skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Revealing High-Temperature Reduction Dynamics of High-Entropy Alloy Nanoparticles via In Situ Transmission Electron Microscopy

Journal Article · · Nano Letters
ORCiD logo [1]; ORCiD logo [2]; ORCiD logo [3];  [4]; ORCiD logo [4]; ORCiD logo [1]; ORCiD logo [4]; ORCiD logo [5]; ORCiD logo [3]; ORCiD logo [6]; ORCiD logo [7]
  1. Univ. of Chicago, IL (United States). Dept. of of Mechanical and Industrial Engineering
  2. Univ. of Maryland, College Park, MD (United States). Dept. of Chemical and Biomolecular Engineering; Univ. of California, Riverside, CA (United States). Dept. of Chemical Engineering and Materials Science
  3. Univ. of Pittsburgh, PA (United States). Dept. of Mechanical Engineering and Materials Science
  4. Northwestern Univ., Evanston, IL (United States). Northwestern University Atomic and Nanoscale Characterization Experimental (NUANCE) Center, Dept. of Materials Science and Engineering, International Institute for Nanotechnology (IIN)
  5. Univ. of California, Riverside, CA (United States). Dept. of Chemical Engineering and Materials Science
  6. Argonne National Lab. (ANL), Argonne, IL (United States). Center for Nanoscale Materials
  7. Department of Mechanical and Industrial Engineering, University of Illinois at Chicago, Chicago, Illinois 60607, United States

Understanding the behavior of high-entropy alloy (HEA) materials under hydrogen (H2) environment is of utmost importance for their promising applications in structural materials, catalysis, and energy-related reactions. Herein, the reduction behavior of oxidized FeCoNiCuPt HEA nanoparticles (NPs) in atmospheric pressure H-2 environment was investigated by in situ gas-cell transmission electron microscopy (TEM). The reduction reaction front was maintained at the external surface of the oxide. During reduction, the oxide layer expanded and transformed into porous structures where oxidized Cu was fully reduced to Cu NPs while Fe, Co, and Ni remained in the oxidized form. In situ chemical analysis showed that the expansion of the oxide layer resulted from the outward diffusion flux of all transition metals (Fe, Co, Ni, Cu). Revealing the H-2 reduction behavior of HEA NPs facilitates the development of advanced multicomponent alloys for applications targeting H2 formation and storage, catalytic hydrogenation, and corrosion removal.

Research Organization:
Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities Division; National Science Foundation (NSF); W.M. Keck Foundation; State of Illinois
Grant/Contract Number:
AC02-06CH11357; DMR-1809439; DMR-1809085
OSTI ID:
1777239
Journal Information:
Nano Letters, Vol. 21, Issue 4; ISSN 1530-6984
Publisher:
American Chemical SocietyCopyright Statement
Country of Publication:
United States
Language:
English

References (47)

