Small-angle X-ray scattering study on the microstructure evolution of zirconia nanoparticles during calcination
- State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China) and College of Material Science and Engineering, Taiyuan University of Science and Technology, Taiyuan 030024 (China) and Graduate School of Chinese Academy of Sciences, Beijing 100039 (China)
- State Key Laboratory of Coal Conversion, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001 (China)
- National Synchrotron Radiation Laboratory, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100039 (China)
Zirconia nanoparticles have been synthesized from zirconium hydroxide precipitates followed by a supercritical CO{sub 2} extraction. The microstructure evolution of these zirconia nanoparticles during the calcination at the moderate temperature has been investigated. Assisted by the analyses of TEM and XRD, small-angle X-ray scattering (SAXS) study offers possibilities to a comprehensive and quantitative characterization of the structural evolution on the nanometer scales. The as-synthesized zirconia sample exhibits a mass fractal structure constructed by the surface fractal particles. Such a structure can be preserved up to 300 deg. C. After calcination at 400 deg. C, considerable structural rearrangement occurs. In the interior of nanoparticles zirconia nanocrystallites emerge. It is the scattering from such zirconia nanoparticles that give rise to the broadened crossover in the ln[J(q)] vs. ln q plot and the scattering peak in the ln[q {sup 3} J(q)] vs. q {sup 2} plot. With a further increase in the calcination temperature, the power-law region at large-q in ln J(q) vs. ln q plot expands, and the peak in ln[q {sup 3} J(q)] vs. q {sup 2} plot shifts towards lower q values, indicating size increases in both the nanocrystallites and nanoparticles. Besides, the mass fractal structure constructed by zirconia nanoparticles can be largely preserved during the moderate temperature calcination.
- OSTI ID:
- 20784944
- Journal Information:
- Journal of Solid State Chemistry, Journal Name: Journal of Solid State Chemistry Journal Issue: 4 Vol. 179; ISSN 0022-4596; ISSN JSSCBI
- Country of Publication:
- United States
- Language:
- English
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