CN105469856B - A kind of low temperature thick film circuit slurry and preparation method thereof - Google Patents
A kind of low temperature thick film circuit slurry and preparation method thereof Download PDFInfo
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- CN105469856B CN105469856B CN201510980658.8A CN201510980658A CN105469856B CN 105469856 B CN105469856 B CN 105469856B CN 201510980658 A CN201510980658 A CN 201510980658A CN 105469856 B CN105469856 B CN 105469856B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses a kind of low temperature thick film circuit slurry and preparation method thereof, the low temperature thick film circuit slurry includes that mass parts are 1% 5% inorganic adhesive phases, 10% 30% organic solvent carriers, 65% 85% high-purity silver powder；Inorganic adhesive mutually includes that mass parts are 40% 60%Bi2O3、20%‑40%B2O3、15%‑20%ZnO、0.5%‑2.5%CuO；Organic solvent carriers include that mass parts are 85% 90% main solvents, 5% 10% thickeners, 1% 5% levelling agents, 0.5% 1.5% thixotropic agent, 0.5% 1% defoamers；Low temperature thick film circuit slurry sintering temperature is low, sintering time is short, resistance value is low, adhesive force is good for this, solderability is good.The processing step of the preparation method is followed successively by：Prepare inorganic adhesive phase, prepare organic solvent carriers, the preparation of low temperature thick film circuit slurry；The preparation method can effectively prepare warm thick film circuit slurry.
Description
Technical field
The present invention relates to technical field of electronic materials, more particularly to a kind of low temperature thick film circuit slurry and preparation method thereof.
Background technology
Circuit slurry be manufacture thick film element basic material, be one kind by solid powder and organic solvent by three rollings
The well mixed paste of system（Can association into appearance such as toothpaste, paint）；Wherein, according to the difference of purposes, circuit slurry can be with
It is divided into dielectric paste, resistance slurry and conductor paste：According to the difference of substrate species, circuit slurry can be divided into ceramic base again
Piece, polymer matrix film, glass substrate, metal-insulator chip circuit slurry etc.；According to the difference of sintering temperature, circuit slurry again may be used
Be divided into high temperature, in gentle low temperature drying circuit slurry；According to the difference of purposes, circuit slurry can be divided into universal circuit slurry again
Material（Make general thick film circuit）With special circuit slurry（Stainless steel substrate circuit slurry, Thermistor）；According to
The price of conductive phase is different, and circuit slurry can be divided into noble metal circuit slurry again（Silver-colored palladium, ruthenium system and gold paste etc.）And base metal
Circuit slurry（Molybdenum manganese slurry）.
There are circuit slurry products miscellaneous in the prior art；However, for existing circuit slurry products,
It is difficult to be provided simultaneously with the combination property that sintering temperature is low, sintering time is short, resistance value is low, adhesive force is good, solderability is good.
The content of the invention
The purpose of the present invention is to solve the shortcomings of the prior art and a kind of low temperature thick film circuit slurry is provided, the low temperature is thick
Film circuit slurry sintering temperature is low, sintering time is short, resistance value is low, adhesive force is good, solderability is good.
Another object of the present invention is to provide a kind of low temperature thick film circuit slurry preparation method, low temperature thick film circuit slurry
Preparation method for material can effectively prepare low temperature thick film circuit slurry, and the low temperature thick film circuit slurry sintering temperature being prepared from
Low, sintering time is short, resistance value is low, adhesive force is good, solderability is good.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 1%-5%
Organic solvent carriers 10%-30%
High-purity silver powder 65%-85%；
Wherein, inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 40%-60%
B2O3 20%-40%
ZnO 15%-20%
CuO 0.5%-2.5%；
Organic solvent carriers include the material of following mass parts, specially：
Main solvent 85%-90%
Thickener 5%-10%
Levelling agent 1%-5%
Thixotropic agent 0.5%-1.5%
Defoamer 0.5%-1%；
Wherein, the main solvent in organic solvent carriers is butyl carbitol, dimethyl adipate or triethylene glycol oxalic acid
Ester.
