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Processing of Cr/Cr stabilized c-ZrO nanoparticles through thermomechanical attrition process

Materials and Manufacturing Processes, ISSN: 1042-6914, Vol: 17, Issue: 4, Page: 529-542
2002
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Conference Paper Description

Stabilized zirconia in nanoparticles in c-ZrO polymorph has been synthesized with a small quantity of (5 mol%) additive of Cr and Cr cations by thermomechanical attrition (MA) process. The MA process allows the chromium cations to dissolve in the precursor in an amorphous state in order to obtain a stabilized phase in c-ZrO. This is not so easily possible by conventional methods. The synthesis process consists of a controlled Cr/Cr:c-ZrO nucleation and growth from an energized amorphous precursor of the metal cations. It involves a reactive milling of dispersed Cr cations by (NH)CrO in an amorphous precipitate of Zr oxyhydroxide. During milling, the Cr reacts with Zr in producing a high-energy solid solution in an amorphous structure. The occurrence in the change from Cr → Cr/Cr oxidation state is promoted by a plastic deformation and mixing between the two types of cations during the milling. The resulting precursor powder undergoes a self-controlled reconstructive thermal decomposition at 500°C and yields Cr/Cr stabilized c-ZrO nanoparticles. Average D ∼ 18 nm crystallite size is estimated from x-ray diffraction peak-widths in sample stabilized by 5 mol% Cr/Cr in 20 hr of milling. The D value decreases from 18 to 15 nm by extending the milling time to 50 hr. The stabilized nanoparticles are found to exist in the c-phase up to a temperature as high as 1000°C. The results are analyzed and discussed in terms of x-ray diffraction, thermal analysis, scanning electron microscopy microstructure, and x-ray photoelectron and optical spectra.

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