CN103165217A - Electric conduction silver paste for mica plate capacitor and preparation method thereof - Google Patents

Electric conduction silver paste for mica plate capacitor and preparation method thereof Download PDF

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Publication number
CN103165217A
CN103165217A CN2011104193067A CN201110419306A CN103165217A CN 103165217 A CN103165217 A CN 103165217A CN 2011104193067 A CN2011104193067 A CN 2011104193067A CN 201110419306 A CN201110419306 A CN 201110419306A CN 103165217 A CN103165217 A CN 103165217A
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silver paste
powder
silver
solvent
mica
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CN103165217B (en
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王洪波
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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BAOYIN ELECTRONIC MATERIAL Co Ltd SHANGHAI
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Abstract

The invention relates to electric conduction silver paste for a mica plate capacitor and a preparation method thereof. The electric conduction silver paste comprises, by weight percentage, 40-55% of metal silver powder, 1-7% of glass powder, 30-45% of organic carrier and 10-20% of solvent, wherein the carrier is prepared by using macromolecule resin and the solvent, and then other components are mixed with the carrier to prepare the electric conduction silver paste for the mica plate capacitor. Compared with the prior art,the electric conduction silver paste has improved electric conduction performance because reasonable matching of ball powder and piece powder is performed so that sintering is compact and an electric conduction network is formed well, and silver content is greatly reduced. SrO and TiO2 are added in the glass powder and are easily melted with a capacitor base body in sintering to form a novel homogeneous phase state, and adhesive force of a silver layer is enhanced. By adding and selecting the glass powder, the adhesive force is improved, a sintering range is further increased, and the sintering temperature is reduced to 490 DEG C.

