journal article·2018-10Open access

Formation of eta carbide in ferrous martensite by room temperature aging

W. Lu, M. Herbig, C.H. Liebscher, L. Morsdorf, R.K.W. Marceau, G. Dehm, D. Raabe

Acta Materialia· Volume 158

Abstract

Abstract For several decades, the formation of carbon(C)-rich domains upon room temperature aging of supersaturated martensite has been a matter of debate. C-rich tweed-like patterns are observed to form after short aging times at room temperature and coarsen upon further aging. Here, we present a systematic atomic-scale investigation of carbide formation in Fe-15Ni-1C (wt.%) martensite after two to three years of isothermal room temperature aging by a combination of atom probe tomography and transmission electron microscopy. Owing to the sub-zero martensite start temperature of −25 °C, a fully austenitic microstructure is maintained at room temperature and the martensitic phase transformation is initiated during quenching in liquid nitrogen. In this way, any diffusion and redistribution of C in martensite is suppressed until heating up the specimen and holding it at room temperature. The microstructural changes that accompany the rearrangement of C atoms have been systematically investigated under controlled isothermal conditions. Our results show that after prolonged room temperature aging nanometer-sized, plate-shaped η-Fe2C carbides form with a macroscopic martensite habit plane close to {521}. The orientation relationship between the η-Fe2C carbides and the parent martensite grain (α′) follows [001]α’//[001]η, ( 1 ¯ 10 ) α’//(020)η. The observation of η-Fe2C–carbide formation at room temperature is particularly interesting, as transition carbides have so far only been reported to form above 100 °C. After three years of room temperature aging a depletion of Fe is observed in the η carbide while Ni remains distributed homogenously. This implies that the substitutional element Fe can diffuse several nanometers in martensite at room temperature within three years.
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OpenAlex topics: Advanced materials and composites · Advanced Materials Characterization Techniques · Metal Extraction and Bioleaching

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References (92)