Wherein, the inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 40%-50%
B2O3 30%-40%
ZnO 15%-20%
CuO 1%-2 %。
Wherein, the inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 50%
B2O3 30%
ZnO 18%
CuO 2 %。
Wherein, the organic solvent carriers include the material of following mass parts, specially：
Main solvent 90%
Thickener 7%
Levelling agent 1%
Thixotropic agent 1%
Defoamer 1%.
Wherein, a kind of low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 3%-5%
Organic solvent carriers 15%-25%
High-purity silver powder 70%-80%.
Wherein, a kind of low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 4%
Organic solvent carriers 20%
High-purity silver powder 76%.
Wherein, the thickener is polyacrylamide or polyvinyl alcohol, and the levelling agent is fluorin modified crylic acid acid stream
Flat agent or P Modification acrylic acid levelling agent, the thixotropic agent are polyamide wax or hydrophobic silica, the defoamer
It is organic silicon modified by polyether or DOW CORNING 1510-US organosilicons.
A kind of low temperature thick film circuit slurry preparation method, includes following processing step, specially：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3, ZnO, CuO be placed in star-like ball mill grinding and obtain glass in 5-8 hours
Glass micro mist, Bi2O3、B2O3, tetra- kinds of materials of ZnO, CuO mass parts be followed successively by：40%-60%、20%-40%、15%-20%、0.5%-
2.5%；
B, prepare organic solvent carriers：By main solvent, thickener, levelling agent, thixotropic agent, defoamer in 30 DEG C -60 DEG C
Water-bath, to obtain the organic solvent carriers that viscosity is 32 dPas -50dPas, main solvent, thickener, levelling agent, thixotroping
Agent, the mass parts of five kinds of materials of defoamer are followed successively by 85%-90%, 5%-10%, 1%-5%, 0.5%-1.5%, 0.5%-1%；
It is prepared by c, low temperature thick film circuit slurry：Inorganic adhesive phase, organic solvent carriers, high-purity silver powder are mixed and is placed in three rollers
Grinder grinds 5-10 times, to obtain the low temperature thick film circuit slurry that viscosity is the dPa s of 200 dPa s- 400, inorganic adhesive
Phase, organic solvent carriers, the mass parts of three kinds of materials of high-purity silver powder are followed successively by 1%-5%, 10%-30%, 65%-85%.
Wherein, the inorganic adhesive phase, the organic solvent carriers, the granularity of high-purity silver powder are respectively smaller than 2 μm.
Beneficial effects of the present invention are：A kind of low temperature thick film circuit slurry of the present invention, it includes following quality
The material of part, specially：Inorganic adhesive phase 1%-5%, organic solvent carriers 10%-30%, high-purity silver powder 65%-85%；Inorganic adhesive
Mutually include the material of following mass parts：Bi2O340%-60%、B2O320%-40%、ZnO15%-20%、CuO0.5%-2.5%；It is organic
Solvent carrier includes the material of following mass parts：Main solvent 85%-90%, thickener 5%-10%, levelling agent 1%-5%, thixotropic agent
0.5%-1.5%, defoamer 0.5%-1%；Wherein, the main solvent in organic solvent carriers is butyl carbitol, dimethyl adipate
Or triethylene-glycol diacetate.By above-mentioned material proportion, low temperature thick film circuit slurry of the invention have sintering temperature it is low, burn
The advantage that the knot time is short, resistance value is low, adhesive force good, solderability is good.
