Abstract
Precipitation age hardening (T6) response of Al-5.8Zn-2.2Mg-2.5Cu alloy in near-net-shaped cast condition was investigated. Cast samples were manufactured using the controlled diffusion solidification (CDS) technology combined with a metallic mold tilt pour gravity casting process. This study was conducted using (1) non-isothermal aging during differential scanning calorimetry (DSC) experiments and (2) isothermal aging during which transient bulk and micro-hardness measurements taken at four aging temperatures of 343, 393, 433 and 473 K. A detailed microstructural investigation combined with a quantitative image analysis was carried out on both DSC and hardness specimens using high-resolution electron microscopy (HREM) and energy-dispersive spectroscopy (EDS) elemental mappings. Hardness measurements were analyzed using a kinetic modeling approach (single state variable combined with a kinetic equation that is valid for the Al-Zn-Mg-Cu alloys). The results confirm the formation of hardening phases of GP zone, intermediate hardening metastable phase η′ and equilibrium phase η. The results of calorimetric measurements, electron microscopy and selected area diffraction patterns are in good agreement and confirm transient precipitation/dissolution sequences. A mean value of activation energy \(Q_{\text{A}}\) of 75 kJ/mol was evaluated for combined bulk diffusion rate of alloying elements during precipitation of strengthening phases within Al matrix.
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Notes
The nominal composition of the material was (at.%): 96.08 Al, 2.30 Zn, 1.38 Mg and 0.09 Si, with Cu, Fe and Mn in the remainder.
Al-6.4Zn-2.2 Mg-2.3Cu (wt.%).
Al-8.5Zn-1.9 Mg-2.2Cu (wt.%).
ImageJ, Image processing and Analysis in Java, 1.42q Java 1.6.0 (32 bits) (https://imagej.net)
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Al-5.5Zn-0.80 Mg-0.16Zr [0.016Cu-0.010Mn-0.008Ti-0.002Cr-0.17Fe-0.05Si] (composition is in wt.%, and minor elements appear in brackets)
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References
D. Saha, S. Shankar, D. Apelian, and M.M. Makhlouf, Casting of Aluminum-Based Wrought Alloys Using Controlled Diffusion Solidification, Metall. Mater. Trans. A, 2004, 35, p 2174–2180
A.A. Khalaf, P. Ashtari, and S. Shankar, Formation of Non-dendritic Primary Al Phase in Hypoeutectic Alloys in CDS: a Hypothesis, Metall. Mater. Trans. B, 2009, 40, p 843–849
A.A. Khalaf and S. Shankar, Favorable Environment for a Nondendritic Morphology in Controlled Diffusion Solidification, Metall. Mater. Trans. A, 2011, 42, p 2456–2465
A.A. Khalaf and S. Shankar, Effect of Mixing Rate on the Morphology of Primary Al Phase in the Controlled Diffusion Solidification (CDS) Process, J. Mater. Sci., 2012, 47, p 8153–8166
K. Symeonidis, The Controlled Diffusion Solidification Process: Fundamentals and Principles, Ph.D. Dissertation, Worcester Polytechnic Institute (WPI), 2009
