CN104143372B - A kind of modified mullite conductive silver paste and preparation method thereof - Google Patents

A kind of modified mullite conductive silver paste and preparation method thereof Download PDF

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CN104143372B
CN104143372B CN201410368700.6A CN201410368700A CN104143372B CN 104143372 B CN104143372 B CN 104143372B CN 201410368700 A CN201410368700 A CN 201410368700A CN 104143372 B CN104143372 B CN 104143372B
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mullite
silver paste
conductive silver
zinc sulfate
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CN104143372A (en
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蒋智谋
周施峰
周梅永
胡加峰
谢水兵
张超
崔海威
吴华
董子侠
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Dongguan Totem Chemical Materials Technology Co.,Ltd.
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Anhui Zhuangyuanlang Electronic Technology Co Ltd
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Abstract

The invention discloses a kind of modified mullite conductive silver paste, it is characterized in that, be prepared by the raw materials in: argentum powder 42 55, mullite 35, boron oxide 24, zinc sulfate 0.4 0.7, chitin 0.6 0.9, carbamide 1.2 3.4, methylpropanol sodium diacelate 1.1 2.5, aluminum phosphate 2.1 3.6, dihydroxy ethyl imidazoline 0.7 1.2, di-n-butyl phosphite 46, auxiliary agent 30 40, suitable quantity of water;The conductive silver paste electric conductivity of the present invention is good, anticorrosive, wear-resisting, high temperature resistant, soldering resistance is strong.

