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

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 [NbCl_6-xO_x] complexes form through exchange of chloride ligands. Heating of the solution results in polymerization, where larger clusters built from multiple edge-sharing [NbCl_6-xO_x] 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.

SUBMITTER: Aalling-Frederiksen O

PROVIDER: S-EPMC8101635 | biostudies-literature | 2021 May

REPOSITORIES: biostudies-literature

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

Aalling-Frederiksen Olivia O Juelsholt Mikkel M Anker Andy S AS Jensen Kirsten M Ø KMØ

Nanoscale 20210323 17

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 benzy ...[more]

PMID: 33956920

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Project description:Interactions of nanoparticles (NPs) with their environment may have a pronounced effect on their structure and shape as well as on their functionality in applications such as catalysis. It is therefore crucial to disentangle the particle-adsorbate and particle-support interaction effects on the particle shape, its local structure, atomic dynamics, and its possible anisotropies. In order to gain insight into the support effect, we carried out an X-ray absorption fine-structure spectroscopy (XAFS) investigation of adsorbate- and ligand-free size-selected Pt NPs deposited on two different supports in ultrahigh vacuum. Polarization-dependent XAFS measurements, neural network-based analysis of X-ray absorption near-edge structure data, and reverse Monte Carlo (RMC) simulations of extended X-ray absorption fine structure (EXAFS) were used to resolve the 3D shape of the NPs and details of their local structure. A synergetic combination of advanced in situ XAFS analysis with atomic force microscopy and scanning tunneling microscopy (STM) imaging provides uniquely detailed information about the particle-support interactions and the NP/support buried interface, not accessible to any experimental technique, when considered alone. In particular, our combined approach reveals differences in the structure of Pt NPs deposited on TiO2(110) and SiO2/Si(111). Pt NPs on SiO2 assume a spherical-like 3D shape and weakly interact with the support. In contrast, the effective shape of analogously synthesized Pt NPs on TiO2(110) after annealing at 600 °C is found to be a truncated octahedron with (100) top and interfacial facets that are encapsulated by the TiO2 support. Modeling disorder effects in these NPs using an RMC approach reveals differences in bond-length distributions for NPs on different supports and allows us to analyze their anisotropy, which may be crucial for the interpretation of support-dependent atomic dynamics and can have an impact on the understanding of the catalytic properties of these NPs.

Dataset Information

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

Publications

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

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