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Method for preparing TiO2 film by utilizing sol-gelatin method

A gel method and sol technology, which is used in devices for coating liquids on surfaces, solid-state chemical plating, coatings, etc. The effect of good surface quality and less cracks

Active Publication Date: 2010-03-03
NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Sol-gel films generally have tiny cracks on the surface, which occur in the film drying and heat treatment stages. The analysis is mainly due to the following four reasons: (1) The sol and gel volatilize too quickly during film coating and heat treatment; (2) The thin film (Gel) Different from the shrinkage rate of the matrix, the gel is an organic mixture that volatilizes quickly when heated, shrinks rapidly, and has a large shrinkage rate, but the matrix is ​​a metal alloy, and the shrinkage rate is relatively small, and the The thermal expansion rate of the gel and the matrix is ​​very different, and stress will also be generated when heating and cooling, so that the film will crack when it is heat-treated at high temperature; (3) The surface layer of the gel will solidify immediately due to contact with air, forming a hard layer. Shell, while the solidification inside the gel is very slow, and during heat treatment, most of the organic matter in the gel will turn into gas, and the gas will expand when heated to break through the hard shell on the surface, resulting in cracks; Destruction, easy to cause film cracks and cracks

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0035] Step 1. TiO 2 Sol preparation

[0036] Chemically pure Ti(OC 4 h 9 ) as TiO 2 The precursor of the sol, adding analytically pure ethylene glycol monomethyl ether CH 3 OCH 2 CH2 OH is used as a solvent, in order to delay Ti(OC 4 h 9 ) strong hydrolysis, add an appropriate amount of analytically pure ethyl acetoacetate (CH 3 COCH 2 COOC 2 h 5 ), while adding analytically pure dry anti-cracking agent formamide (HCONH 2 ); the specific operation steps are: first mix 10ml of Ti(OC 4 h 9 ) dissolved in 50ml of CH 3 OCH 2 CH 2 OH, then add 2ml~6ml of CH 3 COCH 2 COOC 2 h 5 and 1ml~4ml of HCONH 2 , stirred at room temperature on a constant temperature magnetic stirrer for 40min to obtain a mixed solution, then added a pH adjustment solution (the pH adjustment solution was made of HNO 3 Prepare with distilled water, pH is 1~3), add 1ml~3ml of pH adjustment solution to every 100ml of mixed solution, and add in the way of dropwise addition, continue magnetic s...

Embodiment 1

[0044] First, 10ml of Ti(OC 4 h 9 ) dissolved in 50ml of CH 3 OCH 2 CH 2 OH, followed by adding 4ml of CH 3 COCH 2 COOC 2 h 5 and 2ml HCONH 2 . Stir on a constant temperature magnetic stirrer for 40 min at room temperature. Then add pH adjusting solution (pH adjusting solution is prepared by nitric acid and distilled water, pH is 2), the addition amount is to add pH adjusting solution 2ml in every 100ml mixed solution, and add in the mode of dropping. After the pH adjustment solution was added dropwise, magnetic stirring was continued for 3 hours to obtain a uniform, transparent light yellow TiO 2 Sol. The sol was left to stand and aged for 30 hours before use. Put the cleaned coating substrate into the glue homogenizer, the coating substrate is a metal substrate or an inorganic material substrate, and then add the aged sol dropwise on the surface of the sample. Turn on the power supply, the rotating speed is 5000r / min, and the time is 30 seconds. Then the sample...

Embodiment 2

[0046] First, 10ml of Ti(OC 4 h 9 ) dissolved in 50ml of CH 3 OCH 2 CH 2 OH, followed by 4ml of CH 3 COCH 2 COOC 2 h 5 and 2ml of HCONH 2 . Stir on a constant temperature magnetic stirrer for 40 min at room temperature. Then add pH adjusting solution (pH adjusting solution is prepared by nitric acid and distilled water, pH is 2), the addition amount is to add pH adjusting solution 2ml in every 100ml mixed solution, and add in the mode of dropping. After the pH adjustment solution was added dropwise, magnetic stirring was continued for 3 hours to obtain a uniform, transparent light yellow TiO 2 Sol. The sol was left to stand and aged for 30 hours before use. Put the cleaned coating substrate sample into the homogenizer, the coating substrate is a metal substrate or an inorganic material substrate, and then add the aged sol dropwise on the surface of the pure titanium sample. Turn on the power supply, the rotating speed is 5000r / min, and the time is 30 seconds. The...

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PUM

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Abstract

The invention discloses a method for preparing TiO2 film by utilizing a sol-gelatin method. The method comprises the following steps: (1) dissolving Ti (OC4H9) in ethylene glycol monoemethyl ether, then adding acetylacetic ether and methanamide, adding a pH regulator solution after stirring, continuously stirring the mixture to obtain uniform and transparent TiO2 sol with light yellow color, standing and maturing the mixture for later use; (2) dropwise adding the TiO2 sol after maturing to the surface of a substrate to be coated for film coating, putting the substrate in drying cabinet for predrying, putting the substrate in a cabinet-type high temperature resistance furnace for heat treatment, naturally cooling the substrate to a room temperature, putting an obtained film in a high temperature steam kettle for treatment, and then putting the film in boiling water for treatment to obtain the TiO2 film. In the invention, cross-linking agent formamide is added to a sol precursor solution; steam and hydrothermal joint treatment is carried out on the TiO2 film after heat treatment, therefore, internal stress and surface checkmarks of the TiO2 film prepared by the sol-gelatin method areeliminated or weakened, and the film has the advantages of more smooth and compact surface, complete coverage, favorable surface uniformity, uniform thickness and better practical use performance.

Description

technical field [0001] The present invention relates to a kind of TiO 2 The preparation method of thin film, especially relates to a kind of sol-gel method to prepare TiO used for surface anticorrosion, modification or active biology of metal matrix, inorganic material matrix and various parts thereof 2 thin film method. Background technique [0002] The sol-gel process is a method for preparing thin film materials developed in the 1960s. The basic process is that some easily hydrolyzed metal compounds (inorganic salts or metal alkoxides) are mixed with water, different acids and complexing agents in a certain solvent, and are stirred, reacted and aged to form a stable sol, and then The sol is applied to the surface of the cleaned substrate by means of dipping and pulling, spin coating or spraying, and finally a film is formed on the surface of the substrate through post-treatment processes such as drying and roasting. The specific process is as follows: first prepare the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C20/08B05C9/14C03C17/23C04B41/50C01G23/053
Inventor 余森于振涛牛金龙韩建业麻西群刘春潮
Owner NORTHWEST INSTITUTE FOR NON-FERROUS METAL RESEARCH
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