Strategies for Preparing and Analyzing Thin Passive Films With Atom Probe Tomography
Source abstract
Abstract
Abstract Atom probe tomography (APT) provides a unique, three-dimensional map of elemental and isotopic distributions over a wide range of materials with near-atomic scale resolution and is particularly strong at analyzing buried interfaces within materials. However, it is much more difficult to apply atom probe to the analysis of nanoscale surface films, such as those formed during alloy passivation, where unique challenges persist for sample preparation and data collection. Here, we present sample preparation strategies involving the deposition of a <100 nm capping layer that enables reliable characterization of thin passive films ∼2–5 nm thick formed on binary and multiprincipal element alloys via APT. Several capping layer materials (Pt, Ti, and Ni/Cr bilayer) and deposition methods are contrasted. Our results indicate a sputtered Ni/Cr bilayer enables the characterization of the entire passive film and concentration profiles that can easily be interpreted to clearly distinguish base alloy/passive film/capping layer interfaces. Lastly, we highlight ongoing challenges and opportunities for this experimental approach.
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Advanced Materials Characterization Techniques · Hydrogen embrittlement and corrosion behaviors in metals · Fusion materials and technologies
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Energy and Environment Directorate, Pacific Northwest National Laboratory , Richland, WA 99352 ,
Department of Nuclear Engineering, North Carolina State University , Raleigh, NC 27695 ,
Department of Materials Science and Engineering, University of Virginia , Charlottesville, VA 22904 ,
Physical and Computational Sciences Directorate, Pacific Northwest National Laboratory , Richland, WA 99352 ,
Funding
U.S. Department of Energy · Office of Science · Basic Energy Sciences
References (88)
Show source-provided references
1. Investigation of wüstite (fe1−O) by femtosecond laser assisted atom probe tomography10.1016/j.ultramic.2010.11.023 ↗
2. Investigation of O-18 enriched hematite (α-Fe2O3) by laser assisted atom probe tomography10.1016/j.ijms.2012.10.012 ↗
3. Interpreting the presence of an additional oxide layer in analysis of metal oxides–metal interfaces in atom probe tomography10.1021/acs.jpcc.8b10895 ↗
4. 3D atom probe study of gas adsorption and reaction on alloy catalyst surfaces I: Instrumentation10.1016/j.susc.2006.05.026 ↗
5. Oxides film formed on Fe-and Ni-based alloys: An ellipsometry insight10.3390/coatings13050882 ↗
6. An SFG and ERS investigation of the corrosion of CoW0.013C0.001 alloys and WC–Co cermets in CN−-containing aqueous solutions10.1016/j.corsci.2006.10.038 ↗
7. In situ hydride formation in zirconium and titanium during ion milling10.1017/S1431927695111757 ↗
8. Characterizing solute hydrogen and hydrides in pure and alloyed titanium at the atomic scale10.1016/j.actamat.2018.02.064 ↗
9. Ti and its alloys as examples of cryogenic focused ion beam milling of environmentally-sensitive materials10.1038/s41467-019-08752-7 ↗
10. Yield assessment of protective coatings for atom probe analysis10.1017/S1431927622001192 ↗
11. Investigation of native oxide growth on zinc in different atmospheres by spectroscopic ellipsometry10.1002/pssa.201100542 ↗
12. XANES investigation of the role of cerium compounds as corrosion inhibitors for aluminum10.1016/0010-938X(91)90113-4 ↗
13. EELS and atom probe tomography study of the evolution of the metal/oxide interface during zirconium alloy oxidation10.1016/j.jnucmat.2015.03.043 ↗
14. X-ray photoelectron spectroscopy analysis of copper and zinc oxides and sulphides10.1002/sia.740180107 ↗
15. Visualizing the nanoscale oxygen and cation transport mechanisms during the early stages of oxidation of Fe–Cr–Ni alloy using in situ atom probe tomography10.1002/admi.202200134 ↗
16. Role of photoexcitation and field ionization in the measurement of accurate oxide stoichiometry by laser-assisted atom probe tomography10.1021/jz400015h ↗
17. Grain boundary engineering to control the discontinuous precipitation in multicomponent U10Mo alloy10.1016/j.actamat.2018.03.039 ↗
18. Grain boundary segregation in Ni-base alloys: A combined atom probe tomography and first principles study10.1016/j.actamat.2021.117354 ↗