A.A. Khalaf, Controlled Diffusion Solidification: Process Mechanism and Parameter Study, Ph.D. Dissertation, McMaster University, 2010
A.A. Khalaf, Mechanism of Controlled Diffusion Solidification: Mixing, Nucleation and Growth, Acta Mater., 2016, 103, p 301–310
W.A. Tiller, K.A. Jackson, J.W. Rutter, and B. Chalmers, The Redistribution of Solute Atoms During the Solidification of Metals, Acta Metall., 1953, 1(4), p 428–437
D.A. Porter, K.E. Easterling, Phase Transformations in Metals And Alloys. In: Interphase Interfaces, 1st Ed., Von Nostard Reinhold Company, New York, 1981, p 152
R. Ghiaasiaan, and S. Shankar, Effect of Alloy Composition on Microstructure and Tensile Properties of Net-Shaped Castings of Al–Zn–Mg–Cu Alloys, Int. J. Metalcasting, 2019, 13(2), p 300–310
R. Ghiaasiaan, X. Zeng, and S. Shankar, Controlled Diffusion Solidification (CDS) of Al-Zn-Mg-Cu (7050): Microstructure, Heat Treatment and Mechanical Properties, Mater. Sci. Eng. A, 2014, 594, p 260–277
R. Ghiaasiaan, B. Shalchi-Amirkhiz, and S. Shankar, Quantitative Metallography of Precipitating and Secondary Phases After Strengthening Treatment of Net Shaped Casting of Al-Zn-Mg-Cu (7000) Alloys, Mater. Sci. Eng. A, 2017, 698, p 206–217
R. Ghiaasiaan and S. Shankar, Structure-Property Models in Al-Zn-Mg-Cu Alloys: A Critical Experimental Assessment of Shape Castings, Mat. Sci. Eng. A, 2018, 733, p 235–245
I.J. Polmear, Light Alloys From Traditional Alloys to Nano-crystals, Fourth ed., Butterworth-Heinemann is an imprint of Elsevier, Jordan Hill, Oxford, 2006
L.F. Mondolfo, Structure of Aluminum : Magnesium: Zinc Alloys, Metal. Rev., 1971, 95, p 94–124
H. Loffler, I. Kovacs, and J. Lendvai, Review Decomposition Processes in AI-Zn-Mg Alloys, J. Mater. Sci., 1983, 18, p 2215–2240
F.X. Gang, J.D. Ming, M.Q. Chang, Z.B. You, and W. Tao, Evolution of Eutectic Structures in Al-Zn-Mg-Cu Alloys During Heat Treatment, Trans. Nonferr. Met. Soc. China, 2006, 16, p 577–581
D. Dumont, A. Deschamps, Y. Bréachet, C. Sigli, and J.C. Ehrstrom, Characterisation of Precipitation Microstructures in Aluminum Alloys 7040 and 7050 and Their Relationship to Mechanical Behavior, Mater. Sci. Technol., 2004, 20, p 567–576
Maria D. David, Robin D. Foley, John A. Griffin, and Charles A. Monroe, Microstructural Characterization and Thermodynamic Simulation of Cast Al–Zn–Mg–Cu Alloys, Int. J. Metalcasting, 2016, 10(1), p 2–20
L.K. Berg, J. Gjønnes, V. Hansen, X.Z. Li, M. Knutson-Wedel, G. Waterloo, D. Schryvers, and L.R. Wallenberg, GP-Zones in Al-Zn-Mg Alloys and Their Role in artificial ageing, Acta Mater., 2001, 49, p 3443–3451
W.D. Calister, Jr, and D.G. Rethwisch, Material Science and Engineering: An Introduction, 8th ed., Wiley, New York, 2010
J.E. Hatch, Aluminum Properties and Physical Metallurgy, American Society for Metals (ASM), First Printing, Ohio, 1984
