CN104036876A - Preparation method of high-temperature copper electronic paste - Google Patents
Preparation method of high-temperature copper electronic paste Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature copper electronic paste. The preparation method comprises the following steps of: preparing a mixed solvent of copper powders of 1 microns or 15 microns respectively; removing redundant H+ in the mixed solvent of copper powders of 1 microns or 15 microns to obtain pre-coated copper powders of 1 microns or 15 microns; mixing terpilenol, ethyl cellulose, ethyl acetate, polyether defoamer and amino propyl triethoxy silane; heating a mixture in water bath till the mixture is solved completely, obtaining an organic carrier; mixing the pre-coated copper powders of 1 microns, the pre-coated copper powders of 15 microns, glass powders and the organic carrier uniformly, thereby obtaining the high-temperature copper electronic paste. The preparation method of the high-temperature copper electronic paste disclosed by the invention is simple in preparation process flow and can perform production with no need of special equipment, so that a production cost is effectively reduced; the prepared copper electronic paste is not only excellent in conductivity but also available for long-term storage.
Description
Technical field
The invention belongs to electronic package material preparing technical field, be specifically related to a kind of preparation method of high temperature copper electric slurry.
Background technology
Electric slurry is as a kind of new material, excellent in traditional circuit equipment (as resistance wire, electrothermal tube etc.) far away, and has environmental protection, the feature such as efficient and energy-conservation, and its cost also approaches with traditional material, will be main application direction in the future undoubtedly.
Polymorphic type Au, Ag and composite mixed conductive noble metal slurry are developed at present, although electric conductivity excellence, but price is high, low with the adhesive strength of base material, and there is electron transfer phenomenon during for the electrode tip material of the conductive strips of thick film circuit, capacitor, reduce the conductivity of electrocondution slurry.
In metal system, copper source is wide, and cost is low, and Cu has the high frequency characteristics more better than Au and conductivity, and the specific insulation of copper is (1.70 × 10
-10Ω cm) be only second to silver-colored specific insulation (1.62 × 10
-10Ω cm), electric conductivity well be the more important thing is does not have Ag
+the defect of migration.Metallic copper belongs to magnesium-yttrium-transition metal, and its chemical property is very active, and under normal temperature state, contact with air and be just easily oxidized, and, there is easily reunion, and the problem such as substrate combinating strength is low.Therefore, find a kind of Copper Powder Surface modified technique that can improve superfine cupper powder surface oxidation-resistant performance, prepare a kind of can industrial applications, there is excellent conductive capability and environment-friendly high-temperature copper electric slurry that can long-term storage, thereby improve conductivity and the high frequency characteristics of electronic devices and components, reduce the production cost of manufacturer production, enhance competitiveness.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high temperature copper electric slurry, the problem of oxidizable, the easy reunion that has solved that copper electric slurry exists.
The technical solution adopted in the present invention is, a kind of preparation method of high temperature copper electric slurry, and concrete steps are:
Step 1, prepares respectively 1 μ m copper powder mixed solvent and 15 μ m copper powder mixed solvents;
Step 2, unnecessary H in the 1 μ m copper powder mixed solvent that removal step 1 obtains and 15 μ m copper powder mixed solvents
+, obtain being coated in advance 1 μ m copper powder and pre-coated 15 μ m copper powders;
Step 3, mixes terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, until dissolving is complete, obtains organic carrier at 60～90 DEG C of heating water baths;
Step 4, the coated 1 μ m copper powder that step 2 is obtained, the organic carrier that coated 15 μ m copper powders, glass dust and step 3 obtain in advance mix, and obtain high temperature copper electric slurry.
Feature of the present invention is also,
In step 1, the compound method of 1 μ m copper powder mixed solvent and 15 μ m copper powder mixed solvents is: be that 1～3:1～4 mix with the copper powder of 1 μ m copper powder or 15 μ m according to mass ratio by polyethylene glycol, after adopting the centrifugal 10～30min of centrifuge that rotating speed is 5000rpm～10000rpm, leave standstill 1～3h, obtain 1 μ m copper powder mixed solvent or 15 μ m copper powder mixed solvents.