Description

A kind of foil mica capacity conductive silver paste and preparation method thereof
Technical field
The present invention relates to a kind of conductive silver paste and preparation method thereof, especially relate to a kind of foil mica capacity conductive silver paste and preparation method thereof.
Background technology
Foil mica capacity be with the mica sheet material as dielectric, at the battery lead plate that dielectric print electrode on surface silver slurry is done, after pole plate and mica are in layer superimposed, then die casting is made at bakelite powder or in being locked in epoxy resin.The characteristics of foil mica capacity are that dielectric loss is little, and insulation resistance is large, temperature coefficient is little, is suitable for high-frequency circuit.Mica condenser is widely used in radio sending and receiving equipment, precision electronic device, modern communication instrument and meter and equipment, broadcast receiver, power amplifier, television set etc. as basic device.Universal along with household electrical appliance in recent years, electronic product is to miniaturization, microminiaturized development, and the demand of mica condenser increases year by year, also progressively increases as the conductive silver paste demand of mica condenser electrode.
The mica condenser electrode with the present domestic year use amount of conductive silver paste more than 20 tons, the imports silver slurries such as ore deposit, Dupont are lived more by the Japan that use, and mainly have following problem: silver content is high, sintering temperature is high, sintering range is narrow and silver layer and the mica sheet bond strength general.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of sintering more fine and close for the defective that overcomes above-mentioned prior art existence, the foil mica capacity that better improves electric conductivity conductive silver paste and preparation method thereof that conductive network forms.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of foil mica capacity conductive silver paste comprises following component and weight percent content:
Silver powder 40-55;
Glass dust 1-7;
Organic carrier 30-45;
Solvent 10-20.
Described silver powder is spherical silver powder and flake silver powder, and wherein the particle diameter of spherical silver powder is 0.5-1.5 μ m, and tap density is 1.5-2.5g/ml; The particle diameter of flake silver powder is 0.5-1.0 μ m, and tap density is 1.0-2.0g/ml.
Described glass dust is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and weight percent content are:
Bi 2O 3 50-65;
SiO 2 8-13;
ZnO 3-9;
TiO 2 1-6;
SrO 3-10;
Al 2O 3 8-14。
Its component of described organic carrier and content (wt%) are:
Macromolecule resin 10-30;
Solvent 70-90.
Described macromolecule resin is selected from one or more in ethyl cellulose, celluloid or rosin.
Described solvent is selected from one or more mixtures that mix with arbitrary proportion in butyl ether, ten diester alcohol, ethylene glycol ethyl ether, turpentine oil, cyclohexanone or terpinol.
A kind of foil mica capacity preparation method of conductive silver paste comprises the following steps:
(1) preparation of carrier: take macromolecule resin and solvent, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 15000-35000cps, then with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier;
(2) get the raw materials ready according to following component and content (wt%):
Silver powder 40-55,
Glass dust 1-7,
Organic carrier 30-45,
Solvent 10-20;
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30-50Pa.S, makes mica condenser electrode conductive silver paste.
Compared with prior art, the present invention is reasonably combined by ball powder and sheet powder, makes sintering more fine and close, conductive network formation better improve electric conductivity, reduce greatly silver content; Add SrO and TiO2 in glass dust, make the easier congruent melting when sintering of itself and capacitor matrix, form the phase of new homogeneous, strengthened the adhesive force of silver layer; Collocation by glass dust has not only improved adhesive force with selection, has also increased simultaneously the sintering amplitude, and has made sintering temperature be low to moderate 490 ℃; The alternative imported product of present technique.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
A kind of mica condenser electrode preparation method of conductive silver paste, the method comprises the following steps:
(1) preparation of carrier: formulation vehicle 50Kg, take macromolecule resin 12.5Kg, butyl ether 17.5Kg and terpinol 20Kg, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 25000-35000cps, with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier again;
(2) get the raw materials ready, get the raw materials ready according to following component and content (wt%):
Figure BDA0000120086360000031
In silver powder used, the ball powder is 45Kg, sheet powder 5Kg, and ball powder particles particle diameter 1.4 μ m, tap density are 2.4g/ml; Sheet powder particles particle diameter 0.9 μ m, tap density are 1.9g/ml;
Glass dust used is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and content (wt%) are:
Figure BDA0000120086360000041
Solvent for use is butyl ether.
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 40-50Pa.S, makes mica condenser electrode conductive silver paste.
The mode of above-mentioned silver slurry by silk screen printing is printed on mica sheet, carries out sintering, encapsulate and make the foil mica capacity finished product according to the normal process of present industry, made up existing deficiency with silver slurry products made thereby.
Embodiment 2
