CN107068238A - A kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature and preparation method thereof - Google Patents
A kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature and preparation method thereof Download PDFInfo
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- CN107068238A CN107068238A CN201611128842.0A CN201611128842A CN107068238A CN 107068238 A CN107068238 A CN 107068238A CN 201611128842 A CN201611128842 A CN 201611128842A CN 107068238 A CN107068238 A CN 107068238A
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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
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
- H01B1/16—Conductive material dispersed in non-conductive inorganic 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
Abstract
The invention discloses a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature and preparation method thereof, the electrode slurry includes inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier, and inorganic bond is by Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, seven kinds of material compositions of rare earth oxide, organic carrier are made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent.The electrode slurry preparation method is comprised the following steps that:A, inorganic bond are mutually prepared;It is prepared by b, organic carrier;C, prepare electrode slurry.The electrode slurry has good thixotropy, mobility and sintering temperature is low, electrode layer after burning till has the advantages that structure is smooth, fine and close, not ftractureed, pin-free, bubble-free, leadless environment-friendly, while the electrode layer after burning till has the advantages that adhesive force is strong, ageing-resistant, sheet resistance is low, printing characteristic and burn till characteristic good.
Description
Technical field
The present invention relates to thick film circuit technique field, more particularly to a kind of aluminium alloy base plate are complete with thick film circuit intermediate sintering temperature
Silver electrode paste and preparation method thereof.
Background technology
As thick film circuit element is to multiple stratification and the development of miniaturization, corresponding mechanics and thermal property are proposed to substrate
It is required that, the particularly thermal conductivity requirement of substrate;Although BeO, Al2O3, the ceramic substrate such as AlN there is higher thermal conductivity factor, but
BeO substrates are limited because of its toxicity and used, Al2O3With AlN substrate because mechanical performance is poor, assembling is difficult and applies limited.Aluminium is closed
The property such as density that gold base has is small, the cold and hot working processability that ductility is good, thermal conductivity is good, excellent and good toughness
It can make it possible to as baseplate material use;However, due to the thermal coefficient of expansion height of aluminium alloy base plate, while fusing point is low(It is small
In 660 DEG C), therefore high-temperature standard firing process can not be selected(850℃);So, it is desirable to corresponding electric slurry can only be low
In sintering under the fusion temperature of aluminium alloy, and there are good adhesive force, matching, screen printing property so that aluminium base electronics is starched
The development of material becomes extremely difficult.
At present, applied to aluminium alloy base plate thick film circuit electric heating element, especially specialty are used for aluminium alloy base plate system
Electrode slurry, the country report it is less;Wherein, Patent No.:201110118644.7, patent name be:High temperature aluminium alloys base
The Chinese invention patent of rare earth thick film circuit electric heating element and its technology of preparing is thick it discloses a kind of high temperature aluminium alloys base rare earth
Film circuit electric heating element and its technology of preparing, the rare earth electrode slurry are by microcrystalline glass powder, silver-colored aluminium yttrium composite powder and organic
Carrier is constituted, and film forming is sintered after 500 ~ 700 DEG C through silk-screen printing;In addition, patent is well:201310737978.1, proprietary term
Referred to as:The Chinese invention patent of the preparation technology of aluminum bronze Cu+ composite base rare earth thick film circuit intelligent electric-heating chips, it discloses aluminium
The preparation technology of copper Cu+ composite base rare earth thick film circuit intelligent electric-heating chips, and including antibacterial copper Cu+ aluminum composite metals substrate and
The rare earth thick film circuit prepared thereon, the rare earth electrode slurry is made up of silver-colored palladium yttrium composite powder, microcrystalline glass powder and organic carrier,
Through silk-screen printing film forming is sintered after 450 ~ 650 DEG C.
