CN102938269B - Method for preparing copper electronic paste with excellent oxidation resistance - Google Patents
Method for preparing copper electronic paste with excellent oxidation resistance Download PDFInfo
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- CN102938269B CN102938269B CN201210396012.1A CN201210396012A CN102938269B CN 102938269 B CN102938269 B CN 102938269B CN 201210396012 A CN201210396012 A CN 201210396012A CN 102938269 B CN102938269 B CN 102938269B
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- copper powder
- tetraethoxysilane
- deionized water
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- bismuth nitrate
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Abstract
The invention discloses a method for preparing a copper electronic paste with excellent oxidation resistance. The method concretely comprises the following steps of: step 1, preparing a mixed solution of ethyl orthosilicate and anhydrous ethanol, and hydrolyzing the mixed solution to obtain a hydrolyzed solvent; step 2, adding tributyl borate and bismuth nitrate into the hydrolyzed solvent to obtain a mixed solvent; step 3, further hydrolyzing the mixed solvent to obtain a gel; step 4, weighing copper powder, and dispersing the copper powder with ultrasonic waves; step 5, mixing the copper powder and the gel to obtain coated copper powder; and step 6, mixing the coated copper powder and an organic solvent to obtain the copper electronic paste. By using the method for preparing the copper electronic paste with excellent oxidation resistance, the problems that the copper electronic paste is liable to oxidization, and cannot be stored and sintered in the air for a long period of time are solved.
Description
Technical field
The invention belongs to slurry preparing technical field, relate to a kind of preparation method of electrocondution slurry, be specifically related to a kind of preparation method with good oxidation resistance energy copper electric slurry.
Background technology
Along with the develop rapidly of electronics, information, the communications industry, be that the demand of the electric slurry (electrically-conducting paint, conducting resinl) of major function phase is just more and more for the metal dust such as gold, silver, copper, also more and more higher to the requirement of its quality.
China is one of state of manufacturing center of electric slurry, and nowadays much external electronics processing enterprise constantly to China's transfer, makes the demand for electric slurry on market constantly promote.At present, the electric slurry that market uses is mainly silver-colored electronic paste, but constantly rise due to the price of silver, cause the cost of electronics processing enterprise progressively to raise, therefore a lot of electronics processing enterprise is in the urgent need to finding a kind of low cost, easily industrialization, can replacing other system electronic slurries of silver-colored electronic paste.
In numerous metal systems, the specific insulation of metallic copper is 1.70 × 10
-10Ω cm, is only second to the specific insulation 1.62 × 10 of silver
-10Ω cm, therefore likely becomes the excellent replacer of silver-colored electronic paste.But belong to magnesium-yttrium-transition metal due to metallic copper, its chemical property is very active, contact with air under normal temperature state and be just easily oxidized, the copper powder that particularly surface area ratio is larger, the oxide-film of one deck insulation can be formed after oxidation, and this layer of oxide-film conducts electricity hardly, make copper powder, particularly micron-sized copper powder, practical Cheng Du reduces greatly; In addition, if by copper powder long-term storage or in being placed on temperature is higher, humidity is larger environment, then problem of oxidation is even more serious.Therefore the problem of oxidation of copper powder greatly limit the application of copper powder in electric slurry field, need to find a kind of can industrial applications, there is excellent antioxidant performance and can the copper electric slurry of long-term storage.
Summary of the invention
The object of the present invention is to provide a kind of preparation method with good oxidation resistance energy copper electric slurry, solve that copper electric slurry exists oxidizable, can not the problem of long storage time and sintering in atmosphere.
The technical solution adopted in the present invention is, a kind of preparation method with good oxidation resistance energy copper electric slurry, specifically implements according to following steps:
The mixed solution of step 1, configuration tetraethoxysilane and absolute ethyl alcohol, and the solvent after obtaining hydrolysis that mixed solution is hydrolyzed;
Step 2, butyl borate and bismuth nitrate are added the solvent after hydrolysis, obtain mixed solvent;
Step 3, mixed solvent to be hydrolyzed further, to obtain gel;
Step 4, take copper powder, and copper powder ultrasonic wave is disperseed;
Step 5, copper powder to be mixed with gel, obtain coated copper powder;
Step 6, coated copper powder to be mixed with organic solvent, obtain copper electric slurry.