It is of the invention another to have the beneficial effect that：A kind of low temperature thick film circuit slurry preparation method of the present invention, its bag
Following processing step is included, specially：A, prepare inorganic adhesive phase：By Bi2O3、B2O3, ZnO, CuO be placed in star-like ball mill
Grinding obtains glass micro mist, Bi in 5-8 hours2O3、B2O3, tetra- kinds of materials of ZnO, CuO mass parts be followed successively by：40%-60%、20%-
40%、15%-20%、0.5%-2.5%；B, prepare organic solvent carriers：By main solvent, thickener, levelling agent, thixotropic agent, defoamer
In 30 DEG C -60 DEG C of water-bath, to obtain the organic solvent carriers that viscosity is 32 dPas -50dPas, main solvent, thickening
Agent, levelling agent, thixotropic agent, the mass parts of five kinds of materials of defoamer be followed successively by 85%-90%, 5%-10%, 1%-5%, 0.5%-1.5%,
0.5%-1%；It is prepared by c, low temperature thick film circuit slurry：Inorganic adhesive phase, organic solvent carriers, high-purity silver powder are mixed and is placed in three rollers
Grinder grinds 5-10 times, to obtain the low temperature thick film circuit slurry that viscosity is the dPa s of 200 dPa s- 400, inorganic adhesive
Phase, organic solvent carriers, the mass parts of three kinds of materials of high-purity silver powder are followed successively by 1%-5%, 10%-30%, 65%-85%.By above-mentioned
Processing step, low temperature thick film circuit slurry preparation method of the invention can effectively prepare warm thick film circuit slurry, and prepare
Warm thick film circuit slurry sintering temperature it is low, sintering time is short, resistance value is low, adhesive force is good, solderability is good.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
A kind of embodiment one, low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 4%
Organic solvent carriers 20%
High-purity silver powder 76%；
Wherein, inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 50%
B2O3 30%
ZnO 18%
CuO 2%；
Organic solvent carriers include the material of following mass parts, specially：
Main solvent 90%
Thickener 7%
Levelling agent 1%
Thixotropic agent 1%
Defoamer 1%；
Wherein, the main solvent in organic solvent carriers is butyl carbitol, dimethyl adipate or triethylene glycol oxalic acid
Ester, thickener is polyacrylamide or polyvinyl alcohol, and levelling agent is fluorin modified crylic acid acid levelling agent or P Modification propylene
Sour levelling agent, thixotropic agent is polyamide wax or hydrophobic silica, and defoamer is organic silicon modified by polyether or DOW CORNING
1510-US organosilicons.
By above-mentioned material proportion, the low temperature thick film circuit slurry of the present embodiment one has that sintering temperature is low, sintering time
The advantage that short, resistance value is low, adhesive force is good, solderability is good；Wherein, at 380 DEG C -500 DEG C, sintering time is 10 for sintering temperature
Min -30min, specific insulation is in 0.1-2 × 10-5Ω .cm, adhesive force is good, and hardness can reach more than 6H, silver surface shaping
Uniform and smooth complete and easily adhere to tin layers, weldability is good and is not likely to produce the defects such as crackle, stomata.
A kind of embodiment two, low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 5%
Organic solvent carriers 10%
High-purity silver powder 85%；
Wherein, inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 40%
B2O3 40%
ZnO 18%
CuO 2%；
Organic solvent carriers include the material of following mass parts, specially：
Main solvent 85%
Thickener 10%
Levelling agent 4%
Thixotropic agent 0.5%
Defoamer 0.5%；
Wherein, the main solvent in organic solvent carriers is butyl carbitol, dimethyl adipate or triethylene glycol oxalic acid
Ester, thickener is polyacrylamide or polyvinyl alcohol, and levelling agent is fluorin modified crylic acid acid levelling agent or P Modification propylene
Sour levelling agent, thixotropic agent is polyamide wax or hydrophobic silica, and defoamer is organic silicon modified by polyether or DOW CORNING
1510-US organosilicons.
By above-mentioned material proportion, the low temperature thick film circuit slurry of the present embodiment two has that sintering temperature is low, sintering time
The advantage that short, resistance value is low, adhesive force is good, solderability is good；Wherein, at 380 DEG C -500 DEG C, sintering time is 10 for sintering temperature
Min -30min, specific insulation is in 0.1-2 × 10-5Ω .cm, adhesive force is good, and hardness can reach more than 6H, silver surface shaping
Uniform and smooth complete and easily adhere to tin layers, weldability is good and is not likely to produce the defects such as crackle, stomata.