The content of the invention
It is an object of the invention to provide a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, the aluminium
The full silver electrode paste of alloy substrate thick film circuit intermediate sintering temperature has good thixotropy, mobility, and sintering temperature is low and burns
Electrode layer after has the advantages that structure is smooth, fine and close, not ftractureed, pin-free, bubble-free, leadless environment-friendly, while after burning till
Electrode layer have the advantages that adhesive force is strong, ageing-resistant, sheet resistance is low, printing characteristic and burn till characteristic good, and can be well
Match with insulating barrier and the resistance slurry layer of aluminum alloy base material.
Another object of the present invention is to provide a kind of full silver electrode paste of aluminium alloy base plate thick film circuit intermediate sintering temperature
Preparation method, the electrode slurry preparation method, which can be produced effectively, to be prepared the middle temperature of above-mentioned aluminium alloy base plate thick film circuit and burns
Tie full silver electrode paste.
To reach above-mentioned purpose, the present invention is achieved through the following technical solutions.
A kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, includes the material of following parts by weight,
Specially:
Inorganic adhesive phase 1% ~ 5%
Spherical silver powder 35% ~ 40%
Flake silver powder 35% ~ 40%
Organic carrier 20% ~ 25%;
It is preferred that, inorganic bond is mutually by Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, seven kinds of material institute groups of rare earth oxide
Into microcrystalline glass powder, Bi in inorganic adhesive phase2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, the weight of seven kinds of materials of rare earth oxide
Amount part is followed successively by 50% ~ 60%, 15% ~ 25%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%, 1% ~ 5%, 1% ~ 5%;
The mixing that organic carrier is made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent
Organic solvent, macromolecule thickener, dispersant, defoamer, the parts by weight of five kinds of materials of thixotropic agent are followed successively by thing, organic carrier
50%~70%、20%~35%、1%~5%、1%~5%、1%~5%。
It is preferred that, the Nucleating Agent is CaF2、TiO2、ZrO2、P2O5、Sb2O3、V2O5、NiO、Fe2O3In one kind or extremely
Lack two kinds of mixtures constituted.
It is preferred that, the particle size values of the microcrystalline glass powder are 1 μm ~ 3 μm, and softening point is 300 ~ 400 DEG C, average line expansion system
Number is 15 ~ 25 × 10-6/℃。
It is preferred that, the rare earth oxide is La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3
In a kind of or at least two mixtures constituted.
It is preferred that, the particle size values of the spherical silver powder are 1 μm ~ 3 μm, and apparent density is 1.5 ~ 2.5 g/cm3, tap density
For 3.0 ~ 4.0 g/cm3, specific surface area is 0.5 ~ 2.0m2/g;The particle size values of the flake silver powder are 1 μm ~ 3 μm, and apparent density is
1.5~2.0g/cm3, tap density is 3.0 ~ 3.5 g/cm3, specific surface area is 0. 4 ~ 1. 2m2/g。
It is preferred that, the organic solvent is turpentine oil, terpinol, butyl carbitol, butyl carbitol acetate, diethyl two
Alcohol monomethyl ether, dibutyl ethylene glycol ether, ethylene glycol ether acetate, dibutyl phthalate, ATBC, tricresyl phosphate
Butyl ester, Isosorbide-5-Nitrae ~ butyrolactone, mixed dibasic acid ester, N ~ methyl pyrrolidone, N, N ~ dimethylformamide, N, N ~ dimethylacetamide
A kind of or at least two mixtures constituted in amine, dimethyl sulfoxide.
It is preferred that, the macromolecule thickener is ethyl cellulose, NC Nitroncellulose, polyethylene glycol 2000, polyvinyl alcohol
Butyral, polyvinylpyrrolidone, polyvinyl acetate, hydrogenated rosin resin, acrylate, epoxy resin, polyurethane
A kind of or at least two mixtures constituted in resin.
It is preferred that, the dispersant is one in triammonium citrate, polymethyl acid amide, Isosorbide-5-Nitrae ~ dihydroxy sulfanilic acid
Plant or at least two mixtures constituted;The defoamer is organosiloxane, polyethers, polyethylene glycol, ethene ~ acrylic acid
One kind or at least two in copolymer, polyglyceryl fatty acid ester, dimethyl silicone polymer, organic silicon modified by polyether are constituted
Mixture.
