Hydrothermal Crystallization of Niobium Oxide Nanorods Studied by 93Nb Nuclear Magnetic Resonance

doi:10.11938/cjmr20233061

Abstract

Abstract:

The crystallization process of hydrothermally synthesizing niobium oxide nanorods with ammonium niobium oxalate precursor was investigated using ⁹³Nb NMR, combined with X-ray powder diffraction, transmission electron microscopy and quantum chemistry calculations. The results showed that the hydrothermal crystallization of ammonium niobium oxalate underwent a hydrolysis-polymerization reaction, starting with the hydrolysis of ammonium niobium oxalate, followed by the polymerization of the niobium-oxide monomers by condensation, resulting in dimers, trimers and multimers, and finally generating solid niobium oxide nanorods with disordered intra-layer and ordered inter-layer structures. The mechanism of crystallization process is “liquid phase nucleation”, with the layer-structured niobium oxide nanorods being produced within 1 h at 180 ℃. The subsequent hydrothermal treatment does not lead to significant growth of the nanorods, and new solid products are continuously generated independently from the solution.

Key words: ⁹³Nb NMR, nano niobium oxide, ammonium niobium oxalate, hydrothermal, crystallization mechanism

CLC Number:

O482.53

SHEN Changzhi, ZHANG Linlin, LI Xin, SHEN Wanling. Hydrothermal Crystallization of Niobium Oxide Nanorods Studied by ⁹³Nb Nuclear Magnetic Resonance[J]. Chinese Journal of Magnetic Resonance, 2023, 40(4): 376-384.

Figures/Tables 4

References 47

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Hydrothermal Crystallization of Niobium Oxide Nanorods Studied by ⁹³Nb Nuclear Magnetic Resonance

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