Feature of the present invention is also,
Step 1 is specifically implemented according to following steps:
1) in molar ratio for 1:1 takes tetraethoxysilane and absolute ethyl alcohol;
2) by 1) in the tetraethoxysilane that takes be dissolved in absolute ethyl alcohol and be configured to mixed solution;
3) take 2) in the quality W of mixed solution
(tetraethoxysilane and absolute ethyl alcohol), the quality W of deionized water is taken by the quality of mixed solution
(deionized water), wherein the mass ratio of mixed solution and deionized water is W
(tetraethoxysilane and absolute ethyl alcohol): W
(deionized water)=1:1;
4) by 3) in the deionized water that takes all pour in the mixed solution configured the reaction that is hydrolyzed into, after hydrolysis completes, obtain the solvent after being hydrolyzed.
Step 2 is specifically implemented according to following steps:
1) butyl borate, bismuth nitrate is taken respectively, tetraethoxysilane according to the consumption of tetraethoxysilane in step 1: butyl borate: the mol ratio of bismuth nitrate is 20 ~ 10:1 ~ 6:0.5 ~ 3;
2) by 1) in the butyl borate that takes and bismuth nitrate add in the solvent after the hydrolysis that step 1 obtains, obtain mixed solvent.
The purity of the tetraethoxysilane used in step 1 is higher than 99%, and the butyl borate used in step 2, the purity of bismuth nitrate are all higher than 99%.
Step 3 is specifically implemented according to following steps:
1) the quality W of the mixed solvent that step 2 obtains is taken
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate), by the quality W of mixed solvent
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate)take the quality W of deionized water
(deionized water), wherein W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(deionized water)=1:0.05 ~ 0.1;
2) by 1) in whole deionized waters of taking pour in the mixed solvent that step 2 obtains, make mixed solvent produce hydrolysis further, obtain gel.
Step 4 is specifically implemented according to following steps:
1) according to the quality sum W of the tetraethoxysilane used in step 1 and step 2, butyl borate and bismuth nitrate
(tetraethoxysilane+butyl borate+bismuth nitrate)take the quality W of copper powder
copper powder, W
copper powder: W
(tetraethoxysilane+butyl borate+bismuth nitrate)=0.05 ~ 0.3:1;
2) by the quality W of copper powder
copper powdertake deionized water, the mass ratio of copper powder and deionized water is 1:0.3;
3) by 1) in the copper powder that takes pour 2 into) in the deionized water that takes, adopt frequency to be that 35KHz ultrasonic wave disperses copper powder, jitter time is 40min ~ 80min.
Copper powder purity in step 4 is higher than 99%, and grain size is not more than 50 μm.
Step 5 is specifically implemented according to following steps:
1) copper powder of step 4 after ultrasonic wave dispersion is mixed with the gel that step 3 obtains, stir, obtain copper powder mixed solvent;
2) by 1) in the copper powder mixed solvent stirred that obtains carry out drying process, baking temperature is 80 DEG C ~ 150 DEG C, until dry, namely obtains coated copper powder.
Step 6 is specifically implemented according to following steps:
1) take machine solvent by the quality of the coated copper powder obtained in step 5, the mass ratio of coated copper powder and organic solvent is 7 ~ 9:3 ~ 1;
2) the coated copper powder in step 5 is added 1) in the organic solvent that takes, after Homogeneous phase mixing, namely obtain copper electric slurry of the present invention.
Step 6 organic solvent is one or more mixed solvents in triethanolamine, polyethylene glycol, sodium carboxymethylcellulose, sodium hydroxyethlcellulose, acrylic resin, acetylbutyrylcellulose, polyvinyl alcohol.
Beneficial effect of the present invention is,
(1) a kind of preparation method with good oxidation resistance energy copper electric slurry of the present invention has the simple advantage of preparation flow, does not need special equipment to produce, effectively reduces production cost;
(2) the copper electric slurry adopting the inventive method to prepare not only can sinter in atmosphere, and all right long-term storage, has good antioxygenic property.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A kind of preparation method with good oxidation resistance energy copper electric slurry of the present invention, specifically implements according to following steps:
The mixed solution of step 1, configuration tetraethoxysilane and absolute ethyl alcohol, and the solvent after obtaining hydrolysis that mixed solution is hydrolyzed;
1) in molar ratio for 1:1 takes tetraethoxysilane and absolute ethyl alcohol;
2) by 1) in the tetraethoxysilane that takes be dissolved in absolute ethyl alcohol and be configured to mixed solution;
3) take 2) in the quality W of mixed solution
(tetraethoxysilane and absolute ethyl alcohol), the quality W of deionized water is taken by the quality of mixed solution
(deionized water), wherein the mass ratio of mixed solution and deionized water is W
(tetraethoxysilane and absolute ethyl alcohol): W
(deionized water)=1:1;
4) by 3) in the deionized water that takes all pour in the mixed solution configured the reaction that is hydrolyzed into, after hydrolysis completes, obtain the solvent after being hydrolyzed.
