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In-Situ Phase Transition Analysis of Conventional and Laser Beam Melted AlSi10Mg and X5CrNiCuNb16-4 Alloys*

Dedicated to Prof. Dr.-Ing. habil. Peter Mayr on his 80th birthday
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Published/Copyright: December 11, 2018
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HTM Journal of Heat Treatment and Materials
From the journal HTM Journal of Heat Treatment and Materials Volume 73 Issue 6

Abstract

Although metallic materials processed by laser beam melting have significantly different microstructures compared to their conventional counterparts no adjusted heat treatment parameters have been published to date. Conventional heat treatment will therefore not always result in the desired mechanical properties. This project examines the effect of heat treatment on the properties of laser beam melted components produced with AlSi10Mg (EN AC-43000) precipitation hardening cast aluminium alloy and X5CrNiCuNb16-4 (1.4542 or 17-4 PH) martensitic precipitation hardening steel. Comparisons to conventionally manufactured material are made in parallel. The kinetics of phase transformation during heat treatment is analysed in-situ by means of differential scanning calorimetry (AlSi10Mg and X5CrNiCuNb16-4) and dilatometry (X5CrNiCuNb16-4). The results show considerable differences in phase transformation kinetics between laser beam melted and conventionally processed materials.

Kurzfassung

Für mittels Laserstrahlschmelzen verarbeitete metallische Werkstoffe existieren bisher keine angepassten Wärmebehandlungsparameter, obwohl diese Werkstoffe gegenüber ihren konventionellen Pendants signifikant unterschiedliche Gefüge aufweisen. Herkömmliche Wärmebehandlungsparameter führen daher nicht immer zu den gewünschten mechanischen Eigenschaften. In dieser Arbeit wird der Einfluss der Wärmebehandlung auf die Werkstoffeigenschaften laserstrahlgeschmolzener Bauteile aus der aushärtbaren Aluminiumgusslegierung AlSi10Mg (EN AC-43000) und dem martensitischen, ausscheidungshärtenden Stahl X5CrNiCuNb16-4 (1.4542 bzw. 17-4 PH) untersucht. Parallel findet ein Vergleich mit dem jeweiligen konventionell gefertigten Werkstoff statt. Die Kinetik der Phasenumwandlungen während der Wärmebehandlung wird in situ mittels Differential Scanning Calorimetry (AlSi10Mg und X5CrNiCuNb16-4) sowie Dilatometrie (X5CrNiCuNb16-4) analysiert. Die Ergebnisse zeigen einen erheblichen Unterschied der Phasenumwandlungskinetik zwischen laserstrahlgeschmolzenen und konventionell verarbeiteten Werkstoffen.

Keywords: AlSi10Mg; X5CrNiCuNb16-4; differential scanning calorimetry (DSC); dilatometry; LBM; laser beam melting; hardening
Schlüsselwörter: AlSi10Mg; X5CrNiCuNb16-4; Differential Scanning Calorimetry (DSC); Dilatometrie; LBM; Laserstrahlschmelzen; Härten
*

Revised lecture presented by C. Rowolt at the HeatTreatmentCongress, HK 2017, October 25–27, 2017 in Cologne, Germany

5 (corresponding author/Kontakt)

References

1 Gu, D. D.; Meiners, W.; Wissenbach, K.; Poprawe, R.: Laser additive manufacturing of metallic components: materials, processes and mechanisms. Int. Mat. Rev.57 (2012) 3, pp. 133–164, 10.1179/1743280411Y.0000000014Search in Google Scholar

2 Santos, E. C.; Shiomi, M.; Osakada, K.; Laoui, T.: Rapid manufacturing of metal components by laser forming. Int. J. Mach. Tools Manuf.46 (2006) 12–13, pp. 1459–1468, 10.1016/j.ijmachtools.2005.09.005Search in Google Scholar

3 Osakada, K.; Shiomi, M.: Flexible manufacturing of metallic products by selective laser melting of powder. Int. J. Mach. Tools Manuf.46 (2006) 11, pp. 1188–1193, 10.1016/j.ijmachtools.2006.01.024Search in Google Scholar

4 Leuders, S.; Thöne, M.; Riemer, A.; Niendorf, T.; Tröster, T.; Richard, H. A.; Maier, H. J.: On the mechanical behaviour of titanium alloy TiAl6V4 manufactured by selective laser melting: Fatigue resistance and crack growth performance. Int. J. Fatigue48 (2013), pp. 300–307, 10.1016/j.ijfatigue.2012.11.011Search in Google Scholar