Description

A kind of modified mullite conductive silver paste and Manufacture method
Technical field
The present invention relates to conductive silver paste field, be specifically related to a kind of modified mullite conductive silver paste and preparation method thereof.
Background technology
Conductive silver paste refers to be printed on conduction stock, it is allowed to that there is conduction electric current and the silver slurry of eliminating accumulation electrostatic charge ability, usually being imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard, it is made up of electroconductive stuffing, adhesive, solvent and additive.Conductive silver paste needs the characteristic possessed to have: electric conductivity (antistatic behaviour) is good, adhesive force is strong, printing adaptability good and solvent resistance superior properties, and the most existing conductive silver paste has disadvantages that, do not contain only lead, cadmium etc. and poisonous, pollute environment, and when using on conduction stock, adhesive force is low, soldering resistance is the best, and sintering character is poor.
Summary of the invention
It is an object of the invention to provide a kind of modified mullite conductive silver paste and preparation method thereof, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
A kind of modified mullite conductive silver paste, it is characterized in that, be prepared by the raw materials in: argentum powder 42-55, mullite 3-5, boron oxide 2-4, zinc sulfate 0.4-0.7, chitin 0.6-0.9, carbamide 1.2-3.4, methylpropanol sodium diacelate 1.1-2.5, aluminum phosphate 2.1-3.6, dihydroxy ethyl imidazoline 0.7-1.2, di-n-butyl phosphite 4-6, auxiliary agent 30-40, suitable quantity of water.
Described auxiliary agent is prepared from the following raw materials in parts by weight: aluminium sesquioxide 2-3, boron oxide 3-5, polyvinyl alcohol 7-9, Colophonium 14-18,3-aminopropyl trimethoxysilane 1.2-2.4, polydimethylsiloxane 0.3-0.4, acetone 9-14, Ketohexamethylene 7-10, its preparation method is that aluminium sesquioxide, boron oxide are put in calcining furnace and calcined 1-2 hour at 520-610 DEG C, taking-up is cooled to room temperature, adds polyvinyl alcohol and grinds 20-40 minute;By Ketohexamethylene, Colophonium mixing, react 2-3 hour at 100-120 DEG C, be cooled to 40-50 DEG C, add acetone, 3-aminopropyl trimethoxysilane, polydimethylsiloxane, keep temperature to stir 3-4 hour;Above each product is mixed, grinds 2-4 hour prepared 300-400 mesh slurry and get final product.
The preparation method of described a kind of modified mullite conductive silver paste, it is characterised in that comprise the following steps:
(1) take zinc sulfate and add suitable quantity of water stirring to dissolving, make solution of zinc sulfate, mullite is put in calcining furnace calcination processing 2-3 hour at 650-710 DEG C, spray solution of zinc sulfate while hot to all being absorbed, cooling, add carbamide, aluminum phosphate grinds 1-2 hour;
(2) take di-n-butyl phosphite and be heated to 45-55 DEG C, add dihydroxy ethyl imidazoline, methylpropanol sodium diacelate stirring extremely mixing in 30-40 minute, put into chitin, 2-3 hour pulping of Studies of Grinding Process of Boron Oxide;
(3) step (1), (2) reaction mass and other leftover materials being mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is that 10-20 μm starches grain, to obtain final product.
The present invention has following beneficial effect: the conductive silver paste electric conductivity of the present invention is good, anticorrosive, wear-resisting, high temperature resistant, soldering resistance is strong.
Detailed description of the invention
Described a kind of modified mullite conductive silver paste, it is characterized in that, be prepared by the raw materials in: argentum powder 49, mullite 5, boron oxide 4, zinc sulfate 0.4, chitin 0.8, carbamide 1.8, methylpropanol sodium diacelate 1.6, aluminum phosphate 3.6, dihydroxy ethyl imidazoline 0.7, di-n-butyl phosphite 4, auxiliary agent 40, suitable quantity of water.
Described auxiliary agent is prepared from the following raw materials in parts by weight: aluminium sesquioxide 2, boron oxide 4, polyvinyl alcohol 7, Colophonium 15,3-aminopropyl trimethoxysilane 1.5, polydimethylsiloxane 0.3, acetone 13, Ketohexamethylene 8, its preparation method is that aluminium sesquioxide, boron oxide are put in calcining furnace and calcined 1-2 hour at 520-610 DEG C, taking-up is cooled to room temperature, adds polyvinyl alcohol and grinds 20-40 minute;By Ketohexamethylene, Colophonium mixing, react 2-3 hour at 100-120 DEG C, be cooled to 40-50 DEG C, add acetone, 3-aminopropyl trimethoxysilane, polydimethylsiloxane, keep temperature to stir 3-4 hour;Above each product is mixed, grinds 2-4 hour prepared 300-400 mesh slurry and get final product.
Manufacture method comprises the following steps:
(1) take zinc sulfate and add suitable quantity of water stirring to dissolving, make solution of zinc sulfate, mullite is put in calcining furnace calcination processing 2-3 hour at 650-710 DEG C, spray solution of zinc sulfate while hot to all being absorbed, cooling, add carbamide, aluminum phosphate grinds 1-2 hour;
(2) take di-n-butyl phosphite and be heated to 45-55 DEG C, add dihydroxy ethyl imidazoline, methylpropanol sodium diacelate stirring extremely mixing in 30-40 minute, put into chitin, 2-3 hour pulping of Studies of Grinding Process of Boron Oxide;
(3) step (1), (2) reaction mass and other leftover materials being mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is that 10-20 μm starches grain, to obtain final product.
The technical specification being processed the conductive silver paste obtained by above-described embodiment is as follows:
(1) viscosity: 50-100PaS(Brookfield, 10RPM);
(2) adhesive force: > 10N/mm2
(3) sheet resistance: < 5m Ω/c;
(4) solderability excellent, burnt in a heap easily separated, printing adaptability good and solvent resistance is excellent.

