DOE PAGES title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography

Abstract

In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample exposed to molten KCl-MgCl2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl2. Both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and deeper understanding beyond conventional analysis.

Authors:
 [1];  [2]; ORCiD logo [1]; ORCiD logo [1];  [3];  [3];  [3]; ORCiD logo [4]; ORCiD logo [4]; ORCiD logo [5]; ORCiD logo [1];  [3];  [6]; ORCiD logo [1]
  1. Idaho National Lab. (INL), Idaho Falls, ID (United States)
  2. Stony Brook Univ., NY (United States)
  3. Brookhaven National Lab. (BNL), Upton, NY (United States)
  4. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Univ. of Tennessee, Knoxville, TN (United States)
  5. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
  6. Stony Brook Univ., NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)
Publication Date:
Research Org.:
Brookhaven National Laboratory (BNL), Upton, NY (United States); Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States); Idaho National Laboratory (INL), Idaho Falls, ID (United States)
Sponsoring Org.:
USDOE Office of Science (SC); USDOE Office of Nuclear Energy (NE)
OSTI Identifier:
1832023
Alternate Identifier(s):
OSTI ID: 1832937; OSTI ID: 1835199; OSTI ID: 1837226; OSTI ID: 1916452
Report Number(s):
BNL-222427-2021-JAAM; BNL-222518-2021-JAAM; INL/JOU-21-63822-Rev000
Journal ID: ISSN 0010-938X
Grant/Contract Number:  
SC0012704; AC07-05ID14517; AC05-00OR22725
Resource Type:
Accepted Manuscript
Journal Name:
Corrosion Science
Additional Journal Information:
Journal Volume: 195; Journal ID: ISSN 0010-938X
Publisher:
Elsevier
Country of Publication:
United States
Language:
English
Subject:
36 MATERIALS SCIENCE; Molten salt corrosion; quasi in situ TEM; dealloying; X-ray nano-tomography; in situ 12 synchrotron; microstructure; electron microscopy; synchrotron; Nickel alloy

Citation Formats

Bawane, Kaustubh, Liu, Xiaoyang, Gakhar, Ruchi, Woods, Michael, Ge, Mingyuan, Xiao, Xianghui, Lee, Wah-Keat, Halstenberg, Philip, Dai, Sheng, Mahurin, Shannon Mark, Pimblott, Simon M., Wishart, James F., Chen-Wiegart, Yu-chen Karen, and He, Lingfeng. Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography. United States: N. p., 2021. Web. doi:10.1016/j.corsci.2021.109962.
Bawane, Kaustubh, Liu, Xiaoyang, Gakhar, Ruchi, Woods, Michael, Ge, Mingyuan, Xiao, Xianghui, Lee, Wah-Keat, Halstenberg, Philip, Dai, Sheng, Mahurin, Shannon Mark, Pimblott, Simon M., Wishart, James F., Chen-Wiegart, Yu-chen Karen, & He, Lingfeng. Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography. United States. https://doi.org/10.1016/j.corsci.2021.109962
Bawane, Kaustubh, Liu, Xiaoyang, Gakhar, Ruchi, Woods, Michael, Ge, Mingyuan, Xiao, Xianghui, Lee, Wah-Keat, Halstenberg, Philip, Dai, Sheng, Mahurin, Shannon Mark, Pimblott, Simon M., Wishart, James F., Chen-Wiegart, Yu-chen Karen, and He, Lingfeng. Sat . "Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography". United States. https://doi.org/10.1016/j.corsci.2021.109962. https://www.osti.gov/servlets/purl/1832023.
@article{osti_1832023,
title = {Visualizing time-dependent microstructural and chemical evolution during molten salt corrosion of Ni-20Cr model alloy using correlative quasi in situ TEM and in situ synchrotron X-ray nano-tomography},
author = {Bawane, Kaustubh and Liu, Xiaoyang and Gakhar, Ruchi and Woods, Michael and Ge, Mingyuan and Xiao, Xianghui and Lee, Wah-Keat and Halstenberg, Philip and Dai, Sheng and Mahurin, Shannon Mark and Pimblott, Simon M. and Wishart, James F. and Chen-Wiegart, Yu-chen Karen and He, Lingfeng},
abstractNote = {In situ monitoring of corrosion processes is important to fundamentally understand the kinetics and evolution of materials in harsh environments. A quasi in situ transmission electron microscopy technique was utilized to study microstructural and chemical evolution of a Ni-20Cr disc sample exposed to molten KCl-MgCl2 salt for 60 s in consecutive 20 s iterations. In situ synchrotron X-ray nano-tomography was performed to characterize the morphological evolution of a Ni-20Cr microwire exposed to molten KCl-MgCl2. Both techniques captured key corrosion events and revealed mechanisms at different time and length scales, potentially bringing greater insights and deeper understanding beyond conventional analysis.},
doi = {10.1016/j.corsci.2021.109962},
journal = {Corrosion Science},
number = ,
volume = 195,
place = {United States},
year = {Sat Nov 20 00:00:00 EST 2021},
month = {Sat Nov 20 00:00:00 EST 2021}
}

