TY - JOUR

T1 - Formation and growth mechanism for niobium oxide nanoparticles

T2 - Atomistic insight from: In situ X-ray total scattering

AU - Aalling-Frederiksen, Olivia

AU - Juelsholt, Mikkel

AU - Anker, Andy S.

AU - Jensen, Kirsten M.Ø.

N1 - Publisher Copyright: © The Royal Society of Chemistry.

PY - 2021/5/7

Y1 - 2021/5/7

N2 - 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. This journal is

AB - 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. This journal is

U2 - 10.1039/d0nr08299f

DO - 10.1039/d0nr08299f

M3 - Journal article

C2 - 33956920

AN - SCOPUS:85105408964

VL - 13

SP - 8087

EP - 8097

JO - Nanoscale

JF - Nanoscale

SN - 2040-3364

IS - 17

ER -