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

Title: In Situ Heater Design for Nanoscale Synchrotron-Based Full-Field Transmission X-Ray Microscopy

Journal Article · · Microscopy and Microanalysis

Abstract The oxidation of nickel powder under a controlled gas and temperature environment was studied using synchrotron-based full-field transmission X-ray microscopy. The use of this technique allowed for the reaction to be imagedin situat 55 nm resolution. The setup was designed to fit in the limited working distance of the microscope and to provide the gas and temperature environments analogous to solid oxide fuel cell operating conditions. Chemical conversion from nickel to nickel oxide was confirmed using X-ray absorption near-edge structure. Using an unreacted core model, the reaction rate as a function of temperature and activation energy were calculated. This method can be applied to study many other chemical reactions requiring similar environmental conditions.

Research Organization:
Energy Frontier Research Centers (EFRC) (United States). Heterogeneous Functional Materials Center (HeteroFoaM); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Organization:
National Science Foundation (NSF); USDOE Office of Science (SC), Basic Energy Sciences (BES)
DOE Contract Number:
AC02-06CH11357
OSTI ID:
1392066
Journal Information:
Microscopy and Microanalysis, Vol. 21, Issue 02; ISSN 1431-9276
Publisher:
Microscopy Society of America (MSA)
Country of Publication:
United States
Language:
English

References (31)

Transport processes during the growth of oxide films at elevated temperature journal April 1985
In Situ X-Ray Absorption Near-Edge Structure Evidence for Quadrivalent Nickel in Nickel Battery Electrodes journal January 1996
Reduction and Reoxidation Processes of NiO∕YSZ Composite for Solid Oxide Fuel Cell Anodes journal March 2006
Zone-doubled Fresnel zone plates for high-resolution hard X-ray full-field transmission microscopy journal July 2012
Pine-cone morphology and pseudocapacitive behavior of nanoporous nickel oxide journal December 2010
In-situ observation of nickel oxidation using synchrotron based full-field transmission X-ray microscopy journal February 2013
Chemically grown, porous, nickel oxide thin-film for electrochemical supercapacitors journal February 2011
TXM-Wizard : a program for advanced data collection and evaluation in full-field transmission X-ray microscopy journal January 2012
X-Ray Interactions: Photoabsorption, Scattering, Transmission, and Reflection at E = 50-30,000 eV, Z = 1-92 journal July 1993
Thermal analysis of the cyclic reduction and oxidation behaviour of SOFC anodes journal March 2005
Recent advances in synchrotron-based hard x-ray phase contrast imaging journal November 2013
Design of experiment approach applied to reducing and oxidizing tolerance of anode supported solid oxide fuel cell. Part II: Electrical, electrochemical and microstructural characterization of tape-cast cells journal November 2011
Oxidation kinetics of small nickel particles journal January 1999
In Situ Observations of Microstructural Changes in SOFC Anodes during Redox Cycling journal January 2006
A Review of RedOx Cycling of Solid Oxide Fuel Cells Anode journal August 2012
Transport processes in the oxidation of Ni studied using tracers in growing NiO scales journal December 1979
The Hydrogen Evolution and Oxidation Kinetics during Overdischarging of Sealed Nickel-Metal Hydride Batteries journal January 2006
Three-dimensional mapping of nickel oxidation states using full field x-ray absorption near edge structure nanotomography journal April 2011
In situ redox cycle of a nickel–YSZ fuel cell anode in an environmental transmission electron microscope journal August 2010
Dedicated full-field X-ray imaging beamline at Advanced Photon Source
  • Shen, Qun; Lee, Wah-Keat; Fezzaa, Kamel
  • Nuclear Instruments and Methods in Physics Research Section A: Accelerators, Spectrometers, Detectors and Associated Equipment, Vol. 582, Issue 1 https://doi.org/10.1016/j.nima.2007.08.169
journal November 2007
On the high-temperature oxidation of nickel journal January 2003
Solid Oxide Fuel Cells damage mechanisms due to Ni-YSZ re-oxidation: Case of the Anode Supported Cell journal July 2009
Electrochemical and microstructural characterization of the redox tolerance of solid oxide fuel cell anodes journal August 2005
RedOx study of anode-supported solid oxide fuel cell journal August 2009
Redox Cycling of Ni-Based Solid Oxide Fuel Cell Anodes: A Review journal June 2007
Kinetic Model for Solid‐State Reactions journal June 1961
Reduction and Reoxidation Kinetics of Nickel-Based SOFC Anodes journal January 2006
Oxidation failure modes of anode-supported solid oxide fuel cells journal June 2008
Changes in electronic structure by Li ion deintercalation in LiNiO2 from nickel L-edge and O K-edge XANES journal July 2001
The self-diffusion of Ni in NiO and its relevance to the oxidation of Ni journal February 1978
Understanding Nickel Oxidation and Reduction Processes in SOFC Systems
  • Young, Jason L.; Vedahara, Vedasri; Kung, Sherman
  • 10th International Symposium on Solid Oxide Fuel Cells (SOFC-X), ECS Transactions https://doi.org/10.1149/1.2729256
conference January 2007