19. A reproducible method for damage-free site-specific preparation of atom probe tips from interfaces10.1002/jemt.21081 ↗
20. Imaging spectroscopic ellipsometry of MoS210.1088/0953-8984/28/38/385301 ↗
21. Gault · 201210.1007/978-1-4614-3436-8 ↗
22. Behavior of molecules and molecular ions near a field emitter10.1088/1367-2630/18/3/033031 ↗
23. Aqueous passivation of high entropy alloy Ni38Fe20Cr22Mn10Co10: Unexpected high Cr enrichment within the passive film10.1016/j.actamat.2020.07.024 ↗
24. The role of chromium content in aqueous passivation of a non-equiatomic Ni38Fe20CrxMn21-0.5xCo21-0.5x multi-principal element alloy (x= 22, 14, 10, 6 at%) in acidic chloride solution10.1016/j.actamat.2022.118607 ↗
25. Contribution of atom-probe tomography to a better understanding of glass alteration mechanisms: Application to a nuclear glass specimen altered 25 years in a granitic environment10.1016/j.chemgeo.2013.04.001 ↗
26. In situ atomic-scale observation of oxidation and decomposition processes in nanocrystalline alloys10.1038/s41467-018-03288-8 ↗
27. Analysis of three-dimensional atom-probe data by the proximity histogram10.1007/S100050010051 ↗
28. Design and discovery of compositionally complex alloys that include high corrosion resistance10.5006/4451 ↗
29. A more holistic characterisation of internal interfaces in a variety of materials via complementary use of transmission Kikuchi diffraction and atom probe tomography10.1016/j.apsusc.2020.147011 ↗
30. Rapid assessment of structural and compositional changes during early stages of zirconium alloy oxidation10.1038/s41529-020-00133-6 ↗
31. Element redistributions during early stages of oxidation in a Ni38Cr22Fe20Mn10Co10 multi-principal element alloy10.1016/j.scriptamat.2020.10.051 ↗
32. Compositional partitioning during early stages of oxidation of a uranium-molybdenum alloy10.1016/j.scriptamat.2022.114528 ↗
33. Mechanistic insights into selective oxidation and corrosion of multi-principal element alloys from high resolution and in situ microscopy10.1016/j.mtla.2021.101148 ↗
34. Atomic-level studies of diffusion on metal surfaces10.1143/JJAP.32.1463 ↗
35. Atom probe tomography10.1063/1.2709758 ↗
36. An atom probe tomography study of the oxide–metal interface of an oxide intrusion ahead of a crack in a polycrystalline Ni-based superalloy10.1016/j.scriptamat.2014.10.025 ↗
37. Failure mechanisms of silicon-based atom-probe tips10.1016/j.ultramic.2008.11.013 ↗
38. Application of in situ liquid cell transmission electron microscopy in corrosion studies: A critical review of challenges and achievements10.5006/3369 ↗
39. A system for systematically preparing atom-probe field-ion-microscope specimens for the study of internal interfaces10.1063/1.1141590 ↗
40. Nanoscale perspectives of metal degradation via in situ atom probe tomography10.1007/s11244-020-01367-z ↗
41. Effect of analysis direction on the measurement of interfacial mixing in thin metal layers with atom probe tomography10.1016/j.ultramic.2010.12.010 ↗
42. Quantification of oxide particle composition in model oxide dispersion strengthened steel alloys10.1016/j.ultramic.2015.02.013 ↗
43. Comparison of atom probe tomography and transmission electron microscopy analysis of oxide dispersion strengthened steels10.1088/1742-6596/522/1/012028 ↗
44. Unveiling the Re effect on long-term coarsening behaviors of γ′ precipitates in Ni-based single crystal superalloys10.1016/j.actamat.2022.117979 ↗
45. Surface science approach of corrosion phenomena10.1016/S0013-4686(97)00239-9 ↗
46. Atomic level characterization in corrosion studies10.1098/rsta.2016.0414 ↗
47. Determination of the tip temperature in laser assisted atom-probe tomography using charge state distributions10.1063/1.3006017 ↗
48. Evolution of tip shape during field evaporation of complex multilayer structures10.1111/j.1365-2818.2010.03421.x ↗
49. Passive films at the nanoscale10.1016/j.electacta.2012.03.158 ↗
50. Progress in corrosion science at atomic and nanometric scales10.1016/j.pmatsci.2018.03.001 ↗
51. Ex situ STM imaging with atomic resolution of Ni(111) electrodes passivated in sulfuric acid10.1016/0167-2584(93)90955-I ↗
52. Atom probe analysis of AlN interlayers in AlGaN/AlN/GaN heterostructures10.1063/1.4798249 ↗
53. APT characterization of solute segregation to individual dislocations
54. High-resolution chemical and structural characterization of the native oxide scale on a Mg-based alloy10.1016/j.corsci.2023.111776 ↗
