Hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres

A technology of hydrothermal synthesis and zirconium tungstate, applied in the field of ceramic materials, can solve the problems of particle shape influence, high density, difficult shape control, etc., and achieve the effect of uniform particle size and good negative expansion performance.

Active Publication Date: 2015-04-08
SHANGHAI JIAO TONG UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the powder particles obtained by this process are large and dense, and the hydrothermal synthesis reaction time has a significant impact on the particle shape, making it difficult to control the shape

Method used

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  • Hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Press ZrW 2 o 8 The stoichiometric ratio of zirconium oxychloride (ZrOCl 2 ) and ammonium metatungstate ((NH 4 ) 6 W 12 o 39 ), and were dissolved in water respectively to form solution a (zirconium oxychloride aqueous solution) and solution b (ammonium metatungstate aqueous solution). Under the premise of constant stirring of solution b, solution a was added to solution b to make it fully mixed After obtaining the mixed solution c, keep stirring and heating at 60°C for 2h; add 6mol / l hydrochloric acid to the mixed solution c to adjust the pH to 0.2, keep stirring and heat up to 90°C for 3h to obtain a homogeneous precursor suspension. The precursor suspension was transferred into a hydrothermal reaction kettle and heated at 180 °C for 5 h. After cooling, the supernatant was poured out, and the resulting precipitate was washed with deionized water to remove excess Cl - . After drying the precipitate, move it into a horse boiling furnace and calcinate at 900°C fo...

Embodiment 2

[0019] Press ZrW 2 o 8 The stoichiometric ratio of zirconium oxychloride (ZrOCl 2 ) and ammonium metatungstate ((NH 4 ) 6 W 12 o 39 ), and were dissolved in water respectively to form solution a (zirconium oxychloride aqueous solution) and solution b (ammonium metatungstate aqueous solution). Under the premise of constant stirring of solution b, solution a was added to solution b to make it fully mixed After obtaining the mixed solution c, keep stirring and heating at 65°C for 2h; add 6mol / l hydrochloric acid to the mixed solution c to adjust the pH to 0.2, keep stirring and heat up to 90°C for 3h to obtain a homogeneous precursor suspension. The precursor suspension was transferred into a hydrothermal reaction kettle and heated at 180 °C for 5 h. After cooling, the supernatant was poured out, and the resulting precipitate was washed with deionized water to remove excess Cl - . After drying the precipitate, move it into a horse boiling furnace and calcinate at 900°C fo...

Embodiment 3

[0021] Press ZrW 2 o 8 The stoichiometric ratio of zirconium oxychloride (ZrOCl 2 ) and ammonium metatungstate ((NH 4 ) 6 W 12 o 39 ), and were dissolved in water respectively to form solution a (zirconium oxychloride aqueous solution) and solution b (ammonium metatungstate aqueous solution). Under the premise of constant stirring of solution b, solution a was added to solution b to make it fully mixed After obtaining the mixed solution c, keep stirring and heating at 70°C for 2h; add 6mol / l hydrochloric acid to the mixed solution c to adjust the pH to 0.2, keep stirring and heat up to 90°C for 3h to obtain a homogeneous precursor suspension. The precursor suspension was transferred into a hydrothermal reaction kettle and heated at 180 °C for 5 h. After cooling, the supernatant was poured out, and the resulting precipitate was washed with deionized water to remove excess Cl - . After the precipitate is dried, it is transferred into a horse boiling furnace and calcined ...

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Abstract

The invention discloses a hydrothermal synthesis method of nano-scale zirconium tungstate hollow spheres, wherein the hydrothermal synthesis method comprises the following steps: according to the stoichiometric ratio of ZrW2O8, respectively weighing zirconium oxychloride and ammonium metatungstate, and respectively preparing a zirconium oxychloride aqueous solution and an ammonium metatungstate aqueous solution; adding the zirconium oxychloride aqueous solution while stirring the ammonium metatungstate aqueous solution, stirring and preheating at the temperature of 60-70 DEG C, then adding a hydrochloric acid solution, stirring and heating at the temperature of 80-100 DEG C, and thus obtaining a zirconium tungstate precursor suspension liquid; and carrying out a hydrothermal reaction on the zirconium tungstate precursor suspension liquid at the temperature of 170-190 DEG C, then cooling, collecting a precipitate, washing to remove Cl<->, drying the precipitate, calcining at the temperature of 800-1000 DEG C, and thus obtaining the product. The negative-thermal-expansion zirconium tungstate nano hollow spheres are prepared at the low temperature by adopting the hydrothermal synthesis reaction, nano-scale regular particles are obtained, the density of zirconium tungstate is reduced, and the nano-scale zirconium tungstate hollow spheres have a great application potential in the field of aeronautics and astronautics.

Description

technical field [0001] The invention relates to a process for preparing nano zirconium tungstate, in particular to a hydrothermal synthesis method of nano zirconium tungstate hollow spheres, belonging to the field of ceramic materials. Background technique [0002] In recent years, the thermal expansion characteristics of materials have become one of the issues of general concern in the material field. Research and development of zero-expansion or low-expansion materials can significantly improve the thermal geometric stability and impact resistance of materials. Cubic phase zirconium tungstate is one of the hot spots in the research of negative thermal expansion materials. Its negative expansion effect has the widest temperature range, high negative expansion coefficient and isotropy. These excellent properties have laid the foundation for the application of zirconium tungstate. It can be combined with positive expansion materials to form zero-expansion or low-expansion mat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G41/00B82Y30/00
CPCB82Y30/00C01G41/00C01P2004/32C01P2004/64
Inventor 吴一张琳达王浩伟刘预彭思平
Owner SHANGHAI JIAO TONG UNIV
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