Beating hydrogen with its own weapon: Nano-twin gradients enhance embrittlement resistance of a high-entropy alloy journal December 2018
Alloying, thermal stability and strengthening in spark plasma sintered AlxCoCrCuFeNi high entropy alloys journal January 2014
Oxidation Behavior of Al 8 Co 17 Cr 17 Cu 8 Fe 17 Ni 33 , Al 23 Co 15 Cr 23 Cu 8 Fe 15 Ni 15 , and Al 17 Co 17 Cr 17 Cu 17 Fe 17 Ni 17 Compositionally Complex Alloys (High-Entropy Alloys) at Elevated Temperatures in Air : Oxidation Behavior of Al journal June 2015
In Situ Observation of Hydrogen-Induced Surface Faceting for Palladium-Copper Nanocrystals at Atmospheric Pressure journal September 2016
High entropy alloy as a highly active and stable electrocatalyst for hydrogen evolution reaction journal July 2018
Phase equilibria, microstructure, and high temperature oxidation resistance of novel refractory high-entropy alloys journal March 2015
Superior hydrogen storage in high entropy alloys journal November 2016
Carbothermal shock synthesis of high-entropy-alloy nanoparticles journal March 2018
The oxidation behavior of an equimolar FeCoNiCrMn high-entropy alloy at 950°C in various oxygen-containing atmospheres journal July 2016
In Situ TEM Study of Catalytic Nanoparticle Reactions in Atmospheric Pressure Gas Environment journal September 2013
Aerosol Synthesis of High Entropy Alloy Nanoparticles journal February 2020
Hydrogen sorption in TiZrNbHfTa high entropy alloy journal February 2019
Hydrogen embrittlement of an interstitial equimolar high-entropy alloy journal May 2018
In Situ Industrial Bimetallic Catalyst Characterization using Scanning Transmission Electron Microscopy and X-ray Absorption Spectroscopy at One Atmosphere and Elevated Temperature journal July 2017
In situ atomic-scale imaging of the metal/oxide interfacial transformation journal August 2017
X-ray diffraction study of nickel oxide reduction by hydrogen journal June 2003
Structure and Hydrogenation Properties of a HfNbTiVZr High-Entropy Alloy journal February 2018
In‐situ Transmission Electron Microscope Techniques for Heterogeneous Catalysis journal April 2020
Microstructure and mechanical properties of twinned Al0.5CrFeNiCo0.3C0.2 high entropy alloy processed by mechanical alloying and spark plasma sintering journal February 2014
Formation of Oxygen Radical Sites on MoVNbTeOx by Cooperative Electron Redistribution journal August 2017
Nanostructured High-Entropy Alloys with Multiple Principal Elements: Novel Alloy Design Concepts and Outcomes journal May 2004
In Situ Oxidation Studies of High-Entropy Alloy Nanoparticles journal October 2020
Resistance of CoCrFeMnNi high-entropy alloy to gaseous hydrogen embrittlement journal July 2017
Oxidation Behavior of the CrMnFeCoNi High-Entropy Alloy journal March 2016
Real‐Time Imaging of Nanoscale Redox Reactions over Bimetallic Nanoparticles journal July 2019
High-Entropy Alloys: A Critical Review journal April 2014
Revealing Sintering Kinetics of MoS 2 -Supported Metal Nanocatalysts in Atmospheric Gas Environments via Operando Transmission Electron Microscopy journal April 2020
Bimetallic Nanoparticle Oxidation in Three Dimensions by Chemically Sensitive Electron Tomography and in Situ Transmission Electron Microscopy journal July 2018
Three-Dimensional Quantification of the Facet Evolution of Pt Nanoparticles in a Variable Gaseous Environment journal December 2018
Hybrid Monte Carlo/Molecular Dynamics Simulation of a Refractory Metal High Entropy Alloy journal October 2013
High-entropy alloy: challenges and prospects journal July 2016
Microstructure and strengthening mechanisms in an FCC structured single-phase nanocrystalline Co25Ni25Fe25Al7.5Cu17.5 high-entropy alloy journal April 2016
High-entropy alloys journal June 2019
First demonstration of promising selective electron beam melting method for utilizing high-entropy alloys as engineering materials journal November 2015
Reduction of nickel oxide particles by hydrogen studied in an environmental TEM journal November 2012
Ultrahigh-strength CoCrFeMnNi high-entropy alloy wire rod with excellent resistance to hydrogen embrittlement journal August 2018
The use of high-entropy alloys in additive manufacturing journal April 2015
Air-oxidation of FeCoNiCr-based quinary high-entropy alloys at 700–900 °C journal June 2017
Oxidation behavior of arc melted AlCoCrFeNi multi-component high-entropy alloys journal July 2016
Insight by In Situ Gas Electron Microscopy on the Thermal Behaviour and Surface Reactivity of Cobalt Nanoparticles journal July 2018
Additive manufacturing of metals: a brief review of the characteristic microstructures and properties of steels, Ti-6Al-4V and high-entropy alloys journal January 2017
Synthesis of high-entropy alloy nanoparticles on supports by the fast moving bed pyrolysis journal April 2020
Microstructure and hydrogen storage properties of a TiZrNbMoV high entropy alloy synthesized using Laser Engineered Net Shaping (LENS) journal June 2014
In-Situ TEM visualization of vacancy injection and chemical partition during oxidation of Ni-Cr nanoparticles journal January 2014
Relative effects of enthalpy and entropy on the phase stability of equiatomic high-entropy alloys journal April 2013
A review on fundamental of high entropy alloys with promising high–temperature properties journal September 2018
In situ detection of hydrogen-induced phase transitions in individual palladium nanocrystals journal September 2014