Step 2, butyl borate and bismuth nitrate are added the solvent after hydrolysis, obtain mixed solvent;
1) butyl borate, bismuth nitrate is taken respectively, tetraethoxysilane according to the consumption of tetraethoxysilane in step 1: butyl borate: the mol ratio of bismuth nitrate is 20 ~ 10:1 ~ 6:0.5 ~ 3;
2) by 1) in the butyl borate that takes and bismuth nitrate add in the solvent after the hydrolysis that step 1 obtains, obtain mixed solvent.
Step 3, mixed solvent to be hydrolyzed further, to obtain gel;
1) the quality W of the mixed solvent that step 2 obtains is taken
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate), by the quality W of mixed solvent
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate)take the quality W of deionized water
(deionized water), wherein W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(deionized water)=1:0.05 ~ 0.1;
2) by 1) in whole deionized waters of taking pour in the mixed solvent that step 2 obtains, make mixed solvent produce hydrolysis further, obtain gel.
Step 4, take copper powder, and copper powder ultrasonic wave is disperseed;
1) according to the quality sum W of the tetraethoxysilane used in step 1 and step 2, butyl borate and bismuth nitrate
(tetraethoxysilane+butyl borate+bismuth nitrate)take the quality W of copper powder
copper powder, W
copper powder: W
(tetraethoxysilane+butyl borate+bismuth nitrate)=0.05 ~ 0.3:1;
2) by the quality W of copper powder
copper powdertake deionized water, the mass ratio of copper powder and deionized water is 1:0.3;
3) by 1) in the copper powder that takes pour 2 into) in the deionized water that takes, adopt frequency to be that 35KHz ultrasonic wave disperses copper powder, jitter time is 40min ~ 80min.
The copper powder purity wherein adopted is higher than 99%, and grain size is not more than 50 μm.
Step 5, copper powder to be mixed with gel, obtain coated copper powder;
1) copper powder of step 4 after ultrasonic wave dispersion is mixed with the gel that step 3 obtains, stir, obtain copper powder mixed solvent;
2) by 1) in the copper powder mixed solvent stirred that obtains carry out drying process, baking temperature is 80 DEG C ~ 150 DEG C, until dry, namely obtains coated copper powder.
Step 6, coated copper powder to be mixed with organic solvent, obtain copper electric slurry;
1) take machine solvent by the quality of the coated copper powder obtained in step 5, the mass ratio of coated copper powder and organic solvent is 7 ~ 9:3 ~ 1;
2) the coated copper powder in step 5 is added 1) in the organic solvent that takes, after Homogeneous phase mixing, namely obtain copper electric slurry of the present invention.
The organic solvent that step 6 uses is one or more mixed solvents in triethanolamine, polyethylene glycol, sodium carboxymethylcellulose, sodium hydroxyethlcellulose, acrylic resin, acetylbutyrylcellulose, polyvinyl alcohol.
Embodiment 1:
Tetraethoxysilane is dissolved in absolute ethyl alcohol and is configured to mixed solution, the mol ratio of tetraethoxysilane and absolute ethyl alcohol is 1:1, be that 1:1 takes deionized water by the mass ratio of mixed solution and deionized water, and the deionized water taken is poured in mixed solution, mixed solution is hydrolyzed acquisition hydrolysising solvent; Measure butyl borate and bismuth nitrate according to the consumption of tetraethoxysilane, the mol ratio of tetraethoxysilane, butyl borate and bismuth nitrate is 20:1:0.5, the butyl borate measured and bismuth nitrate is poured in the solvent after said hydrolyzed and obtains mixed solvent; Quality according to mixed solvent takes deionized water, W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(go ionized water)=1:0.05, is poured in the mixed solvent of acquisition by the deionized water taken, and mixed solvent is hydrolyzed further, obtains gel; According to the quality sum W of tetraethoxysilane, butyl borate and bismuth nitrate
(tetraethoxysilane+butyl borate+bismuth nitrate)take copper powder W
copper powder, W
copper powder: W
(positive silicic acid second ester+butyl borate+bismuth nitrate)=0.05:1, then take deionized water according to the quality of copper powder, the mass ratio of copper powder and deionized water is 1:0.3, the copper powder taken is placed in the ultrasonic wave dispersion 40min that deionized water adopts 35KHz; Copper powder after being disperseed by ultrasonic wave carries out mixing rear stirring with the gel of acquisition, carries out drying, obtain coated copper powder under 80 DEG C of conditions; The coated copper powder of preparation is mixed according to the ratio that mass ratio is 7:3 with organic solvent triethanolamine, obtains copper electric slurry.