5 Aboulkhair, N. T.; Maskery, I.; Tuck, C.; Ashcroft, I. A.; Everitt, N. M.: The microstructure and mechanical properties of selectively laser melted AlSi10Mg: The effect of a conventional T6-like heat treatment. Mat. Sci. Eng.667A (2016), pp. 139–146, 10.1016/j.msea.2016.04.092Search in Google Scholar

6 Yadollahi, A.; Shamsaei, N.; Thompson, S. M.; Elwany, A.; Bian, L.: Mechanical and microstructural properties of selective laser melted 17-4 PH stainless steel. Proc. ASME Int. Mech. Eng. Congr. and Exp. ASME 2015, 13–19.11.15, Houston, Texas, USA. The American Society of Mechanical Engineers, New York, N. Y., USA, 201610.1115/IMECE2015-52362Search in Google Scholar

7 Brandl, E.; Heckenberger, U.; Holzinger, V.; Buchbinder, D.: Additive manufactured AlSi10Mg samples using Selective Laser Melting (SLM): Microstructure, high cycle fatigue, and fracture behavior. Mater. Design34 (2012), pp. 159–169, 10.1016/j.matdes.2011.07.067Search in Google Scholar

8 Thijs, L.; Kempen, K.; Kruth, J. P.; van Humbeeck, J.: Fine-structured aluminium products with controllable texture by selective laser melting of pre-alloyed AlSi10Mg powder. Acta Mater.61 (2013) 5, pp. 1809–1819, 10.1016/j.actamat.2012.11.052Search in Google Scholar

9 Rafi, H. K.; Pal, D.; Patil, N.; Starr, T. L.; Stucker, B. E.: Microstructure and Mechanical Behavior of 17-4 Precipitation Hardenable Steel Processed by Selective Laser Melting. J. Mater. Eng. Perform.23 (2014) 12, pp. 4421–4428, 10.1007/s11665-014-1226-ySearch in Google Scholar

10 Murr, L. E.; Martinez, E.; Hernandez, J.; Collins, S.; Amato, K. N.; Gaytan, S. M.; Shindo, P. W.: Microstructures and Properties of 17-4 PH Stainless Steel Fabricated by Selective Laser Melting. J. Mater. Res. Technol.1 (2012) 3, pp. 167–177, 10.1016/S2238-7854(12)70029-7Search in Google Scholar

11 Milkereit, B.; Kessler, O.; Schick, C.: Recording of continuous cooling precipitation diagrams of aluminium alloys. Thermochim. Acta492 (2009) 1–2, pp. 73–78, 10.1016/j.tca.2009.01.027Search in Google Scholar

12 Osten, J.; Milkereit, B.; Schick, C.; Kessler, O.: Dissolution and Precipitation Behaviour during Continuous Heating of Al–Mg–Si Alloys in a Wide Range of Heating Rates. Materials8 (2015) 5, pp. 2830–2848, 10.3390/ma8052830Search in Google Scholar

13 Antony, K. C.: Aging reactions in precipitation hardenable stainless steel. J. Metals15 (1963), pp. 922–927, 10.1007/BF03397271Search in Google Scholar

14 Hsiao, C. N.; Chiou, C. S.; Yang, J. R.: Aging reactions in a 17-4 PH stainless steel. Mater. Chem. Phys.74 (2002) 2, pp. 134–142, 10.1016/S0254-0584(01)00460-6Search in Google Scholar

15 Goller, G. N.; Clarke, W. C.: New Precipitation-Hardening Stainless Steel. Iron Age165 (1950), pp. 79–83; 86–89Search in Google Scholar

16 Rack, H. J.; Kalish, D.: The strength, fracture toughness, and low cycle fatigue behavior of 17-4 PH stainless steel. Metall. Trans.5 (1974) 7, pp. 1595–1605, 10.1007/BF02646331Search in Google Scholar

17 Irvine, K. J.; Llewellyn, D. T.; Pickering, F. B.: Controlled-transformation stainless steels. J. Iron Steel Inst.192 (1959) 7, pp. 218–238Search in Google Scholar

18 Viswanathan, U. K.; Banerjee, S.; Krishnan, R.: Effects of aging on the microstructure of 17-4 PH stainless steel. Mat. Sci. Eng. A.104 (1988), pp. 181–189, 10.1016/0025-5416(88)90420-XSearch in Google Scholar

