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

Published online by Cambridge University Press:  05 March 2015

Andrew M. Kiss
Affiliation:
Department of Mechanical Engineering, University of Connecticut, Storrs, CT 06269-3139, USA
William M. Harris
Affiliation:
Department of Mechanical Engineering, University of Connecticut, Storrs, CT 06269-3139, USA
Arata Nakajo
Affiliation:
Department of Mechanical Engineering, University of Connecticut, Storrs, CT 06269-3139, USA
Steve Wang
Affiliation:
Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA
Joan Vila-Comamala
Affiliation:
Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA
Alex Deriy
Affiliation:
Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439, USA
Wilson K. S. Chiu*
Affiliation:
Department of Mechanical Engineering, University of Connecticut, Storrs, CT 06269-3139, USA
*
*Corresponding author.wchiu@engr.uconn.edu
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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 imaged in situ at 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.

Type
Equipment Development
Copyright
© Microscopy Society of America 2015 

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References

Atkinson, A. (1985). Transport processes during the growth of oxide films at elevated temperature. Rev Mod Phys 57, 437470.Google Scholar
Atkinson, A. & Taylor, R.I. (1978). The self-diffusion of Ni in NiO and its relevance to the oxidation of Ni. J Mater Sci 13, 427432.Google Scholar
Atkinson, A., Taylor, R.I. & Goode, P.D. (1979). Transport processes in the oxidation of Ni studied using tracers in growing NiO scales. Oxid Met 13, 519543.Google Scholar
Ayeb, A., Otten, W.M., Mank, A.J.G. & Notten, P.H.L. (2006). The hydrogen evolution and oxidation kinetics during overdischarging of sealed nickel-metal hydride batteries. J Electrochem Soc 153, 20552065.Google Scholar
Carter, R.E. (1961). Kinetic model for solid-state reactions. J Chem Phys 34, 20102015.Google Scholar
Faes, A., Hessler-Wyser, A., Zryd, A. & Van Herle, J. (2012). A review of redox cycling of solid oxide fuel cells anode. Membranes 2, 585664.Google Scholar
Faes, A., Nakajo, A., Hessler-Wyser, A., Dubois, D., Brisse, A., Modena, S. & Van Herle, J. (2009). Redox study of anode-supported solid oxide fuel cell. J Power Sources 193, 5564.Google Scholar
Faes, A., Wuillemin, Z., Tanasini, P., Accardo, N., Modena, S., Schindler, H.J., Cantoni, M., Lübbe, H., Diethelm, S., Hessler-Wyser, A. & Van Herle, J. (2011). 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. J Power Sources 196, 89098917.CrossRefGoogle Scholar
Green, D.W. & Perry, R.H. (2008). Perry’s Chemical Engineers’ Handbook. New York, NY: McGraw-Hill.Google Scholar
Haugsrud, R. (2003). On the high-temperature oxidation of nickel. Corros Sci 45, 211235.Google Scholar
Henke, B.L., Gullikson, E.M. & Davis, J.C. (1993). X-ray interactions: Photoabsorption, scattering, transmission, and reflection at E=50-30000eV, Z=1-92. At Data Nucl Data Tables 54(2), 181342.Google Scholar
Inamdar, A.I., Kim, Y., Pawar, S.M., Kim, J.H., Im, H. & Kim, H. (2011). Chemically grown, porous, nickel oxide thin-film for electrochemical supercapacitors. J Power Sources 196, 23932397.Google Scholar
Jeangros, Q., Faes, A., Wagner, J.B., Hansen, T.W., Aschauer, U., Van Herle, J., Hessler-Wyser, A. & Dunin-Borkowski, R.E. (2010). In situ redox cycle of a nickel–YSZ fuel cell anode in an environmental transmission electron microscope. Acta Mater 58, 45784589.Google Scholar
Karmhag, R., Niklasson, G.A. & Nygren, M. (1999). Oxidation kinetics of small nickel particles. J Appl Phys 85, 11861191.CrossRefGoogle Scholar