The specific implementation method of step 2 is: in the 1 μ m copper powder mixed solvent obtaining to step 1 or 15 μ m copper powder mixed solvents, add absolute ethyl alcohol; then after adopting speed magnetic agitation 10～30min of 5000～10000rpm, leave standstill 20～50min; outwell a layer clear liquid; after repeating 2～3 times, under the atmosphere of nitrogen protection, be dried processing, obtain pre-coated 1 μ m copper powder and pre-coated 15 μ m copper powders.
Baking temperature is 100 DEG C～150 DEG C, time 2～4h.
In step 3, the volume ratio of terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane is 60～80:6～10:6～15:2～5:2～5.
Pre-coated 1 μ m copper powder in step 4, the mass ratio of coated 15 μ m copper powders, glass dust and organic carrier is 13～16:54～60:5～12:5～25 in advance.
The invention has the beneficial effects as follows,
1. the preparation method of high temperature copper electric slurry of the present invention, utilize polyethylene glycol coated in advance to copper powder in the aqueous solution as reducing agent, dispersant and stabilizer, remove surperficial oxide layer, through magnetic agitation, the standing pre-cladding of copper powder that obtains, then dry and obtain coated copper powder; Then adopt terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, glass dust to prepare high temperature copper electric slurry, the copper slurry that slurry prepares is screen-printed on alumina ceramic substrate, adopt suitable temperature and time to dry sintered copper slurry, obtain can be used for the conductive copper films of Electronic Packaging coating.
2. the preparation method of high temperature copper electric slurry of the present invention, preparation flow is simple, does not need special equipment to produce, and effectively reduces production cost; Not only electric conductivity excellence of the copper electric slurry of preparing, can also long-term storage.
3. the preparation method of high temperature copper electric slurry of the present invention, the copper electric slurry of preparing can high temperature sintering, and not leaded cadmium composition is pollution-free, can be used for the high temperature copper electric slurry that ceramic electronic component and vitreous electricity sub-element and thick-film conductor band etc. require.
Embodiment
Below in conjunction with embodiment, the present invention is described in detail.
The preparation method of high temperature copper electric slurry of the present invention, specifically implements according to following steps:
Step 1, prepares respectively 1 μ m copper powder mixed solvent and 15 μ m copper powder mixed solvents;
Be that 1～3:1～4 mix with the copper powder of 1 μ m copper powder or 15 μ m according to mass ratio by polyethylene glycol, after adopting the centrifugal 10～30min of centrifuge that rotating speed is 5000rpm～10000rpm, leave standstill 1～3h, obtain 1 μ m copper powder mixed solvent or 15 μ m copper powder mixed solvents;
Step 2, unnecessary H in the 1 μ m copper powder mixed solvent that removal step 1 obtains and 15 μ m copper powder mixed solvents
+, obtain being coated in advance 1 μ m copper powder and pre-coated 15 μ m copper powders;
In the 1 μ m copper powder mixed solvent obtaining to step 1 or 15 μ m copper powder mixed solvents, add absolute ethyl alcohol, then after adopting speed magnetic agitation 10～30min of 5000～10000rpm, leave standstill 20～50min, outwell a layer clear liquid, after repeating 2～3 times, under the atmosphere of nitrogen protection, be dried processing, baking temperature is 100 DEG C～150 DEG C, time 2～4h, obtains pre-coated 1 μ m copper powder and pre-coated 15 μ m copper powders;
Step 3, be that mix 60～80:6～10:6～15:2～5:2～5 by volume by terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, until dissolving is complete, obtain organic carrier at 60～90 DEG C of heating water baths;
Step 4, the coated 1 μ m copper powder that step 2 is obtained, the organic carrier that coated 15 μ m copper powders, glass dust and step 3 obtain are in advance that 13～16:54～60:5～12:5～25 mix in mass ratio, obtain high temperature copper electric slurry.
The preparation method of high temperature copper electric slurry of the present invention, utilize polyethylene glycol coated in advance to copper powder in the aqueous solution as reducing agent, dispersant and stabilizer, remove surperficial oxide layer, through magnetic agitation, the standing pre-cladding of copper powder that obtains, then dry and obtain coated copper powder; Then adopt terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, glass dust to prepare high temperature copper electric slurry, the copper slurry that slurry prepares is screen-printed on alumina ceramic substrate, adopt suitable temperature and time to dry sintered copper slurry, obtain can be used for the conductive copper films of Electronic Packaging coating.
