journal article·2021-12Open access

In situ high-energy X-ray diffraction of precipitation and dissolution reactions during heating of Al alloys

Hannes Fröck, Christian Rowolt, Benjamin Milkereit, Michael Reich, Wolfgang Kowalski, Andreas Stark, Olaf Kessler

Journal of Materials Science· Volume 56· Issue 35

Abstract

Abstract During heating of Al alloys, typically a sequence of precipitation and dissolution reactions occurs and the single (partly opposing) reactions superimpose. Differential scanning calorimetry (DSC) is one common technique to analyse the kinetic development of precipitation and dissolution in Al alloys, but the superposition of the exothermic precipitation and endothermic dissolution reactions complicates the DSC signal interpretation, as DSC measures the sum of any heat effect. Synchrotron high-energy X-ray diffraction (HEXRD) allows the kinetic development of phase transformations to be obtained and can support the separation of superimposed DSC signals. HEXRD results from this work offer a new approach to separate part of the superimposed reactions and their kinetic development for the equilibrium phases β-Mg2Si in EN AW-6082 and η-Mg(Zn,Cu,Al)2 in EN AW-7150. Comparing DSC and HEXRD results confirms serious overlap issues. Common DSC evaluation methods alone, using zero crossing between endothermic and exothermic heat flow or peak positions can be misleading regarding individual reaction start and finish temperatures as well as regarding reaction intensities, which can be unambiguously determined by in situ HEXRD.
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Research context

OpenAlex topics: Aluminum Alloy Microstructure Properties · X-ray Diffraction in Crystallography · Corrosion Behavior and Inhibition

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References (32)