It is preferred that, the thixotropic agent is hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organic swelling
A kind of or at least two mixtures constituted in soil or aerosil.
A kind of preparation method of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, includes following technique
Step, be specially:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, rare earth oxide are in three-dimensional material mixer
It is well mixed, Bi in mixture2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, the parts by weight of seven kinds of materials of rare earth oxide are followed successively by
50%~60%、15%~25%、10%~20%、5%~10%、5%~10%、1%~5%、1%~5%;Treat Bi2O3、B2O3、CaO、ZnO、K2O, nucleus
After agent, rare earth oxide are well mixed, then by Bi2O3、B2O3、CaO、ZnO、K2It is mixed that O, Nucleating Agent, rare earth oxide are constituted
Compound is placed in progress melting processing in smelting furnace, and smelting temperature is 1200 ~ 1400 DEG C, and soaking time is 2 ~ 4 hours, to obtain glass
Liquation;Glass melts are then subjected to Water Quenching, to obtain glass dregs, ball finally is carried out to glass dregs by medium of distilled water
Mill processing, the ball-milling treatment time is 4 ~ 6 hours, to obtain particle size values as 1 μm ~ 3 μm of leadless crystallizing glass powder;
B, prepare organic carrier:By organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent in 80 DEG C of water bath conditions
It is lower to be dissolved, to obtain organic carrier, and by adjusting the content of macromolecule thickener so that the viscosity of organic carrier is controlled
In the range of the mPas of 200 mPas ~ 300, then organic carrier is filtered by 200 mesh nylon leaching nets to go again
The removal of impurity;Wherein, organic solvent, macromolecule thickener, dispersant, defoamer, the weight of five kinds of materials of thixotropic agent in organic carrier
Amount part is followed successively by 50% ~ 70%, 20% ~ 35%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%;
It is prepared by c, electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, and
After be placed in three-roll grinder and grind repeatedly, to obtain the full silver that range of viscosities is less than 5 μm as 80 ~ 150Pas, average fineness
Electrode slurry, then carries out filtration treatment to go the removal of impurity by the nylon leaching net of 500 mesh to electrode slurry again;Wherein, electrode
In slurry inorganic adhesive phase, spherical silver powder, flake silver powder, the parts by weight of four kinds of materials of organic carrier be followed successively by 1% ~ 5%, 35% ~
40%、35%~40%、20%~25%。
Beneficial effects of the present invention are:A kind of aluminium alloy base plate of the present invention full silver electricity of thick film circuit intermediate sintering temperature
Pole slurry, it includes the material of following parts by weight:Inorganic adhesive phase 1% ~ 5%, spherical silver powder 35% ~ 40%, flake silver powder 35% ~
40%th, organic carrier 20% ~ 25%;Inorganic bond is mutually by Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, seven kinds of rare earth oxide
Bi in the microcrystalline glass powder that material is constituted, inorganic adhesive phase2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, seven kinds of rare earth oxide
The parts by weight of material are followed successively by 50% ~ 60%, 15% ~ 25%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%, 1% ~ 5%, 1% ~ 5%;Organic carrier
In the mixture being made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent, organic carrier
Organic solvent, macromolecule thickener, dispersant, defoamer, the parts by weight of five kinds of materials of thixotropic agent are followed successively by 50% ~ 70%, 20% ~
35%、1%~5%、1%~5%、1%~5%.By above-mentioned material proportion, aluminium alloy base plate of the invention is complete with thick film circuit intermediate sintering temperature
Silver electrode paste has advantages below, is specially:
1st, from Bi2O3-B2O3- CaO-ZnO be unleaded, low softening point microcrystalline glass powder as Binder Phase, by Bi2O3-
B2O3The thermal coefficient of expansion of-CaO-ZnO microcrystalline glass in series powder, glass transition temperature, the regulation of softening temperature are allowed to and rare-earth oxidation
The thermal coefficient of expansion and aluminium base of the compound thick membrane electrode track layer constituted of thing, spherical silver powder, flake silver powder, organic carrier insulate
Layer, aluminium base resistance slurry match and with good binding ability, while electrode layer can be made to be burnt between 450 ~ 550 DEG C
Knot, it is to avoid lead is researching and developing, the injury that uses and caused after discarded to environment, human body, can solve high-power electrode or electric heating
Element manufacturing urgent problem, meets RoHS Directive(2002/95/EC)It is required that;
