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From nanoparticles to bulk crystalline solid: Nucleation, growth kinetics and crystallisation of mixed oxide ZrxTi1-xO2 nanoparticles

Abstract

We describe the preparation of mixed metal oxide nanoparticles of a desirable composition and their transformation to the crystalline solids ZrxTi1-xO2 (0.0≤x≤1.0) after heat treatment. The correlation analysis between the size of the nucleus, crystalline phase and elemental composition of the solid is presented. Mixed metal oxide zirconium-titanium-oxo-alkoxy (ZTOA) nanopaticles of different elemental compositions 0≤x=CZr/(CZr+CTi)≤1 were prepared via sol-gel method in a reactor with rapid micromixing of n-propanol fluids containing the precursors and water. The structural transformation of the nanoparticles takes place in two temperatures ranges: 210-250 °C and 380-680 °C, which sensitively depends on the elemental composition. In the range 0.3≤x≤0.6, stable ZTOA nanoparticles with a radius of 2.1±0.05 nm appeared at the hydrolysis ratio H≤1.5. The heat treatment results in a single orthorhombic ZrxTi1-xO2 phase. The crystallization onset temperature was the highest in this range of x attaining 680 °C at x=0.5. In the range 0≤x≤0.2, the particles radius decreased to 1.6 nm for pure titanium-oxo-alkoxy nuclei (TOA, x=0); their heat treatment resulted in a single TiO2 anatase phase. In the range 0.7≤x≤1, the particles radius decreased to 1.8 nm of pure zirconium-oxo-alkoxy nuclei (ZOA, x=1); their heat treatment resulted in mixed monoclinic and tetragonal ZrO2 phases. The crystalline cell parameters of the observed phases underwent a continuous variation with x. TEM images evidenced the nanoporous structure of submicronic orthorhombic ZrxTi1-xO2 monocrystals with a mean pore size of about that of the ZTOA nanoparticles.

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Publication details

The article was received on 15 Mar 2017, accepted on 12 Jun 2017 and first published on 12 Jun 2017


Article type: Paper
DOI: 10.1039/C7CE00505A
Citation: CrystEngComm, 2017, Accepted Manuscript
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    From nanoparticles to bulk crystalline solid: Nucleation, growth kinetics and crystallisation of mixed oxide ZrxTi1-xO2 nanoparticles

    K. Cheng, K. Chhor, O. Brinza, D. Vrel and A. Kanaev , CrystEngComm, 2017, Accepted Manuscript , DOI: 10.1039/C7CE00505A

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