Elsevier S & T

Methods for Phase Diagram Determination

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Table of contents
  • Copyright Pageiv
  • Table of Contentsv
  • Prefacevii
  • Chapter 1 Introduction to Phase Diagrams1
  • 1 Introduction1
  • 2 J. Willard Gibbs and the First Equilibrium Diagram3
  • 3 Twentieth Century Developments5
  • 4 The CALPHAD Method and Its Need for Data8
  • 5 Thermodynamic Constraints on Phase Diagrams10
  • 6 Experimental Considerations17
  • References20
  • Chapter 2 The Role of Phase Transformation Kinetics in Phase Diagram Determination and Assessment22
  • 1 Introduction22
  • 2 Phase Transformation Kinetics During Cooling and Heating as Related to Phase Diagram Determination24
  • 2.1 Shifting of Transformation-Start Temperature with Cooling Rate26
  • 2.2 Formation of Metastable Phases During Cooling27
  • 2.3 Shifting of Transformation-Start Temperature with Heating Rate30
  • 2.4 Analyses of Examples from Cooling and Heating Experiments35
  • 3 Isothermal Phase Transformation Kinetics as Related to Phase Diagram Determination41
  • 3.1 Precipitation of Phases from Quenched Alloys41
  • 3.2 Kinetics and Phase Formation in Diffusion Couples/Multiples46
  • 4 Concluding Remarks48
  • Acknowledgments48
  • References49
  • Chapter 3 Correct and Incorrect Phase Diagram Features51
  • 1 Introduction52
  • 2 Phase Rule Violations53
  • 2.1 Typical Phase Rule Violations53
  • 3 Guidelines for Finding Less Obvious Phase Diagram Errors56
  • 3.1 Problems Connected with Phase Boundary Curvatures56
  • 3.2 Summary of Improbable Phase Diagram Situations57
  • 3.3 Van’t Hoff Relationship and Charles’ Law59
  • 3.4 Form of the Liquidus of a Compound Near a Pure Element Side61
  • 3.5 Sharpness of the Liquidus of a Compound and its Relation to a Possible Eutectoid Temperature63
  • 3.6 Two Compounds with Very Similar Compositions Are Unlikely to Coexist in a Wide Temperature Range65
  • 3.7 Asymmetry of the Liquidus Around the Melting Point of a Compound65
  • 3.8 Narrowing of the Width of a Two-Phase Field When the Boundaries Are Extrapolated Toward Higher T68
  • 3.9 An Abrupt Change of Slope70
  • 3.10 An Excessive Slope Change Associated with a Polymorphic Transformation72
  • 3.11 Shape of a Miscibility Gap73
  • 3.12 Displaced Miscibility Gap74
  • 3.13 An Inverse Miscibility Gap76
  • 3.14 Almost Symmetric Syntectic Reaction76
  • 3.15 Metastable Melting Point of a Pure Element77
  • 4 Examples of Phase Diagrams with Improbable Features79
  • 4.1 Ag–Pr80
  • 4.2 Al–B80
  • 4.3 Al–Mn82
  • 4.4 Al–Pu82
  • 4.5 Al–Se83
  • 4.6 Au–La83
  • 4.7 Au–U84
  • 4.8 B–Bi86
  • 4.9 B–W86
  • 4.10 C–Ge87
  • 4.11 Ca–Eu87
  • 4.12 Ce–Pr87
  • 4.13 Cr–Ni89
  • 4.14 Cu–Hf90
  • 4.15 Ir–Rh92
  • 4.16 Lu–Th92
  • 4.17 Mg–Sb92
  • 4.18 Mn–Y94
  • 4.19 Mo–Ru94
  • 4.20 Nd–Pu96
  • 4.21 Ni–Sr96
  • 4.22 Np–Zr97
  • 4.23 Pd–Zr97
  • 4.24 Pt–Zr99
  • 5 Unusual but Correct Phase Diagrams100
  • 5.1 Apparent Four-Phase Equilibrium100
  • 5.2 Apparent Five-Phase Equilibrium100
  • 5.3 Pointed Liquidus102
  • 5.4 A Straight Line Liquidus102
  • 5.5 Off-Stoichiometric Melting104
  • 6 Phase Diagram Below 0°C105
  • 7 Conclusion105
  • References105
  • Chapter 4 Determination of Phase Diagrams Using Equilibrated Alloys108
  • 1 Introduction108
  • 2 Alloy Preparation109
  • 2.1 High-Temperature Melting of Alloys109
  • 2.2 Arc Melting110
  • 2.3 Induction Melting111
  • 2.4 Powder Metallurgy Method112
  • 3 Homogenization Heat Treatment113
  • 4 Determination of Phase Equilibria: Isothermal Experiments vs. Cooling/Heating Experiments114
  • 4.1 Analysis of Quenched Samples to Construct Isothermal Sections (Static Method)115
