CN104658633A - Formula and preparation method of conductive copper paste for automotive glass heater wire - Google Patents
Formula and preparation method of conductive copper paste for automotive glass heater wire Download PDFInfo
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- CN104658633A CN104658633A CN201310585286.XA CN201310585286A CN104658633A CN 104658633 A CN104658633 A CN 104658633A CN 201310585286 A CN201310585286 A CN 201310585286A CN 104658633 A CN104658633 A CN 104658633A
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Abstract
The invention relates to a formula and a preparation method of conductive copper paste for an automotive glass heater wire. The formula of the conductive copper paste for the automotive glass heater wire comprises the following components in percentage by mass: 80-90 percent of ultrafine mixed metal powder, 4-9.5 percent of glass powder, 5.5-10.5 percent of an organic carrier, 0.1-1.0 percent of an organic additive, wherein the sum of the mass percents of the components is 100%. The preparation method of the conductive copper paste for the automotive glass heater wire comprises the following steps: uniformly mixing the ultrafine mixed metal powder with the quantitative organic carrier and organic additive and rolling to paste, and uniformly mixing the glass powder with the quantitative organic carrier and organic additive and rolling to paste; dispersing the two kinds of paste through a high-shear dispersion machine to obtain a viscous paste finished product, namely the conductive copper slurry. The conductive copper paste can replace automotive glass heater wire silver paste, and is subjected to silk-screen printing on automotive glass and sintered under N2 atmosphere, so that the obtained glass heater wire has good electrical property, adhesion fastness, thermal shock resistance and resistance to oxidation; meanwhile, the conductive copper paste can also replace the silver paste for similar purposes, and the cost is greatly reduced compared with that of the silver paste.
Description
Technical field
The present invention relates to a kind of electric slurry, be specifically related to a kind of formula and preparation method of vehicle glass hot line conductive copper paste, the printing manufacture of conductive silver paste for vehicle glass hot line can be substituted, and obtain good electrical property, attachment fastness, resistance to sudden heating, non-oxidizability; Simultaneously this conductive copper paste also alternative silver slurry be used for other similar purposes, belong to electronic material and Micron-nano composites field.
Background technology
At present, vehicle glass hot line generally adopts the printing of silver slurry, although adopt silver slurry to be printed in manufacturing process and performance all bring various facility, silver belongs to precious metal, expensive, to cost bringing huge pressure.At present, field is manufactured at ceramic capacitor, many manufacturers start to consider to adopt copper slurry to substitute part silver slurry, to reduce costs, such as in MLCC multilayer ceramic capacitor field, the basic base metal that all adopts is as electrode material, and in the manufacture field of the electronic devices and components such as wafer capacitance, piezo-resistance, the lowpriced metallization of its electrode material is to be adopted by increasing producer.
In vehicle glass hot line field, main electrical property, attachment fastness, acid resistance, resistance to sudden heating, the non-oxidizability paying close attention to its wiring; The present invention improves high-copper powder content by adopting, and adds certain additive, adopts special glass dust system, makes its above-mentioned various performance reach silver-colored pulp-water and puts down, considerably reduce cost simultaneously.
Summary of the invention
Vehicle glass hot line, to the particular/special requirement of wiring character, comprises conductivity, attachment fastness, acid resistance, sulfur resistive voltinism, non-oxidizability etc.
The object of the invention is to be achieved through the following technical solutions:
The formula of vehicle glass hot line conductive copper paste, it is characterized in that: each constituent mass percentage is: ultra-fine mixed metal powder 80 ~ 90%, glass dust 4 ~ 9.5%, organic carrier 5.5 ~ 10.5%, organic additive 0.1 ~ 1.0%, each constituent mass percentage sum is 100%;
Described ultra-fine mixed metal powder is made up of the raw material of following mass percent: blister copper powder 90 ~ 95%, thin copper powder 5 ~ 10%, low-melting alloy powder 0.5 ~ 2%.