The preparation method of high temperature copper electric slurry of the present invention, preparation flow is simple, does not need special equipment to produce, and effectively reduces production cost; Not only electric conductivity excellence of the copper electric slurry of preparing, can also long-term storage.
The preparation method of high temperature copper electric slurry of the present invention, the copper electric slurry of preparing can high temperature sintering, and not leaded cadmium composition is pollution-free, can be used for the high temperature copper electric slurry that ceramic electronic component and vitreous electricity sub-element and thick-film conductor band etc. require.
Embodiment 1
Step 1, is that 1:1 mix with the copper powder of 1 μ m according to mass ratio by polyethylene glycol, after the centrifugal 30min of centrifuge that employing rotating speed is 5000rpm, leaves standstill 1h, obtains 1 μ m copper powder mixed solvent;
Step 2, is that 1:1 mix with the copper powder of 15 μ m according to mass ratio by polyethylene glycol, after the centrifugal 30min of centrifuge that employing rotating speed is 5000rpm, leaves standstill 1h, obtains 15 μ m copper powder mixed solvents;
Step 3, adds absolute ethyl alcohol in the 5 μ m copper powder mixed solvents that the 1 μ m copper powder mixed solvent obtaining or step 2 obtain to step 1, leaves standstill 30min after then adopting the speed magnetic agitation 10min of 8000rpm, outwells a layer clear liquid, repeats 3 times, removes unnecessary H
+, prevent that copper powder is by secondary oxidation, then under the atmosphere of nitrogen protection, be dried processing, baking temperature is 100 DEG C, time 120min obtains pre-coated 1 μ m or is coated in advance 15 μ m copper powders;
Step 4, by terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, by volume for 80:6:8:3:3 mixes, 80 DEG C of heating water baths are until dissolving completely, obtains organic carrier;
Step 5, the pre-coated 1 μ m copper powder that step 3 is obtained, coated 15 μ m copper powders, glass dust and step 4 obtain in advance organic carrier, in mass ratio for 15.8:59.2:5:20 mixes, obtain high temperature copper electric slurry.
Embodiment 2
Step 1, is that 3:2 mix with the copper powder of 1 μ m according to mass ratio by polyethylene glycol, after the centrifugal 10min of centrifuge that employing rotating speed is 8000rpm, leaves standstill 2h, obtains 1 μ m copper powder mixed solvent;
Step 2, is that 3:2 mix with the copper powder of 15 μ m according to mass ratio by polyethylene glycol, after the centrifugal 10min of centrifuge that employing rotating speed is 8000rpm, leaves standstill 2h, obtains 15 μ m copper powder mixed solvents;
Step 3, adds absolute ethyl alcohol in the 15 μ m copper powder mixed solvents that the 1 μ m copper powder mixed solvent obtaining or step 2 obtain to step 1, leaves standstill 20min after then adopting the speed magnetic agitation 30min of 5000rpm, outwells a layer clear liquid, repeats 3 times, removes unnecessary H
+, prevent that copper powder is by secondary oxidation, then under the atmosphere of nitrogen protection, be dried processing, baking temperature is 120 DEG C, time 3h obtains pre-coated 1 μ m or is coated in advance 15 μ m copper powders;
Step 4, by terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, by volume for 76:8:11:2:3 mixes, 60 DEG C of heating water baths are until dissolving completely, obtains organic carrier;
Step 5, the pre-coated 1 μ m copper powder that step 3 is obtained, coated 15 μ m copper powders, glass dust and step 4 obtain in advance organic carrier, in mass ratio for 13:54:7:5 mixes, obtain high temperature copper electric slurry.
