阅读说明：本技术 一种陶瓷基导电胶材料的制备方法 (Preparation method of ceramic-based conductive adhesive materials ) 是由 沈丽尧 于 2018-10-26 设计创作，主要内容包括：本发明提供了一种陶瓷基导电胶材料的制备方法,包括以下步骤：S1.制备石墨烯基碳包覆TiB<Sub>2</Sub>；S2.将制备悬浮液A；S3.制备导电TiB<Sub>2</Sub>-C-PANI；S4.将E-51环氧树脂,甘油环氧树脂,有机硅消泡剂KS-603,甲基六氢邻苯二甲酸酐和2-乙基-4-甲基咪唑以质量比为100-120：25-35：3-5：40-50：1-4混合作为基体树脂；S5.将步骤S3中制备得到导电TiB<Sub>2</Sub>-C-PANI加入基体树脂中,将上述材料混合均匀得到未固化的导电胶。本陶瓷胶导电材料具有优异的导电性能,同时使用时不易出现变形和热老化的问题。(The invention provides a preparation method of ceramic-based conductive adhesive materials, which comprises the following steps of S1, preparing graphene-based carbon-coated TiB 2 (ii) a S2, preparing a suspension A; s3, preparing conductive TiB 2 -C-PANI; s4, mixing E-51 epoxy resin, glycerin epoxy resin, an organic silicon defoamer KS-603, methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole in a mass ratio of 100-: 25-35: 3-5: 40-50: 1-4 as a matrix resin; s5, preparing the conductive TiB prepared in the step S3 2 Adding the-C-PANI into the matrix resin, and uniformly mixing the materials to obtain the uncured conductive adhesive. The ceramic adhesive conductive material has excellent conductive performance, and is not easy to deform in useAnd heat aging problems.)

1, kinds of ceramic base conductive glue material's preparation method, characterized by, including the following steps:

s1, mixing TiB₂Dissolving nano powder in ethanol, performing ultrasonic dispersion uniformly, adding the solution into liquid polyacrylonitrile oligomer, performing ball milling uniformly in a ball mill to obtain a mixture, pre-oxidizing the mixture in air at 160-260 ℃ to obtain a cured substance, and sintering the cured substance at 800-1200 ℃ to obtain the graphene-based carbon-coated TiB₂；

S2, dissolving aniline monomer in 0.045mol/L sodium dodecyl benzene sulfonate water solution, and adding the water solution into S1 to prepare the graphene-based carbon-coated TiB₂Ultrasonically homogenizing to obtain a suspension A;

s3, dissolving ammonium persulfate in 0.1-0.15mol/L hydrochloric acid aqueous solution to obtain 0.2-0.25mol/L solution B, then dropwise adding the solution B into the suspension A, reacting for 4-6h, standing for 12h, washing and drying to obtain the conductive TiB₂-C-PANI；

S4, mixing E-51 epoxy resin, glycerin epoxy resin, an organic silicon defoamer KS-603, methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole in a mass ratio of 100-: 25-35: 3-5: 40-50: 1-4 as a matrix resin;

s5, preparing the conductive TiB prepared in the step S3₂Adding the-C-PANI into the matrix resin, wherein the content of the filler is 30-50%, and uniformly mixing the materials to obtain the uncured conductive adhesive.

2. The method for preparing ceramic-based conductive adhesive materials according to claim 1, wherein the rotation speed of the ball mill in the step S1 is 500-700r/min, and the ball milling time is 2-4 h.

3. The method for preparing ceramic-based conductive paste materials according to claim 1, wherein the sintering time in step S1 is 2-6 h.

4. The ceramic-based conductive paste material of claim 1The preparation method is characterized by comprising the following steps: in the step S2, 2mL of aniline and 0.2-0.4g of graphene-based carbon-coated TiB are added into each 100mL of sodium dodecyl benzene sulfonate aqueous solution₂。

5. The method for preparing ceramic-based conductive paste materials according to claim 1, wherein in step S4, E-51 epoxy resin, glycerin epoxy resin, silicone defoamer KS-603, methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole are mixed in a mass ratio of 105-.