2nd, the addition of rare earth oxide, can not only reduce the cost of microcrystalline glass powder and improve the comprehensive utilization effect of rare earth resources
Benefit, can also reduce Bi2O3-B2O3The glass transition temperature of-CaO-ZnO microcrystalline glass in series powder, softening temperature, while improving its heat
The coefficient of expansion, makes it preferably relatively low with fusing point(660℃), thermal coefficient of expansion(23×10-6/℃)Very high aluminium alloy base plate phase
Matching;
3rd, spherical silver powder is used as complex function phase, the conduction of continuity and electronic component to silver layer after sintering with flake silver powder
Performance serves vital, it is therefore desirable to select the metal-powder of good dispersion, wherein spherical silver powder requires specific surface area
For 0.5 ~ 2.0m2/ g, the specific surface area of flake silver powder is 0.4 ~ 1.2m2Why/g, select spherical and flake silver powder combination,
It is, because the space that can effectively fill up between spherical silver powder of flake silver powder, to make that the conductive layer after sintering is relatively compact, ensure element electricity
Gas performance;
4th, the electrode slurry being made using unleaded, low softening point, high thermal expansion coefficient microcrystalline glass powder as one of raw material, itself and aluminium base
Insulating barrier, aluminium base resistance slurry matching performance are good, and with good thixotropy, mobility, the electrode layer after burning till has
Structure is smooth, fine and close, do not ftracture, pin-free, bubble-free, the advantage of leadless environment-friendly, while the film layer after burning till has adhesive force
By force, conduct electricity very well, solderability is good, the good advantage of anti-weldering dissolubility, and its preparation method is simple, process conditions gentle, to equipment
It is required that low, economic and environment-friendly.
The another of the present invention has the beneficial effect that:A kind of aluminium alloy base plate of the present invention is complete with thick film circuit intermediate sintering temperature
The preparation method of silver electrode paste, it includes following processing step:A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、
ZnO、K2O, Nucleating Agent, rare earth oxide are well mixed in three-dimensional material mixer, Bi in mixture2O3、B2O3、CaO、ZnO、K2O、
Nucleating Agent, the parts by weight of seven kinds of materials of rare earth oxide are followed successively by 50% ~ 60%, 15% ~ 25%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%,
1%~5%、1%~5%;Treat Bi2O3、B2O3、CaO、ZnO、K2After O, Nucleating Agent, rare earth oxide are well mixed, then by Bi2O3、B2O3、
CaO、ZnO、K2The mixture that O, Nucleating Agent, rare earth oxide are constituted is placed in progress melting processing in smelting furnace, and smelting temperature is
1200 ~ 1400 DEG C, soaking time is 2 ~ 4 hours, to obtain glass melts;Glass melts are then subjected to Water Quenching, to obtain
Glass dregs are obtained, finally by medium of distilled water glass dregs are carried out with ball-milling treatment, the ball-milling treatment time is 4 ~ 6 hours, to obtain
Particle size values are 1 μm ~ 3 μm of leadless crystallizing glass powder;B, prepare organic carrier:By organic solvent, macromolecule thickener, disperse
Agent, defoamer, thixotropic agent are dissolved under 80 DEG C of water bath conditions, to obtain organic carrier, and are thickened by adjusting macromolecule
The content of agent is so that the viscosity control of organic carrier then passes through 200 mesh again in the range of the mPas of 200 mPas ~ 300
Nylon leaching net is filtered to go the removal of impurity to organic carrier;Wherein, organic solvent in organic carrier, macromolecule thickener, point
Powder, defoamer, the parts by weight of five kinds of materials of thixotropic agent are followed successively by 50% ~ 70%, 20% ~ 35%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%;c、
It is prepared by electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, then it is placed in
Ground repeatedly in three-roll grinder, the full silver electrode for being less than 5 μm as 80 ~ 150Pas, average fineness to obtain range of viscosities is starched
Material, then carries out filtration treatment to go the removal of impurity by the nylon leaching net of 500 mesh to electrode slurry again;Wherein, in electrode slurry
Inorganic adhesive phase, spherical silver powder, flake silver powder, the parts by weight of four kinds of materials of organic carrier are followed successively by 1% ~ 5%, 35% ~ 40%, 35% ~
40%、20%~25%.Designed by above-mentioned processing step, the electrode slurry preparation method, which can be produced effectively, prepares above-mentioned aluminium conjunction
The gold base full silver electrode paste of thick film circuit intermediate sintering temperature.