Described blister copper powder equivalent sphere particle diameter is D
50=2 ~ 4 μm, S.S.A=0.5 ~ 1.0m
2/ g.
Described thin copper powder equivalent sphere particle diameter is D
50=80 ~ 200nm, S.S.A=6 ~ 15m
2/ g.
The fusing point of described low-melting alloy powder is 130 ~ 230 DEG C, and it comprises one or more in signal bronze, sn-bi alloy.
Described glass dust is a kind of B-Bi-Si-P glass frit, and its point of incipient sintering is 450 ~ 550 DEG C, obvious melt temperature higher than 600 DEG C, equivalent sphere particle diameter D
50=1 ~ 3 μm, S.S.A=4 ~ 10m
2/ g.
The each constituent mass percentage of described B-Bi-Si-P glass frit is: B
2o
310 ~ 15%, Bi
2o
375 ~ 85%, SiO
25 ~ 15%, P
2o
50 ~ 5%, BaO 0 ~ 5%, inorganic additive 0 ~ 0.5%, each constituent mass percentage sum is 100%.
Described inorganic additive adds in the process of glass dust powder process.
Described inorganic additive is made up of one or more in following material: zinc oxide, di-iron trioxide, iron sulfide, zirconia, cupric oxide, copper sulfide, cuprous sulfide, tungsten oxide, titanium dioxide, molybdenum oxide, rare earth oxide.
The each constituent mass percentage of described organic carrier is: acrylic resin 10 ~ 15%, terpinol 50 ~ 65%, tributyl citrate 15 ~ 20%, alcohol ester 12 ~ 10%, butyl carbitol 5 ~ 8%, rilanit special 0.3 ~ 0.6%, and each constituent mass percentage sum is 100%.
Described organic additive is the high molecular surfactant of a class with special end group, and it is made up of one or more in following material: the long chain alkane of acrylic resin, higher mercaptan, band sulfydryl, the long chain alkane of band hydrosulfamine base.
A kind of vehicle glass hot line conductive copper paste and preparation method thereof, it is characterized in that: preparation process is: (1) by ultra-fine mixed metal powder, glass dust respectively with the organic carrier of corresponding mass ratio and organic additive high-speed stirred even, rolling becomes viscous paste, obtains metal pulp and glass paste respectively; (2) by metal pulp and glass paste mixing, adopt high shear dispersion machine to carry out dispersed with stirring, obtain uniform viscous paste, be finished automotive glass hot line conductive copper paste.
Embodiment
Formula Design and the preparation process of conductive copper paste involved in the present invention will be described in detail below with application example.
Embodiment one
Mixed metal powder chooses preparation according to parameter shown in table 1 and ratio, mixes, for subsequent use.
The specification of table 1 mixed metal powder and proportioning
| Powder type | D50 | S.S.A/ | Mass fraction |
| Blister copper powder | 3.75μm | 0.55m 2/g | 94.5% |
| Thin copper powder | 80nm | 10.0m 2/g | 5% |
| Signal bronze powder | 3.90 | 0.67m 2/g | 0.5% |
Glass dust, according to the ratio precise shown in table 2, mixed 30 mesh sieves, and in 1150 DEG C of constant temperature 15min, shrend, adds the super fine zinc oxide of 0.5%, powder process; Obtaining glass dust specifications parameter is: D50=1.49 μm, S.S.A=6.45m2/g, and the point of incipient sintering is 490 DEG C.
Each component proportion of table 2 glass dust and specification
| Oxide | Bi2O3 | B2O3 | SiO2 | P2O5 | BaO |
| Mass fraction/% | 70 | 15 | 9.5 | 3 | 2.5 |
Organic carrier, according to the ratio precise shown in table 3, mixes, and stirs 2h in 75 DEG C of constant temperature, crosses 80 order stainless steel mesh, obtains the thick liquid clarified.