  • 4.2 Analysis of Samples by Heating and Cooling Experiments to Construct Vertical Sections and Liquid122
  • 5 Examples of Phase Diagram Determination Using Equilibrated Alloys129
  • 5.1 The Cu–Nd Binary System130
  • 5.2 The Al–Be–Si Ternary System131
  • 5.3 The Al–Mn–Si Ternary System135
  • 5.4 Multicomponent Phase Diagram and the Al–C–Si–Ti System137
  • 6 Crystal Structure Identification of New Phases140
  • 7 Pitfalls145
  • 7.1 Verification of the Establishment of True Equilibrium145
  • 7.2 Inconsistency Between the Result from DTA Measurement and that from XRD and Microscopy Observati147
  • 7.3 Identification of Degenerated Phase Equilibrium148
  • References149
  • Chapter 5 DTA and Heat-Flux DSC Measurements of Alloy Melting and Freezing151
  • 1 Introduction152
  • 1.1 Focus of this Chapter152
  • 1.2 Information Sought from DTA/Heat-Flux DSC Measurements153
  • 1.3 Relevant Standards154
  • 1.4 Major Points155
  • 2 Instruments and Operation155
  • 2.1 Variations Among Instruments155
  • 2.2 Samples159
  • 2.3 Reference Materials164
  • 2.4 Calibration and DTA Signal from Pure Metals164
  • 2.5 Major Points169
  • 3 Analysis of DTA Data for Binary Alloys169
  • 3.1 General Behavior for a Binary Eutectic System: Example Ag–Cu Alloy Melting171
  • 3.2 Problems with Solidus Determination on Heating177
  • 3.3 Problems with Liquidus Determination on Heating180
  • 3.4 Supercooling Problem with Liquidus Determination on Cooling186
  • 3.5 Eutectic Reactions vs. Peritectic Reactions191
  • 3.6 Major Points192
  • 4 Analysis of DTA Data for Ternary Alloys194
  • 4.1 Al-Rich Corner of Al–Cu–Fe Phase Diagram194
  • 4.2 Al–20% Cu–0.5% Fe195
  • 4.3 Al–6% Cu–0.5% Fe197
  • 4.4 Major Points200
  • 5 Concluding Remarks200
  • Appendix A: Glossary201
  • Appendix B: Recommended Reading204
  • Appendix C: Model for Simulating DTA Response for Melting and Solidification of Materials with Known205
  • Appendix D: Expressions for the Rate Dependence of Melting Onset Temperatures for a Pure Metal208
  • Appendix E: Enthalpy vs. Temperature Relations for Dilute Binary Solid Solution Alloy211
  • Appendix F: Binary Phase Diagrams and DTA Response213
  • Appendix G: Tutorial on Melting and Freezing of Multicomponent Alloys213
  • G.1 Aluminum Alloy 2219213
  • G.2 Udimet 700218
  • References220
  • Chapter 6 Application of Diffusion Couples in Phase Diagram Determination222
  • 1 Introduction222
  • 2 General Principles of the Diffusion Couple Method223
  • 3 Experimental Procedures225
  • 3.1 Preparation of Diffusion Couples225
  • 3.2 Analytical Techniques and Specimen Preparation226
  • 3.3 Preparation of Diffusion Couple Specimens for EPMA227
  • 4 Variations of the Diffusion Couple Technique228
  • 5 Error Sources Encountered in the Diffusion Couple Experiments236
  • 6 Concluding Remarks244
  • References244
  • Chapter 7 Phase Diagram Determination Using Diffusion Multiples246
  • 1 Introduction246
  • 2 Diffusion-Multiple Fabrication248
  • 3 Analysis of Diffusion Multiples and Extraction of Phase Diagram Data256
  • 3.1 Imaging Examination and Phase Analysis256
  • 3.2 EPMA Profiling257
  • 3.3 Extraction of Equilibrium Tie Lines259
  • 4 Sources of Errors266
  • 5 Concluding Remarks269
  • Acknowledgments271
  • References272
  • Chapter 8 Application of Computational Thermodynamics to Rapidly Determine Multicomponent Phase Diag273
  • 1 Introduction273
  • 2 Ternary Mg–Al–Sr System275
  • 2.1 Experimental Method276
  • 2.2 Thermodynamic Models276
  • 2.3 Experimental Results and Discussion277
  • 3 Quaternary Mo–Si–B–Ti System282
  • 4 Concluding Remarks289
  • Acknowledgment290
  • References290
  • Chapter 9 Determination of Phase Diagrams with Reactive or Volatile Elements292