19 Reich, M.; Milkereit, B.; Bader, M.; Oehmigen, H. G.; Kessler, O.: Calorimetric and Dilatometric Study of Tempering Behavior in the Heat Affected Zone of T24 Welding Seams. HTM J. Heat Treatm. Mat.68 (2013) 6, pp. 274–282, 10.3139/105.110202Search in Google Scholar

20 Stahl-Eisen-Prüfblatt SEP 1681:1993: Richtlinien für Vorbereitung, Durchführung und Auswertung dilatometrischer Umwandlungsuntersuchungen an Eisenlegierungen. Verein Deutscher Eisenhüttenleute, Stahleisen m.b.H., Düsseldorf, 1993Search in Google Scholar

21 Calvet, E.; Prat, H.; Skinner, H. (eds.): Recent progress in microcalorymetry. Pergamon Press, Oxford, 1963Search in Google Scholar

22 Weck, E.; Leistner, E.: Metallographische Anleitung zum Farbätzen nach dem Tauchverfahren Teil III: Nichteisenmetalle, Hartmetalle und Eisenwerkstoffe, Nickel-Basis- und Kobalt-Basis-Legierungen. Fachbuchreihe Schweißtechnik 77/3, Dt. Verl. f. Schweißtechnik, Düsseldorf, 1986Search in Google Scholar

23 ASM International: Metallography and Microstructures. Metals Handbook Vol. 9, ASM Int., Ohio, USA, 1992Search in Google Scholar

24 Weck, E.; Leistner, E.: Metallographische Anleitung zum Farbätzen nach dem Tauchverfahren Teil II: Farbätzmittel nach Beraha und ihre Abwandlungen. Fachbuchreihe Schweißtechnik 77/2, Dt. Verl. f. Schweißtechnik, Düsseldorf, 1983Search in Google Scholar

25 Rometsch, P. A.; Schaffer, G. B.: Quench modelling of Al-7Si-Mg casting alloys. Int. J. Cast Metal. Res.12 (2000) 6, pp. 431–439, 10.1080/13640461.2000.11819380Search in Google Scholar

26 Zhang, D. L.; Zheng, L.: The quench sensitivity of cast Al-7 Wt Pct Si-0.4 Wt pct Mg alloy. Metall. Mater. Trans. A:27A (1996) 12, pp. 3983–3991, 10.1007/BF02595647Search in Google Scholar

27 Wang, G.; Yan, L.; Ren, G.; Zhao, Z.: Analyzing as-cast age hardening of 356 cast alloy. J. Mater. Eng. Perform.20 (2011) 3, pp. 399–404, 10.1007/s11665-010-9708-zSearch in Google Scholar

28 Schumacher, P.; Pogatscher, S.; Starink, M. J.; Schick, C.; Mohles, V.; Milkereit, B.: Quench-induced precipitates in Al–Si alloys: Calorimetric determination of solute content and characterisation of microstructure. Thermochim. Acta602 (2015), pp. 63–73, 10.1016/j.tca.2014.12.023Search in Google Scholar

29 Milkereit, B.; Starink, M. J.: Quench sensitivity of Al-Mg-Si alloys: A model for linear cooling and strengthening. Mater. Design76 (2015), pp. 117–129, 10.1016/j.matdes.2015.03.055Search in Google Scholar

30 Milkereit, B.; Wanderka, N.; Schick, C.; Kessler, O.: Continuous cooling precipitation diagrams of Al–Mg–Si alloys. Mat. Sci. Eng. A550 (2012), pp. 87–96, 10.1016/j.msea.2012.04.033Search in Google Scholar

31 Mondolfo, L. F.: Aluminum alloys. Structure and properties. Butterworths, London, 197610.1016/B978-0-408-70932-3.50008-5Search in Google Scholar

32 Schumacher, P.; Reich, M.; Mohles, V.; Pogatscher, S.; Uggowitzer, P. J.; Milkereit, B.: Correlation between supersaturation of solid solution and mechanical behaviour of two binary Al-Si-Alloys. Mater. Sci. Forum794/796 (2014), pp. 508–514, 10.4028/www.scientific.net/MSF.794-796.508Search in Google Scholar

33 Milkereit, B.; Fröck, H.; Schick, C.; Kessler, O.: Continuous cooling precipitation diagram of cast aluminium alloy Al-7Si-0.3Mg. Trans. Nonferr. Metal. Soc. China24 (2014) 7, pp. 2025–2033, 10.1016/S1003-6326(14)63308-2Search in Google Scholar