A kind of embodiment three, low temperature thick film circuit slurry, includes the material of following mass parts, specially：
Inorganic adhesive phase 5%
Organic solvent carriers 30%
High-purity silver powder 65%；
Wherein, inorganic adhesive mutually includes the material of following mass parts, specially：
Bi2O3 60%
B2O3 20%
ZnO 19%
CuO 1%；
Organic solvent carriers include the material of following mass parts, specially：
Main solvent 90%
Thickener 7%
Levelling agent 1%
Thixotropic agent 1%
Defoamer 1%；
Wherein, the main solvent in organic solvent carriers is butyl carbitol, dimethyl adipate or triethylene glycol oxalic acid
Ester, thickener is polyacrylamide or polyvinyl alcohol, and levelling agent is fluorin modified crylic acid acid levelling agent or P Modification propylene
Sour levelling agent, thixotropic agent is polyamide wax or hydrophobic silica, and defoamer is organic silicon modified by polyether or DOW CORNING
1510-US organosilicons.
By above-mentioned material proportion, the low temperature thick film circuit slurry of the present embodiment three has that sintering temperature is low, sintering time
The advantage that short, resistance value is low, adhesive force is good, solderability is good；Wherein, at 380 DEG C -500 DEG C, sintering time is 10 for sintering temperature
Min -30min, specific insulation is in 0.1-2 × 10-5Ω .cm, adhesive force is good, and hardness can reach more than 6H, silver surface shaping
Uniform and smooth complete and easily adhere to tin layers, weldability is good and is not likely to produce the defects such as crackle, stomata.
A kind of example IV, low temperature thick film circuit slurry preparation method, includes following processing step, specially：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3, ZnO, CuO be placed in star-like ball mill grinding and obtain glass in 5-8 hours
Glass micro mist, Bi2O3、B2O3, tetra- kinds of materials of ZnO, CuO mass parts be followed successively by：50%、30%、18%、2%；
B, prepare organic solvent carriers：By main solvent, thickener, levelling agent, thixotropic agent, defoamer in 30 DEG C -60 DEG C
Water-bath, to obtain the organic solvent carriers that viscosity is 32 dPas -50dPas, main solvent, thickener, levelling agent, thixotroping
Agent, the mass parts of five kinds of materials of defoamer are followed successively by 90%, 7%, 1%, 1%, 1%；
It is prepared by c, low temperature thick film circuit slurry：Inorganic adhesive phase, organic solvent carriers, high-purity silver powder are mixed and is placed in three rollers
Grinder grinds 5-10 times, to obtain the low temperature thick film circuit slurry that viscosity is the dPa s of 200 dPa s- 400, inorganic adhesive
Phase, organic solvent carriers, the mass parts of three kinds of materials of high-purity silver powder are followed successively by 4%, 20%, 76%.
Wherein, inorganic adhesive phase, organic solvent carriers, the granularity of high-purity silver powder are respectively smaller than 2 μm.
By above-mentioned processing step, the low temperature thick film circuit slurry preparation method of the present embodiment four can effectively prepare temperature
Thick film circuit slurry, and the warm thick film circuit slurry sintering temperature being prepared from is low, sintering time is short, resistance value is low, adhesive force
Good, solderability is good.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to of the invention
Thought, will change in specific embodiments and applications, and this specification content should not be construed as to the present invention
Limitation.
