIER DE
L'HISTOIRE DU BAS-EMPIRE.
Introduction Page 1.
LIVRE PREMIER.
1. Date de la naissance de Constantin. 2. Sa patrie. 3. Son origine.
4. Qualité de sa mère. 5. Noms de Constantin. 6. Ses premières
années. 7. Portrait de ce prince. 8. Sa chasteté. 9. Son savoir. 10.
Galérius est jaloux de Constantin. 11. Il cherche à le perdre. 12.
Constantin s'échappe des mains de Galérius. 13. Il joint son père.
14. Il lui succède. 15. Proclamation de Constantin. 16. Sépulture de
Constance. 17. Projets de Galérius. 18. Ses cruautés, 19; contre les
chrétiens, 20; contre les païens mêmes. 21. Rigueur des
impositions. 22. Les crimes de ses officiers doivent lui être imputés.
23. Il refuse à Constantin le titre d'Auguste et le donne à Sévère. 24.
Maxence élevé à l'empire. 25. Maximien reprend le titre d'Auguste.
26. Maximin ne prend point de part à ces mouvements. 27.
Occupations de Constantin. 28. Sa victoire sur les Francs. 29. Il
achève de les dompter. 30. Il met à couvert les terres de la Gaule.
31. Sévère trahi. 32. Sa mort. 33. Mariage de Constantin. 34.
Galérius vient assiéger Rome. 35. Il est contraint de se retirer. 36. Il
ruine tout sur son passage. 37. Maximien revient à Rome, d'où il est
chassé. 38. Maxence lui ôte le consulat. 39. Maximien va trouver
Constantin et ensuite Galérius. 40. Portrait de Licinius. 41. Dioclétien
refuse l'empire. 42. Licinius Auguste. 43. Maximin continue à
persécuter les chrétiens. 44. Punition d'Urbanus et de Firmilianus.
45. Maximin prend le titre d'Auguste. 46. Maximien consul. 47.
Alexandre est nommé empereur à Carthage. 48. Maximien quitte la
pourpre pour la seconde fois. 49. Il la reprend. 50. Constantin
marche contre lui. 51. Il s'assure de sa personne. 52. Mort de
Maximien. 53. Ambition et vanité de Maximien. 54. Consulats. 55.
Constantin fait des offrandes à Apollon. 56. Il embellit la ville de
Trèves. 57. Guerre contre les Barbares. 58. Nouvelles exactions de
Galérius. 59. Sa maladie. 60. Édit de Galérius en faveur des
chrétiens. 61. Mort de Galérius. 62. Différence de sentiments au
sujet de Galérius. 63. Consulats de cette année. 64. Partage de
Maximin et de Licinius. 65. Débauches de Maximin. 66. Maximin fait
cesser la persécution. 67. Délivrance des chrétiens. 68. Artifices
contre les chrétiens. 69. Édit de Maximin. 70. La persécution
recommence. 71. Passion de Maximin pour les sacrifices. 72.
Calomnies contre les chrétiens. 73. Divers martyrs. 74. Famine et
peste en Orient. 75. Guerre contre les Arméniens. 76. État du
christianisme en Italie. 77. Guerre contre Alexandre. 78. Défaite
d'Alexandre. 79. Désolation de l'Afrique. 80. Massacre dans Rome.
81. Avarice de Maxence. 82. Ses rapines. 83. Ses débauches. 84.
Mort de Sophronie. 85. Superstition de Maxence. 86. Constantin se
prépare à la guerre. 87. Il soulage la ville d'Autun. 88. Il retourne à
Trèves. 89. Outrages qu'il reçoit de Maxence. 90. Ils s'appuient tous
deux par des alliances. 91. Préparatifs de Maxence. 92. Forces de
Constantin. 93. Inquiétudes de ce prince. 94. Réflexions qui le
portent au christianisme. 95. Apparition de la croix. 96. Constantin
fait faire le labarum. 97. Culte de cette enseigne. 98. Protection
divine attachée au labarum. 99. Sur le lieu où parut ce prodige. 100.
Discussion sur la vérité de ce miracle. 101. Raisons pour le
combattre. 102. Raisons pour l'appuyer. 103. Constantin se fait
instruire. 104. Conversion de sa famille. 105. Fable de Zosime
réfutée. Page 23.
LIVRE DEUXIÈME.