Table 3 organic carrier formula table
| Component | Acrylic resin | Terpinol | Tributyl citrate | Alcohol ester 12 | Butyl carbitol | Rilanit special |
| Mass fraction/% | 12 | 60 | 16 | 5 | 6.7 | 0.3 |
Wet end furnish is in table 4.
Table 4 conductive copper paste formula
| Component | Mixed metal powder | Glass dust | Organic carrier | Acrylic resin dispersant |
| Mass fraction/% | 85.4 | 5.9 | 8.3 | 0.4 |
The preparation technology of slurry is as follows:
A, by metal mixed powder and glass dust precise respectively, mix 2h with three-dimensional mixer, as solid-state point;
B, by organic carrier and acrylic resin dispersant precise, stir, divide as liquid state;
C, by described in (a) solid-state point respectively and (b) described in liquid state divide mixing, stir 30min with homogenizer, fully mix, obtain two kinds of pastel, be called metal pastel and glass paste thing;
D, by kind of the pastel of two described in (c) respectively cross three-high mill, fineness controlled at 10 ~ 15 μm, viscosity controls at 80 ~ 120Pa.S, obtains bronzing pasty masses, is metal pulp; Linen paste is glass paste;
E, by the high shear dispersion machine high-speed stirred dispersion of the metal pulp described in (d) and glass paste, obtain bronzing pasty masses, be finished product conductive copper paste;
By the finished product conductive copper paste of gained, on the glass substrate, through silk screen printing, obtain bronzing wiring; Under N2 atmosphere protection, at 600 DEG C sinter, obtain the wiring having copper metallic luster of copper red look, after testing its performance reach silver-colored pulp-water put down.Its performance parameter is as table 5.
Table 5 copper slurry wiring performance test results
Embodiment two
Mixed metal powder chooses preparation according to parameter shown in table 6 and ratio, mixes, for subsequent use.
The specification of table 6 mixed metal powder and proportioning
| Powder type | D50 | S.S.A/ | Mass fraction |
| Blister copper powder | 3.87μm | 0.67m 2/g | 93.5% |
| Thin copper powder | 80nm | 9.20m 2/g | 6% |
| Sn-bi alloy powder | 3.67μm | 0.50m 2/g | 0.5% |
Glass dust, according to the ratio precise shown in table 7, mixed 30 mesh sieves, and in 1150 DEG C of constant temperature 15min, shrend, adds the super fine zinc oxide of 0.5%, powder process; Obtaining glass dust specifications parameter is: D50=1.47 μm, S.S.A=6.40m2/g, and the point of incipient sintering is 480 DEG C.
Each component proportion of table 7 glass dust and specification
| Oxide | Bi2O3 | B2O3 | SiO2 | P2O5 | BaO |
| Mass fraction/% | 72 | 13 | 7.5 | 3 | 4.5 |
Organic carrier, according to the ratio precise shown in table 8, mixes, and stirs 2h in 75 DEG C of constant temperature, crosses 80 order stainless steel mesh, obtains the thick liquid clarified.
Table 8 organic carrier formula table
| Component | Acrylic resin | Terpinol | Tributyl citrate | Alcohol ester 12 | Butyl carbitol | Rilanit special |
| Mass fraction/% | 12 | 60 | 16 | 5 | 6.4 | 0.6 |
Wet end furnish is in table 9.
Table 9 conductive copper paste formula
| Component | Mixed metal powder | Glass dust | Organic carrier | Acrylic resin dispersant |
| Mass fraction/% | 82.6 | 7.4 | 10 | 0.4 |
The preparation technology of slurry is identical with blank preparation technics in embodiment one, and size performance parameter is as table 10.
Table 10 copper slurry wiring performance test results
Embodiment three
Mixed metal powder chooses preparation according to parameter shown in table 11 and ratio, mixes, for subsequent use.