Embodiment 2
Tetraethoxysilane is dissolved in absolute ethyl alcohol and is configured to mixed solution, the mol ratio of tetraethoxysilane and absolute ethyl alcohol is 1:1, be that 1:1 takes deionized water by the mass ratio of mixed solution and deionized water, and the deionized water taken is poured in mixed solution, mixed solution is hydrolyzed acquisition hydrolysising solvent; Measure butyl borate and bismuth nitrate according to the consumption of tetraethoxysilane, the mol ratio of tetraethoxysilane, butyl borate and bismuth nitrate is 10:6:3, the butyl borate measured and bismuth nitrate is poured in the solvent after said hydrolyzed and obtains mixed solvent; Quality according to mixed solvent takes deionized water, W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(go ionized water)=1:0.1, is poured in the mixed solvent of acquisition by the deionized water taken, and mixed solvent is hydrolyzed further, obtains gel; According to the quality sum W of tetraethoxysilane, butyl borate and bismuth nitrate
(tetraethoxysilane+butyl borate+bismuth nitrate)take copper powder W
copper powder, W
copper powder: W
(positive silicic acid second ester+butyl borate+bismuth nitrate)=0.3:1, then take deionized water according to the quality of copper powder, the mass ratio of copper powder and deionized water is 1:0.3, the copper powder taken is placed in the ultrasonic wave dispersion 60min that deionized water adopts 35KHz; ; Copper powder after being disperseed by ultrasonic wave carries out mixing rear stirring with the gel of acquisition, carries out drying, obtain coated copper powder under 90 DEG C of conditions; The coated copper powder of preparation is mixed according to the ratio that mass ratio is 9:1 with organic solvent acrylic resin, obtains copper electric slurry.
Embodiment 3
Tetraethoxysilane is dissolved in absolute ethyl alcohol and is configured to mixed solution, the mol ratio of tetraethoxysilane and absolute ethyl alcohol is 1:1, be that 1:1 takes deionized water by the mass ratio of mixed solution and deionized water, and the deionized water taken is poured in mixed solution, mixed solution is hydrolyzed acquisition hydrolysising solvent; Measure butyl borate and bismuth nitrate according to the consumption of tetraethoxysilane, the mol ratio of tetraethoxysilane, butyl borate and bismuth nitrate is 15:3:2, the butyl borate measured and bismuth nitrate is poured in the solvent after said hydrolyzed and obtains mixed solvent; Quality according to mixed solvent takes deionized water, W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(go from sub-water)=1:0.1, is poured in the mixed solvent of acquisition by the deionized water taken, and mixed solvent is hydrolyzed further, obtains gel; According to the quality sum W of tetraethoxysilane, butyl borate and bismuth nitrate
(tetraethoxysilane+butyl borate+bismuth nitrate)take copper powder W
copper powder, W
copper powder: W
(tetraethoxysilane+ butyl borate+bismuth nitrate)=0.1:1, then take deionized water according to the quality of copper powder, the mass ratio of copper powder and deionized water is 1:0.3, the copper powder taken is placed in the ultrasonic wave dispersion 80min that deionized water adopts 35KHz; Copper powder after being disperseed by ultrasonic wave carries out mixing rear stirring with the gel of acquisition, carries out drying, obtain coated copper powder under 120 DEG C of conditions; The coated copper powder of preparation is mixed according to the ratio that mass ratio is 4:1 with organic solvent polyethylene glycol, obtains copper electric slurry.