Embodiment 3
Step 1, is that 1:4 mix with the copper powder of 1 μ m according to mass ratio by polyethylene glycol, after the centrifugal 20min of centrifuge that employing rotating speed is 6000rpm, leaves standstill 3h, obtains 1 μ m copper powder mixed solvent;
Step 2, is that 1:4 mix with the copper powder of 15 μ m according to mass ratio by polyethylene glycol, after the centrifugal 20min of centrifuge that employing rotating speed is 6000rpm, leaves standstill 3h, obtains 15 μ m copper powder mixed solvents;
Step 3, adds absolute ethyl alcohol in the 15 μ m copper powder mixed solvents that the 1 μ m copper powder mixed solvent obtaining or step 2 obtain to step 1, leaves standstill 40min after then adopting the speed magnetic agitation 20min of 10000rpm, outwells a layer clear liquid, repeats 2 times, removes unnecessary H
+, prevent that copper powder is by secondary oxidation, then under the atmosphere of nitrogen protection, be dried processing, baking temperature is 130 DEG C, time 4h obtains pre-coated 1 μ m copper powder or is coated in advance 15 μ m copper powders;
Step 4, by terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, by volume for 60:7:6:2:2 mixes, 90 DEG C of heating water baths are until dissolving completely, obtains organic carrier;
Step 5, the pre-coated 1 μ m copper powder that step 3 is obtained, coated 15 μ m copper powders, glass dust and step 4 obtain in advance organic carrier, in mass ratio for 14:56:12:18 mixes, obtain high temperature copper electric slurry.
Embodiment 4
Step 1, is that 2:3 mix with the copper powder of 1 μ m according to mass ratio by polyethylene glycol, after the centrifugal 25min of centrifuge that employing rotating speed is 10000rpm, leaves standstill 2.5h, obtains 1 μ m copper powder mixed solvent;
Step 2, is that 2:3 mix with the copper powder of 15 μ m according to mass ratio by polyethylene glycol, after the centrifugal 25min of centrifuge that employing rotating speed is 10000rpm, leaves standstill 2.5h, obtains 15 μ m copper powder mixed solvents;
Step 3, adds absolute ethyl alcohol in the 15 μ m copper powder mixed solvents that the 1 μ m copper powder mixed solvent obtaining or step 2 obtain to step 1, leaves standstill 50min after then adopting the speed magnetic agitation 25min of 6000rpm, outwells a layer clear liquid, repeats 2 times, removes unnecessary H
+, prevent that copper powder is by secondary oxidation, then under the atmosphere of nitrogen protection, be dried processing, baking temperature is 150 DEG C, time 2.5h obtains pre-coated 1 μ m copper powder or is coated in advance 15 μ m copper powders;
Step 4, by terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, by volume for 70:10:15:5:5 mixes, 70 DEG C of heating water baths are until dissolving completely, obtains organic carrier;
Step 5, the pre-coated 1 μ m copper powder that step 3 is obtained, coated 15 μ m copper powders, glass dust and step 4 obtain in advance organic carrier, in mass ratio for 16:60:10:25 mixes, obtain high temperature copper electric slurry.
After the high temperature copper electric slurry of embodiment 1～4 preparation is printed on aluminium oxide ceramic substrate with screen printing technique, be positioned in the Muffle furnace of 300 DEG C sintering in air, gained sample is tested with four point probe tester, and gained resistance is as shown in table 1.
The resistance of the high temperature copper electric slurry of table 1 embodiment 1～4 preparation
| Example number | Sheet resistance (m Ω/) |
| 1 | 36.03 |
| 2 | 36.29 |
| 3 | 18.23 |
| 4 | 22.39 |
Claims (6)
1. a preparation method for high temperature copper electric slurry, is characterized in that, concrete steps are:
Step 1, prepares respectively 1 μ m copper powder mixed solvent and 15 μ m copper powder mixed solvents;
Step 2, unnecessary H in the 1 μ m copper powder mixed solvent that removal step 1 obtains and 15 μ m copper powder mixed solvents
+, obtain being coated in advance 1 μ m copper powder and pre-coated 15 μ m copper powders;
Step 3, mixes terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane, until dissolving is complete, obtains organic carrier at 60～90 DEG C of heating water baths;
Step 4, the coated 1 μ m copper powder that step 2 is obtained, the organic carrier that coated 15 μ m copper powders, glass dust and step 3 obtain in advance mix, and obtain high temperature copper electric slurry.
2. the preparation method of high temperature copper electric slurry according to claim 1, it is characterized in that, in step 1, the compound method of 1 μ m copper powder mixed solvent and 15 μ m copper powder mixed solvents is: be that 1～3:1～4 mix with the copper powder of 1 μ m copper powder or 15 μ m according to mass ratio by polyethylene glycol, after adopting the centrifugal 10～30min of centrifuge that rotating speed is 5000rpm～10000rpm, leave standstill 1～3h, obtain 1 μ m copper powder mixed solvent or 15 μ m copper powder mixed solvents.