Show source-provided references
1. Osten J, Milkereit B, Schick C, Kessler O (2015) Dissolution and precipitation behaviour during continuous heating of Al-Mg-Si alloys in a wide range of heating rates. Mater 8(5):2830–2848. https://doi.org/10.3390/ma805283010.3390/ma8052830 ↗
2. Milkereit B, Österreich M, Schuster P, Kirov G, Mukeli E, Kessler O (2018) Dissolution and precipitation behaviour for hot forming of 7021 and 7075 aluminum alloys. Metals 8(7):531. https://doi.org/10.3390/met807053110.3390/met8070531 ↗
3. Milkereit B, Starink MJ, Rometsch PA, Schick C, Kessler O. 2019 Review of the quench sensitivity of aluminium alloys: analysis of the kinetics and nature of quench-induced precipitation. Materials 12 (24). https://doi.org/10.3390/ma12244083.10.3390/ma12244083 ↗
4. Birol Y (2006) DSC Analysis of the precipitation reactions in the alloy AA6082. J Therm Anal Calorim 83(1):219–22210.1007/s10973-005-6950-y ↗
5. Birol Y (2008) DSC analysis of the precipitation reaction in AA6005 alloy. J Therm Anal Calorim 93(3):977–98110.1007/s10973-007-8686-3 ↗
6. Dutta I, Allen SM (1991) A calorimetric study of precipitation in commercial aluminium alloy 6061. J Mater Sci Lett 10(6):323–32610.1007/BF00719697 ↗
7. Barrena MI, Gómez de Salazar JM, Pascual L, Soria A (2013) Determination of the kinetic parameters in magnesium alloy using TEM and DSC techniques. J Therm Anal Calorim. https://doi.org/10.1007/s10973-012-2791-710.1007/s10973-012-2791-7 ↗
8. Heugue P, Larouche D, Breton F, Martinez R, Chen XG (2019) Evaluation of the growth kinetics of θ′ and θ-Al2Cu precipitates in a binary Al-3.5 Wt Pct Cu Alloy. Metallurgical and Materials Transactions A. https://doi.org/10.1007/s11661-019-05227-810.1007/s11661-019-05227-8 ↗
9. Khalfallah A, Raho AA, Amzert S, Djemli A. Precipitation kinetics of GP zones, metastable η′ phase and equilibrium η phase in Al−5.46wt.%Zn−1.67wt.%Mg alloy. T Nonferr Metal Soc 2019; 29(2): 233–41. https://doi.org/10.1016/S1003-6326(19)64932-0.10.1016/S1003-6326(19)64932-0 ↗
10. Serradj F, Farh H, Belfarhi B (2019) Study of precipitation hardening in two Al-Mg-Si alloys with and without copper and excess silicon using kissinger and boswell methods. DDF 397:101–11010.4028/www.scientific.net/DDF.397.101 ↗
11. Belhouchet H, Fatmi M, Sahnoune F, Heraiz M, Saheb N (2018) Dilatometric and DSC study of the kinetics of discontinuous precipitation of Ag2Al intermetallic in Al – 10% Ag Alloy. Met Sci Heat Treat 60(3–4):185–189. https://doi.org/10.1007/s11041-018-0258-610.1007/s11041-018-0258-6 ↗
12. Hu X, Fang L, Zhou J, Zhang X, Hu H (2017) Characterization and kinetic modeling of secondary phases in squeeze cast Al alloy A380 by DSC thermal analysis. China Foundry 14(2):98–107. https://doi.org/10.1007/s41230-017-6092-410.1007/s41230-017-6092-4 ↗
13. Hamdi I, Boumerzoug Z (2016) The Natural Aging Effect on the Activation Energy of the Precipitation Processes in the Al-Mg-Si Alloy. KEM 723:27–3110.4028/www.scientific.net/KEM.723.27 ↗
14. Hamdi I, Boumerzoug Z, Chabane F. STUDY OF PRECIPITATION KINETICS OF AN AL-MG-SI ALLOY USING DIFFERENTIAL SCANNING CALORIMETRY. Acta Metall. Slovaca 2017;23(2):155. https://doi.org/10.12776/ams.v23i2.908.10.12776/ams.v23i2.908 ↗
15. Yin Y, Luo B-H, Bai Z-H, Jing H-B (2019) Quench sensitivity of Al–Cu–Mg alloy thick plate. Rare Met. https://doi.org/10.1007/s12598-018-1196-610.1007/s12598-018-1196-6 ↗
16. Kissinger HE (1957) Reaction kinetics in differential thermal analysis. Anal Chem 29(11):1702–1706. https://doi.org/10.1021/ac60131a04510.1021/ac60131a045 ↗
17. Kemsies RH, Milkereit B, Lindemann A, Schick C, Kessler O (2020) In situ investigation of precipitation in aluminium alloys via thermal diffusivity from laser flash analysis. J Therm Anal Calor 140:725–733. https://doi.org/10.1007/s10973-019-08880-810.1007/s10973-019-08880-8 ↗
18. Poulsen HF, Garbe S, Lorentzen T, Juul Jensen D, Poulsen FW, Andersen NH et al (1997) Applications of high-energy synchrotron radiation for structural studies of polycrystalline materials. J Synchrotron Radiat 4(Pt 3):147–154. https://doi.org/10.1107/S090904959700202110.1107/S0909049597002021 ↗
19. Liss K-D, Bartels A, Schreyer A, Clemens H (2003) High-Energy X-rays: a tool for advanced bulk investigations in materials science and physics. Textures and Microstructures 35(3–4):219–252. https://doi.org/10.1080/0730330031000163495210.1080/07303300310001634952 ↗
20. Liss K-D, Bartels A, Clemens H, Bystrzanowski S, Stark A, Buslaps T et al (2006) Recrystallization and phase transitions in a γ-TiAl-based alloy as observed by ex situ and in situ high-energy X-ray diffraction. Acta Mater 54(14):3721–3735. https://doi.org/10.1016/j.actamat.2006.04.00410.1016/j.actamat.2006.04.004 ↗
21. Andrews RN, Serio J, Muralidharan G, Ilavsky J (2017) An in situ USAXS-SAXS-HEXRD study of precipitate size distribution evolution in a model Ni-based alloy. J Appl Crystallogr 50(3):734–740. https://doi.org/10.1107/S160057671700644610.1107/S1600576717006446 ↗
22. Haas S, Andersson J, Fisk M, Park J-S, Lienert U (2018) Correlation of precipitate evolution with Vickers hardness in Haynes® 282® superalloy: In-situ high-energy SAXS/HEXRD investigation. Mater Sci Eng A 711:250–258. https://doi.org/10.1016/j.msea.2017.11.03510.1016/j.msea.2017.11.035 ↗
23. Tsao C-S, Huang E-W, Wen M-H, Kuo T-Y, Jeng S-L, Jeng U-S et al (2013) Phase transformation and precipitation of an Al-Cu alloy during non-isothermal heating studied by in situ small-angle and wide-angle scattering. J Alloys Compd 579:138–146. https://doi.org/10.1016/j.jallcom.2013.04.20110.1016/j.jallcom.2013.04.201 ↗
24. Rowolt C, Fröck H, Milkereit B, Reich M, Kowalski W, Stark A et al (2020) In-situ analysis of continuous cooling precipitation in Al alloys by wide-angle X-ray scattering. Sci Technol Adv Mater 21(1):205–218. https://doi.org/10.1080/14686996.2020.173955410.1080/14686996.2020.1739554 ↗
25. Kemsies RH, Milkereit B, Wenner S, Holmestad R, Kessler O (2018) In situ DSC investigation into the kinetics and microstructure of dispersoid formation in Al-Mn-Fe-Si(-Mg) alloys. Mater Des 146:96–107. https://doi.org/10.1016/j.matdes.2018.03.00710.1016/j.matdes.2018.03.007 ↗
26. Schell N, King A, Beckmann F, Fischer T, Müller M, Schreyer A (2013) The High Energy Materials Science Beamline (HEMS) at PETRA III. Mater Sci Forum 772:57–6110.4028/www.scientific.net/MSF.772.57 ↗
27. Bruker AXS GmbH. DIFFRACplus PDFMaint database 15.0.0.0: Bruker-AXS 1996–2009.
28. Starink MJ, Milkereit B, Zhang Y, Rometsch PA (2015) Predicting the quench sensitivity of Al-Zn-Mg-Cu alloys: A model for linear cooling and strengthening. Mater Des 88:958–971. https://doi.org/10.1016/j.matdes.2015.09.05810.1016/j.matdes.2015.09.058 ↗
29. Polmear IJ (2006) Light alloys: From traditional alloys to nanocrystals, 4th edn. Elsevier Butterworth-Heinemann, Amsterdam
30. Wiechmann P, Panwitt H, Heyer H, Reich M, Sander M, Kessler O (2018) Combined calorimetry thermo-mechanical analysis and tensile test on welded EN AW-6082 Joints. Mater. https://doi.org/10.3390/ma1108139610.3390/ma11081396 ↗
31. Adler PN, DeIasi R (1977) Calorimetric studies of 7000 series aluminum alloys: II Comparison of 7075, 7050 and RX720 alloys. Metall Trans A. https://doi.org/10.1007/BF0266740410.1007/BF02667404 ↗
32. Park JK, Ardell AJ (1989) Correlation between microstructure and calorimetric behaviour of aluminum alloy 7075 and AlZnMg alloys in various tempers. Mater Sci Eng A. https://doi.org/10.1016/0921-5093(89)90859-910.1016/0921-5093(89)90859-9 ↗