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Thermal behavior of the composite xerogels of zirconium oxyhydroxide and silicic acid

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Abstract

Gels were prepared via sol–gel method by addition of zirconium oxychloride solution into sodium metasilicate (SZ) and sodium metasilicate solution into zirconium oxychloride (ZS) at varying final pH. Si/Zr molar ratio equaled 1/1. Synthesized gels were dried with calcium chloride until they reached a constant mass. SEM and nitrogen adsorption analysis have shown that SZ gels have surface area 175–200 mg−1, consist of 20–30 nm grains. ZS samples have surface area about 1 mg−1, consist of grains smaller than 10 nm. Thermal and X-ray phase analysis have shown that transition of amorphous ZrO2 to crystalline form shifts from 430 to 850–870 °C for SZ gels. Unlike zirconia gels phase transitions that proceed in order: “amorphous (430 °C)—tetragonal (800 °C)—monoclinic (1,000 °C) phases”, the monoclinic phase in ZS gels appears immediately after transition from amorphous to crystalline state; the tetragonal phase in SZ samples is stable until 1,000 °C.

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Acknowledgements

The study is carried out within the Federal Goal-oriented Programme “Scientific and scientific pedagogical personnel of innovative Russia” for 2009–2013, gov.contract. No. 16.740.11.0332.

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Correspondence to Viacheslav V. Avdin.

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Avdin, V.V., Krivtsov, I.V., Dyachuk, V.V. et al. Thermal behavior of the composite xerogels of zirconium oxyhydroxide and silicic acid. J Therm Anal Calorim 109, 1261–1265 (2012). https://doi.org/10.1007/s10973-012-2531-z

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