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Synthetic method of superhigh temperature resistant zirconium carbide ceramic precursor

A technology of ceramic precursors and synthesis methods, applied in carbon compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of toxicity of raw materials, poor compatibility between materials, poor stability, etc., and achieves low solvent toxicity and improved products. Performance, effect of low synthesis temperature

Inactive Publication Date: 2014-03-12
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to provide a method for synthesizing an ultra-high temperature resistant zirconium carbide ceramic precursor, which solves the problems of toxic raw materials, poor stability and poor compatibility between materials when synthesizing ZrC ceramic precursors

Method used

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  • Synthetic method of superhigh temperature resistant zirconium carbide ceramic precursor
  • Synthetic method of superhigh temperature resistant zirconium carbide ceramic precursor

Examples

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Effect test

Embodiment 1

[0017] Example 1: 6.44 g of zirconium oxychloride was dissolved in 50 mL of anhydrous methanol, stirred at room temperature to dissolve, then cooled in an ice bath, 2.48 g of salicyl alcohol was added dropwise, and finally 4.24 g of triethylamine was added dropwise at a rate of 1 Drops / second, magnetic stirring is performed during the dropping process. After the dropwise addition, the ice bath was removed, and the reaction was carried out at room temperature for 4 h. The solvent was evaporated by rotary evaporation for 10 min, 50 mL of tetrahydrofuran was added, stirred at room temperature for 2 h, filtered with suction, and the precipitate of triethylamine hydrochloride was filtered off. The solvent was evaporated from the filtrate by rotary evaporation for 15 min, and 100 mL of n-hexane was added, stirred at room temperature for 12-48 h, filtered to obtain a light yellow precipitate, and vacuum-dried at 50 °C for 3 h to obtain the zirconium carbide precursor. The precursor ...

Embodiment 2

[0019] Example 2: 6.44 g of zirconium oxychloride was dissolved in 50 mL of anhydrous methanol, stirred at room temperature to dissolve, then cooled in an ice bath, 3.47 g of salicyl alcohol was added dropwise, and finally 4.24 g of triethylamine was added dropwise at a rate of 1 Drops / second, magnetic stirring is performed during the dropping process. After the dropwise addition, the ice bath was removed, and the reaction was carried out at room temperature for 4 h. Rotary steam for 10 min to remove the solvent, add 50 mL of tetrahydrofuran, stir at room temperature for 2 h, and filter with suction to remove the precipitate of triethylamine hydrochloride. The solvent was evaporated from the filtrate by rotary evaporation for 15 min, and 100 mL of n-hexane was added, stirred at room temperature for 12-48 h, filtered to obtain a light yellow precipitate, and vacuum-dried at 50 °C for 3 h to obtain the zirconium carbide precursor. The precursor is easily soluble in organic solv...

Embodiment 3

[0020] Example 3: 6.44 g of zirconium oxychloride was dissolved in 50 mL of anhydrous methanol, stirred at room temperature to dissolve, then cooled in an ice bath, 3.22 g of salicyl alcohol was added dropwise, and finally 4.24 g of triethylamine was added dropwise at a rate of 1 Drops / second, magnetic stirring is performed during the dropping process. After the dropwise addition, the ice bath was removed, and the reaction was carried out at room temperature for 4 h. Rotary steam for 10 min to remove the solvent, add 50 mL of tetrahydrofuran, stir at room temperature for 2 h, and filter with suction to remove the precipitate of triethylamine hydrochloride. The solvent was evaporated from the filtrate by rotary evaporation for 15 min, and 100 mL of n-hexane was added, stirred at room temperature for 12-48 h, filtered to obtain a light yellow precipitate, and vacuum-dried at 50 °C for 3 h to obtain the zirconium carbide precursor. The precursor is easily soluble in organic solv...

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Abstract

A synthetic method of a superhigh temperature resistant zirconium carbide ceramic precursor belongs to preparation methods of ceramic precursors. The synthetic method includes firstly, dissolving 6.44g zirconium oxychloride in 50 mL absolute methanol, stirring the mixture at a room temperature for dissolving, subjecting the mixture to ice bath for cooling, dropwise adding 2.4g-3.47g saligenin, finally dropwise adding 4.24g triethylamine at a dropping speed of 1 droplet per second, and subjecting the mixture to magnetic stirring in the process of the dropping adding; after the dropping adding, removing the ice bath and stirring the mixture at a room temperature for 4 hours; then subjecting the mixture to rotary evaporation for 10 minutes to evaporate solvents, adding 50 mL tetrahydrofuran, stirring the mixture at a room temperature for 2 hours, and performing suction filtration to remove a precipitation of triethylamine hydrochloride; subjecting the mixture to rotary evaporation for 15 minutes to evaporate the solvents of colatuie, adding 100 mL hexyl hydride, stirring the mixture at a room temperature for 12-48 hours, performing filtration to obtain a pale yellow precipitation, and subjecting the pale yellow precipitation to vacuum drying for three hours to obtain the zirconium carbide ceramic precursor. The synthetic method of the superhigh temperature resistant zirconium carbide ceramic precursor has the advantages that the even dispersing of modular zirconium components in precursor reins is achieved, the solidification group saligenin are contained in the ceramic precursor so that crosslinking solidification is facilitated, the synthesis temperature is low, the reaction speed is rapid, and the toxicity of solvents is small.

Description

technical field [0001] The invention relates to a preparation method of a ceramic precursor, in particular to a synthesis method of an ultra-high temperature resistant zirconium carbide ceramic precursor. Background technique [0002] At present, the preparation of ZrC mostly adopts solid-phase method and gas-phase method, mainly including the reduction synthesis method of oxide and carbon reaction, the chemical method of metal and carbon reaction, and the vapor phase deposition method. The main method for industrialized preparation of ZrC is to reduce metal oxide powder with solid carbon, the reaction temperature is 1900-2300°C, and the prepared ZrC powder has a relatively large size. The precursor conversion method is a newly developed new process and new technology for preparing ceramics and ceramic matrix composites. Compared with traditional ceramic preparation methods, the main characteristics of the preparation of ceramic materials by the precursor method are: ①The ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B31/30C04B35/56C01B32/914
Inventor 陶雪钰邱文丰赵彤陈龙阁刘帆
Owner CHINA UNIV OF MINING & TECH
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