1. Triomphe de la religion chrétienne. 2. Prise de Suze. 3. Bataille de
Turin. 4. Suites de la victoire. 5. Siége de Vérone. 6. Bataille de
Vérone. 7. Prise de Vérone. 8. Constantin devant Rome. 9. Maxence
se tient enfermé dans Rome. 10. Pont de bateaux. 11. Songe de
Constantin. 12. Sentiment de Lactance. 13. Bataille contre Maxence.
14. Fuite de Maxence. 15. Suites de la victoire. 16. Entrée de
Constantin dans Rome. 17. Fêtes, réjouissances, honneurs rendus à
Constantin. 18. Dispositions de Maximin. 19. Précautions de
Constantin. 20. Conduite sage et modérée après la victoire. 21. Lois
contre les délateurs. 22. Il répare les maux qu'avait fait Maxence. 23.
Libéralités de Constantin. 24. Embellissements et réparations des
villes. 25. Établissement des indictions. 26. Raisons de cet
établissement. 27. Conduite de Constantin par rapport au
christianisme. 28. Progrès du christianisme. 29. Honneurs que
Constantin rend à la religion. 30. Églises bâties et ornées. 31.
Constantin arrête la persécution de Maximin. 32. Consulats de cette
année. 33. Mariage de Licinius. 34. Mort de Dioclétien. 35. Édit de
Milan. 36. Guerre contre les Francs. 37. Constantin comble de
bienfaits l'église d'Afrique. 38. Exemption des fonctions municipales,
accordée aux clercs. 39. Abus occasionés par ces exemptions, et
corrigés par Constantin. 40. Lois sur le gouvernement civil. 41. Lois
pour la perception des tributs. 42. Lois pour l'administration de la
justice. 43. Maximin commence la guerre contre Licinius. 44. Licinius
vient à sa rencontre. 45. Bataille entre Licinius et Maximin. 46.
Licinius à Nicomédie. 47. Mort de Maximin. 48. Suites de cette mort.
49. Aventures de Valéria, de Prisca et de Candidianus. 50. Valéria
fuit Licinius, et est persécutée par Maximin. 51. Supplice de trois
dames innocentes. 52. Dioclétien redemande Valéria. 53. Mort de
Candidianus, de Prisca et de Valéria. 54. Jeux séculaires. 55. Paix
universelle de l'église. 56. Origine du schisme des Donatistes. 57.
Conciliabule de Carthage, où Cécilien est condamné. 58. Ordination
de Majorinus. 59. Constantin prend connaissance de cette querelle.
60. Concile de Rome. 61. Suites de ce concile. 62. Plaintes des
Donatistes. 63. Convocation du concile d'Arles. 64. Concile d'Arles.
65. Les Donatistes appellent du concile à l'empereur. Page 98.
LIVRE TROISIÈME.
1. Consuls de cette année. 2. Première guerre entre Constantin et
Licinius. 3. Bataille de Cibales. 4. Suites de cette bataille. 5. Bataille
de Mardie. 6. Traité de paix et de partage. 7. Loi en faveur des
officiers du palais. 8. Décennales de Constantin. 9. Révolte des Juifs
réprimée. 10. Lois en l'honneur de la croix. 11. Constantin en Gaule.
12. Il se détermine à juger de nouveau les Donatistes. 13. Nouveaux
troubles en Afrique. 14. Jugement rendu à Milan. 15.
Mécontentement des Donatistes. 16. Violences des Donatistes. 17.
Silvanus exilé et rappelé. 18. Le schisme dégénère en hérésie. 19.
Donatistes à Rome, 20. Circoncellions. 21. Constantin en Illyrie. 22.
Nomination des trois Césars. 23. Lactance chargé de l'instruction de
Crispus. 24. Naissance de Constance. 25. Éducation du jeune
Constantin, consul avec son père. 26. Persécution de Licinius. 27.
Victoire de Crispus sur les Francs. 28. Quinquennales des Césars.
29. Consuls. 30. Les Sarmates vaincus. 31. Pardon accordé aux
criminels. 32. Lois de Constantin. 33. Loi pour la célébration du
dimanche. 35. Loi en faveur du célibat. 35. Loi de tolérance. 36. Loi
en faveur des ministres de l'église. 37. Lois qui regardent les
mœurs. 38. Lois concernant les officiers du prince et ceux des villes.
39. Lois sur la police générale et sur le gouvernement civil. 40. Lois
sur l'administration de la justice. 41. Lois sur la perception des
impôts. 42. Lois pour l'ordre militaire. 43. Causes de la guerre entre
Constantin et Licinius. 44. Préparatifs de guerre. 45. Piété de
Constantin et superstition de Licinius. 46. Approches des deux
armées. 47. Harangue de Licinius. 48. Bataille d'Andrinople. 49.