The specification of table 6 mixed metal powder and proportioning
| Powder type | D50 | S.S.A/ | Mass fraction |
| Blister copper powder | 2.70μm | 1.07m 2/g | 97.5% |
| Thin copper powder | 100nm | 6.70m 2/g | 2% |
| Sn-bi alloy powder | 3.67μm | 0.50m 2/g | 0.5% |
Glass dust, according to the ratio precise shown in table 12, mixed 30 mesh sieves, and in 1150 DEG C of constant temperature 15min, shrend, adds the copper sulfide of 0.5%, powder process; Obtaining glass dust specifications parameter is: D50=1.45 μm, S.S.A=6.40m
2/ g, the point of incipient sintering is 480 DEG C.
Each component proportion of table 12 glass dust and specification
| Oxide | Bi2O3 | B2O3 | SiO2 | P2O5 | BaO |
| Mass fraction/% | 75 | 15 | 2.5 | 3 | 4.5 |
Organic carrier, according to the ratio precise shown in table 13, mixes, and stirs 2h in 75 DEG C of constant temperature, crosses 80 order stainless steel mesh, obtains the thick liquid clarified.
Table 13 organic carrier formula table
| Component | Acrylic resin | Terpinol | Tributyl citrate | Alcohol ester 12 | Butyl carbitol | Rilanit special |
| Mass fraction/% | 12 | 60 | 16 | 5 | 6.4 | 0.6 |
Wet end furnish is in table 14.
Table 9 conductive copper paste formula
| Component | Mixed metal powder | Glass dust | Organic carrier | Acrylic resin dispersant |
| Mass fraction/% | 82.4 | 7.5 | 10.1 | 0.4 |
The preparation technology of slurry is identical with blank preparation technics in embodiment one, and size performance parameter is as table 15.
Table 15 copper slurry wiring performance test results
Claims (10)
1. a formula for vehicle glass hot line conductive copper paste, is characterized in that: each constituent mass percentage is:
Ultra-fine mixed metal powder 80 ~ 90%, glass dust 4 ~ 9.5%, organic carrier 5.5 ~ 10.5%, organic additive 0.1 ~ 1.0%, each constituent mass percentage sum is 100%.
2. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 1, is characterized in that:
Described ultra-fine mixed metal powder is made up of the raw material of following mass percent: blister copper powder 90 ~ 95%, thin copper powder 5 ~ 10%, low-melting alloy powder 0.5 ~ 2%.
3. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 2, is characterized in that:
Described blister copper powder equivalent sphere particle diameter is D
50=2 ~ 4 μm, S.S.A=0.5 ~ 1.0m
2/ g, thin copper powder equivalent sphere particle diameter is D
50=80 ~ 200nm, S.S.A=6 ~ 15m
2/ g.
4. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 2, is characterized in that:
The fusing point of described low-melting alloy powder is 130 ~ 230 DEG C, and it comprises one or more in signal bronze, sn-bi alloy.
5. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 1, is characterized in that:
Described glass dust is a kind of B-Bi-Si-P glass frit, and its point of incipient sintering is 450 ~ 550 DEG C, obvious melt temperature higher than 600 DEG C, equivalent sphere particle diameter D
50=1 ~ 3 μm, S.S.A=4 ~ 10m
2/ g.
6. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 6, is characterized in that:
The each constituent mass percentage of described B-Bi-Si-P glass frit is: B
2o
310 ~ 15%, Bi
2o
375 ~ 85%, SiO
25 ~ 15%, P
2o
50 ~ 5%, BaO0 ~ 5%, inorganic additive 0 ~ 0.5%, each constituent mass percentage sum is 100%.
7. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 7, is characterized in that:
Described inorganic additive is made up of one or more in following material: zinc oxide, di-iron trioxide, iron sulfide, zirconia, cupric oxide, copper sulfide, cuprous sulfide, tungsten oxide, titanium dioxide, molybdenum oxide, rare earth oxide.
8. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 1, it is characterized in that: each constituent mass percentage of described organic carrier is: acrylic resin 10 ~ 15%, terpinol 50 ~ 65%, tributyl citrate 15 ~ 20%, alcohol ester 12 ~ 10%, butyl carbitol 5 ~ 8%, rilanit special 0.3 ~ 0.6%, each constituent mass percentage sum is 100%.
9. the formula of a kind of vehicle glass hot line conductive copper paste according to claim 1, it is characterized in that: described organic additive is the high molecular surfactant of a class with special end group, and it is made up of one or more in following material: the long chain alkane of acrylic resin, higher mercaptan, band sulfydryl, the long chain alkane of band hydrosulfamine base.
10. the formula of a vehicle glass hot line conductive copper paste and preparation method, it is characterized in that: preparation process is: (1) by ultra-fine mixed metal powder, glass dust respectively with the organic carrier of corresponding mass ratio and organic additive high-speed stirred even, rolling becomes viscous paste, obtains metal pulp and glass paste respectively;
(2) by metal pulp and glass paste mixing, adopt high shear dispersion machine to carry out dispersed with stirring, obtain uniform viscous paste, be finished automotive glass hot line conductive copper paste.
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|---|---|---|---|
| CN201310585286.XA CN104658633A (en) | 2013-11-20 | 2013-11-20 | Formula and preparation method of conductive copper paste for automotive glass heater wire |
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|---|---|---|---|
| CN201310585286.XA CN104658633A (en) | 2013-11-20 | 2013-11-20 | Formula and preparation method of conductive copper paste for automotive glass heater wire |
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Cited By (3)
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| CN107056282A (en) * | 2016-12-22 | 2017-08-18 | 广东风华高新科技股份有限公司 | The preparation method of yttrium stable zirconium oxide slurry, its preparation method and yttrium stable zirconium oxide base substrate |
| CN109785991A (en) * | 2017-11-10 | 2019-05-21 | 上海宝银电子材料有限公司 | A kind of anti-oxidant silver paste of car windshield and preparation method thereof |
| CN110428926A (en) * | 2019-08-07 | 2019-11-08 | 东南大学 | Copper-based composite conducting slurry, preparation method and applications |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056282A (en) * | 2016-12-22 | 2017-08-18 | 广东风华高新科技股份有限公司 | The preparation method of yttrium stable zirconium oxide slurry, its preparation method and yttrium stable zirconium oxide base substrate |
| CN107056282B (en) * | 2016-12-22 | 2020-05-12 | 广东风华高新科技股份有限公司 | Yttrium-stabilized zirconia slurry, preparation method thereof and preparation method of yttrium-stabilized zirconia blank |
| CN109785991A (en) * | 2017-11-10 | 2019-05-21 | 上海宝银电子材料有限公司 | A kind of anti-oxidant silver paste of car windshield and preparation method thereof |
| CN109785991B (en) * | 2017-11-10 | 2020-07-31 | 上海宝银电子材料有限公司 | Antioxidant silver paste for front windshield of passenger car and preparation method thereof |
| CN110428926A (en) * | 2019-08-07 | 2019-11-08 | 东南大学 | Copper-based composite conducting slurry, preparation method and applications |
| CN110428926B (en) * | 2019-08-07 | 2020-10-02 | 东南大学 | Copper-based composite conductive slurry, preparation method and application thereof |
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Address after: No. 8 and Simpson science and Technology Park in Hunan province Zhuzhou City Jinlong Road 412007 Tianyuan District 2. Applicant after: HUNAN LEED THICK FILM PASTE CO., LTD. Address before: 412007 Hunan Province, Zhuzhou city Tianyuan district the Yellow River Road No. 78 Leadbeater Industrial Park Applicant before: Hunan Leed Thick Film Paste Co., Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: HUNAN LEED THICK FILM PASTE CO., LTD. TO: HUNAN LEED ELECTRONIC INK CO., LTD. |
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Application publication date: 20150527 |
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