Embodiment
With reference to specific embodiment, the present invention will be described.
Embodiment 1, a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, by weight percentage,
Including following components:
Inorganic adhesive phase 1%
Spherical silver powder 40%
Flake silver powder 39%
Organic carrier 20%;
The inorganic adhesive phase, by weight percentage, including following components:
Bi2O3 50%
B2O3 25%
CaO 10%
ZnO 5%
K2O 5%
TiO2 2.5%
Y2O32.5%;
The organic carrier, by weight percentage, including following components:
Butyl carbitol acetate 70%
Ethyl cellulose 20%
Triammonium citrate 4%
Organic silicon modified by polyether 3%,
Rilanit special 3%.
A kind of aluminium alloy base plate preparation method of the full silver electrode paste of thick film circuit intermediate sintering temperature, comprises the following steps:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O、TiO2And Y2O3Mixed in three-dimensional material mixer equal
Then at smelting furnace melting after even, smelting temperature is 1250 DEG C, and soaking time is to obtain glass melts in 3 hours, then melts glass
Liquid carries out water quenching and simultaneously obtains glass dregs, finally by medium of distilled water to glass dregs ball milling 6 hours, that is, obtain particle size values be 1 μm ~
3 μm of microcrystalline glass powder;
B, prepare organic carrier:By butyl carbitol acetate, ethyl cellulose, triammonium citrate, organic silicon modified by polyether, hydrogen
Change castor oil to dissolve in 80 DEG C of water bath conditions to obtain organic carrier, then the removal of impurity is gone by 200 mesh nylon leaching nets, there is airborne
The viscosity of body is 200 ± 20 mPas;
C, prepare electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, and
After be placed in three-roll grinder and grind repeatedly, to obtain the thick film that range of viscosities is less than 5 μm as 110 ± 20Pas, average fineness
Electrode slurry, then the filter cloth by 500 mesh or filter screen removal of impurities;It is the all-silver electronic paste good dispersion of gained, superior performance, unleaded
Environmental protection.
Embodiment 2, a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, by weight percentage, including
Following components:
Inorganic adhesive phase 3%
Spherical silver powder 37.5%
Flake silver powder 37.5%
Organic carrier 22%;
The inorganic adhesive phase, by weight percentage, including following components:
Bi2O3 60%
B2O3 15%
CaO 10%
ZnO 5%
K2O 5%
ZrO2 2.5%
La2O32.5%;
The organic carrier, by weight percentage, including following components:
Butyl carbitol acetate 70%
Polyurethane resin 20%
Polymethyl acid amide 4%
Organic silicon modified by polyether 3%
Thixotropy alkyd resin 3%.
