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Stabilization of tetragonal zirconia nanocrystallites using an original supercritical-based synthesis route

DOI: 10.1021/acs.chemmater.0c01550 DOI Help

Authors: Aimery Auxemery (CNRS, Université de Bordeaux, Bordeaux INP, ICMCB) , Gilles Philippot (CNRS, Université de Bordeaux, Bordeaux INP, ICMCB) , Matthew R. Suchomel (CNRS, Université de Bordeaux, Bordeaux INP, ICMCB) , Denis Testemale (CNRS, Université Grenoble Alpes, Institut NEEL) , Cyril Aymonier (CNRS, Université de Bordeaux, Bordeaux INP, ICMCB)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemistry Of Materials

State: Published (Approved)
Published: September 2020
Diamond Proposal Number(s): 22774

Abstract: To understand the importance of the crystallite size on the stabilization of metastable tetragonal ZrO2, ultra-fine ZrO2 nanocrystallites were synthesized via: (i) the precipitation method in supercritical water using nitrate precursors, (ii) the sol-gel method in a supercritical ethanol-water mixture and (iii) the borderline non-hydrolytic sol-gel route in supercritical ethanol using propoxide precursors. The obtained nanocrystals displayed a variation of the monoclinic versus tetragonal molar frac-tions from 100 wt. % down to ≈ 10 wt. % of monoclinic. This variation was concomitant with an overall size decrease of the nanocrystals, ranging from 7 to 2 nm depending on the synthesis procedures. Phase contents were quantified by refinement analysis of X-ray scattering datasets, and crosschecked with Raman spectroscopy. Our results suggest that an upper limit of ≈ 90 wt. %, of tetragonal ZrO2 phase is possible, even for ultra-fine nanoparticles (2 nm). These findings thus question the exist-ence of any critical size limit below which stabilization of pure t-ZrO2 is attainable at low temperatures.

Subject Areas: Chemistry, Materials

Instruments: I15-1-X-ray Pair Distribution Function (XPDF)

Other Facilities: ESRF