掺钒六方铷钨青铜的合成与表征

H. Simol, Istiak Hossain, T. Debnath, P. K. Bakshi, R. A. Jahan, Claus H Ruscher, Altaf Hussain
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摘要

我们尝试合成了掺钒铷六方钨青铜,其标称成分为 RbxVyW1-yO3(x = 0.30、0.25 和 0.0 ≤ y ≤ x)。样品是在 700°C 的真空(10-2 托)条件下,在硅玻璃管中用固态合成法合成的。X 射线衍射测量结果表明,只要用 V5+ 替代 60% 的 W5+,就能形成纯六方钨青铜(HTB)相。X 射线衍射数据的里特维尔德结构细化也揭示了钒在 HTB 晶格中的系统性结合,以及 V/W-O 键在 xy 平面上长度的减少和这些键在晶体学 c 方向上长度的延长。氧化相的傅立叶变换红外吸收光谱支持 XRD 结果。此外,随着 W5+ 最终被 V5+ 取代,吸收特征随 y 的变化而发展,强度显著增加,这表明类似金属的贡献大大降低,并揭示了化合物的非金属性质。元素分析表明与标称值十分吻合,表明钒被系统地掺入到 RbxVyW1-yO3 体系中:77-84, 2024 (January)
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Synthesis and Characterization of Vanadium Doped Hexagonal Rubidium Tungsten Bronze
Attempts have been made to synthesize vanadium doped rubidium hexagonal tungsten bronzes with the nominal composition RbxVyW1-yO3 (x = 0.30, 0.25, and 0.0 ≤ y ≤ x). The samples were synthesized using the solid state synthesis method in a silica glass tube under vacuum at (10-2 Torr) 700°C. The X-ray diffraction measurements reveal that a pure hexagonal tungsten bronze (HTB) phase can be formed with a 60% replacement of W5+ by V5+. The systematic incorporation of vanadium into the HTB lattice, as well as the reduction of V/W-O bond lengths in the xy plane and the lengthening of these bonds in the crystallographic c direction, are also revealed by Rietveld structure refinement of XRD data. The XRD results are supported by FTIR absorption spectra of the oxidized phases. Furthermore, an absorption signature develops as a function of y and exhibits a considerable increase in intensity with the eventual replacement of W5+ by V5+, showing a large decrease in the metallic like contribution and revealing the compounds' nonmetallic nature. Elemental analysis indicates good agreement with nominal values, demonstrating that vanadium was systematically incorporated into the RbxVyW1-yO3 system. Dhaka Univ. J. Sci. 72(1): 77-84, 2024 (January)
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