CN103021572A - Method for preparing conductive paste containing thermoplastic acrylic resin - Google Patents

Method for preparing conductive paste containing thermoplastic acrylic resin Download PDF

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CN103021572A
CN103021572A CN2012105508641A CN201210550864A CN103021572A CN 103021572 A CN103021572 A CN 103021572A CN 2012105508641 A CN2012105508641 A CN 2012105508641A CN 201210550864 A CN201210550864 A CN 201210550864A CN 103021572 A CN103021572 A CN 103021572A
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raw material
acrylic resin
thermoplastic acrylic
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organic carrier
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CN103021572B (en
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孔祥伟
宋强
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Anhui Jinda Instrument Co Ltd
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Anhui Jinda Instrument Co Ltd
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Abstract

The invention discloses a method for preparing conductive paste containing thermoplastic acrylic resin. The conductive paste is prepared from raw materials including, by weight, 76-79 parts of materials A, 18-21 parts of materials B, 1.4-2.3 parts of silane coupling agents KH560, 2-3 parts of organic silicon leveling agents, 0.3-0.5 part of organic silicon oil, 1-2 parts of zinc stearate and 0.4-0.8 part of trioctyl trimellitate. The conductive paste is lead-free, completely meets environmental protection requirements, and can form silver powder with large adhesive force, high cell photoelectric conversion efficiency and different particle sizes on the surface of a solar cell when applied to solar cell production. The contact area of particles is increased, so that conductivity of the paste is improved.