34 Starink, M. J.; Milkereit, B.; Zhang, Y.; Rometsch, P. A.: Predicting the quench sensitivity of Al-Zn-Mg-Cu alloys: A model for linear cooling and strengthening. Mater. Design88 (2015), pp. 958–971, 10.1016/j.matdes.2015.09.058Search in Google Scholar

35 Yang, B.; Milkereit, B.; Zhang, Y.; Rometsch, P. A.; Kessler, O.; Schick, C.: Continuous cooling precipitation diagram of aluminium alloy AA7150 based on a new fast scanning calorimetry and interrupted quenching method. Mater. Charact.120 (2016), pp. 30–37, 10.1016/j.matchar.2016.08.016Search in Google Scholar

36 Palm, F.: Material quality in laser powderbed melting has to be manufactured directly – and not assured by NDI. AEROMAT2016, 27th Aeromat Conf. & Exp., 23–25.05.2016, Bellevue, WA, USA, 2016Search in Google Scholar

37 Hitzler, L.; Hirsch, J.; Heine, B.; Merkel, M.; Hall, W.; Öchsner, A.: On the Anisotropic Mechanical Properties of Selective Laser-Melted Stainless Steel. Materials10 (2017) 10; 10.3390/ma10101136Search in Google Scholar PubMed PubMed Central

38 Amato, K. N.; Gaytan, S. M.; Murr, L. E.; Martinez, E.; Shindo, P. W.; Hernandez, J.; Collins, S.; Medina, F.: Microstructures and mechanical behavior of Inconel 718 fabricated by selective laser melting. Acta Mater.60 (2012) 5, pp. 2229–2239, 10.1016/j.actamat.2011.12.032Search in Google Scholar

39 Thijs, L.; Verhaeghe, F.; Craeghs, T.; van Humbeeck, J.; Kruth, J. P.: A study of the microstructural evolution during selective laser melting of Ti-6Al-4 V. Acta Mater.58 (2010) 9, pp. 3303–3312, 10.1016/j.actamat.2010.02.004Search in Google Scholar

40 Gülsoy, H. Ö.; Salman, S.: Microstructures and mechanical properties of injection molded 17-4 PH stainless steel powder with nickel boride additions. J. Mater. Sci.40 (2005) 13, pp. 3415–3421, 10.1007/s10853-005-0432-2Search in Google Scholar

41 Irrinki, H.: Mechanical properties and microstructure evolution of 17-4 PH stainless steel processed by laser-powered bed fusion. Electronic Theses and Dissertations, University of Louisville: ThinkIR: The University of Louisville‘s Institutional Repository, 2016Search in Google Scholar

42 Slaby, S. A.; Kraft, O.; Eberl, C.: Fatigue properties of conventionally manufactured and micro-powder-injection-moulded 17-4PH micro-components. Fatigue Fract. Eng. M.39 (2016) 6, pp. 780–789, 10.1111/ffe.12416Search in Google Scholar

43 Christien, F.; Telling, M. T. F.; Knight, K. S.: A comparison of dilatometry and in-situ neutron diffraction in tracking bulk phase transformations in a martensitic stainless steel. Mater. Charact. (2013), pp. 50–57, 10.1016/j.matchar.2013.05.002Search in Google Scholar

44 Christien, F.; Saindrenan, G.; Le Gall, R.; Boursier, J. M.: Some aspects of interfacial segregation in martensitic stainless steel 17-4 PH. In: EDEM 99, Proc. Int. Conf. on Environmental Degradation of Engineering Materials, 19–23.09.99, Gdaňsk-Jurata, PL, 1999, pp. 99–104Search in Google Scholar

45 Maruyama, N.; Sugiyama, M.; Hara, T.Tamehiro, H.: Precipitation and phase transformation of copper particles in low alloy ferritic and martensitic steels. Mater. Trans. JIM40 (1999) 4, pp. 268–277, 10.2320/matertrans1989.40.268Search in Google Scholar

46 Kapoor, R.; Batra, I. S.: On the α' to γ transformation in maraging (grade 350), PH 13-8 Mo and 17-4 PH steels. Mat. Sci. Eng. A371 (2004) 1–2, pp. 324–334, 10.1016/j.msea.2003.12.023Search in Google Scholar

47 Kapoor, R.; Kumar, L.; Batra, I. S.: Dilatometric study of the continuous heating transformations in 18wt.% Ni maraging steel of grade 350. Mat. Sci. Eng. A352 (2003) 1–2, pp. 318–324, 10.1016/S0921-5093(02)00934-6Search in Google Scholar

