Method for preparing aluminium titanate film by non-hydrolytic sol-gel process

A technology of aluminum titanate and sol, which is applied in chemical instruments and methods, titanium compounds, inorganic chemistry, etc., can solve the problems of demand and high equipment cost, and achieve the effects of simple process, low synthesis temperature, and shortened preparation cycle

Inactive Publication Date: 2008-10-01
JINGDEZHEN CERAMIC INSTITUTE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Thin Solid Films 2005, Volume 487, pages 109-115, reported that using aluminum sec-butoxide and titanium tetrachloride as raw materials, using chemical vapor deposition, using a vertical cold-wall CVD reactor, and strictl

Method used

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  • Method for preparing aluminium titanate film by non-hydrolytic sol-gel process

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Prepare aluminum titanate sol according to the molar ratio of aluminum to titanium of 2:1, weigh 2.667g of anhydrous aluminum trichloride (analytical pure) and dissolve in 3.4ml tetrabutyl titanate (analytical pure), then add 0.037g KI (analytical pure) ) heated and stirred to AlCl 3 After completely dissolving with KI, reflux at 110°C for 0.5h to obtain a black-brown precursor mixture; add 0.050g of tetrabutylammonium bromide (analytical pure) to 50.0ml of AGSE (industrial pure), heat and stir until completely dissolved to obtain tetrabutylammonium bromide AGSE solution of butyl ammonium bromide, sealed for use; measure 50.0ml of AGSE and add it to the refluxed precursor mixture, stir evenly, and then slowly add the prepared tetrabutylammonium bromide-AGSE solution to it to obtain bright yellow For transparent aluminum titanate sol, add 5.0ml diethyl phthalate as a drying control additive, stir at room temperature for 1 hour, and age at 110°C for 24 hours to obtain lig...

Embodiment 2

[0028] Prepare aluminum titanate sol according to the molar ratio of aluminum to titanium of 2:1, weigh 4.005g of anhydrous aluminum trichloride (analytical pure) and dissolve in 5.1ml tetrabutyl titanate (analytical pure), then add 0.067g NaI (analytical pure) ) heated and stirred to AlCl3 After completely dissolving with NaI, reflux at 110°C for 24 hours to obtain a dark brown precursor mixed solution; add 0.300g tetrabutylammonium bromide (analytical pure) to 50.0ml AGSE (industrial pure), heat and stir until completely dissolved to obtain tetrabutylammonium bromide The AGSE solution of butylammonium bromide, sealed for use; then measure 50.0ml of AGSE and add it to the precursor mixture that has been refluxed, stir evenly, and then slowly add the prepared AGSE solution of tetrabutylammonium bromide to obtain orange Red transparent aluminum titanate sol, then add 5.0ml diethyl phthalate as a drying control additive, stir at room temperature for 1h, and age at 110°C for 12h t...

Embodiment 3

[0030] Prepare aluminum titanate sol according to the molar ratio of aluminum to titanium of 2:1, weigh 5.336g of anhydrous aluminum trichloride (analytical pure) and dissolve in 6.8ml tetrabutyl titanate (analytical pure), then add 0.084gMgI 2 (analytical pure) heated and stirred to AlCl 3 and MgI 2 After completely dissolving, reflux at 110°C for 12 hours to obtain a dark brown precursor mixture; add 0.300g tetrabutylammonium bromide (analytical pure) to 50.0ml AGSE (industrial pure), heat and stir until completely dissolved to obtain tetrabutylammonium bromide The AGSE solution of ammonium bromide, sealed for use, then measure 50.0ml of AGSE and add it to the refluxed precursor mixture, stir evenly, and then slowly add the prepared AGSE solution of tetrabutylammonium bromide to it to obtain orange-red transparent Aluminum titanate sol, then add 5.0ml dimethyl phthalate as a drying control additive, stir at room temperature for 1h, and age at 110°C for 12h to obtain dark re...

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Abstract

The invention discloses a method for preparing an aluminum titanate film by a non-hydrolytic sol-gel technique. Anhydrous aluminum chloride and titanium tetrachloride are taken as precursors and low-carbon alcohol is taken as an oxygen donor; or the anhydrous aluminum chloride and titanium alkoxide are taken as the precursors and precursor mixing liquid is prepared according to the stoichiometry of aluminum titanate; a catalyzer is added into the precursor mixing liquid for backflow at 110 DEG C for 0.5h to 24h; then a solvent AGSE and a quaternary ammonium salt AGSE solution are added into the precursor mixing liquid to prepare aluminum titanate sol; a drying control chemical additive is added to prepare aluminum titanate filming sol after aging; the aluminum titanate filming sol is then filmed and dried to prepare an aluminum titanate dried gel film; filming can be carried out for a plurality of times till required film thickness is obtained and finally heat treatment at 750 DEG C is carried out to obtain the even and compact aluminum titanate film. The method has the advantages of low synthesizing temperature, simple technique, low cost of raw materials, etc. of the aluminum titanate film.

Description

technical field [0001] The invention belongs to the technical field of inorganic thin film preparation, and in particular relates to a method for preparing an aluminum titanate thin film by a non-hydrolytic sol-gel process. Background technique [0002] Aluminum titanate (Al 2 TiO 5 , referred to as AT) not only has a high melting point (1860 ° C) and low expansion (α<1.5×10 -6 / ℃), but also has the characteristics of low thermal conductivity (1.5W / m·K), good thermal shock resistance and strong corrosion resistance. Aluminum titanate films have broad application prospects in many fields, such as: (1) as a high-temperature anti-corrosion and anti-oxidation protective coating to prevent Si 3 N 4 High-temperature oxidation and hot salt corrosion of ceramic materials such as SiC; (2) In the metallurgical industry, aluminum titanate films can be used as protective coatings for continuous steel casting molds, protection against molten steel erosion and blast furnace slag er...

Claims

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Application Information

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IPC IPC(8): C01G23/00C04B41/50
Inventor 江伟辉冯果魏恒勇彭永烽谭训彦包镇红
Owner JINGDEZHEN CERAMIC INSTITUTE
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