A. Deschamps, A. Bigot, F. Livet, P. Auger, Y. Bréachet, and D. Blavette, A Comparative Study of Precipitate Composition and Volume Fraction in an Al–Zn–Mg Alloy Using Tomographic Atom Probe and Small-Angle X-Ray Scattering, Philos. Mag., 2001, 81(10), p 2391–2414
S.K. Maloney, K. Hono, I.J. Polmear, and S.P. Ringer, The Effects of a Trace Addition of Silver Upon Elevated Temperature Ageing of an Al+Zn+Mg Alloy, Micron, 2001, 32, p 741–747
J.A. Wert, Identification of Precipitates In 7075 After High-Temperature Aging, Scr. Metal., 1981, 15, p 445–447
T. Engdahl, V. Hansen, P.J. Warren, and K. Stiller, Investigation of Fine Scale Precipitates in Al–Zn–Mg Alloys After Various Heat Treatments, Mater. Sci. Eng. A, 2002, 327, p 59–64
G. Sha and A. Cerezo, Early-Stage Precipitation in Al–Zn–Mg–Cu Alloy (7050), Acta Mater., 2004, 52, p 4503–4516
K. Stiller, P.J. Warren, V. Hansen, J. Angenete, and J. Gjønnes, Investigation of Precipitation in an Al–Zn–Mg Alloy After Two-Step Ageing Treatment at 100° and 150°C, Mater. Sci. Eng. A, 1999, 270, p 55–63
N.Q. Chinh, J. Lendvai, D.H. Ping, and K. Hono, The Effect of Cu on Mechanical and Precipitation Properties of Al–Zn–Mg Alloys, J. Alloys Compd., 2004, 378, p 52–60
T. Marlaud, A. Deschamps, F. Bley, W. Lefebvre, and B. Baroux, Influence of Alloy Composition and Heat Treatment on Precipitate Composition in Al–Zn–Mg–Cu Alloys, Acta Mater., 2010, 58, p 248–260
J. Malek, The Applicability of Johnson-Mehl-Avrami Model in the Thermal Analysis of the Crystallization Kinetics of Glasses, Thermochim. Acta, 1995, 267, p 61–73
M.J. Starink, Kinetic Equations for Diffusion-Controlled Precipitation Reactions, J. Mater. Sci., 1997, 32, p 4061–4070
H.R. Shercliff and M.F. Ashby, A Process Model for Age Hardening of Aluminium Alloys—I. The Model, Acta Metall. Mater., 1990, 38(10), p 1789–1802
H.R. Shercliff and M.F. Ashby, A Process Model for Age Hardening of Aluminium Alloys—II. Applications of the Model, Acta Metal. Mater., 1990, 38(10), p 1803–1812
J.C. Ion, K.E. Easterling, and M.F. Ashby, A Second Report on Diagrams of Microstructure and Hardness for Heat-Affected Zones in Welds, Acra Metaria, 1984, 32(11), p 1949–1962
X. Zeng, C. Fergusson, K. Sadayappan, and S. Shankar, Effect of Titanium Levels on the Hot Tearing Sensitivity and Abnormal Grain Growth After T4 Heat Treatment of Al–Zn–Mg–Cu Alloys, Int. J. Metalcast., 2018, 12, p 457–468
Standard Test Methods for Tension Testing Wrought and Cast Aluminum- and Magnesium-Alloy Products, ASTM B557-15, ASTM International, West Conshohocken, PA, 2015, www.astm.org
Standard Practice for Conducting Force Controlled Constant Amplitude Axial Fatigue Tests of Metallic Materials, ASTM E466-96, ASTM International, West Conshohocken, PA, 1996, www.astm.org
Standard Test Methods for Vickers Hardness and Knoop Hardness of Metallic Materials, ASTM E92-17, ASTM International, West Conshohocken, PA, 2017, www.astm.org
Standard Test Methods for Rockwell Hardness of Metallic Materials”, ASTM E18-18a, ASTM International, West Conshohocken, PA, 2018, www.astm.org.
