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. This journal is
Originalsprog | Engelsk |
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Tidsskrift | Nanoscale |
Vol/bind | 13 |
Udgave nummer | 17 |
Sider (fra-til) | 8087-8097 |
Antal sider | 11 |
ISSN | 2040-3364 |
DOI | |
Status | Udgivet - 7 maj 2021 |
Bibliografisk note
Funding Information:Kirsten M. Ø. Jensen is an associ- ate professor at Department of Chemistry at University of Copenhagen. She received her Ph.D. in Chemistry from Aarhus University in 2013. Following a postdoc position at Columbia University, she started her research group in Copenhagen in 2015. Her group’s work is sup- ported by the European Research Council (ERC Starting Grant, 2017) and the Villum Foundation (Villum Young Investigator Award, 2016), and in 2019 she received the L’Oreal-UNESCO International Rising Talent Award. The research in her group concerns nanomaterials, focusing especially on the use of X-ray and neutron scattering to elucidate the structure and formation mechanisms of nanoparticles. Her group are in particular frequent users of large scale synchrotron facilities for in situ studies of chemical reactions, and works in both nanoparticle synthesis and development of data analysis methods for Pair Distribution Function studies.
Funding Information:
We are grateful to the Villum Foundation for financial support through a Villum Young Investigator grant (VKR00015416). This work is part of a project that has received funding from the European Research Council (ERC) under the European Union’s Horizon 2020 research and innovation programme, (Grant agreement No. 804066). We acknowledge the Carlsberg Foundation for financial support through grants CF14-0652 and CF17-0976. Funding from the Danish Ministry of Higher Education and Science through the SMART Lighthouse is gratefully acknowledged. We thank DANSCATT (supported by the Danish Agency for Science and Higher Education) for support. We acknowledge DESY (Hamburg, Germany), a member of the Helmholtz Association HGF, for the provision of experimental facilities. Parts of this research were carried out at P02.1 and we would like to thank Martin Etter for assist- ance in using the beamline. This work was performed in part at DTU Nanolab, the National Centre for Nano Fabrication and Characterization at the Technical University of Denmark.
Publisher Copyright:
© The Royal Society of Chemistry.