  • 1 Introduction293
  • 2 Solid–Solid Equilibria299
  • 2.1 Thermal Analysis299
  • 2.2 Zone Melting300
  • 2.3 Microstructural Analysis of Quenched Samples301
  • 2.4 X-Ray Diffraction302
  • 2.5 Densitometry302
  • 2.6 Dilatometry303
  • 2.7 Interdiffusion303
  • 2.8 Hardness304
  • 2.9 Calorimetry304
  • 2.10 Electrical Resistivity305
  • 2.11 Superconductivity305
  • 2.12 Electromotive Force306
  • 2.13 Coulometric Titration307
  • 2.14 Galvanic Polarization309
  • 2.15 Magnetic Susceptibility310
  • 2.16 Vapor Pressure311
  • 2.17 Gaseous Thermal Extraction314
  • 3 Solid–Liquid Equilibria315
  • 3.1 Weight Loss of a Solid After Equilibration with a Liquid315
  • 3.2 Chemical Analysis of a Separated Liquid316
  • 3.3 Chemical Analysis of Quenched Samples318
  • 3.4 Thermal Analysis319
  • 3.5 Electromotive Force320
  • 3.6 Electrical Resistivity321
  • 3.7 Anodic Oxidation321
  • 3.8 Magnetic Susceptibility323
  • 3.9 Densitometry325
  • 3.10 Enthalpy of Dilution325
  • 3.11 Kinetics of Alloy Decomposition or Formation325
  • 3.12 Diffusion Coefficient327
  • 3.13 Vapor Pressure327
  • 3.14 X-Ray Absorption Spectrometry327
  • 3.15 Viscosity328
  • 3.16 Optical Reflectivity328
  • 3.17 Corrosion Tests328
  • 3.18 Motion of Liquid Metal Inclusions in Ionic Crystals330
  • 4 Liquid–Liquid Equilibria330
  • 4.1 Chemical Analysis of Separated Liquids330
  • 4.2 Thermal Analysis330
  • 4.3 Calorimetry331
  • 4.4 Densitometry by X-Ray Attenuation332
  • 4.5 Neutron Transmission332
  • 4.6 Electromotive Force332
  • 4.7 Electrical Resistivity332
  • 4.8 Magnetic Susceptibility333
  • 4.9 Vapor Pressure333
  • 5 Solid–Vapor Equilibria334
  • 5.1 Vapor Pressure334
  • 5.2 Thermogravimetry335
  • 6 Liquid–Vapor Equilibria336
  • 6.1 Vapor Pressure336
  • 7 Liquid–Fluid Equilibria337
  • 8 Concluding Remarks337
  • References338
  • Chapter 10 Phase Diagram Determination of Ceramic Systems341
  • 1 Introduction341
  • 2 Ex Situ Methods342
  • 2.1 Sample Preparation and Equilibration343
  • 2.2 Phase and Compositional Analysis350
  • 2.3 Identification of New Phases354
  • 3 In Situ Methods354
  • 3.1 Thermal Analysis355
  • 3.2 Coulometric Titration356
  • 3.3 High-Temperature X-Ray Diffraction358
  • 3.4 Thermomicroscopy and Other Optical Techniques358
  • 3.5 Oscillation Method of Phase Analysis358
  • 3.6 In Situ Electrical, Dielectric, and Magnetic Measurements359
  • 4 Concluding Remarks359
  • References359
  • Chapter 11 Determination of Phase Diagrams Involving Order–Disorder Transitions361
  • 1 Introduction361
  • 2 ER and Thermal Analysis Methods362
  • 2.1 ER Method (Resistometric Study)362
  • 2.2 Thermal Analysis364
  • 3 Singular Point Method366
  • 3.1 Origin of Singularity366
  • 3.2 Examples of SPM368
  • 4 Concentration Gradient Method374
  • 4.1 Basics of CGM376
  • 4.2 Examples of CGM376
  • 5 Concluding Remarks380
  • References382
  • Chapter 12 Determination of Phase Diagrams Involving Magnetic Transitions383
  • 1 Introduction383
  • 2 The Basics of Magnetism and the Traditional Methods of Mapping Magnetic Phase Diagrams384
  • 2.1 Basics of Magnetism384
  • 2.2 Measurements of Magnetism385
  • 2.3 Effects of Magnetism on Phase Diagrams389
  • 3 Combinatorial and High-Throughput Mapping of Magnetic Phase Diagrams396
  • 3.1 Introduction to the Combinatorial Approach396
  • 3.2 Combinatorial Mapping of Magnetic Phase Diagrams in Metallic Systems396
  • 3.3 Combinatorial Mapping of Oxide Systems404
  • 4 Concluding Remarks409
  • Acknowledgments409
  • References409
  • Chapter 13 Determination of Pressure-Dependent Phase Diagrams412
  • 1 Introduction412
  • 2 High-Pressure Devices413
  • 2.1 Diamond-Anvil Cells413