A kind of aluminium alloy base plate preparation method of the full silver electrode paste of thick film circuit intermediate sintering temperature, comprises the following steps:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O、ZrO2And La2O3Mixed in three-dimensional material mixer
Then at smelting furnace melting after uniform, smelting temperature is 1300 DEG C, and soaking time is to obtain glass melts in 2 hours, then by glass
Liquation carries out water quenching and simultaneously obtains glass, finally by medium of distilled water to glass ball milling 6 hours, that is, it is 1 μm ~ 3 μ to obtain particle size values
M microcrystalline glass powder;
B, prepare organic carrier:By butyl carbitol acetate, polyurethane resin, polymethyl acid amide, polyether-modified organic
Silicon, thixotropy alkyd resin dissolve to obtain organic carrier in 80 DEG C of water bath conditions, then go removal of impurities by 200 mesh nylon leaching nets
Matter, the viscosity of organic carrier is 200 ± 20 mPas;
C, prepare electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, and
After be placed in three-roll grinder and grind repeatedly, to obtain the thick film that range of viscosities is less than 5 μm as 110 ± 20Pas, average fineness
Electrode slurry, then the filter cloth by 500 mesh or filter screen removal of impurities;It is the all-silver electronic paste good dispersion of gained, superior performance, unleaded
Environmental protection.
Embodiment 3, a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, by weight percentage, including
Following components:
Inorganic adhesive phase 4%
Spherical silver powder 38%
Flake silver powder 38%
Organic carrier 20%;
The inorganic adhesive phase, by weight percentage, including following components:
Bi2O3 55%
B2O3 20%
CaO 10%
ZnO 5%
K2O 5%
TiO2 2.5%
Sm2O32.5%;
The organic carrier, by weight percentage, including following components:
Butyl carbitol acetate 65%
Acrylate 25%
1,4 ~ dihydroxy sulfanilic acid 4%
Dimethyl silicone polymer 3%
Rilanit special 3%.
A kind of aluminium alloy base plate preparation method of the full silver electrode paste of thick film circuit intermediate sintering temperature, comprises the following steps:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O、ZrO2And Sm2O3Mixed in three-dimensional material mixer
Then at smelting furnace melting after uniform, smelting temperature is 1400 DEG C, and soaking time is to obtain glass melts in 2 hours, then by glass
Liquation carries out water quenching and simultaneously obtains glass, finally by medium of distilled water to glass ball milling 6 hours, that is, it is 1 μm ~ 3 μ to obtain particle size values
M microcrystalline glass powder;
B, prepare organic carrier:By butyl carbitol acetate, acrylate, 1,4 ~ dihydroxy sulfanilic acid, poly dimethyl
Siloxanes, rilanit special dissolve to obtain organic carrier in 80 DEG C of water bath conditions, then go removal of impurities by 200 mesh nylon leaching nets
Matter, the viscosity of organic carrier is 200 ± 20 mPas;
C, prepare electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, then
It is placed in three-roll grinder and grinds repeatedly, obtains the thick membrane electrode that range of viscosities is less than 5 μm as 110 ± 20Pas, average fineness
Slurry, then the filter cloth by 500 mesh or filter screen removal of impurities;All-silver electronic paste good dispersion, superior performance, the leadless environment-friendly of gained.
Embodiment 4, a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, by weight percentage, including
Following components:
Inorganic adhesive phase 5%
Spherical silver powder 35%
Flake silver powder 35%
Organic carrier 25%;
The inorganic adhesive phase, by weight percentage, including following components:
Bi2O3 60%
B2O3 15%
CaO 10%
ZnO 5%
K2O 5%
CaF2 2.5%
Eu2O32.5%;
The organic carrier, by weight percentage, including following components:
Ethylene glycol ether acetate 70%
Polyvinyl butyral resin 20%
1,4 ~ dihydroxy sulfanilic acid 5%
Organic silicon modified by polyether 2.5%
Thixotropy alkyd resin 2.5%.