Show source-provided references
1. The strength of ferrous martensite10.1016/0001-6160(68)90137-5 ↗
2. Martensite in steel strength and structure10.1016/S0921-5093(99)00288-9 ↗
3. Toward a new interpretation of the mechanical behavior of as quenched low alloyed martensitic steels10.2355/isijinternational.52.717 ↗
4. Bhadeshia · 2006
5. Matensite lattice changes during tempering10.1007/BF02653487 ↗
6. A study of the early stages of tempering of iron-carbon martensites by atom probe field ion microscopy10.1007/BF02642333 ↗
7. Ageing of Fe-Ni-C martensite
8. Ageing and tempering of ferrous martensites
9. Spinodal decomposition during aging of Fe-Ni-C martensites10.1007/BF02670166 ↗
10. Carbide precipitation during stage 1 tempering of Fe-Ni-C martensites10.1007/BF02670168 ↗
11. Tempering of iron-carbon-nitrogen martensites: (Re) distributin of interstitial atoms10.4028/www.scientific.net/MSF.318-320.103 ↗
12. Three-dimensional atom probe characterization of alloy element partitioning in cementite during tempering of alloy steel10.1016/j.ultramic.2007.02.033 ↗
13. The morphology of secondary-hardening carbides in a martensitic steel at the peak hardness by 3DFIM10.1016/j.ultramic.2008.11.010 ↗
14. Atom probe tomography investigation of assisted precipitation of secondary hardening carbides in a medium carbon martensitic steels10.1111/j.1365-2818.2011.03537.x ↗
15. Microstructures and hardness of as-quenched martensites (0.1–0.5%C)10.1016/j.actamat.2011.05.061 ↗
16. Cementite-free martensitic steels: a new route to develop high strength/high toughness grades by modifying the conventional precipitation sequence during tempering10.1016/j.actamat.2012.07.030 ↗
17. Studies of dislocations by field ion microscopy and atom probe tomography10.1080/14786435.2013.818257 ↗
18. Microstructural heterogeneity and its relationship to the strength of martensite10.1016/j.msea.2015.04.088 ↗
19. 3D structural and atomic-scale analysis of lath martensite: effect of the transformation sequence10.1016/j.actamat.2015.05.023 ↗
20. Characterization of transition carbides in quench and partitioned steel microstructures by Mossbauer spectroscopy and complementary techniques10.1016/j.actamat.2015.01.024 ↗
21. Investigation of solute/interphase interaction during ferrite growth10.1016/j.actamat.2016.11.035 ↗
22. An atom study of the aging of Iron-Nickle-Carbon martensite
23. Crystallographic study of the tempering of martensitic carbon steel by electron microscopy and diffraction10.1007/BF02659851 ↗
24. Early stages of aging and tempering of ferrous martensites10.1007/BF02670444 ↗
25. Low temperature aging of the freshly formed martensite in an Fe-Ni-C alloy10.1007/BF02670362 ↗
26. Aging of freshly formed Fe-based martensites at low temperatures10.1007/BF02652265 ↗
27. Electron diffraction study of aging processes in Fe-1.83 wt pct martensite at room temperature10.1007/BF02670672 ↗
28. Aging and tempering behavior of iron-nickel-carbon and iron-carbon martensite
29. Initial stages of Fe-C martensite decomposition10.1080/01418610108212169 ↗
30. Thermodynamics of stable and metastable structures in Fe–C system10.1016/j.calphad.2014.03.004 ↗
31. Thermodynamic aspects of carbon redistribution during ageing and tempering of Fe–Ni–C alloys10.1080/14786435.2016.1211790 ↗
32. Mössbauer measurements on the aging of iron-carbon martensite10.1016/0001-6160(73)90036-9 ↗
33. Carbide characterization in low-temperature tempered steels10.1016/j.ultramic.2008.12.007 ↗
34. Static and dynamical ageing processes at room temperature in a Fe25Ni0.4C virgin martensite: effect of C redistribution at the nanoscale10.1080/09500839.2012.742590 ↗
35. The aging and tempering of iron-nickel-carbon martensite10.1007/BF02659847 ↗
36. Atomic-scale quantification of grain boundary segregation in nanocrystalline material10.1103/PhysRevLett.112.126103 ↗
37. Combining structural and chemical information at the nanometer scale by correlative transmission electron microscopy and atom probe tomography10.1016/j.ultramic.2015.02.003 ↗
38. Herbig · 2017
39. A novel approach for site-specific atom probe specimen preparation by focused ion beam and transmission electron backscatter diffraction10.1016/j.ultramic.2014.04.003 ↗
40. A hierarchical microstructure due to chemical ordering in the bcc lattice: early stages of formation in a ferritic Fe–Al–Cr–Ni–Ti alloy10.1016/j.actamat.2015.03.043 ↗
41. Quantitative analysis of carbon content in cementite in steel by atom probe tomography10.1016/j.ultramic.2011.03.024 ↗
42. Understanding the detection of carbon in austenitic high-Mn steel using atom probe tomography10.1016/j.ultramic.2013.01.010 ↗
43. Combined atom probe tomography and density functional theory investigation of the Al off-stoichiometry of κ-carbides in an austenitic Fe–Mn–Al–C low density steel10.1016/j.actamat.2016.01.007 ↗
44. Stadelmann · 2016
45. Study of metallic carbides by electron diffraction10.1143/JPSJ.12.482 ↗