48 Brezina, P.: Martensitische CrNi-Stähle mit tiefem Kohlenstoffgehalt. Escher Wyss Mitteilungen53 (1980) 1–2, pp. 218–236Search in Google Scholar

49 Kulmburg, A.; Korntheuer, F.; Koren, M.; Gründler, O.; Hutterer, K.: Umwandlungs- und Ausscheidungsverhalten von weichmartensitischen und hochfesten korrosionsbeständigen Stählen. BHM Berg- u. Hüttenmännische Monatshefte126 (1981) 3, pp. 104–108Search in Google Scholar

50 Salje, G.; Feller-Kniepmeier, M.: The diffusion and solubility of copper in iron. J. Appl. Phys.48 (1977) 5, pp. 1833–1839, 10.1063/1.323934Search in Google Scholar

51 Hornbogen, E.: The role of strain energy during precipitation of copper and gold from alpha iron. Acta Metall. Mater.10 (1962) 5, pp. 525–533, 10.1016/0001-6160(62)90197-9Search in Google Scholar

52 Othen, P. J.; Jenkins, M. L.; Smith, G. D. W.; Phythian, W. J.: Transmission electron microscope investigations of the structure of copper precipitates in thermally-aged Fe-Cu and Fe-Cu-Ni. Phil. Mag. Lett.64 (1991) 6, pp. 383–391, 10.1080/09500839108215121Search in Google Scholar

53 Othen, P. J.; Jenkins, M. L.; Smith, G. D. W.: High-resolution electron microscopy studies of the structure of Cu precipitates in α-Fe. Phil. Mag. A:70A (1994) 1, pp. 1–24, 10.1080/01418619408242533Search in Google Scholar

54 Goodman, S. R.; Brenner, S. S.; Low, J. R.: An FIM-Atom Probe Study of the Precipitation of Copper from Iron-1.4 At. Pct Copper. Part II: Atom Probe Analyses. Metall. Trans.4 (1973) 10, pp. 2371–2378, 10.1007/BF02669377Search in Google Scholar

55 Habibi Bajguirani, H. R.; Jenkins, M. L.: High-resolution electron microscopy analysis of the structure of copper precipitates in a martensitic stainless steel of type PH 15-5. Phil. Mag. Lett.73 (1996) 4, pp. 155–162, 10.1080/095008396180786Search in Google Scholar

Published Online: 2018-12-11
Published in Print: 2018-12-12

© 2018, Carl Hanser Verlag, München

Articles in the same Issue

  1. Praxis-Informationen/From and for Practice
  2. AWT Info
  3. HTM-Praxis
  4. Kurzfassungen/Abstracts
  5. Kurzfassungen
  6. Inhalt/Contents
  7. Inhalt
  8. Editorial
  9. Professor Dr.-Ing. habil. Peter Mayr on the occasion of his 80th birthday
  10. Scientific Contributions/Fachbeiträge
  11. Surface Layer Microstructure of Carburised and Bainitically Transformed Parts and their Mechanical Properties*
  12. In-Situ Phase Transition Analysis of Conventional and Laser Beam Melted AlSi10Mg and X5CrNiCuNb16-4 Alloys*
  13. Investigation of the Tempering Effect during Nitriding*
  14. Multistage Eccentric Rotary Swaging
  15. Successive Spray Forming and Selective Heat Treatment of Composite Tool Steels
https://doi.org/10.3139/105.110366
Keywords for this article
AlSi10Mg; X5CrNiCuNb16-4; differential scanning calorimetry (DSC); dilatometry; LBM; laser beam melting; hardening

Articles in the same Issue

  1. Praxis-Informationen/From and for Practice
  2. AWT Info
  3. HTM-Praxis
  4. Kurzfassungen/Abstracts
  5. Kurzfassungen
  6. Inhalt/Contents
  7. Inhalt
  8. Editorial
  9. Professor Dr.-Ing. habil. Peter Mayr on the occasion of his 80th birthday
  10. Scientific Contributions/Fachbeiträge
  11. Surface Layer Microstructure of Carburised and Bainitically Transformed Parts and their Mechanical Properties*
  12. In-Situ Phase Transition Analysis of Conventional and Laser Beam Melted AlSi10Mg and X5CrNiCuNb16-4 Alloys*
  13. Investigation of the Tempering Effect during Nitriding*
  14. Multistage Eccentric Rotary Swaging
  15. Successive Spray Forming and Selective Heat Treatment of Composite Tool Steels
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