A kind of mica condenser electrode preparation method of conductive silver paste, the method comprises the following steps:
(1) preparation of carrier: formulation vehicle 50Kg, take macromolecule resin 15Kg, butyl ether 15Kg and terpinol 20Kg, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 25000-35000cps, with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier again;
(2) get the raw materials ready, get the raw materials ready according to following component and content (wt%):
Figure BDA0000120086360000042
In silver powder used, the ball powder is 40Kg, sheet powder 5Kg, and ball powder particles particle diameter 1.2 μ m, tap density are 2.3g/ml; Sheet powder particles particle diameter 0.8 μ m, tap density are 1.8g/ml;
Glass dust used is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and content (wt%) are:
Figure BDA0000120086360000043
Figure BDA0000120086360000051
Solvent for use is 12 ester alcohol.
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 40-50Pa.S, makes mica condenser electrode conductive silver paste.
Embodiment 3
A kind of mica condenser electrode preparation method of conductive silver paste, the method comprises the following steps:
(1) preparation of carrier: formulation vehicle 50Kg, take macromolecule resin 10Kg, butyl ether 20Kg and terpinol 20Kg, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 25000-30000cps, with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier again;
(2) get the raw materials ready, get the raw materials ready according to following component and content (wt%):
Figure BDA0000120086360000052
In silver powder used, the ball powder is 35Kg, sheet powder 5Kg, and ball powder particles particle diameter 1.0 μ m, tap density are 1.8g/ml; Sheet powder particles particle diameter 0.6 μ m, tap density are 1.2g/ml;
Glass dust used is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and content (wt%) are:
Figure BDA0000120086360000053
Solvent for use is 12 ester alcohol.
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30-40Pa.S, makes mica condenser electrode conductive silver paste.
Embodiment 4
A kind of mica condenser electrode preparation method of conductive silver paste, the method comprises the following steps:
(1) preparation of carrier: formulation vehicle 50Kg, take macromolecule resin 8Kg, butyl ether 20Kg and terpinol 22Kg, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 25000-30000cps, with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier again;
(2) get the raw materials ready, get the raw materials ready according to following component and content (wt%):
Figure BDA0000120086360000061
In silver powder used, the ball powder is 50Kg, sheet powder 5Kg, and ball powder particles particle diameter 1.4 μ m, tap density are 2.4g/ml; Sheet powder particles particle diameter 0.9 μ m, tap density are 1.8g/ml;
Glass dust used is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and content (wt%) are:
Figure BDA0000120086360000062
Solvent for use is ethylene glycol ethyl ether.
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30-40Pa.S, makes mica condenser electrode conductive silver paste.
Embodiment 5
A kind of foil mica capacity conductive silver paste, comprise following component and content: silver powder 50kg, glass dust 1kg, organic carrier 45kg, solvent 14kg, silver powder is spherical silver powder and flake silver powder, and wherein the particle diameter of spherical silver powder is 0.5 μ m, and tap density is 1.5g/ml; The particle diameter of flake silver powder is 0.5 μ m, and tap density is 1.0g/ml.
Glass dust is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and weight percent content are: Bi 2O 365%, SiO 210%, ZnO 3%, TiO 22%, SrO 10%, Al 2O 310%.
Its component of organic carrier and content (wt%) are: macromolecule resin 10%, solvent 90%.
The macromolecule resin that uses is the mixture of ethyl cellulose and celluloid, and solvent is the mixture of the ten pure and mild ethylene glycol ethyl ethers of diester.
The foil mica capacity preparation method of conductive silver paste comprises the following steps:
(1) preparation of carrier: take macromolecule resin and solvent, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 15000cps, then with resin filtering and impurity removing on 300 purpose screen cloths, obtain carrier;
(2) get the raw materials ready according to above component and content;
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30Pa.S, makes mica condenser electrode conductive silver paste.
Embodiment 6
A kind of foil mica capacity conductive silver paste, comprise following component and content: silver powder 41kg, glass dust 7kg, organic carrier 32kg, solvent 20kg, silver powder is spherical silver powder and flake silver powder, and wherein the particle diameter of spherical silver powder is 1.5 μ m, and tap density is 2.5g/ml; The particle diameter of flake silver powder is 1.0 μ m, and tap density is 2.0g/ml.
Glass dust is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and weight percent content are: Bi 2O 362%, SiO 210%, ZnO 3%, TiO 22%, SrO 10%, Al 2O 313%.
Its component of organic carrier and content (wt%) are: macromolecule resin 30%, solvent 70%.
The macromolecule resin that uses is rosin, and solvent is turpentine oil.
The foil mica capacity preparation method of conductive silver paste comprises the following steps:
(1) preparation of carrier: take macromolecule resin and solvent, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 35000cps, then with resin filtering and impurity removing on 400 purpose screen cloths, obtain carrier;
(2) get the raw materials ready according to above component and content;
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30Pa.S, makes mica condenser electrode conductive silver paste.