Journal Article:

Figures / Tables:

Fig. 1 Fig. 1: Experimental setup for (a) quasi in situ molten salt corrosion of TEM sample, (b) in situ X-ray nano-tomography experiment setup for observing the 3D morphology evolution of Ni-20Cr in molten KCl-MgCl2 at 500 °C.

Save / Share:

Works referenced in this record:

Investigating local oxidation processes in Fe thin films in a water vapor environment by in situ liquid cell TEM
journal, February 2020


In Situ Transmission Electron Microscopy of High-Temperature Inconel-625 Corrosion by Molten Chloride Salts
journal, May 2021

  • Pragnya, Prachi; Gall, Daniel; Hull, Robert
  • Journal of The Electrochemical Society, Vol. 168, Issue 5
  • DOI: 10.1149/1945-7111/ac0225

Corrosion behavior of 316SS and Ni-based alloys in a ternary NaCl-KCl-MgCl2 molten salt
journal, September 2018


Molten chloride salts for next generation CSP plants: Electrolytical salt purification for reducing corrosive impurity level
journal, September 2019


Volume and Grain Boundary Diffusion of Chromium in Ni-Base Ni-Cr-Fe Alloys
journal, January 2003

  • Chen, Tien-Fu; Tiwari, Gyanendra Prasad; Iijima, Yoshiaki
  • MATERIALS TRANSACTIONS, Vol. 44, Issue 1
  • DOI: 10.2320/matertrans.44.40

Oxidation of Ni-20 Cr alloy and stainless steels in the presence of chlorides
journal, January 1970


Molten chloride salts for next generation CSP plants: Selection of promising chloride salts & study on corrosion of alloys in molten chloride salts
conference, January 2019

  • Ding, Wenjin; Bonk, Alexander; Bauer, Thomas
  • SOLARPACES 2018: International Conference on Concentrating Solar Power and Chemical Energy Systems, AIP Conference Proceedings
  • DOI: 10.1063/1.5117729

Early stages during localized corrosion of AA2024 TEM specimens in chloride environment: Early stages during localized corr. of AA2024 TEM specimens in Cl env
journal, December 2012

  • Malladi, S. R. K.; Xu, Q.; Tichelaar, F. D.
  • Surface and Interface Analysis, Vol. 45, Issue 10
  • DOI: 10.1002/sia.5193

Corrosion in the molten fluoride and chloride salts and materials development for nuclear applications
journal, August 2018


Proton irradiation-decelerated intergranular corrosion of Ni-Cr alloys in molten salt
journal, July 2020


Investigating corrosion behavior of Ni and Ni-20Cr in molten ZnCl2
journal, February 2021


Corrosion evaluation of eutectic chloride molten salt for new generation of CSP plants. Part 2: Materials screening performance
journal, June 2020


Developments in synchrotron x-ray computed microtomography at the National Synchrotron Light Source
conference, September 1999

  • Dowd, Betsy A.; Campbell, Graham H.; Marr, Robert B.
  • SPIE's International Symposium on Optical Science, Engineering, and Instrumentation, SPIE Proceedings
  • DOI: 10.1117/12.363725

Corrosion behavior and mechanism of austenitic stainless steels in a new quaternary molten salt for concentrating solar power
journal, June 2019


Corrosion-induced microstructural developments in 316 stainless steel during exposure to molten Li2BeF4(FLiBe) salt
journal, December 2016


Effect of Surface Roughness on Pitting Corrosion of AZ31 Mg Alloy
journal, May 2020

  • Mitchell, Jeffrey; Crow, Natalie; Nieto, Andy
  • Metals, Vol. 10, Issue 5
  • DOI: 10.3390/met10050651

Effect of surface roughness on corrosion behavior of the superalloy IN718 in simulated marine environment
journal, April 2018