Claims (1)
1. a kind of low temperature thick film circuit slurry preparation method, it is characterised in that include following processing step, specially：
A, prepare inorganic adhesive phase：By Bi2O3、B2O3, ZnO, CuO be placed in star-like ball mill grinding to obtain glass within 5-8 hours micro-
Powder, Bi2O3、B2O3, tetra- kinds of materials of ZnO, CuO mass parts be followed successively by：40%-60%、20%-40%、15%-20%、0.5%-2.5%；
B, prepare organic solvent carriers：By main solvent, thickener, levelling agent, thixotropic agent, defoamer in 30 DEG C -60 DEG C of water-bath,
To obtain the organic solvent carriers that viscosity is 32 dPas -50dPas, main solvent, thickener, levelling agent, thixotropic agent, disappear
The mass parts of five kinds of materials of infusion are followed successively by 85%-90%, 5%-10%, 1%-5%, 0.5%-1.5%, 0.5%-1%；
It is prepared by c, low temperature thick film circuit slurry：Inorganic adhesive phase, organic solvent carriers, high-purity silver powder are mixed and is placed in the grinding of three rollers
Machine grinds 5-10 times, to obtain the low temperature thick film circuit slurry that viscosity is the dPa s of 200 dPa s- 400, inorganic adhesive phase, has
Machine solvent carrier, the mass parts of three kinds of materials of high-purity silver powder are followed successively by 1%-5%, 10%-30%, 65%-85%.
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| CN105810291A (en) * | 2016-04-07 | 2016-07-27 | 东莞珂洛赫慕电子材料科技有限公司 | Rare-earth resistance paste of medium- and low-resistance high-power thick film circuit and preparation method of rare-earth resistance paste |
| CN105869706A (en) * | 2016-05-11 | 2016-08-17 | 东莞珂洛赫慕电子材料科技有限公司 | Low-temperature sintering thick film paste applied to PI films and preparation method of low-temperature sintering thick film paste |
| CN105873248B (en) * | 2016-05-11 | 2019-06-07 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of heating film low-temperature sintering slurry and preparation method thereof |
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| CN106252272B (en) * | 2016-10-13 | 2019-01-15 | 珠海市华晶微电子有限公司 | The connecting process of laminate patch multilayer thick film circuit |
| CN107068238A (en) * | 2016-12-09 | 2017-08-18 | 东莞珂洛赫慕电子材料科技有限公司 | A kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature and preparation method thereof |
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| KR100613406B1 (en) * | 2004-01-17 | 2006-08-17 | 한국과학기술연구원 | Composite ceramics having matched shrinkage |
| CN101377966B (en) * | 2008-09-27 | 2012-05-09 | 彩虹集团公司 | Method for preparing leadless silver electrode slurry for glass substrates |
| CN102010127A (en) * | 2009-09-07 | 2011-04-13 | 上海歌灵新材料科技有限公司 | Lead-free solder glass |
| CN101728439B (en) * | 2009-12-01 | 2011-07-20 | 洛阳神佳电子陶瓷有限公司 | Aluminum pulp composition of crystal silicon solar cell and preparation method thereof |
| CN102136308B (en) * | 2010-11-23 | 2012-11-14 | 湖南威能新材料科技有限公司 | Organic carrier for silver paste and preparation method thereof as well as silver paste containing organic carrier and solar cell manufactured from silver paste |
| CN102629496B (en) * | 2012-04-27 | 2015-02-18 | 西安银泰新能源材料科技有限公司 | Crystalline silicon solar battery front side electrode lead-free conductive lead slurry and preparation method of crystalline silicon solar battery front side electrode lead-free conductive lead slurry |
| CN103258584B (en) * | 2013-01-09 | 2018-04-10 | 深圳市创智材料科技有限公司 | A kind of conductive silver paste and preparation method thereof |
| CN104425053A (en) * | 2013-09-06 | 2015-03-18 | 湖南利德电子浆料有限公司 | Resistance slurry used for thick film circuit and based on ceramic tile and preparation process thereof |
| CN104021842B (en) * | 2014-06-25 | 2016-09-28 | 西安工程大学 | A kind of Graphene complex copper thick film conductor paste and preparation method thereof |
| CN104966761B (en) * | 2015-07-08 | 2017-04-05 | 四川银河星源科技有限公司 | A kind of manufacture method of crystal silicon solar energy battery |
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