Guerre sur mer. 50. Licinius passe à Chalcédoine. 51. Bataille de
Chrysopolis. 52. Suites de la bataille. 53. Mort de Licinius. Page 159.
LIVRE QUATRIÈME.
1. Aventures d'Hormisdas. 2. Il se réfugie auprès de Constantin. 3.
Récit de Zonare. 4. Constantin seul maître de tout l'empire. 5. Il
profite de sa victoire pour étendre le christianisme. 6. Lettre de
Constantin aux peuples d'Orient. 7. Il défend les sacrifices. 8. Édit de
Constantin pour tout l'Orient. 9. Tolérance de Constantin. 10. Piété
de Constantin, 11. Corruption de sa cour. 12. Discours de
Constantin. 13. Troubles de l'arianisme. 14. Commencements
d'Arius. 15. Son portrait. 16. Progrès de l'arianisme. 17. Premier
concile d'Alexandrie contre Arius. 18. Eusèbe de Nicomédie. 19.
Eusèbe de Césarée. 20. Mouvements de l'arianisme. 21. Concile en
faveur d'Arius. 22. Lettre de Constantin à Alexandre et à Arius. 23.
Second concile d'Alexandrie. 24. Généreuse réponse de Constantin.
25. Convocation du concile de Nicée. 26. Occupation de Constantin
jusqu'à l'ouverture du concile. 27. Les évêques se rendent à Nicée.
28. Évêques orthodoxes. 29. Évêques ariens. 30. Philosophes
païens confondus. 31. Trait de sagesse de Constantin. 32.
Conférences préliminaires. 33. Séances du concile. 34. Constantin
au concile. 35. Discours de Constantin. 36. Liberté du concile. 37.
Consubstantialité du Verbe. 38. Jugement du concile. 39. Question
de la Pâque terminée. 40. Réglement au sujet des Mélétiens et des
Novatiens. 41. Canons et symbole de Nicée. 42. Lettres du concile
et de Constantin. 43. Vicennales de Constantin. 44. Conclusion du
concile. 45. Exil d'Eusèbe et de Théognis. 46. Saint Athanase,
évêque d'Alexandrie 47. Lois de Constantin. 48. Mort de Crispus. 49.
Mort de Fausta. 50. Insultes que Constantin reçoit à Rome. 51.
Constantin quitte Rome pour n'y plus revenir. 52. Consuls. 53.
Découverte de la croix. 54. Église du saint Sépulcre. 55. Piété
d'Hélène. 56. Retour d'Hélène. 57. Sa mort. 58. Guerres contre les
Barbares. 59. Destruction des idoles. 60. Temple d'Aphaca. 61.
Autres débauches et superstitions abolies. 62. Chêne de Mambré.
63. Églises bâties. 64. Arad et Maïuma deviennent chrétiennes. 65.
Conversions des Éthiopiens et des Ibériens. 66. Établissement des
monastères. 67. Restes de l'idolâtrie. 68. Date de la fondation de
Constantinople. 69. Motifs de Constantin pour bâtir une nouvelle
ville. 70. Il veut bâtir à Troie. 71. Situation de Byzance. 72. Abrégé
de l'histoire de Byzance jusqu'à Constantin. 73. État du christianisme
à Byzance. 74. Nouvelle enceinte de C. P. 75. Bâtiments faits à
Constantinople. 76. Places publiques. 77. Palais. 78. Autres
ouvrages. 79. Statues. 80. Églises bâties. 81. Égouts de
Constantinople. 82. Prompte exécution de ces ouvrages. 83.
Maisons bâties à Constantinople. 84. Nom et division de
Constantinople. Page 222.
LIVRE CINQUIÈME.
1. Changement dans le gouvernement. 2. Dédicace de C. P. 3.
Précautions de Constantin pour la subsistance de C. P. 4.
Chrysargyre. 5. Priviléges de C. P. 6. Autres établissements. 7.
Nouvel ordre politique. 8. Nouvelle division de l'empire. 9. Quatre
préfets du prétoire établis. 10. Des maîtres de la milice. 11. Patrices.
12. Des ducs et des comtes. 13. Multiplication des titres. 14. Luxe de
Constantin. 15. Suite de l'histoire de Constantin. 16. Guerre contre
les Goths. 17. Sarmates vaincus. 18. Delmatius consul. 19. Peste et
famine en Orient. 20. Mort de Sopater. 21. Ambassades envoyées à
Constantin. 22. Lettre de Constantin à Sapor. 23. Préparatifs de
guerre faits par les Perses. 24. Constantin écrit à saint Antoine. 25.