46. Crystal structure and morphology of the carbide precipitated from martensitic high carbon during the first stage pf tempering10.1016/0001-6160(72)90020-X ↗
47. X-ray diffraction and Mössbauer studies of the (Fe1-xNix)4N compounds (0≤x≤0.5)x10.1016/0304-8853(95)00371-1 ↗
48. Microstructure of a Damascene sabre after annealing10.1515/ijmr-2006-0184 ↗
49. Substructures of lenticular martensites with different martensite start temperatures in ferrous alloys10.1016/j.actamat.2008.09.030 ↗
50. Nakamura · 1986 · vol. 27 · 842
51. Spatially correlated electron microscopy and atom probe tomography: current possibilities and future perspectives10.1016/j.scriptamat.2017.03.017 ↗
52. Brundle · 1992
53. Microstructures and hardness of as-quenched martensites (0.1-0.5%C)10.1016/j.actamat.2011.05.061 ↗
54. Atomic-scale quantification of grain boundary segregation in nanocrystalline material10.1103/PhysRevLett.112.126103 ↗
55. Carbon supersaturation of ferrite in a nanocrystalline bainitic steel10.1016/j.actamat.2009.12.020 ↗
56. Evolution of strength and microstructure during annealing of heavily cold-drawn 6.3 GPa hypereutectoid pearlitic steel wire10.1016/j.actamat.2012.03.006 ↗
57. An electron transmission study of the tempering of martensite in a Fe-Ni-C alloy10.1016/0001-6160(64)90009-4 ↗
58. Orientation relationships between ferrite and cementite by edge-to-edge matching principle10.1016/S1005-0302(11)60094-7 ↗
59. Homogenous formation of epsilon carbides within the austenite during the isothermal transformation of a ductile iron at 410 ºC10.1007/BF02670600 ↗
60. Electron microscopy study of the aging and first stage of tempering of high-carbon Fe-C martensite10.1007/BF02658989 ↗
61. Krauss · 2005
62. Carbon diffusion in carbon-supersaturated ferrite and austenite10.1016/j.jallcom.2013.10.058 ↗
63. Metallography of bainitic transformation in silicon containing steels10.1007/BF02646868 ↗
64. Competition between formation of carbides and reversed austenite during tempering of a medium-manganese steel studied by thermodynamic-kinetic simulations and atom probe tomography10.1016/j.actamat.2018.01.022 ↗
65. On the morphology of the modulated precipitation of extended mutiplets and Fe9C4 epsilon or eta carbide obtained by aging and tempering in Fe-C martensite10.1007/BF02647716 ↗
66. Electron microscopy and diffraction study of the carbide precipitated from martensitic low and high nickel steels at the first stge of tempering10.2320/matertrans1960.17.503 ↗
67. Atomic-scale mechanisms of deformation-induced cementite decomposition in pearlite10.1016/j.actamat.2011.03.022 ↗
68. Quantitative atom probe analysis of carbides10.1016/j.ultramic.2010.12.024 ↗
69. Gault · 2012
70. Atomic scale investigation of redistribution of alloying elements in pearlitic steel wires upon cold-drawing and annealing10.1016/j.ultramic.2012.10.010 ↗
71. Segregation stabilizes nanocrystalline bulk steel with near theoretical strength10.1103/PhysRevLett.113.106104 ↗
72. Quantitative measurement of carbon content in Fe–C binary alloys by atom probe tomography10.1016/j.scriptamat.2012.09.007 ↗
73. Local magnification effects in the atom probe10.1016/0039-6028(91)90449-3 ↗
74. Clustering and local magnification effects in atom probe tomography: a statistical approach, Microscopy and microanalysis10.1017/S1431927610000449 ↗
75. Improved resistance to hydrogen embrittlement in a high-strength steel by quenching–partitioning–tempering treatment10.1016/j.scriptamat.2014.10.030 ↗
76. Lattice changes of iron-carbon martensite on aging at room temperature10.1007/BF02669863 ↗
77. Edington · 1976
78. Structure of magnetite (Fe3O4) below the verwey transition temperature10.1107/S0567740882008176 ↗
79. Williams · 2009
80. Review of lattice diffusion substitutional impurtites in iron, A Summary Report
81. Heumann · 1992
82. Effect of partitioning of Mn and Si on the growth kinetics of cementite in tempered Fe–0.6 mass% C martensite10.1016/j.actamat.2007.05.023 ↗
83. Mehrer · 2007
84. Campbell · 2008
85. First-principles calculations on stabilization of iron carbides (Fe3C, Fe5C2, and η-Fe2C) in steels by common alloying elements10.1007/s11661-012-1229-y ↗
86. Review of lattice diffusion substitutional impurtites in iron, A Summary Report
87. Roberts · 1998
88. Early stages of decomposition in iron-carbon and iron-nitrogen martensites diffraction analysis using synchrotron radiation10.1007/BF02666331 ↗
89. Mossbauer spectroscopy of iron carbides: from prediction to experimental confirmation10.1038/srep26184 ↗
90. Stability and crystal structures of iron carbides: a comparison between the semi-empirical modified embedded atom method and quantum-mechanical DFT calculations10.1103/PhysRevB.85.054116 ↗
91. Structure and stability of Fe2C phases from density-functional theory calculations10.1016/j.scriptamat.2010.04.042 ↗
92. Crystalline, electronic, and magnetic structures of θ-Fe3C, χ-Fe5C2, and η-Fe2C from first principle calculation10.1063/1.2194118 ↗