Low-Temperature Synthesis of Tungsten Silicates with Pyrochlore and Tungsten Bronze Structure

IF 0.6 4区材料科学 Q4 MATERIALS SCIENCE, CERAMICS

Glass and Ceramics Pub Date : 2024-11-11 DOI:10.1007/s10717-024-00708-8

Ya.A. Moroz, N. S. Lozinskii, A. N. Lopanov, K. A. Chebyshev, M. Yu. Zelenskii, E. A. Fanina

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Abstract

Polyoxotungstosilicates with the general formulas Cat₄[SiW₁₂O₄₀] · mH₂O and Cat₆[SiW₁₁O₃₉Ni(H₂O)] · nH₂O were synthesized, where Cat = Rb⁺, Cs⁺, (CH₃)₄N⁺. By means of IR spectroscopy and x-ray diffraction analysis, it was shown that the compounds have the Keggin anion structure. The thermolysis of the obtained compounds within the temperature range of 600 – 800°C resulted in the formation of previously unknown pyrochlore-structure phases Rb_12/13Si_2/13W_22/13Ni_2/13O₆ and Cs_12/13Si_2/13W_22/13Ni_2/13O₆ with the with the unit cell parameters a of 10.284 and 10.309 Å, as well as phases with tungsten bronze structure Rb_12/20Si_3/20W_36/20O₆ and Si_3/38W_36/38O₃. The synthesis of tungsten silicates with pyrochlore and tungsten bronze structure through thermolysis of polyoxotungstosilicates reduces the temperature of their preparation to 600 – 650°C and heating time to 1 h, thus extending the ranges of chemical compositions and their morphological diversity.

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具有火成岩和钨青铜结构的硅酸钨的低温合成

合成了通式为 Cat4[SiW12O40] - mH2O 和 Cat6[SiW11O39Ni(H2O)] - nH2O 的多氧钨硅酸盐，其中 Cat = Rb+、Cs+、(CH3)4N+。红外光谱和 X 射线衍射分析表明，这些化合物具有凯金阴离子结构。在 600 - 800°C 的温度范围内对获得的化合物进行热解，形成了之前未知的热绿石结构相 Rb12/13Si2/13W22/13Ni2/13O6 和 Cs12/13Si2/13W22/13Ni2/13O6 （单胞参数 a 为 10.284 和 10.309 Å），以及钨青铜结构相 Rb12/20Si3/20W36/20O6 和 Si3/38W36/38O3。通过热解多氧钨硅酸盐合成具有热绿体和钨青铜结构的硅酸钨，可将制备温度降低到 600 - 650°C，加热时间缩短到 1 小时，从而扩大了化学成分的范围及其形态的多样性。

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来源期刊

Glass and Ceramics 工程技术-材料科学：硅酸盐

CiteScore

1.00

自引率

16.70%

发文量

审稿时长

6-12 weeks

期刊介绍： Glass and Ceramics reports on advances in basic and applied research and plant production techniques in glass and ceramics. The journal''s broad coverage includes developments in the areas of silicate chemistry, mineralogy and metallurgy, crystal chemistry, solid state reactions, raw materials, phase equilibria, reaction kinetics, physicochemical analysis, physics of dielectrics, and refractories, among others.