Kiss, A.M., Harris, W.M., Wang, S., Vila-Comamala, J., Deriy, A. & Chiu, W.K.S. (2013). In-situ observation of nickel oxidation using synchrotron based full-field transmission X-ray microscopy. Appl Phys Lett 102, 053902.CrossRefGoogle Scholar
Klemensø, T., Appel, C.C. & Mogensen, M. (2006). In situ observations of microstructural changes in SOFC anodes during redox cycling. Electrochem Solid-State Lett 9, A403A407.Google Scholar
Laurencin, J., Delette, G., Morel, B., Lefebvre-Joud, F. & Dupeux, M. (2009). Solid oxide fuel cells damage mechanisms due to Ni-YSZ re-oxidation: Case of the anode supported cell. J Power Sources 192, 344352.Google Scholar
Levenspiel, O. (1972). Chemical Reaction Engineering, 2nd ed. New York, NY: Wiley.Google Scholar
Liu, Y., Nelson, J., Holzner, C., Andrews, J.C. & Pianetta, P. (2013). Recent advances in synchrotron-based hard X-ray phase contrast imaging. J Phys D 46, 494001.Google Scholar
Liu, Y., Meirer, F., Williams, P.A., Wang, J., Andrews, J.C. & Pianetta, P. (2012). TXM-Wizard: A program for advanced data collection and evaluation in full-field transmission X-ray microscopy. J Synchrotron Radiat 19, 281287.Google Scholar
Meher, S.K., Justin, P. & Rao, G.R. (2010). Pine-cone morphology and pseudocapacitive behavior of nanoporous nickel oxide. Electrochim Acta 55, 83888396.Google Scholar
Modena, S., Ceschini, S., Tomasi, A., Montinaro, D. & Sglavo, V.M. (2006). Reduction and reoxidation processes of NiO/YSZ composite for solid oxide fuel cell anodes. J Fuel Cell Sci Technol 3, 487491.Google Scholar
Nelson, G.J., Harris, W.M., Izzo, J.R. Jr., Grew, K.N., Chiu, W.K.S., Chu, Y.S., Yi, J., Andrews, J.C., Liu, Y. & Pianetta, P. (2011). Three-dimensional mapping of nickel oxidation states using full field X-ray absorption near edge structure nanotomography. Appl Phys Lett 98, 173109.Google Scholar
O’Grady, W.E., Pandya, K.I., Swider, K.E. & Corrigan, D.A. (1996). In situ X-ray absorption near-edge structure evidence for quadrivalent nickel in nickel battery electrodes. J Electrochem Soc 143, 16131616.Google Scholar
Sarantaridis, D. & Atkinson, A. (2007). Redox cycling of Ni-based solid oxide fuel cell anodes: A review. Fuel Cells 7, 246258.Google Scholar
Sarantaridis, D., Rudkin, R.A. & Atkinson, A. (2008). Oxidation failure modes of anode-supported solid oxide fuel cells. J Power Sources 180, 704710.Google Scholar
Shen, Q., Lee, W., Fezzaa, K., Chu, Y.S., De Carlo, F., Jemian, P., Ilavsky, J., Erdmann, M. & Long, G.G. (2007). Dedicated full-field X-ray imaging beamline at advanced photon source. Nucl Instrum Methods Phys Res 582, 7779.Google Scholar
Tikekar, N.M., Armstrong, T.J. & Virkar, A.V. (2006). Reduction and reoxidation kinetics of nickel-based SOFC anodes. J Electrochem Soc 153, A654A663.Google Scholar
Uchimoto, Y., Sawada, H. & Yao, T. (2001). Changes in electronic structure by Li ion deintercalation in LiNiO2 from nickel L-edge and O K-edge XANES. J Power Sources 97–98, 326327.Google Scholar
Vila-Comamala, J., Pan, Y., Lombardo, J.J., Harris, W.M., Chiu, W.K.S., David, C. & Wang, Y. (2012). Zone-doubled Fresnel zone plates for high-resolution hard X-ray full-field transmission microscopy. J Synchrotron Radiat 19, 705709.Google Scholar
Waldbillig, D., Wood, A. & Ivey, D.G. (2005 a). Electrochemical and microstructural characterization of the redox tolerance of solid oxide fuel cell anodes. J Power Sources 145, 206215.Google Scholar
Waldbillig, D., Wood, A. & Ivey, D.G. (2005 b). Thermal analysis of the cyclic reduction and oxidation behaviour of SOFC anodes. Solid State Ionics 176, 847859.Google Scholar
Young, J.L., Vedahara, V., Kung, S., Xia, S. & Birss, V. (2007). Understanding nickel oxidation and reduction processes in SOFC systems. In ECS Trans, Eguchi, K., Mizusaki, J., Singhal, S. & Yokokawa, H. (Eds.), pp. 15111519. Pennington, NJ: The Electrochemical Society Proceedings Series.Google Scholar