Technical Field

The invention relates to the field of novel conductive adhesive materials, in particular to a preparation method of ceramic-based conductive adhesive materials.

Background

The conductive adhesive is special adhesives with conductive performance, which mainly comprises base resin and conductive filler, wherein the conductive filler is the basis of the conductive adhesive for realizing the conductive connection effect, the base resin mainly plays a supporting and bearing role and connects the conductive filler to form a conductive path through the bonding effect to realize the conductive connection of the connected materialsConductive paste used in high-tip fields has a volume resistivity of of 10^-4Q cm, partial high-temperature cured conductive adhesive can reach 10^-5Q · cm, however, has a limited range of use because the electronic components may be deformed by heating, or may be deteriorated by heat deterioration, or the like, and the performance of the electronic components may be affected. The metal powder has a very low resistance but is easily oxidized, so that in order to obtain a low resistance value and overcome the defect that the metal powder is easily oxidized, the conductive ceramic powder with excellent conductivity and oxidation resistance is gradually the focus of recent research.

Disclosure of Invention

The invention aims to provide ceramic-based conductive adhesive materials which have excellent conductive performance and are not easy to deform and thermally age when in use.

The preparation method of ceramic-based conductive adhesive materials comprises the following steps:

s1, mixing TiB₂Dissolving nano powder in ethanol, performing ultrasonic dispersion uniformly, adding the solution into liquid polyacrylonitrile oligomer, performing ball milling uniformly in a ball mill to obtain a mixture, pre-oxidizing the mixture in air at 160-260 ℃ to obtain a cured substance, and sintering the cured substance at 800-1200 ℃ to obtain the graphene-based carbon-coated TiB₂；

S2, dissolving aniline monomer in 0.045mol/L sodium dodecyl benzene sulfonate water solution, and adding the water solution into S1 to prepare the graphene-based carbon-coated TiB₂Ultrasonically homogenizing to obtain a suspension A;

s3, dissolving ammonium persulfate in 0.1-0.15mol/L hydrochloric acid aqueous solution to obtain 0.2-0.25mol/L solution B, then dropwise adding the solution B into the suspension A, reacting for 4-6h, standing for 12h, washing and drying to obtain the conductive TiB₂-C-PANI；

S4, mixing E-51 epoxy resin, glycerin epoxy resin, an organic silicon defoamer KS-603, methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole in a mass ratio of 100-: 25-35: 3-5: 40-50: 1-4 as a matrix resin;

s5, preparing the product obtained in the step S3Conductive TiB₂Adding the-C-PANI into the matrix resin, wherein the content of the filler is 30-50%, and uniformly mixing the materials to obtain the uncured conductive adhesive.

, in the ceramic-based conductive adhesive materials preparation method, the rotation speed of the ball mill in the step S1 is 500-.

, in the ceramic-based conductive adhesive materials preparation method, the sintering time in the step S1 is 2-6 h.

, in the ceramic-based conductive adhesive materials preparing method, 2mL aniline and 0.2-0.4g graphene-based carbon-coated TiB are added into each 100mL sodium dodecyl benzene sulfonate aqueous solution in the step S2₂。

, the ceramic-based conductive adhesive materials are prepared by mixing E-51 epoxy resin, glycerin epoxy resin, an organic silicon defoamer KS-603, methylhexahydrophthalic anhydride and 2-ethyl-4-methylimidazole in a mass ratio of 105-115: 28-32: 3-5: 45-50: 2-3 as matrix resin in the step S4.

Has the advantages that: the invention has the following advantages: the invention takes ceramic material as a conductive substrate, and among a plurality of ceramic materials, TiB is found₂Has excellent conductive effect, and simultaneously forms the TiB coated by the graphene through the sintering function₂Then polyaniline is generated by an in-situ polymerization method, and TiB is coated by graphene₂Controlling TiB in the using process₂The expansion of the polyaniline leads to the reduction of the conductivity, which is beneficial to the stability of the material structure, the polyaniline is not only conductive, but also has a three-dimensional network structure, and the step is TiB₂Provides a receiving space.

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