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Issue 17, 2021

Formation and growth mechanism for niobium oxide nanoparticles: atomistic insight from in situ X-ray total scattering

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Abstract

Understanding the mechanisms for nanoparticle nucleation and growth is crucial for the development of tailormade nanomaterials. Here, we use X-ray total scattering and Pair Distribution Function analysis to follow the formation and growth of niobium oxide nanoparticles. We study the solvothermal synthesis from niobium chloride in benzyl alcohol, and through investigations of the influence of reaction temperature, a formation pathway can be suggested. Upon dissolution of niobium chloride in benzyl alcohol, octahedral [NbCl6−xOx] complexes form through exchange of chloride ligands. Heating of the solution results in polymerization, where larger clusters built from multiple edge-sharing [NbCl6−xOx] octahedra assemble. This leads to the formation of a nucleation cluster with the ReO3 type structure, which grows to form nanoparticles of the Wadsley–Roth type H-Nb2O5 structure, which in the bulk phase usually only forms at high temperature. Upon further growth, structural defects appear, and the presence of shear-planes in the structure appears highly dependent on nanoparticle size.

Graphical abstract: Formation and growth mechanism for niobium oxide nanoparticles: atomistic insight from in situ X-ray total scattering

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Article information


Submitted
20 Nov 2020
Accepted
14 Mar 2021
First published
15 Mar 2021

This article is Open Access

Nanoscale, 2021,13, 8087-8097
Article type
Paper

Formation and growth mechanism for niobium oxide nanoparticles: atomistic insight from in situ X-ray total scattering

O. Aalling-Frederiksen, M. Juelsholt, A. S. Anker and K. M. Ø. Jensen, Nanoscale, 2021, 13, 8087 DOI: 10.1039/D0NR08299F

This article is licensed under a Creative Commons Attribution 3.0 Unported Licence. You can use material from this article in other publications without requesting further permissions from the RSC, provided that the correct acknowledgement is given.

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