NiAl Oxidation Reaction Processes Studied In Situ Using MEMS-Based Closed-Cell Gas Reaction Transmission Electron Microscopy

Unocic, Kinga A.; Shin, Dongwon; Unocic, Raymond R.; Allard, Jr., Lawrence Frederick

doi:10.1007/s11085-016-9676-2

NiAl Oxidation Reaction Processes Studied In Situ Using MEMS-Based Closed-Cell Gas Reaction Transmission Electron Microscopy

Journal Article · Tue Feb 07 00:00:00 EST 2017 · Oxidation of Metals

DOI:https://doi.org/10.1007/s11085-016-9676-2· OSTI ID:1394581

^[1]; ^[1]; ^[2]; ^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Center for Nanophase Materials Sciences Div., Oak Ridge, TN (United States)

The nanoscale oxidation mechanisms and kinetics of a model β-NiAl system were investigated using in situ closed-cell gas reaction scanning transmission electron microscopy (STEM). Here, we directly visualize the dynamic structural and chemical changes that occur during high-temperature oxidation at a high spatial resolution of 50.3Ni–49.7Al (at.%) nanoparticles under static air conditions at 730 Torr with heating up to 750 °C at 5 °C/s. A MEMS-based gas cell system, with microfabricated heater devices and a gas delivery system, was used to reveal site-specific oxidation initiation sites. Through time-resolved annular dark-field STEM imaging, we tracked the nanoscale oxidation kinetics of Al₂O₃. After oxidation at 750 °C, nucleation of voids at the Ni/Al₂O₃ interface was observed along a NiAl grain boundary, followed by the formation of faceted NiO crystals. Small faceted cubic crystals of NiO were formed at the initial stage of oxidation at high PO₂ due to the outward self-diffusion of Ni²⁺ ions, followed by the formation of a mixture of metastable and stable α-Al₂O₃ at the oxide/metal interface that is attributed to a PO₂ decrease with oxidation time, which agreed with thermodynamic modeling calculations. Furthermore, the results from these in situ oxidation experiments in the β-NiAl system are in agreement with the established oxidation mechanisms; however, with in situ closed-cell gas microscopy it is now feasible to investigate nanoscale oxidation mechanisms and kinetics in real time and at high spatial resolution and can be broadly applied to understand the basic high-temperature oxidation mechanisms for a wide range of alloy compositions.

View Accepted Manuscript (DOE)

Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Fossil Energy (FE)

Grant/Contract Number:: AC05-00OR22725

OSTI ID:: 1394581

Journal Information:: Oxidation of Metals, Journal Name: Oxidation of Metals Journal Issue: 3-4 Vol. 88; ISSN 0030-770X

Publisher:: SpringerCopyright Statement

Country of Publication:: United States

Language:: English

References (21)