Description

A kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin
Technical field
The present invention relates to the electrocondution slurry field, exactly is a kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin.
Background technology
Electrocondution slurry is electronic devices and components encapsulation, electrode and interconnected critical material, mainly comprises burning infiltration type electrocondution slurry and curing type conducting resinl (electrically conductive ink) two large classes.
Burning infiltration type electrocondution slurry mainly is used in the industries such as solar cell, makes electrode behind the sintering and uses, and the curing type electrically conductive ink is widely used in the industries such as printed circuit and Electronic Packaging.
Electrocondution slurry is different according to filler wherein, can be divided into carbon slurry (graphite conductor), metal paste (bronze, silver powder, copper powder, yellow gold), and the ceramic size of modification.
The conductive silver slurry refers to be printed on the conduction stock, and the silver that makes it to have conduction current and get rid of the accumulate static charge ability is starched, and generally is to be imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard.
Summary of the invention
The object of the present invention is to provide a kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin.
Above-mentioned purpose realizes by following scheme:
A kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin is characterized in that, may further comprise the steps:
(1) takes by weighing each raw material for preparing glass dust: K by following weight portion 2O 2-4, AS 2O 36.5-8.2, Co 2O 33-5, SnO 23.5-5.8, V 2O 58-12, B 2O 35-7, ZrO 26-8, SiO 212-15, Sb 2O 33-4, Na 2O 7-9, MgO 1-2, CuO 4-6;
(2) will prepare required each raw material blending of glass dust, afterwards in 1100-1200 ℃ of lower sintering 1.5-3h, again the gained melting charge is poured in the cold water and quenched, ball milling, sieving, obtain the glass dust of 10-15 μ m, is that the hydrochloric acid solution of 10-12% soaked 2-4 hour with concentration again, then be washed till neutrality with deionized water, dry to such an extent that 10-15 μ m glass dust is for subsequent use;
(3) take by weighing each raw material for preparing C5 Petropols organic carrier by following weight portion: C5 Petropols 8-10, polyvinylpyrrolidone 2.9-4.5, polyethylene glycol 1-2, butyl carbitol 18-19, diethylene glycol ether acetate 15-18, dioctyl phthalate 1.3-1.8;
(4) will prepare each raw material blending of C5 Petropols organic carrier after, in 50-65 ℃ of lower stirring and dissolving, cross 300-500 order filter cloth, it is for subsequent use namely to get C5 Petropols organic carrier;
(5) take by weighing each raw material for preparing the thermoplastic acrylic resin organic carrier by following weight portion: thermoplastic acrylic resin 8-10, tricresyl phosphate 0.5-0.7,2-octanol 8-12, ethyl acetate 16-18, turpentine oil 8-10;
(6) will prepare each raw material blending of thermoplastic acrylic resin organic carrier after, in 63-68 ℃ of lower stirring and dissolving, cross 300-500 order filter cloth, it is for subsequent use namely to get the thermoplastic acrylic resin organic carrier;
(7) take by weighing each raw material that preparation A expects by following weight portion: 10-15 μ m glass dust 10-12, C5 Petropols organic carrier 20-23, di-n-octyl phthalate 1.5-2.8, chlorinated paraffin wax 0.2-0.3 that 1-5 μ m silver powder 25-28,61-90nm silver powder 25-28,16-25 μ m silver powder 20-25, step (2) make;
With each raw material blending of preparation A material, obtain the A material;
(8) take by weighing each raw material that preparation B expects by following weight portion: 10-15 μ m glass dust 10-12, thermoplastic acrylic resin organic carrier 22-25, castor oil 2-3 that 1-5 μ m aluminium powder 32-34,61-90nm aluminium powder 10-15,11-15 μ m copper powder 24-28, step (2) make;
With each raw material blending of preparation B material, obtain the B material;
(9) take by weighing each raw material that preparation contains the electrocondution slurry of thermoplastic acrylic resin by following weight portion:
A expects 76-79, and B expects 18-21, silane coupler KH560 1.4-2.3, organosilicon levelling agent 2-3, organic silicone oil 0.3-0.5, zinc stearate 1-2, trioctyl trimellitate (TOTM) 0.4-0.8;