3. the preparation method of high temperature copper electric slurry according to claim 1; it is characterized in that; the specific implementation method of step 2 is: in the 1 μ m copper powder mixed solvent obtaining to step 1 or 15 μ m copper powder mixed solvents, add absolute ethyl alcohol; then after adopting speed magnetic agitation 10～30min of 5000～10000rpm, leave standstill 20～50min; outwell a layer clear liquid; after repeating 2～3 times, under the atmosphere of nitrogen protection, be dried processing, obtain pre-coated 1 μ m copper powder and pre-coated 15 μ m copper powders.
4. the preparation method of high temperature copper electric slurry according to claim 3, is characterized in that, baking temperature is 100 DEG C～150 DEG C, time 2～4h.
5. the preparation method of high temperature copper electric slurry according to claim 1, it is characterized in that, in step 3, the volume ratio of terpinol, ethyl cellulose, ethyl acetate, polyether antifoam agent, aminopropyl triethoxysilane is 60～80:6～10:6～15:2～5:2～5.
6. the preparation method of high temperature copper electric slurry according to claim 1, is characterized in that, pre-coated 1 μ m copper powder in step 4, the mass ratio of coated 15 μ m copper powders, glass dust and organic carrier is 13～16:54～60:5～12:5～25 in advance.
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Cited By (8)
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| CN104361950A (en) * | 2014-10-21 | 2015-02-18 | 西安工程大学 | Preparation method of carbon-clad copper electronic paste |
| CN105834418A (en) * | 2016-03-17 | 2016-08-10 | 西安工程大学 | Processing method for ethyl cellulose microcapsules of copper powder in electronic slurry |
| CN106548822A (en) * | 2016-10-31 | 2017-03-29 | 上海新益电力线路器材有限公司 | A kind of high temperature resistant composite conductor and preparation method thereof |
| CN106782885A (en) * | 2016-12-19 | 2017-05-31 | 西安工程大学 | A kind of preparation method of nano silver wire copper chopped fiber copper composite electron slurry |
| CN106876005A (en) * | 2017-01-11 | 2017-06-20 | 西安工程大学 | Sn Cu composite electron slurries and preparation method thereof |
| CN108231281A (en) * | 2017-12-20 | 2018-06-29 | 西安工程大学 | A kind of preparation method of titanium aluminium carbon/copper electric slurry |
| CN108766619A (en) * | 2018-05-28 | 2018-11-06 | 原晋波 | A kind of electronic component electrode slurry and preparation method thereof |
| CN111540503A (en) * | 2020-05-29 | 2020-08-14 | 南京凯泰化学科技有限公司 | Conductive copper paste and using method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104361950A (en) * | 2014-10-21 | 2015-02-18 | 西安工程大学 | Preparation method of carbon-clad copper electronic paste |
| CN105834418A (en) * | 2016-03-17 | 2016-08-10 | 西安工程大学 | Processing method for ethyl cellulose microcapsules of copper powder in electronic slurry |
| CN105834418B (en) * | 2016-03-17 | 2018-01-05 | 西安工程大学 | The ethyl cellulose microcapsule processing method of copper powder in a kind of electric slurry |
| CN106548822A (en) * | 2016-10-31 | 2017-03-29 | 上海新益电力线路器材有限公司 | A kind of high temperature resistant composite conductor and preparation method thereof |
| CN106782885A (en) * | 2016-12-19 | 2017-05-31 | 西安工程大学 | A kind of preparation method of nano silver wire copper chopped fiber copper composite electron slurry |
| CN106782885B (en) * | 2016-12-19 | 2018-07-03 | 西安工程大学 | A kind of preparation method of nano silver wire-copper staple fiber-copper composite electron slurry |
| CN106876005A (en) * | 2017-01-11 | 2017-06-20 | 西安工程大学 | Sn Cu composite electron slurries and preparation method thereof |
| CN108231281A (en) * | 2017-12-20 | 2018-06-29 | 西安工程大学 | A kind of preparation method of titanium aluminium carbon/copper electric slurry |
| CN108766619A (en) * | 2018-05-28 | 2018-11-06 | 原晋波 | A kind of electronic component electrode slurry and preparation method thereof |
| CN111540503A (en) * | 2020-05-29 | 2020-08-14 | 南京凯泰化学科技有限公司 | Conductive copper paste and using method thereof |
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