A kind of aluminium alloy base plate preparation method of the full silver electrode paste of thick film circuit intermediate sintering temperature, comprises the following steps:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O、CaF2And Eu2O3Mixed in three-dimensional material mixer
Then at smelting furnace melting after uniform, smelting temperature is 1250 DEG C, and soaking time is to obtain glass melts in 3 hours, then by glass
Liquation carries out water quenching and simultaneously obtains glass, finally by medium of distilled water to glass ball milling 6 hours, that is, it is 1 μm ~ 3 μ to obtain particle size values
M microcrystalline glass powder;
B, prepare organic carrier:Ethylene glycol ether acetate, polyvinyl butyral resin, 1,4 ~ dihydroxy sulfanilic acid, polyethers are changed
Property organosilicon, thixotropy alkyd resin dissolve to obtain organic carrier in 80 DEG C of water bath conditions, then pass through 200 mesh nylon leaching nets
The removal of impurity is gone, the viscosity of organic carrier is 200 ± 20 mPas;
C, prepare electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, and
After be placed in three-roll grinder and grind repeatedly, to obtain the thick film that range of viscosities is less than 5 μm as 110 ± 20Pas, average fineness
Electrode slurry, then the filter screen removal of impurities for passing through 500 mesh.All-silver electronic paste good dispersion, superior performance, the leadless environment-friendly of gained.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's
Thought, will change in specific embodiments and applications, and this specification content should not be construed as to the present invention
Limitation.
Claims (10)
1. a kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature, it is characterised in that include following weight
The material of part, be specially:
Inorganic adhesive phase 1% ~ 5%
Spherical silver powder 35% ~ 40%
Flake silver powder 35% ~ 40%
Organic carrier 20% ~ 25%;
Wherein, inorganic bond is mutually by Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, seven kinds of materials of rare earth oxide are constituted
Bi in microcrystalline glass powder, inorganic adhesive phase2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, the parts by weight of seven kinds of materials of rare earth oxide
It is followed successively by 50% ~ 60%, 15% ~ 25%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%, 1% ~ 5%, 1% ~ 5%;
The mixing that organic carrier is made up of organic solvent, macromolecule thickener, dispersant, defoamer, five kinds of materials of thixotropic agent
Organic solvent, macromolecule thickener, dispersant, defoamer, the parts by weight of five kinds of materials of thixotropic agent are followed successively by thing, organic carrier
50%~70%、20%~35%、1%~5%、1%~5%、1%~5%。
2. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The Nucleating Agent is CaF2、TiO2、ZrO2、P2O5、Sb2O3、V2O5、NiO、Fe2O3In one kind or at least two groups
Into mixture.
3. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The particle size values of the microcrystalline glass powder are 1 μm ~ 3 μm, and softening point is 300 ~ 400 DEG C, and average coefficient of linear expansion is 15 ~ 25
×10-6/℃。
4. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The rare earth oxide is La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3In one kind or
The mixture that person at least two is constituted.
5. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The particle size values of the spherical silver powder are 1 μm ~ 3 μm, and apparent density is 1.5 ~ 2.5 g/cm3, tap density is 3.0 ~ 4.0
g/cm3, specific surface area is 0.5 ~ 2.0m2/g;The particle size values of the flake silver powder are 1 μm ~ 3 μm, and apparent density is 1.5 ~ 2.0g/
cm3, tap density is 3.0 ~ 3.5 g/cm3, specific surface area is 0. 4 ~ 1. 2m2/g。
6. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The organic solvent be turpentine oil, terpinol, butyl carbitol, butyl carbitol acetate, diethylene glycol monomethyl ether,
Dibutyl ethylene glycol ether, ethylene glycol ether acetate, dibutyl phthalate, ATBC, tributyl phosphate, Isosorbide-5-Nitrae ~
Butyrolactone, mixed dibasic acid ester, N ~ methyl pyrrolidone, N, N ~ dimethylformamide, N, N ~ dimethyl acetamide, dimethyl sulfoxide
In a kind of or at least two mixtures constituted.
7. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The macromolecule thickener is ethyl cellulose, NC Nitroncellulose, polyethylene glycol 2000, polyvinyl butyral resin, poly- second
One kind in alkene pyrrolidone, polyvinyl acetate, hydrogenated rosin resin, acrylate, epoxy resin, polyurethane resin
Or at least two mixtures constituted.
8. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The dispersant is triammonium citrate, polymethyl acid amide, one kind in 1,4 ~ dihydroxy sulfanilic acid or at least
Two kinds of mixtures for being constituted;The defoamer is organosiloxane, polyethers, polyethylene glycol, ethene ~ acrylic copolymer, poly-
A kind of or at least two mixtures constituted in fatty acid glyceride, dimethyl silicone polymer, organic silicon modified by polyether.
9. a kind of aluminium alloy base plate according to claim 1 full silver electrode paste of thick film circuit intermediate sintering temperature, its feature
It is:The thixotropic agent is hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organobentonite or gas phase two
A kind of or at least two mixtures constituted in silica.
10. a kind of aluminium alloy base plate preparation method of the full silver electrode paste of thick film circuit intermediate sintering temperature, it is characterised in that including
There is following processing step, be specially:
A, prepare inorganic adhesive phase:By Bi2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, rare earth oxide are mixed in three-dimensional material mixer
Close uniform, Bi in mixture2O3、B2O3、CaO、ZnO、K2O, Nucleating Agent, the parts by weight of seven kinds of materials of rare earth oxide are followed successively by
50%~60%、15%~25%、10%~20%、5%~10%、5%~10%、1%~5%、1%~5%;Treat Bi2O3、B2O3、CaO、ZnO、K2O, nucleus
After agent, rare earth oxide are well mixed, then by Bi2O3、B2O3、CaO、ZnO、K2It is mixed that O, Nucleating Agent, rare earth oxide are constituted
Compound is placed in progress melting processing in smelting furnace, and smelting temperature is 1200 ~ 1400 DEG C, and soaking time is 2 ~ 4 hours, to obtain glass
Liquation;Glass melts are then subjected to Water Quenching, to obtain glass dregs, ball finally is carried out to glass dregs by medium of distilled water
Mill processing, the ball-milling treatment time is 4 ~ 6 hours, to obtain particle size values as 1 μm ~ 3 μm of leadless crystallizing glass powder;
B, prepare organic carrier:By organic solvent, macromolecule thickener, dispersant, defoamer, thixotropic agent in 80 DEG C of water bath conditions
It is lower to be dissolved, to obtain organic carrier, and by adjusting the content of macromolecule thickener so that the viscosity of organic carrier is controlled
In the range of the mPas of 200 mPas ~ 300, then organic carrier is filtered by 200 mesh nylon leaching nets to go again
The removal of impurity;Wherein, organic solvent, macromolecule thickener, dispersant, defoamer, the weight of five kinds of materials of thixotropic agent in organic carrier
Amount part is followed successively by 50% ~ 70%, 20% ~ 35%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%;
It is prepared by c, electrode slurry:By inorganic adhesive phase, spherical silver powder, flake silver powder, organic carrier dispersed with stirring in container, and
After be placed in three-roll grinder and grind repeatedly, to obtain the full silver that range of viscosities is less than 5 μm as 80 ~ 150Pas, average fineness
Electrode slurry, then carries out filtration treatment to go the removal of impurity by the nylon leaching net of 500 mesh to electrode slurry again;Wherein, electrode
In slurry inorganic adhesive phase, spherical silver powder, flake silver powder, the parts by weight of four kinds of materials of organic carrier be followed successively by 1% ~ 5%, 35% ~
40%、35%~40%、20%~25%。
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CN201611128842.0A CN107068238A (en) | 2016-12-09 | 2016-12-09 | A kind of aluminium alloy base plate full silver electrode paste of thick film circuit intermediate sintering temperature and preparation method thereof |
PCT/CN2016/113346 WO2018103164A1 (en) | 2016-12-09 | 2016-12-30 | Medium-temperature sintered all-silver electrode paste for thick film circuit for use in aluminum alloy substrate |
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CN201611128842.0A CN107068238A (en) | 2016-12-09 | 2016-12-09 | 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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