  • Pradhan, Dhananjay; Mahobia, Girija Shankar; Chattopadhyay, Kausik
  • Journal of Alloys and Compounds, Vol. 740
  • DOI: 10.1016/j.jallcom.2018.01.042

Introducing and Controlling Water Vapor in Closed-Cell In Situ Electron Microscopy Gas Reactions
journal, March 2020

  • Unocic, Kinga A.; Walden, Franklin S.; Marthe, Nelson L.
  • Microscopy and Microanalysis, Vol. 26, Issue 2
  • DOI: 10.1017/S1431927620000185

Application of a Quasi In Situ Experimental Approach to Estimate 3-D Pitting Corrosion Kinetics in Stainless Steel
journal, January 2016

  • Almuaili, F. A.; McDonald, S. A.; Withers, P. J.
  • Journal of The Electrochemical Society, Vol. 163, Issue 13
  • DOI: 10.1149/2.0381613jes

TomoPy: a framework for the analysis of synchrotron tomographic data
journal, August 2014

  • Gürsoy, Dogˇa; De Carlo, Francesco; Xiao, Xianghui
  • Journal of Synchrotron Radiation, Vol. 21, Issue 5
  • DOI: 10.1107/S1600577514013939

Molten-Salt Reactor Chemistry
journal, February 1970


Influence of graphite-alloy interactions on corrosion of Ni-Mo-Cr alloy in molten fluorides
journal, May 2018


Inconel 617 corrosion in FLiNaK molten salts: An in situ X-ray diffraction study
journal, April 2021


The molten salt reactor (MSR) in generation IV: Overview and perspectives
journal, November 2014


Effect of CrF 3 on the corrosion behaviour of Hastelloy-N and 316L stainless steel alloys in FLiNaK molten salt
journal, February 2018


Stabilized Nanoporous Metals by Dealloying Ternary Alloy Precursors
journal, December 2008

  • Snyder, Josh; Asanithi, Piyapong; Dalton, Alan B.
  • Advanced Materials, Vol. 20, Issue 24, p. 4883-4886
  • DOI: 10.1002/adma.200702760

Elucidating Ionic Correlations Beyond Simple Charge Alternation in Molten MgCl 2 –KCl Mixtures
journal, November 2019

  • Wu, Fei; Roy, Santanu; Ivanov, Alexander S.
  • The Journal of Physical Chemistry Letters, Vol. 10, Issue 24
  • DOI: 10.1021/acs.jpclett.9b02845

Identification of MnCr2O4 nano-octahedron in catalysing pitting corrosion of austenitic stainless steels
journal, September 2010


Revealing 3D Morphological and Chemical Evolution Mechanisms of Metals in Molten Salt by Multimodal Microscopy
journal, March 2020

  • Ronne, Arthur; He, Lingfeng; Dolzhnikov, Dmitriy
  • ACS Applied Materials & Interfaces, Vol. 12, Issue 15
  • DOI: 10.1021/acsami.9b19099

Advanced heat exchanger development for molten salts
journal, December 2014


Quasi-in-situ STEM-EDS insight into the role of Ag in the corrosion behaviour of Mg-Gd-Zr alloys
journal, May 2018


Cellular automata simulation on the corrosion behavior of Ni-base alloy in chloride molten salt
journal, December 2019


Aggregation and data analysis of corrosion studies in molten chloride and fluoride salts
journal, December 2018


Time-sequential corrosion behaviour observation of micro-alloyed Mg-0.5Zn-0.2Ca alloy via a quasi-in situ approach
journal, September 2019


Materials corrosion in molten LiF–NaF–KF salt
journal, January 2009


Electrochemical monitoring of high-temperature molten-salt corrosion
journal, February 1990

  • Gao, G.; Stott, F. H.; Dawson, J. L.
  • Oxidation of Metals, Vol. 33, Issue 1-2
  • DOI: 10.1007/BF00665670

Determining oxidation states of transition metals in molten salt corrosion using electron energy loss spectroscopy
journal, May 2021


One-minute nano-tomography using hard X-ray full-field transmission microscope
journal, August 2018

  • Ge, Mingyuan; Coburn, David Scott; Nazaretski, Evgeny
  • Applied Physics Letters, Vol. 113, Issue 8
  • DOI: 10.1063/1.5048378

Molten salt reactors: A new beginning for an old idea
journal, June 2010


Corrosion of alloys in a chloride molten salt (NaCl-LiCl) for solar thermal technologies
journal, December 2016


Synergistic effect of irradiation and molten salt corrosion: Acceleration or deceleration?
journal, June 2021


Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.