Segregation studies of oxidized Y and Zr doped NiAl Schumann, E.; Yang, J. C.; Rühle, M. Materials and Corrosion/Werkstoffe und Korrosion, Vol. 46, Issue 4 https://doi.org/10.1002/maco.19950460405	journal	April 1995
The effect of Y and Zr on the Oxidation of NiAl Schumann, E.; Yang, J. C.; Graham, M. J. Materials and Corrosion/Werkstoffe und Korrosion, Vol. 47, Issue 11 https://doi.org/10.1002/maco.19960471107	journal	November 1996
High Temperature Materials Based on the Intermetallic Compound NiAl Reinforced by Refractory Metals for Advanced Energy Conversion Technologies Frommeyer, Georg; Rablbauer, Ralf steel research international, Vol. 79, Issue 7 https://doi.org/10.1002/srin.200806159	journal	July 2008
18O/SIMS characterization of the growth mechanism of doped and undoped ?-Al2O3 Pint, B. A.; Martin, J. R.; Hobbs, L. W. Oxidation of Metals, Vol. 39, Issue 3-4 https://doi.org/10.1007/BF00665610	journal	April 1993
TEM studies of oxidized NiAl and Ni3Al cross sections Doychak, J.; R�hle, M. Oxidation of Metals, Vol. 31, Issue 5-6 https://doi.org/10.1007/BF00666466	journal	June 1989
On the formation of interfacial and internal voids inα-Al2O3 scales Pint, B. A. Oxidation of Metals, Vol. 48, Issue 3-4 https://doi.org/10.1007/BF01670505	journal	October 1997
The effect of various oxide dispersions on the phase composition and morphology of Al2O3 scales grown on β-NiAl Pint, B. A.; Treska, M.; Hobbs, L. W. Oxidation of Metals, Vol. 47, Issue 1-2 https://doi.org/10.1007/BF01682369	journal	February 1997
Transient oxidation of Single-Crystal β-NiAl Doychak, J.; Smialek, J. L.; Mitchell, T. E. Metallurgical Transactions A, Vol. 20, Issue 3 https://doi.org/10.1007/BF02653930	journal	March 1989
Characterization of alumina interfaces in TBC systems Pint, B. A.; More, K. L. Journal of Materials Science, Vol. 44, Issue 7 https://doi.org/10.1007/s10853-008-3221-x	journal	April 2009
The oxidation behaviour of NiAl-I. Phase transformations in the alumina scale during oxidation of NiAl and NiAl-Cr alloys Brumm, M. W.; Grabke, H. J. Corrosion Science, Vol. 33, Issue 11 https://doi.org/10.1016/0010-938X(92)90002-K	journal	November 1992
The oxidation of NiAl-III. Internal and intergranular oxidation Brumm, M. W.; Grabke, H. J.; Wagemann, B. Corrosion Science, Vol. 36, Issue 1 https://doi.org/10.1016/0010-938X(94)90107-4	journal	January 1994
Z-contrast stem for materials science Pennycook, S. J. Ultramicroscopy, Vol. 30, Issue 1-2 https://doi.org/10.1016/0304-3991(89)90173-3	journal	June 1989
Transient oxidation of Ni-base alloys Wood, G. C.; Chattopadhyay, B. Corrosion Science, Vol. 10, Issue 7 https://doi.org/10.1016/S0010-938X(70)80032-4	journal	July 1970
Oxidation of NiAl and FeAl Grabke, H. J. Intermetallics, Vol. 7, Issue 10 https://doi.org/10.1016/S0966-9795(99)00037-0	journal	October 1999
Oxidation mechanism of nickel particles studied in an environmental transmission electron microscope Jeangros, Q.; Hansen, T. W.; Wagner, J. B. Acta Materialia, Vol. 67 https://doi.org/10.1016/j.actamat.2013.12.035	journal	April 2014
Novel MEMS-Based Gas-Cell/Heating Specimen Holder Provides Advanced Imaging Capabilities for In Situ Reaction Studies Allard, Lawrence F.; Overbury, Steven H.; Bigelow, Wilbur C. Microscopy and Microanalysis, Vol. 18, Issue 4 https://doi.org/10.1017/S1431927612001249	journal	July 2012
Controlled _{In Situ} Gas Reaction Studies of Catalysts at High Temperature and Pressure with Atomic Resolution Allard, L. F.; Bigelow, W. C.; Zhang, S. Microscopy and Microanalysis, Vol. 20, Issue S3 https://doi.org/10.1017/S1431927614009593	journal	August 2014
Computer-Controlled In Situ Gas Reactions via a MEMS-based Closed-Cell System Allard, L. F.; Bigelow, W. C.; Wu, Z. Microscopy and Microanalysis, Vol. 21, Issue S3 https://doi.org/10.1017/S1431927615001282	journal	August 2015
Direct in Situ TEM Observation of Modification of Oxidation by the Injected Vacancies for Ni–4Al Alloy Using a Microfabricated Nanopost Wang, Chong-Min; Schreiber, Daniel K.; Olszta, Matthew J. ACS Applied Materials & Interfaces, Vol. 7, Issue 31 https://doi.org/10.1021/acsami.5b04341	journal	July 2015
Oxidation induced lifetime limits of thin walled, iron based, alumina forming, oxide dispersion strengthened alloy components Quadakkers, w. J.; Bennett, M. J. Materials Science and Technology, Vol. 10, Issue 2 https://doi.org/10.1179/026708394790163807	journal	February 1994
Oxidation induced lifetime limits of thin walled, iron based, alumina forming, oxide dispersion strengthened alloy components Quadakkers, w. J.; Bennett, M. J. Materials Science and Technology, Vol. 10, Issue 2 https://doi.org/10.1179/mst.1994.10.2.126	journal	February 1994

Cited By (2)

In Situ S/TEM Reduction Reaction of Ni-Mo2C Catalyst for Biomass Conversion Unocic, Kinga A.; Choi, Jae-Soon; Ruddy, Daniel A. Microscopy and Microanalysis, Vol. 24, Issue S1 https://doi.org/10.1017/s1431927618002106	journal	August 2018
Thermally Introduced Bismuth Clustering in Ga(P,Bi) Layers under Group V Stabilised Conditions Investigated by Atomic Resolution In Situ (S)TEM Straubinger, R.; Widemann, M.; Belz, J. Scientific Reports, Vol. 8, Issue 1 https://doi.org/10.1038/s41598-018-27286-4	journal	June 2018

Similar Records

Electrochemical passivation of ordered NiAl

Journal Article · Mon Jun 01 00:00:00 EDT 1998 · Journal of the Electrochemical Society · OSTI ID:653353

A structural study of oxidation in a zirconia-toughened alumina fiber-reinforced NiAl composite

Journal Article · Wed Jun 01 00:00:00 EDT 1994 · Metallurgical Transactions, A (Physical Metallurgy and Materials Science); (United States) · OSTI ID:7174391

Duplex Oxide Formation during Transient Oxidation of Cu-5%Ni(001) Investigated by In situ UHV-TEM and XPS

Conference · Sun May 20 00:00:00 EDT 2012 · OSTI ID:1037702

Related Subjects

36 MATERIALS SCIENCE
In situ TEM
MEMS-based closed-cell gas
NiAl
Oxidation

NiAl Oxidation Reaction Processes Studied In Situ Using MEMS-Based Closed-Cell Gas Reaction Transmission Electron Microscopy

Citation Formats

References (21)

Cited By (2)

Similar Records

Related Subjects