Claims (3)
1. there is a preparation method for good oxidation resistance energy copper electric slurry, it is characterized in that, specifically implement according to following steps:
The mixed solution of step 1, preparation tetraethoxysilane and absolute ethyl alcohol, and the solvent after obtaining hydrolysis that mixed solution is hydrolyzed, specifically implement according to following steps:
Step 1.1, in molar ratio for 1:1 takes tetraethoxysilane and absolute ethyl alcohol;
Step 1.2, the tetraethoxysilane taken is dissolved in absolute ethyl alcohol is mixed with mixed solution in step 1.1;
Step 1.3, take the quality W of mixed solution in step 1.2
(tetraethoxysilane and absolute ethyl alcohol), the quality W of deionized water is taken by the quality of mixed solution
(deionized water), wherein the mass ratio of mixed solution and deionized water is W
(tetraethoxysilane and absolute ethyl alcohol): W
(deionized water)=1:1;
Step 1.4, the deionized water taken in step 1.3 all poured in the mixed solution that configures into the reaction that is hydrolyzed, after hydrolysis completes, obtain the solvent after being hydrolyzed;
Step 2, butyl borate and bismuth nitrate are added the solvent after hydrolysis, obtain mixed solvent, specifically implement according to following steps:
Step 2.1, take butyl borate, bismuth nitrate respectively, tetraethoxysilane according to the consumption of tetraethoxysilane in step 1: butyl borate: the mol ratio of bismuth nitrate is 20 ~ 10:1 ~ 6:0.5 ~ 3;
Step 2.2, the butyl borate taken in step 2.1 and bismuth nitrate to be added in the solvent after hydrolysis that step 1 obtains, obtain mixed solvent;
Step 3, mixed solvent to be hydrolyzed further, to obtain gel, specifically implement according to following steps:
Step 3.1, take the quality W of mixed solvent that step 2 obtains
(tetraethoxysilane+absolute ethyl alcohol+boric acid three fourth ester+bismuth nitrate), by the quality W of mixed solvent
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate)take the quality W of deionized water
(deionized water), wherein W
(tetraethoxysilane+absolute ethyl alcohol+butyl borate+bismuth nitrate): W
(deionized water)=1:0.05 ~ 0.1;
Step 3.2, the whole deionized waters taken in step 3.1 to be poured in mixed solvent that step 2 obtains, make mixed solvent produce hydrolysis further, obtain gel;
Step 4, take copper powder, and copper powder ultrasonic wave disperseed, specifically implement according to following steps:
The quality sum W of step 4.1, tetraethoxysilane, butyl borate and bismuth nitrate according to using in step 1 and step 2
(tetraethoxysilane+butyl borate+bismuth nitrate)take the quality W of copper powder
copper powder, W
copper powder: W
(tetraethoxysilane+butyl borate+bismuth nitrate)=0.05 ~ 0.3:1;
Step 4.2, quality W by copper powder
copper powdertake deionized water, the mass ratio of copper powder and deionized water is 1:0.3;
Step 4.3, to be poured into by the copper powder taken in step 4.1 in the deionized water that takes in step 4.2, adopt frequency to be that 35KHz ultrasonic wave disperses copper powder, jitter time is 40min ~ 80min;
Step 5, copper powder to be mixed with gel, obtains coated copper powder, specifically implement according to following steps:
Step 5.1, the copper powder of step 4 after ultrasonic wave dispersion to be mixed with the gel that step 3 obtains, stir, acquisition copper powder mixed solvent;
Step 5.2, the copper powder mixed solvent stirred obtained in step 5.1 carried out drying process, baking temperature is 80 DEG C ~ 150 DEG C, until dry, namely obtains coated copper powder;
Step 6, coated copper powder to be mixed with organic solvent, obtains copper electric slurry, specifically implement according to following steps:
Step 6.1, take organic solvent by the quality of coated copper powder obtained in step 5, the mass ratio of coated copper powder and organic solvent is 7 ~ 9:3 ~ 1;
Step 6.2, the coated copper powder in step 5 to be added in organic solvent that step 6.1 takes, after Homogeneous phase mixing, namely obtain copper electric slurry;
Described step 6 organic solvent is the one in triethanolamine, polyethylene glycol, sodium carboxymethylcellulose, sodium hydroxyethlcellulose, acrylic resin, acetylbutyrylcellulose, polyvinyl alcohol.
2. the preparation method with good oxidation resistance energy copper electric slurry according to claim 1, it is characterized in that, the purity of the tetraethoxysilane used in described step 1 is higher than 99%, and the butyl borate used in described step 2, the purity of bismuth nitrate are all higher than 99%.
3. the preparation method with good oxidation resistance energy copper electric slurry according to claim 1, is characterized in that, the copper powder purity in described step 4 is higher than 99%, and grain size is not more than 50 μm.
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| WO2016104232A1 (en) * | 2014-12-26 | 2016-06-30 | ハリマ化成株式会社 | Conductive paste |
| JP6777548B2 (en) * | 2015-01-29 | 2020-10-28 | ハリマ化成株式会社 | Conductive paste |
| CN105679408B (en) * | 2016-03-17 | 2017-08-29 | 西安工程大学 | The acrylic acid microcapsules processing method of copper powder in a kind of electric slurry |
| CN105957642B (en) * | 2016-06-08 | 2017-11-28 | 天津大学 | A kind of preparation method of coated with silica copper electric slurry for ltcc substrate |
| CN107337965B (en) * | 2017-08-28 | 2020-03-10 | 厦门大学 | Preparation method of antioxidant copper-based conductive ink |
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