Issue 28, 2017

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, the crystalline phase and the elemental composition of the solid is presented. Mixed metal oxide zirconium–titanium-oxo-alkoxy (ZTOA) nanoparticles of different elemental compositions 0 ≤ x = CZr/(CZr + CTi) ≤ 1 were prepared via the sol–gel method in a reactor by rapid micromixing of n-propanol fluids containing the precursors and water. The structural transformation of the nanoparticles takes place in two temperature 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 crystallisation 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 particle 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 particle radius decreased to 1.8 nm for 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.

Graphical abstract: From nanoparticles to bulk crystalline solid: nucleation, growth kinetics and crystallisation of mixed oxide ZrxTi1−xO2 nanoparticles

Article information

Article type
Paper
Submitted
15 Mar 2017
Accepted
12 Jun 2017
First published
12 Jun 2017

CrystEngComm, 2017,19, 3955-3965

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, 19, 3955 DOI: 10.1039/C7CE00505A

To request permission to reproduce material from this article, please go to the Copyright Clearance Center request page.

If you are an author contributing to an RSC publication, you do not need to request permission provided correct acknowledgement is given.

If you are the author of this article, you do not need to request permission to reproduce figures and diagrams provided correct acknowledgement is given. If you want to reproduce the whole article in a third-party publication (excluding your thesis/dissertation for which permission is not required) please go to the Copyright Clearance Center request page.

Read more about how to correctly acknowledge RSC content.

Social activity

Spotlight

Advertisements