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In situ total scattering experiments of nucleation and crystallisation of tantalum-based oxides: from highly dilute solutions via cluster formation to nanoparticles

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Onur Şahin,  Ezgi
Research Group Weidenthaler, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Tüysüz,  Harun
Research Group Tüysüz, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Chan,  Candace K.
Research Group Tüysüz, Max-Planck-Institut für Kohlenforschung, Max Planck Society;
Materials Science and Engineering, School for Engineering of Matter, Transport and Energy (SEMTE), Arizona State University;

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Moon,  Gun-Hee
Research Group Tüysüz, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Dai,  Yitao
Research Group Tüysüz, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Schmidt,  Wolfgang
Research Group Schmidt, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Lim,  Joohyun
Nanoanalytics and Interfaces, Independent Max Planck Research Groups, Max-Planck-Institut für Eisenforschung GmbH, Max Planck Society;

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Scheu,  Christina
Nanoanalytics and Interfaces, Independent Max Planck Research Groups, Max-Planck-Institut für Eisenforschung GmbH, Max Planck Society;

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Weidenthaler,  Claudia
Research Group Weidenthaler, Max-Planck-Institut für Kohlenforschung, Max Planck Society;

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Citation

Onur Şahin, E., Tüysüz, H., Chan, C. K., Moon, G.-H., Dai, Y., Schmidt, W., et al. (2021). In situ total scattering experiments of nucleation and crystallisation of tantalum-based oxides: from highly dilute solutions via cluster formation to nanoparticles. Nanoscale, 13(1), 150-162. doi:10.1039/D0NR07871A.


Cite as: http://hdl.handle.net/21.11116/0000-0007-AB1C-A
Abstract
The exact formation mechanism of tantalum oxides (and in general, metal/mixed metal oxides) from alkoxide precursors is still not fully understood, particularly when forming cluster-like or amorphous materials. The structural evolution of Ta-based oxides was studied in detail using X-ray total scattering experiments along with subsequent pair distribution function (PDF) analyses. Starting from a tantalum alkoxide precursor (Ta2(OEt)10), the formation of hydrolysed TaxOyHz clusters in highly diluted aqueous solution was analysed. From the PDF data, the connectivity and arrangement of TaxOy octahedra in the cluster could be deduced as well as the approximate size of the clusters (<1 nm). Construction of cluster models allowed for identification of common structural motifs in the TaxOyHz clusters, ruling out the formation of chain- or ring-like clusters. More likely, bulky clusters with a high number of corner-sharing octahedra are formed. After separation of the amorphous solid from the liquid, temperature-induced crystallisation processes were monitored via in situ total scattering experiments. Between room temperature and 600 °C, only small rearrangements of the amorphous structure are observed. At about 610 °C, amorphous TaxOyHz transforms directly into crystalline orthorhombic L-Ta2O5 without formation of any crystalline intermediate structures.