Standard Practice for Determining the Inclusion or Second-Phase Constituent Content of Metals by Automatic Image Analysis, ASTM E1245-03, ASTM International, West Conshohocken, PA, 2003, www.astm.org
G.A. Botton, G. L’esperance, C.E. Gallerneault, and M.D. Ball, Volume Fraction Measurement of Dispersoids in a Thin Foil by Parallel Energy-Loss Spectroscopy: Development and Assessment of the Technique, J. Microsc., 1995, 180, p 217–229
E. Celebi, J. Chen, E.S. Gopi, A. Neustein, and H.V. Poor, Signals and Communication Technology, ISSN: 1860-4862, Springer, Dordrecht, 2010
X.H. Zhu, High-Resolution (Scanning) Transmission Electron Microscopy and Related Techniques for Structural Analysis of Transition Metal Oxide Nanowires. In: Current Microscopy Contributions to Advances in Science and Technology, FORMATEX Microscopy Series No 5, vol. 1, Edited by A. Méndez-Vila, FORMATEX RESEARCH CENTER - C/Zurbaran 1, 2nd Floor, Office 1, 06002 Badajoz, Spain, 2012, p 1190–1203
M.J. Starink, Analysis of Aluminum Based Alloys by Calorimetry: Quantitative Analysis of Reactions and Reaction Kinetics, Int. Mater. Rev., 2004, 49(3–4), p 191–226
R.C. Dorward, Precipitate Coarsening During Overaging of Al–Zn–Mg–Cu Alloy, Mater. Sci. Technol., 1999, 15, p 1133–1138
N. Kamp, I. Sinclair, and M.J. Starink, Toughness-Strength Relations in the Over-aged 7449 Al-Based Alloy, Met. Mater. Trans. A, 2002, 33, p 1125–1136
W. Huo, L. Hou, Y. Lang, H. Cui, L. Zhuang, and J. Zhang, Improved Thermo-Mechanical Processing for Effective Grain Refinement of High-Strength AA 7050 Al Alloy, Mater. Sci. Eng. A, 2015, 626, p 86–93
L.K. Berg, J. Gjønnes, V. Hansen, X.Z. Li, M. Knutson-Wedel, G. Waterloo, D. Schryvers, and L.R. Wallenberg, GP-Zones in Al–Zn–Mg Alloys and Their Role in Artificial Aging, Acta Mater., 2001, 49, p 3443–3451
J.D. Embury and R.B. Nicholson, The Nucleation of Precipitates: The System Al-Zn-Mg, Acta Metal., 1965, 13, p 403–417
T.-Y. Ahn, J.-G. Jung, E.-J. Baek, S.S. Hwang, and K. Euh, Temporal Evolution of Precipitates in Multicomponent Al–6Mg–9Si–10Cu–10Zn–3Ni Alloy Studied by Complementary Experimental Methods, J. Alloys Compd., 2017, 701(15), p 660–668
X. Peng, Q. Guo, X. Liang, Y. Deng, G. Yi, X. Guofu, and Z. Yin, Mechanical Properties, Corrosion Behavior and Microstructures of a Non-isothermal Ageing Treated Al-Zn-Mg-Cu Alloy, Mater. Sci. Eng. A, 2017, 688(14), p 146–154
J. Zheng, Z. Li, R. Luo, and B. Chen, Precipitation in an Al-Zn-Mg-Cu Alloy During Isothermal Aging: Atomic-Scale HAADF-STEM Investigation, Mater. Sci. Eng. A, 2017, 691(13), p 60–70
X.Z. Li, V. Hansen, J. Gjønnes, and L.R. Wallenberg, HREM Study and Structure Modeling of the η′ Phase, the Hardening Precipitates in Commercial Al–Zn–Mg Alloys, Acta Mater., 1999, 47, p 2651–2659
J. Buha, R.N. Lumley, and A.G. Crosky, Secondary Ageing in an Aluminum Alloy 7050, Mater. Sci. Eng. A, 2008, 492, p 1–10
E. Druschitz, R.D. Foley, J. A. Griffin, High Strength Cast Al-Zn-Cu-Mg Aluminum: Solution Treating and Aging Study, Transactions of the American Foundry Society, 117th Annual Metalcasting Congress, 2013, Paper No. 13-1568, p 231–241
H. Akhyar and Husaini, Study on Cooling Curve Behavior During Solidification and Investigation of Impact Strength and Hardness of Recycled, Int. J. Metalcasting, 2016, 10(4), p 452–456
G. Sha, Y.B. Wang, X.Z. Liao, Z.C. Duan, S.P. Ringer, and T.G. Langdon, Influence of Equal-Channel Angular Pressing on Precipitation in an Al–Zn–Mg–Cu Alloy, Acta Mater., 2009, 57(10), p 3123–3132