Preparation is contained each raw material mixing by weight of the electrocondution slurry of thermoplastic acrylic resin, ball milling is ground to the slurry fineness less than 10 μ m, transfers after the viscosity and get final product;
Described a kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin is characterized in that: transfer viscosity to 150-200Pas in the step (9).
Beneficial effect of the present invention is: the electrocondution slurry of gained of the present invention is not leaded, meet environmental requirement fully, when the production that is applied to solar cell, can form strong adhesion, cell photoelectric conversion efficiency height in solar cell surface, selected simultaneously the silver powder of different-grain diameter, increase interparticle contact area, thereby improved the conductive capability of slurry.
Embodiment
A kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin may further comprise the steps:
(1) by following weight portion (kg) take by weighing the preparation glass dust each raw material: K 2O 4, AS 2O 36.5, Co 2O 33, SnO 25.8, V 2O 512, B 2O 37, ZrO 28, SiO 215, Sb 2O 34, Na 2O 9, MgO2, and CuO 6;
(2) will prepare required each raw material blending of glass dust, afterwards in 1200 ℃ of lower sintering 3h, again the gained melting charge is poured in the cold water and quenched, ball milling, sieving, obtain the glass dust of 10-15 μ m, is that 10% hydrochloric acid solution soaked 4 hours with concentration again, then be washed till neutrality with deionized water, dry to such an extent that 10-15 μ m glass dust is for subsequent use;
(3) take by weighing each raw material for preparing C5 Petropols organic carrier by following weight portion: C5 Petropols 10, polyvinylpyrrolidone 4.5, polyethylene glycol 2, butyl carbitol 19, diethylene glycol ether acetate 15, dioctyl phthalate 1.8;
(4) will prepare each raw material blending of C5 Petropols organic carrier after, in 50 ℃ of lower stirring and dissolving, cross 300 order filter clothes, it is for subsequent use namely to get C5 Petropols organic carrier;
(5) take by weighing each raw material for preparing the thermoplastic acrylic resin organic carrier by following weight portion: thermoplastic acrylic resin 8, tricresyl phosphate 0.7,2-octanol 12, ethyl acetate 18, turpentine oil 10;
(6) will prepare each raw material blending of thermoplastic acrylic resin organic carrier after, in 63 ℃ of lower stirring and dissolving, cross 300 order filter clothes, it is for subsequent use namely to get the thermoplastic acrylic resin organic carrier;
(7) take by weighing each raw material that preparation A expects by following weight portion: 10-15 μ m glass dust 12, C5 Petropols organic carrier 23, di-n-octyl phthalate 2.8, chlorinated paraffin wax 0.3 that 1-5 μ m silver powder 28,61-90nm silver powder 25,16-25 μ m silver powder 25, step (2) make;
With each raw material blending of preparation A material, obtain the A material;
(8) take by weighing each raw material that preparation B expects by following weight portion: 10-15 μ m glass dust 12, thermoplastic acrylic resin organic carrier 23, castor oil 3 that 1-5 μ m aluminium powder 32,61-90nm aluminium powder 15,11-15 μ m copper powder 28, step (2) make;
With each raw material blending of preparation B material, obtain the B material;
(9) by each raw material of electrocondution slurry that preparation contains thermoplastic acrylic resin that takes by weighing of following weight portion (kg):
A material 76, B material 18, silane coupler KH560 2.1, organosilicon levelling agent 3, organic silicone oil 0.5, zinc stearate 2, trioctyl trimellitate (TOTM) 0.8;
Preparation is contained each raw material mixing by weight of the electrocondution slurry of thermoplastic acrylic resin, ball milling is ground to the slurry fineness less than 10 μ m, transfers after the viscosity and get final product;
Adopt screen process press that the silver slurry is printed on 125mm * 125mm Si substrate, then 180 ℃ of dryings, carry out quick fired electrodes lead-in wire at 880 ℃ again, the contact conductor surface silvery white of making behind the high temperature sintering, smooth zero defect, peel strength 13 N/cm, soldering is functional, sheet resistance<10 Siements/sq, the solar cell photoelectric transformation efficiency of preparation is 18.8%, the tensile test result is adhesive force〉14N/mm 2