Claims (7)

1. a foil mica capacity conductive silver paste, is characterized in that, this conductive silver paste comprises following component and weight percent content:
Silver powder 40-55;
Glass dust 1-7;
Organic carrier 30-45;
Solvent 10-20.
2. a kind of foil mica capacity conductive silver paste according to claim 1, is characterized in that, described silver powder is spherical silver powder and flake silver powder, and wherein the particle diameter of spherical silver powder is 0.5-1.5 μ m, and tap density is 1.5-2.5g/ml; The particle diameter of flake silver powder is 0.5-1.0 μ m, and tap density is 1.0-2.0g/ml.
3. a kind of foil mica capacity conductive silver paste according to claim 1, is characterized in that, described glass dust is lead-free glass powder, and sintering temperature is 490-700 ℃, and its component and weight percent content are:
Bi 2O 3 50-65;
SiO 2 8-13;
ZnO 3-9;
TiO 2 1-6;
SrO 3-10;
Al 2O 3 8-14。
4. a kind of foil mica capacity conductive silver paste according to claim 1, is characterized in that, its component of described organic carrier and content (wt%) are:
Macromolecule resin 10-30;
Solvent 70-90.
5. a kind of foil mica capacity conductive silver paste according to claim 1, is characterized in that, described macromolecule resin is selected from one or more in ethyl cellulose, celluloid or rosin.
6. according to claim 1 or 4 described a kind of foil mica capacity conductive silver pastes, it is characterized in that, described solvent is selected from one or more mixtures that mix with arbitrary proportion in butyl ether, ten diester alcohol, ethylene glycol ethyl ether, turpentine oil, cyclohexanone or terpinol.
7. the preparation method of a foil mica capacity use conductive silver paste as claimed in claim 1, is characterized in that, the method comprises the following steps:
(1) preparation of carrier: take macromolecule resin and solvent, then be heated and be warming up to 80 ℃ and constant temperature, until resin constant temperature is dissolved to 15000-35000cps, then with resin filtering and impurity removing on 300-400 purpose screen cloth, obtain carrier;
(2) get the raw materials ready according to following component and content (wt%):
Silver powder 40-55,
Glass dust 1-7,
Organic carrier 30-45,
Solvent 10-20;
(3) preparation of silver slurry: take silver powder, glass dust, it is fully mixed in batch mixer with organic carrier, solvent, using high speed dispersor to carry out high speed dispersion, obtain uniform slurry;
(4) production of silver paste: above-mentioned slurry is ground at three rollers grind, the fine setting by roller is that silver slurry fineness is controlled at below 10 μ m, and viscosity is 30-50Pa.S, makes mica condenser electrode conductive silver paste.
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Cited By (8)

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CN109671516A (en) * 2019-01-24 2019-04-23 日照众邦电子有限公司 A kind of method of preparation and use of electric heating resistance slurry
TWI676194B (en) * 2018-09-21 2019-11-01 鈺冠科技股份有限公司 Stacked capacitor without carbon layer and method of manufacturing the same, and siliver silver paste layer
CN110942917A (en) * 2018-09-21 2020-03-31 钰冠科技股份有限公司 Capacitor packaging structure, capacitor and polymer composite layer
CN110942918A (en) * 2018-09-21 2020-03-31 钰冠科技股份有限公司 Stacked capacitor, manufacturing method thereof and silver colloid layer
TWI690957B (en) * 2018-09-21 2020-04-11 鈺冠科技股份有限公司 Stacked capacitor package structure without carbon layer and stacked capacitor thereof, and conductive polymer layer
CN112562884A (en) * 2019-11-07 2021-03-26 陕西彩虹新材料有限公司 Preparation method of low-sheet-resistance conductive silver paste
CN115483025A (en) * 2022-09-30 2022-12-16 安徽锐光电子科技有限公司 Preparation process of mica sheet capacitor
CN115650767A (en) * 2022-09-30 2023-01-31 安徽锐光电子科技有限公司 Mica sheet silver spraying heat treatment color changing method

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TWI676194B (en) * 2018-09-21 2019-11-01 鈺冠科技股份有限公司 Stacked capacitor without carbon layer and method of manufacturing the same, and siliver silver paste layer
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CN115650767A (en) * 2022-09-30 2023-01-31 安徽锐光电子科技有限公司 Mica sheet silver spraying heat treatment color changing method
CN115650767B (en) * 2022-09-30 2024-04-19 安徽锐光电子科技有限公司 Silver spraying heat treatment color-changing method for mica sheet

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