Constant César. 26. Consuls. 27. Les Sarmates chassés par leurs
esclaves. 28. Consuls. 29. Tricennales de Constantin. 30. Delmatius
César. 31. Partage des états de Constantin. 32. Comète. 33.
Consuls. 34. Mariage de Constance. 35. Ambassade des Indiens.
36. Rappel d'Arius. 37. Retour d'Eusèbe et de Théognis. 38.
Déposition d'Eustathius. 39. Troubles d'Antioche. 40. Eusèbe de
Césarée refuse l'évêché d'Antioche. 41. Athanase refuse de recevoir
Arius. 42. Calomnies contre Athanase. 43. Accusation au sujet
d'Arsénius. 44. Eusèbe s'empare de l'esprit de l'empereur. 45.
Concile de Tyr. 46. Accusateurs confondus. 47. Conclusion du
Concile de Tyr. 48. Dédicace de l'église du Saint-Sépulcre. 49.
Concile de Jérusalem. 50. Athanase s'adresse à l'empereur. 51. Exil
d'Athanase. 52. Concile de C. P. 53. Efforts d'Eusèbe pour faire
recevoir Arius par Alexandre. 54. Mort d'Arius. 55. Constantin refuse
de rappeler Athanase. 56. Lois contre les hérétiques. 57. Loi sur la
juridiction épiscopale. 58. Lois sur les mariages. 59. Autres lois sur
l'administration civile. 60. Les Perses rompent la paix. 61. Maladie
de Constantin. 62. Son baptême. 63. Vérité de cette histoire. 64.
Mort de Constantin. 65. Deuil de sa mort. 66. Ses funérailles. 67.
Fidélité des légions. 68. Inhumation de Constantin. 69. Deuil à
Rome. 70. Honneurs rendus à sa mémoire par l'église. 71.
Caractère de Constantin. 72. Reproches mal fondés de la part des
païens. 73. Ses filles. Page 309.
LIVRE SIXIÈME.
1. Caractère des fils de Constantin. 2. Massacre des frères et des
neveux de Constantin. 3. Autres Massacres. 4. Crédit de l'eunuque
Eusèbe. 5. Suites de la mort de Delmatius et d'Hanniballianus. 6.
Nouveau partage. 7. Rétablissement de saint Athanase. 8. Rappel
de saint Paul de Constantinople. 9. Constance retourne en Orient.
10. Antiquités de Nisibe. 11. Sapor lève le siége de Nisibe. 12.
Préparatifs pour la guerre de Perse. 13. Première expédition de
Constance. [14. Révolutions arrivées en Arménie.] 15. Troubles de
l'arianisme. 16. Mort d'Eusèbe de Césarée. 17. Consulat
d'Acyndinus et de Proculus. 18. Mort du jeune Constantin. 19. Lois
des trois princes. 20. Nouvelles calomnies contre saint Athanase.
21. Concile d'Antioche. 22. Grégoire intrus sur le siége d'Alexandrie.
23. Violences à l'arrivée de Grégoire. 24. Précaution pour cacher ces
excès à l'empereur. 25. Les catholiques maltraités par toute l'Égypte.
26. Violences exercées ailleurs. 27. Athanase va à Rome. 28. Paul
rétabli et chassé de nouveau. 29. Athanase va trouver Constant. 30.
Synode de Rome. 31. Amid fortifiée. 32. Terrible tremblement de
terre. 33. Courses des Francs. 34. Ils sont réprimés par Constant.
35. Constant dans la Grande-Bretagne. 36. Tremblements de terre.
37. Conversion des Homérites. 38. Inquiétudes des Ariens. 39.
Marche de Constance vers la Perse. 40. Port de Séleucie. 41.
Sédition à Constantinople. 42. Concile de Milan. 43. Concile de
Sardique. 44. Les Ariens se séparent. 45. Jugement du concile. 46.
Faux concile de Sardique. 47. Concile de Milan. 48. Députés
envoyés à Constance. 49. Guerre des Perses. 50. Bataille de
Singara. 51. Nouveaux troubles des Donatistes apaisés en Afrique.
52. Violences des Ariens. 53. Lettres de Constance à saint
Athanase. 54. Insigne fourberie d'Étienne, évêque d'Antioche. 55.
Constance rappelle de nouveau saint Athanase. 56. Athanase à
Antioche. 57. Retour d'Athanase à Alexandrie. Page 392.

FIN DE LA TABLE DU TOME PREMIER.

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