Claims (2)

1. a preparation method who contains the electrocondution slurry of thermoplastic acrylic resin is characterized in that, may further comprise the steps:
(1) takes by weighing each raw material for preparing glass dust: K by following weight portion 2O 2-4, AS 2O 36.5-8.2, Co 2O 33-5, SnO 23.5-5.8, V 2O 58-12, B 2O 35-7, ZrO 26-8, SiO 212-15, Sb 2O 33-4, Na 2O 7-9, MgO 1-2, CuO 4-6;
(2) will prepare required each raw material blending of glass dust, afterwards in 1100-1200 ℃ of lower sintering 1.5-3h, again the gained melting charge is poured in the cold water and quenched, ball milling, sieving, obtain the glass dust of 10-15 μ m, is that the hydrochloric acid solution of 10-12% soaked 2-4 hour with concentration again, then be washed till neutrality with deionized water, dry to such an extent that 10-15 μ m glass dust is for subsequent use;
(3) take by weighing each raw material for preparing C5 Petropols organic carrier by following weight portion: C5 Petropols 8-10, polyvinylpyrrolidone 2.9-4.5, polyethylene glycol 1-2, butyl carbitol 18-19, diethylene glycol ether acetate 15-18, dioctyl phthalate 1.3-1.8;
(4) will prepare each raw material blending of C5 Petropols organic carrier after, in 50-65 ℃ of lower stirring and dissolving, cross 300-500 order filter cloth, it is for subsequent use namely to get C5 Petropols organic carrier;
(5) take by weighing each raw material for preparing the thermoplastic acrylic resin organic carrier by following weight portion: thermoplastic acrylic resin 8-10, tricresyl phosphate 0.5-0.7,2-octanol 8-12, ethyl acetate 16-18, turpentine oil 8-10;
(6) will prepare each raw material blending of thermoplastic acrylic resin organic carrier after, in 63-68 ℃ of lower stirring and dissolving, cross 300-500 order filter cloth, it is for subsequent use namely to get the thermoplastic acrylic resin organic carrier;
(7) take by weighing each raw material that preparation A expects by following weight portion: 10-15 μ m glass dust 10-12, C5 Petropols organic carrier 20-23, di-n-octyl phthalate 1.5-2.8, chlorinated paraffin wax 0.2-0.3 that 1-5 μ m silver powder 25-28,61-90nm silver powder 25-28,16-25 μ m silver powder 20-25, step (2) make;
With each raw material blending of preparation A material, obtain the A material;
(8) take by weighing each raw material that preparation B expects by following weight portion: 10-15 μ m glass dust 10-12, thermoplastic acrylic resin organic carrier 22-25, castor oil 2-3 that 1-5 μ m aluminium powder 32-34,61-90nm aluminium powder 10-15,11-15 μ m copper powder 24-28, step (2) make;
With each raw material blending of preparation B material, obtain the B material;
(9) take by weighing each raw material that preparation contains the electrocondution slurry of thermoplastic acrylic resin by following weight portion:
A expects 76-79, and B expects 18-21, silane coupler KH560 1.4-2.3, organosilicon levelling agent 2-3, organic silicone oil 0.3-0.5, zinc stearate 1-2, trioctyl trimellitate (TOTM) 0.4-0.8;
Preparation is contained each raw material mixing by weight of the electrocondution slurry of thermoplastic acrylic resin, ball milling is ground to the slurry fineness less than 10 μ m, transfers after the viscosity and get final product.
2. a kind of preparation method who contains the electrocondution slurry of thermoplastic acrylic resin according to claim 1 is characterized in that: transfer viscosity to 150-200Pas in the step (9).
CN201210550864.1A 2012-12-18 2012-12-18 A kind of preparation method of the electrocondution slurry that contains thermoplastic acrylic resin Active CN103021572B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104143377A (en) * 2014-06-30 2014-11-12 永利电子铜陵有限公司 PCB conductive silver paste and preparing method thereof
CN104575675A (en) * 2014-12-23 2015-04-29 合肥中南光电有限公司 Conductive silver paste for flexible circuit board
CN104575683A (en) * 2015-01-08 2015-04-29 安徽凤阳德诚科技有限公司 Conductive silver paste long in service life
CN104575664A (en) * 2014-12-23 2015-04-29 合肥中南光电有限公司 Electric conduction silver paste with high adhesive force
CN110838383A (en) * 2019-10-29 2020-02-25 深圳顺络电子股份有限公司 Flexible outer electrode of chip component and manufacturing method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356731A (en) * 2001-03-30 2002-12-13 Nippon Tungsten Co Ltd Substrate for semiconductor
JP2005123141A (en) * 2003-10-20 2005-05-12 Murata Mfg Co Ltd Conductive paste and piezoelectric ceramic electronic component
CN101692410A (en) * 2009-08-21 2010-04-07 广东风华高新科技股份有限公司 Silver paste of MLCC terminal electrode
CN101728001A (en) * 2009-11-12 2010-06-09 东南大学 Lead-free and low-silver photosensitive silver paste and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356731A (en) * 2001-03-30 2002-12-13 Nippon Tungsten Co Ltd Substrate for semiconductor
JP2005123141A (en) * 2003-10-20 2005-05-12 Murata Mfg Co Ltd Conductive paste and piezoelectric ceramic electronic component
CN101692410A (en) * 2009-08-21 2010-04-07 广东风华高新科技股份有限公司 Silver paste of MLCC terminal electrode
CN101728001A (en) * 2009-11-12 2010-06-09 东南大学 Lead-free and low-silver photosensitive silver paste and preparation method thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104143377A (en) * 2014-06-30 2014-11-12 永利电子铜陵有限公司 PCB conductive silver paste and preparing method thereof
CN104575675A (en) * 2014-12-23 2015-04-29 合肥中南光电有限公司 Conductive silver paste for flexible circuit board
CN104575664A (en) * 2014-12-23 2015-04-29 合肥中南光电有限公司 Electric conduction silver paste with high adhesive force
CN104575683A (en) * 2015-01-08 2015-04-29 安徽凤阳德诚科技有限公司 Conductive silver paste long in service life
CN110838383A (en) * 2019-10-29 2020-02-25 深圳顺络电子股份有限公司 Flexible outer electrode of chip component and manufacturing method thereof
CN110838383B (en) * 2019-10-29 2021-04-23 深圳顺络电子股份有限公司 Flexible outer electrode of chip component and manufacturing method thereof

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