  • 2.2 Large-Volume Presses416
  • 3 Pressure Measurement418
  • 3.1 Pressure Measurement Using Ruby Fluorescence418
  • 3.2 Pressure Measurement Using X-Rays419
  • 4 High Pressure and Temperature421
  • 4.1 X-Rays at High Pressure421
  • 4.2 Heating at High Pressure in a DAC422
  • 5 Examples of Phase Diagrams Determined Using LVPs431
  • 5.1 Phase Relations in Univariant Systems432
  • 5.2 Phase Relations in Complex Systems434
  • 6 Phase Diagrams Using DAC436
  • 7 Industrial Solids438
  • Acknowledgments438
  • References439
  • Chapter 14 The Determination of Phase Diagrams For Slag Systems442
  • 1 Introduction442
  • 2 The CaO–Al[sub(2)]O[sub(3)]–SiO[sub(2)] System443
  • 2.1 The CaO–SiO[sub(2)] System443
  • 2.2 The Al[sub(2)]O[sub(3)]–SiO[sub(2)] System447
  • 2.3 The CaO–Al[sub(2)]O[sub(3)]–SiO[sub(2)] System452
  • 3 The CaO–"FeO"–SiO[sub(2)] System453
  • 4 The FeO-Fe[sub(2)]O[sub(3)]-SiO[sub(2)] System455
  • References457
  • Chapter 15 Determination of Phase Diagrams for Hydrogen-Containing Systems459
  • 1 Introduction459
  • 2 Phase Diagram Representations of M–H Systems462
  • 2.1 Binary M–H Systems462
  • 2.2 Multi-component Systems466
  • 3 Some Useful Rules Relating Phase Diagrams and Reaction Enthalpies for M–H Systems471
  • 4 Techniques Employed for Phase Diagram Determination of M–H Systems473
  • 4.1 Open Systems474
  • 4.2 Closed Systems477
  • 4.3 Electron Diffraction and TEM480
  • 4.4 Magnetic Susceptibility480
  • 4.5 Electric Resistivity480
  • 4.6 Dilatometry480
  • Acknowledgements481
  • References481
  • Chapter 16 Miscellaneous Topics on Phase Diagrams483
  • 1 Introduction483
  • 2 Ever-Increasing Interplay of Modeling and Experiment484
  • 3 Phase Diagrams for Functional Materials485
  • 4 High-Throughput Approaches to Phase Diagram Determination486
  • 5 Low-Temperature Phase Diagrams487
  • 6 Phase Diagram Determination: A Never-Ending Task488
  • 7 Some Suggestions489
  • Further Reading490
  • General Phase Diagram Introduction490
  • Specimen Purity and Preparation490
  • Diffusion as Related to Phase Diagrams and Phase Diagram Determination490
  • Interplay of Ordering, Magnetic Transitions, and Phase Equilibria491
  • Ceramic Phase Diagram Determination491
  • Theoretical/Modeling Work491
  • The CALPHAD Approach491
  • Miscellaneous Recommended Papers on Phase Diagram Determination491
  • Some Current Phase Diagram Compilations492
  • Elemental and Metallic Systems492
  • Ceramic Systems493
  • Other Miscellaneous Compilations/Books493
  • Some Useful Websites493
  • References494
  • Index495
  • A495
  • B495
  • C495
  • D496
  • E497
  • F498
  • G498
  • H498
  • I499
  • K500
  • L500
  • M500
  • N501
  • O501
  • P501
  • Q503
  • R504
  • S504
  • T505
  • U505
  • V505
  • W505
  • X505
  • Z505
  • Color Plates507
Book details
  • Vendor Elsevier S & T
  • SKU 9780080446295
  • ISBN-13 9780080549965

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Phase diagrams are "maps" materials scientists often use to design new materials. They define what compounds and solutions are formed and their respective compositions and amounts when several elements are mixed together under a certain temperature and pressure. This monograph is the most comprehensive reference book on experimental methods for phase diagram determination. It covers a wide range of methods that have been used to determine phase diagrams of metals, ceramics, slags, and hydrides.

* Extensive discussion on methodologies of experimental measurements and data assessments
* Written by experts around the world, covering both traditional and combinatorial methodologies
* A must-read for experimental measurements of phase diagrams