Mechanism of synthesizing hexaniobate cluster by microwave-assisted hydrothermal reaction

IF 5.3 2区化学 Q1 CHEMISTRY, APPLIED

Catalysis Today Pub Date : 2025-10-07 DOI:10.1016/j.cattod.2025.115593

Nattamon Panichakul , Hiroki Nagakari , Soichi Kikkawa , Shuntaro Tsubaki , Kotaro Higashi , Tomoya Uruga , Hideyuki Kawasoko , Seiji Yamazoe

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引用次数: 0

Abstract

Anionic hexaniobate clusters [Nb₆O₁₉]^8 −, which act as a superbase catalyst, could be synthesized by the microwave-assisted hydrothermal method at 180℃ within 10 min with high purity, whereas the conventional hydrothermal synthesis method requires a long reaction time (>24 h). In this study, the mechanism of synthesizing [Nb₆O₁₉]⁸⁻ by the microwave-assisted hydrothermal method was investigated by in situ quick-scan X-ray absorption fine structure and electrospray ionization time-of-flight mass spectroscopy. This revealed rapid [Nb₆O₁₉]⁸⁻ nucleation along with dissolution of Nb₂O₅∙nH₂O accompanied by the formation of mononuclear Nb species at 160℃. The unveiled mechanistic insights provide the controllability in products during microwave-assisted hydrothermal synthesis of polyoxoniobate clusters.

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微波辅助水热反应合成己酸酯簇的机理

作为超碱催化剂的阴离子型己酸盐簇[Nb6O19]8 −通过微波辅助水热合成法在180℃下仅需10 min即可合成出高纯度的[Nb6O19]，而传统的水热合成法需要较长的反应时间（>24 h）。本研究采用原位快速扫描x射线吸收精细结构和电喷雾电离飞行时间质谱对微波辅助水热法合成[Nb6O19]8−的机理进行了研究。结果表明，在160℃下，[Nb6O19]快速成核，Nb2O5∙nH2O溶解，同时形成单核Nb。揭示的机理见解提供了微波辅助水热合成多氧氧酸盐簇过程中产品的可控性。

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来源期刊

Catalysis Today 化学-工程：化工

CiteScore

11.50

自引率

3.80%

发文量

573

审稿时长

2.9 months

期刊介绍： Catalysis Today focuses on the rapid publication of original invited papers devoted to currently important topics in catalysis and related subjects. The journal only publishes special issues (Proposing a Catalysis Today Special Issue), each of which is supervised by Guest Editors who recruit individual papers and oversee the peer review process. Catalysis Today offers researchers in the field of catalysis in-depth overviews of topical issues. Both fundamental and applied aspects of catalysis are covered. Subjects such as catalysis of immobilized organometallic and biocatalytic systems are welcome. Subjects related to catalysis such as experimental techniques, adsorption, process technology, synthesis, in situ characterization, computational, theoretical modeling, imaging and others are included if there is a clear relationship to catalysis.