Claims (2)

1. a modified mullite conductive silver paste, it is characterized in that, be prepared by the raw materials in: argentum powder 42-55, mullite 3-5, boron oxide 2-4, zinc sulfate 0.4-0.7, chitin 0.6-0.9, carbamide 1.2-3.4, methylpropanol sodium diacelate 1.1-2.5, aluminum phosphate 2.1-3.6, dihydroxy ethyl imidazoline 0.7-1.2, di-n-butyl phosphite 4-6, auxiliary agent 30-40, suitable quantity of water;
Described auxiliary agent is prepared from the following raw materials in parts by weight: aluminium sesquioxide 2-3, boron oxide 3-5, polyvinyl alcohol 7-9, Colophonium 14-18,3-aminopropyl trimethoxysilane 1.2-2.4, polydimethylsiloxane 0.3-0.4, acetone 9-14, Ketohexamethylene 7-10, its preparation method is that aluminium sesquioxide, boron oxide are put in calcining furnace and calcined 1-2 hour at 520-610 DEG C, taking-up is cooled to room temperature, adds polyvinyl alcohol and grinds 20-40 minute;By Ketohexamethylene, Colophonium mixing, react 2-3 hour at 100-120 DEG C, be cooled to 40-50 DEG C, add acetone, 3-aminopropyl trimethoxysilane, polydimethylsiloxane, keep temperature 40-50 DEG C to stir 3-4 hour;Above each product is mixed, grinds 2-4 hour prepared 300-400 mesh slurry and get final product.
The manufacture method of a kind of modified mullite conductive silver paste the most according to claim 1, it is characterised in that comprise the following steps:
(1) take zinc sulfate and add suitable quantity of water stirring to dissolving, make solution of zinc sulfate, mullite is put in calcining furnace calcination processing 2-3 hour at 650-710 DEG C, spray solution of zinc sulfate while hot to all being absorbed, cooling, add carbamide, aluminum phosphate grinds 1-2 hour;
(2) take di-n-butyl phosphite and be heated to 45-55 DEG C, add dihydroxy ethyl imidazoline, methylpropanol sodium diacelate stirring extremely mixing in 30-40 minute, put into chitin, 2-3 hour pulping of Studies of Grinding Process of Boron Oxide;
(3) step (1), (2) reaction mass and other leftover materials being mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is that 10-20 μm starches grain, to obtain final product.
CN201410368700.6A 2014-07-30 2014-07-30 A kind of modified mullite conductive silver paste and preparation method thereof Active CN104143372B (en)

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CN104575681A (en) * 2015-01-08 2015-04-29 安徽凤阳德诚科技有限公司 Conducting silver paste with cobalt powder
CN105772705A (en) * 2016-03-22 2016-07-20 苏州捷德瑞精密机械有限公司 Conductive silver powder and preparation method thereof
CN106087009A (en) * 2016-08-16 2016-11-09 王世群 A kind of Graphene scaffold composite plating solution
CN113470864B (en) * 2021-09-01 2022-03-11 西安宏星电子浆料科技股份有限公司 Thick film resistor paste with low size effect

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07254308A (en) * 1994-03-16 1995-10-03 Alps Electric Co Ltd Conductive paste
US5951918A (en) * 1995-02-08 1999-09-14 Hitachi Chemical Company, Ltd. Composite electroconductive powder, electroconductive paste, process for producing electroconductive paste, electric circuit and process for producing electric circuit
CN1467571A (en) * 2002-06-26 2004-01-14 富士施乐株式会社 Electrophotographic photoreceptor, electrophotographic member, process cartridge and image forming apparatus
CN103123812A (en) * 2013-02-20 2013-05-29 江苏晨电太阳能光电科技有限公司 Crystalline silicon solar cell aluminum paste

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH07254308A (en) * 1994-03-16 1995-10-03 Alps Electric Co Ltd Conductive paste
US5951918A (en) * 1995-02-08 1999-09-14 Hitachi Chemical Company, Ltd. Composite electroconductive powder, electroconductive paste, process for producing electroconductive paste, electric circuit and process for producing electric circuit
CN1467571A (en) * 2002-06-26 2004-01-14 富士施乐株式会社 Electrophotographic photoreceptor, electrophotographic member, process cartridge and image forming apparatus
CN103123812A (en) * 2013-02-20 2013-05-29 江苏晨电太阳能光电科技有限公司 Crystalline silicon solar cell aluminum paste

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