55. Hydrogen bonding interactions of H2O and SiOH on a boroaluminosilicate glass corroded in aqueous solution10.1038/s41529-019-0105-2 ↗
56. On the field evaporation behavior of dielectric materials in three-dimensional atom probe: A numeric simulation10.1017/S1431927610093888 ↗
57. A surface enhanced Raman spectroscopic study of the passive films formed in borate buffer on iron, nickel, chromium and stainless steel10.1016/0010-938X(94)00102-C ↗
58. In-situ synchrotron GIXRD study of passive film evolution on duplex stainless steel in corrosive environment10.1016/j.corsci.2018.06.040 ↗
59. Passivation of a corrosion-resistant high entropy alloy in non-oxidizing sulfate solutions10.1016/j.actamat.2018.10.026 ↗
60. Passive film formation on the new biocompatible non-equiatomic Ti21Nb24Mo23Hf17Ta15 high entropy alloy before and after resting in simulated body fluid10.1016/j.corsci.2022.110607 ↗
61. Use of in situ atomic force microscopy to image corrosion at inclusions10.1149/1.2054943 ↗
62. Structure, dissolution, and passivation of Ni(111) electrodes in sulfuric acid solution: An in situ STM, X-ray scattering, and electrochemical study10.1016/S0013-4686(02)00827-7 ↗
63. Electrochemical behavior of Cr2O3/Fe2O3 artificial passive films studied by in situ XANES10.1149/1.1838347 ↗
64. Revealing the complexity of high temperature oxide formation in a 38Ni-21Cr-20Fe-13Ru-6Mo-2W (at%) multi-principal element alloy10.1016/j.scriptamat.2021.114419 ↗
65. Considerations for using calibration curves to infer oxide stoichiometry from atom probe tomography data10.1093/mam/ozae044.018 ↗
66. Grain boundary depletion and migration during selective oxidation of Cr in a Ni–5Cr binary alloy exposed to high-temperature hydrogenated water10.1016/j.scriptamat.2014.06.022 ↗
67. Examinations of oxidation and sulfidation of grain boundaries in alloy 600 exposed to simulated pressurized water reactor primary water10.1017/S1431927613000421 ↗
68. A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography10.1016/j.ultramic.2018.07.010 ↗
69. In situ metallic coating of atom probe specimen for enhanced yield, performance, and increased field-of-view10.1093/mam/ozae006 ↗
70. Corrosion chemistry closing comments: Opportunities in corrosion science facilitated by operando experimental characterization combined with multi-scale computational modelling10.1039/C5FD00075K ↗
71. Surface properties probed by second-harmonic and sum-frequency generation10.1038/337519a0 ↗
72. Facilitating the systematic nanoscale study of battery materials by atom probe tomography through in-situ metal coating10.1002/batt.202300403 ↗
73. Atom probe tomography of oxide scales10.1007/s11085-012-9330-6 ↗
74. Resolving iron(II) sorption and oxidative growth on hematite (001) using atom probe tomography10.1021/acs.jpcc.7b11989 ↗
75. Visualizing the iron atom exchange front in the Fe (II)-catalyzed recrystallization of goethite by atom probe tomography10.1073/pnas.1816620116 ↗
76. In situ site-specific specimen preparation for atom probe tomography10.1016/j.ultramic.2006.06.008 ↗
77. Atomic structure of the passive oxide film formed on iron10.1103/PhysRevLett.79.4282 ↗
78. Quantitative investigations of atomic processes on metal surfaces at atomic resolution10.1016/0079-6816(80)90001-5 ↗
79. Critical review on the passive film formation and breakdown on iron electrode and the models for the mechanisms underlying passivity10.1016/j.jelechem.2016.12.020 ↗
80. Modeling image distortions in 3DAP10.1017/S1431927604040486 ↗
81. Study of the surface oxides and corrosion behaviour of an equiatomic CoCrFeMnNi high entropy alloy by XPS and ToF-SIMS10.1016/j.corsci.2020.108507 ↗
82. Origin of enhanced passivity of Cr–Fe–Co–Ni–Mo multi-principal element alloy surfaces10.1038/s41529-023-00330-z ↗
83. A versatile and reproducible cryo-sample preparation methodology for atom probe studies10.1093/micmic/ozad120 ↗
84. Radiation-enhanced anion transport in hematite10.1021/acs.chemmater.0c04235 ↗
85. Variable-angle spectroscopic ellipsometry of InAlP native oxide dielectric layers for GaAs metal–oxide–semiconductor field effect transistor applications10.1063/1.4794817 ↗
86. Unmasking chloride attack on the passive film of metals10.1038/s41467-018-04942-x ↗
87. Ziegler · 2013
88. SRIM—The stopping and range of ions in matter (2010)10.1016/j.nimb.2010.02.091 ↗