D.B. Williams and C.B. Carter, Transmission Electron Microscopy: A Textbook for Material Science III, Plenum Press, New York, 1996, p 444–450
D. Su and Y. Zhu, Scanning Moiré Fringe Imaging by Scanning Transmission Electron Microscopy, Ultramicroscopy, 2010, 110(3), p 229–233
D.K. Xu, N. Birbilis, and P.A. Rometsch, The Effect of Pre-ageing Temperature and Retrogression Heating Rate on the Strength and Corrosion Behaviour of AA7150, Corros. Sci., 2012, 54, p 17–25
M. Nicolas and A. Deschamps, Characterisation and Modelling of Precipitate Evolution in an Al–Zn–Mg Alloy During Non-isothermal Heat Treatments, Acta Mater., 2003, 51, p 6077–6094
M. Nicolas, Precipitation Evolution in an Al-Zn-Mg Alloy During Non-isothermal Heat Treatments and in the Heat-Affected Zone of Welded Joints, Ph.D. Dissertation, Institute National Polytechnique de Grenoble – INPG (2002)
R.W. Siegel, Vacancy Concentrations in Metals, J. Nucl. Mater., 1978, 69–70, p 117–146
A. Deschamps, F. Livet, and Y. Bréachet, Influence of Predeformation on Ageing in an Al–Zn–Mg Alloy—I. Microstructure Evolution and Mechanical Properties, Acta Materialia, 1998, 47, p 281–292
A. Deschamps and Y. Bréachet, Influence of Predeformation and Ageing of an Al–Zn–Mg alloy—II. Modeling of Precipitation Kinetics and Yield Stress, Acta Materialia, 1998, 47, p 293–305
J.C. Werenskiold, A. Deschamps, and Y. Bréachet, Characterization and Modeling of Precipitation Kinetics in an Al–Zn–Mg Alloy, Mater. Sci. Eng. A, 2000, 293, p 267–274
D. Wang and Z.Y. Ma, Effect of Pre-strain on Microstructure and Stress Corrosion Cracking of Over-Aged 7050 Aluminum Alloy, J. Alloys Compd., 2009, 469, p 445–450
A. Deschamps, G. Fribourg, Y. Bréachet, J.L. Chemin, and C.R. Hutchinson, In Situ Evaluation of Dynamic Precipitation During Plastic Straining of an Al–Zn–Mg–Cu Alloy, Acta Mater., 2012, 60, p 1905–1916
C.C. Kammerer, N.S. Kulkarni, B. Warmack, and Y.H. Sohn, Interdiffusion in Ternary Magnesium Solid Solutions of Aluminum and Zinc, J. Phase Equilibria Diffus., 2016, 37, p 65–74
M. Vlach, V. Kodetová, B. Smola, J. Čízek, T. Kekule, M. Cieslar, H. Kudrnová, L. Bajtošová, M. Leibner, and I. Procházka, Characterization of Phase Development in Commercial Al-Zn-Mg(-Mn, Fe) Alloy with and Without Sc,Zr-Addition, Kovove Mater., 2018, 56, p 367–377
E. Donoso, Calorimetric Study of the Dissolution of Guinier-Preston Zones and η’ Phase in Al-4.5at%Zn-1.75at%Mg, Mater. Sci. Eng., 1985, 74, p 39–46
C. García-Cordovilla and E. Louis, Kinetics of Retrogression in Al-Zn-Mg-(Cu) Alloys, Metall. Trans. A, 1990, 21A, p 2277–2280
Acknowledgments
The authors express their gratitude to the Natural Sciences and Engineering Research Council (NSERC) of Canada for their financial support through the Discovery Grant program. Further, the first author would like to express his gratitude to Professor Hugh Shercliff (Senior Lecturer, Department of Engineering, University of Cambridge, Cambridge, UK) and Dr. Marjan Rajabi (Assistant Professor, Department of Advanced Materials and Renewable Energy, Iranian Research Organization for Science and Technology, Tehran, Iran) for their invaluable comments on this work.
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Ghiaasiaan, S.R., Shalchi Amirkhiz, B. & Shankar, S. High-Resolution Electron Microscopy and Kinetic Studies of Precipitation Hardening Reactions in Cast Al-5.8Zn-2.2Mg-2.5Cu. J. of Materi Eng and Perform 28, 4630–4646 (2019). https://doi.org/10.1007/s11665-019-04219-4
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DOI: https://doi.org/10.1007/s11665-019-04219-4