Method for preparing zirconium silicate whisker by employing non-hydrolytic sol-gel technology combined with molten-salt growth method

A technology of zirconium silicate whisker and zirconium silicate, which is applied in the directions of self-gelling state, chemical instruments and methods, and self-melting solvent melt, etc., can solve the problem of high price, increase the difficulty of operation, and is not suitable for mass production Use and other problems to achieve the effect of low synthesis temperature, broad market space, cheap and easy-to-obtain raw materials

Active Publication Date: 2014-02-05
JINGDEZHEN CERAMIC INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method can prepare zirconium silicate whiskers, because the gas-phase catalyst used is anhydrous zirconium fluoride, etc., it is not only expensive, but also easily reacts with oxygen and water vapor in the air, so the zirconium silicate whiskers The heat treatment process must be carried out under the protection of inert gas, which increases the difficulty of operation, so it is not suitable for mass production

Method used

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  • Method for preparing zirconium silicate whisker by employing non-hydrolytic sol-gel technology combined with molten-salt growth method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] with anhydrous ZrCl 4 (industrial pure), Si(OC 2 h 5 ) 4 (chemically pure) is the reaction precursor, LiF (chemically pure) is the mineralizer, absolute ethanol (chemically pure) is the solvent, Na 2 MoO 4 (chemically pure) is a molten salt. First weigh 0.280 g LiF and put it in a dry Erlenmeyer flask, then add 8 ml Si(OC 2 h 5 ) 4 , 7.040 g ZrCl 4 , 30 ml of absolute ethanol, heated and magnetically stirred for 20 min to obtain a zirconium silicate precursor mixed solution; then put the mixed solution in an oil bath at 110 ℃ to condense and reflux for 24 h to obtain a transparent zirconium silicate sol; place the sol in Dry in an oven at 100 °C for 24 h to obtain zirconium silicate xerogel, then pre-fire it in an electric furnace at 400 °C and keep it warm for 30 min to obtain zirconium silicate xerogel powder; mix xerogel powder with Na 2 MoO 4 The mixture was ball-milled at a mass ratio of 1:4, placed in an alumina crucible, heat-treated at 900 °C and kept ...

Embodiment 2

[0025] With anhydrous Zr(OC 3 h 7 ) 4 (industrial pure), Si(OC 2 h 5 ) 4 (chemically pure) is the precursor, LiF (chemically pure) is the mineralizer, anhydrous n-butanol (chemically pure) is the solvent, and LiF (chemically pure) is the solvent. 2 MoO 4 for molten salt. The technological process and experimental conditions used to prepare zirconium silicate whiskers are the same as in Example 1, except that the amount of LiF used is 0.187 g, the amount of anhydrous n-butanol is 25 ml, the pre-calcination temperature is 300 ° C for 60 min, and the heat treatment temperature is 750 °C. ℃ for 3 h.

Embodiment 3

[0027] with anhydrous ZrCl 4 (industrial pure), Si(OC 2 h 5 ) 4 (chemically pure) is the precursor, LiCl (chemically pure) is the mineralizer, anhydrous dichloromethane (chemically pure) is the solvent, Na 2 MoO 4 for molten salt. The process flow and experimental conditions used to prepare zirconium silicate whiskers are the same as in Example 1, except that the amount of LiCl is 0.458 g, the mass ratio of dry gel powder to molten salt is 1:2, the pre-calcination temperature is 800 °C and the temperature is kept for 60 min. The temperature was kept at 1000 °C for 2 h.

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Abstract

The invention discloses a method for preparing a zirconium silicate whisker by employing a non-hydrolytic sol-gel technology combined with a molten-salt growth method. The method comprises the following steps: firstly, mixing an anhydrous silica source with a mineralizer; orderly adding an anhydrous zirconium source and a solvent; heating and evenly stirring, and then forming zirconium silicate sol by condensation and reflux; mixing and ball-milling zirconium silicate dry gel powder obtained by drying and pre-sintering the sol with fused salt; and finally preparing the zirconium silicate whisker by thermal treatment, washing and drying processes. The zirconium silicate whisker is prepared by adopting the non-hydrolytic sol-gel technology combined with the molten-salt growth method for the first time at home and abroad; the zirconium silicate whisker has outstanding advantages of being low in preparation temperature, simple in process, low in price, available in raw materials and the like. Therefore, the method disclosed by the invention has a broad application prospect.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a method for preparing zirconium silicate whiskers by combining a non-hydrolytic sol-gel process with a molten salt method. Background technique [0002] Whiskers refer to a fibrous single crystal material with a certain length-to-diameter ratio (generally greater than 10) and a highly ordered arrangement of atoms. It has a small diameter, few internal defects, and its strength is close to the theoretical value of a complete crystal. Because the whisker-reinforced composite material has the potential to achieve high strength, its research and development are highly valued by countries all over the world. Although there are hundreds of whisker experimental samples developed, the only whisker that has been industrialized is silicon carbide. , silicon nitride, aluminum oxide, titanium nitride, potassium titanate, aluminum borate, magnesium borate and mullite and a few varietie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/34C30B29/62C30B5/00C30B9/00
Inventor 江伟辉张涛刘健敏冯果陈婷张权吴倩苗立锋
Owner JINGDEZHEN CERAMIC INSTITUTE
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