Method for preparing nano metal oxide ceramic thin/thick film

A technology of oxide ceramics and nano-metals, applied in instruments, analytical materials, measuring devices, etc., can solve problems such as being unfavorable to obtain fine-grained and uniform nano-metal oxide films, achieve mutual contact and agglomeration inhibition, high efficiency, The effect of strong universality and generality

Inactive Publication Date: 2008-07-23
HUAZHONG UNIV OF SCI & TECH
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Problems solved by technology

This method includes the steps of preparation of nano-metal particles, oxidation of metal particles, in-situ drip injection film formation, and sintering. It needs to undergo multiple heat treatments, which is not conducive to obtaining fine and uniform nano-metal oxide films. This document also The final obtained SnO 2 Specific characterization of film particle size

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  • Method for preparing nano metal oxide ceramic thin/thick film

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preparation example Construction

[0016] Conventional water-soluble metal inorganic salts (including one or more, such as doping) for preparing metal oxide ceramic film layers can be used as raw materials of the present invention. The organic monomer is acrylamide (AM); the crosslinking agent is N, N'-methylenebisacrylamide (MBAM); the initiator is ammonium persulfate (APS); every 100 ml of mixed solution contains metal inorganic salt 15-25 grams, 15-25 grams of organic monomer, the mass ratio of crosslinking agent to organic monomer is 0.01:1-0.1:1; the mass ratio of initiator to organic monomer is 0.02:1-0.05:1.

[0017] (2) Catalytic initiation to form a gel. In the above mixed solution, add the catalyst dropwise, and add 1.2 to 3 ml of N, N, N', N'-tetramethylethylenediamine (TEMED) per 100 ml of the mixed solution as a catalyst to initiate crosslinking of the organic monomer Copolymerize to form a three-dimensional network-like polymer, so that the mixed solution turns into a gel.

[0018] (3) Preparati...

Embodiment 1

[0024] (1) Preparation containing Sn 4+ , a mixed solution of organic monomers, crosslinking agents and initiators. 20 g tin tetrachloride pentahydrate SnCl 4 ·5H 2 O was dissolved in 100 ml of deionized water, 15 g of AM, 1.5 g of MBAM, and 0.6 g of APS were added, stirred evenly by magnetic force, and a stable mixed solution was obtained.

[0025] (2) Catalytic initiation to form a gel. In the above mixed solution, 1.5 milliliters of TEMED was added dropwise to initiate cross-linking and copolymerization of organic monomers to form a polymer with a three-dimensional network structure, turning the mixed solution into a gel.

[0026] (3) Preparation of slurry suitable for film coating. In order to facilitate film coating, 2 milliliters of a premix solution containing a water-soluble organic binder and a plasticizer was added to the above-mentioned gel, and its component distribution ratio was 18 grams of PVA: 6 milliliters of glycerin: 100 milliliters of deionized water. ...

Embodiment 2

[0031] (1) Preparation containing Sn 4+ , Sb 3+ , a mixed solution of organic monomers, crosslinking agents and initiators. 25 g tin tetrachloride pentahydrate SnCl 4 ·5H 2 O and 1.3 g antimony trichloride SbCl 3 Dissolve in 100 ml of deionized water, add 25 g of AM, 2.0 g of MBAM and 0.5 g of APS, and mix evenly with magnetic stirring to obtain a stable mixed solution.

[0032] (2) Catalytic initiation to form a gel. In the above mixed solution, 1.8 milliliters of TEMED was added dropwise to initiate cross-linking and copolymerization of organic monomers to form a polymer with a three-dimensional network structure, so that the mixed solution turned into a gel.

[0033] (3) Preparation of slurry suitable for film coating. In order to facilitate film coating, 2.5 milliliters of a premix solution containing a water-soluble organic binder and a plasticizer was added to the above-mentioned gel, and its component distribution ratio was 15 grams of PVA: 6 milliliters of glycer...

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Abstract

The invention discloses a preparation method for nanometer metal oxide ceramic thin or thick coating, comprising steps in sequence: first, a mixed solution with metallic cation, organic monomers, cross-bonding agents, and initiating agents is prepared; second, gelatin is catalyzed; third, sizing agent is prepared for coating; fourth, coating is carried out; fifth, heat treatment is carried out. By adopting the cheap inorganic salts as raw materials, the nanometer metal oxide ceramic thin or thick coating has the advantages of simple technical process, easy operation, high efficiency, excellent repeatability, easy control for the size of the metal oxide grain and the thickness of the coating by adjusting the technological parameters, effectively avoiding mutual contact and agglomeration of the grains, meanwhile overcoming the shortcomings of high requirements upon experimental facilities and high cost in the common film preparing technique, thus providing with excellent universality and commonality, and also applicable to the preparation of the multi-layer composite nano-metal oxide thin or thick ceramic coating. In addition, the prepared thin or thick coating has a net-type loose porous structure, and the crystallization is excellent. The crystallized grains with narrowly distributed sizes are in sphere or sphere-like shapes, and are particularly suitable for the preparation of gas or humidity sensors.

Description

technical field [0001] The invention belongs to the technical field of electronic ceramic materials and preparation thereof, and in particular relates to a method for preparing nanometer metal oxide ceramic thin / thick films. The method uses the three-dimensional structure of the polymer network to solidify and disperse the metal cations in situ, and forms a nanometer metal oxide ceramic thin / thick film after heat treatment. The film is especially suitable for gas and humidity sensors. The metal oxide ceramic film is the core unit of the semiconductor ceramic gas sensor and humidity sensor. It uses the characteristic that its resistance value changes with the external gas or humidity to realize the detection of gas or humidity. Background technique [0002] Human's daily life and production activities are closely related to the atmospheric environment. Gas sensors and humidity sensors are mainly used to measure and control the atmospheric environment and its humidity changes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/624C04B35/63C04B35/01G01N27/12G01N27/407
Inventor 周东祥龚树萍刘欢郑志平胡云香傅邱云
Owner HUAZHONG UNIV OF SCI & TECH
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