CN104078095A - Conductive oxygen-free ceramic powder/nano-graphite composite conductive silver paste and preparing method thereof - Google Patents
Conductive oxygen-free ceramic powder/nano-graphite composite conductive silver paste and preparing method thereof Download PDFInfo
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- CN104078095A CN104078095A CN201410303512.5A CN201410303512A CN104078095A CN 104078095 A CN104078095 A CN 104078095A CN 201410303512 A CN201410303512 A CN 201410303512A CN 104078095 A CN104078095 A CN 104078095A
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Abstract
The invention discloses conductive oxygen-free ceramic powder/nano-graphite composite conductive silver paste. The conductive silver paste is characterized by being prepared from, by weight, 40-50 parts of silver powder, 1.5-2.6 parts of aluminum oxide, 2.1-3.2 parts of boron oxide, 1.2-2.9 parts of citric acid, 0.7-1.5 parts of polyvinyl butyral, 2-3 parts of nano-graphite, 2-4 parts of polyethylene glycol, 0.4-0.8 part of calcium nitrate, 1-3 parts of ethidene diamine, 2-5 parts of conductive oxygen-free ceramic powder and 30-40 parts of auxiliaries. Due to the fact that the conductive oxygen-free ceramic powder is added into the conductive silver paste, consumption of silver powder is reduced and cost is reduced. Meanwhile, the improved production technology is adopted, operation is easy and convenient, and the prepared conductive silver paste is unleaded, low in toxicity and free of pollution to the environment and is novel environmentally friendly conductive silver paste.
Description
Technical field
The present invention relates to conductive silver paste field, be specifically related to a kind of compound conductive silver paste of anaerobic ceramic powder/nano-graphite and preparation method thereof that conducts electricity.
Background technology
Conductive silver paste refers to and is printed on conduction stock, make it the silver slurry that there is conduction current and get rid of accumulate static charge ability, be to be generally imprinted on the non-conductive stocks such as plastics, glass, pottery or cardboard, it is made up of electroconductive stuffing, binder, solvent and additive.The characteristic that need to possess when conductive silver paste has: conductivity (antistatic behaviour) is good, strong adhesion, printing adaptability are good and the excellent characteristic of solvent resistance, and existing conductive silver paste has a lot of shortcomings in the market, not only contain lead, cadmium etc. and poisonous, contaminated environment, and use conduction stock on time adhesive force low, soldering resistance is not good, sintering character is poor.
Summary of the invention
Object of the present invention is just to provide a kind of compound conductive silver paste of anaerobic ceramic powder/nano-graphite and preparation method thereof that conducts electricity, to overcome the deficiencies in the prior art.
The object of the present invention is achieved like this:
A kind of compound conductive silver paste of anaerobic ceramic powder/nano-graphite that conducts electricity, it is characterized in that, made by the raw material of following weight portion: silver powder 40-50, aluminium oxide 1.5-2.6, boron oxide 2.1-3.2, citric acid 1.2-2.9, polyvinyl butyral resin 0.7-1.5, nano-graphite 2-3, polyethylene glycol 2-4, calcium nitrate 0.4-0.8, ethylenediamine 1-3, conduction anaerobic ceramic powder 2-5, auxiliary agent 30-40.
Described auxiliary agent is made up of following raw materials in part by weight: bismuth oxide 2-3, boron oxide 3-4, ethyl cellulose 0.8-1.4, lauryl sodium sulfate 0.3-0.4, repefral 0.2-0.4, lecithin 0.3-0.5, polysiloxanes 0.2-0.3, terpinol 20-25, its preparation method is bismuth oxide and boron oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds ethyl cellulose to grind 20-40 minute; Repefral, terpinol are stirred and evenly mixed, at 140-190 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add lecithin, polysiloxanes, lauryl sodium sulfate, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
Described a kind of preparation method of conducting electricity the compound conductive silver paste of anaerobic ceramic powder/nano-graphite, is characterized in that comprising the following steps:
(1) get ethylenediamine, conduction anaerobic ceramic powder mixed grinding makes 200-300 order slurry for 2-3 hour, adds aluminium oxide, boron oxide to continue to grind 3-4 hour, spraying is dry, dries, and sends in calciner sintering 1-2 hour at 450-510 DEG C;
(2) taking polyethylene glycol is put into reactor and is heated to 55-65 DEG C, adds polyvinyl butyral resin, keeps temperature to stir 2-3 hour, dissolve completely to polyvinyl butyral resin, add calcium nitrate, citric acid, nano-graphite, insulation 30-50 minute, grinds pulping again;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
The present invention has following beneficial effect: in conductive silver paste slurry of the present invention, add conduction anaerobic ceramic powder, reduce the consumption of silver powder, reduce cost, also improved production technology of the present invention simultaneously, easy and simple to handle, the conductive silver paste that makes is unleaded, low toxicity, environmentally safe, is a kind of novel conductive silver slurry of environmental protection.
Embodiment
Described a kind of compound conductive silver paste of anaerobic ceramic powder/nano-graphite that conducts electricity, it is characterized in that, made by the raw material of following weight portion: silver powder 43, aluminium oxide 2.6, boron oxide 3.2, citric acid 2.5, polyvinyl butyral resin 1.5, nano-graphite 3, polyethylene glycol 2, calcium nitrate 0.8, ethylenediamine 1, conduction anaerobic ceramic powder 5, auxiliary agent 40.
Described auxiliary agent is made up of following raw materials in part by weight: bismuth oxide 2, boron oxide 3, ethyl cellulose 0.9, lauryl sodium sulfate 0.3, repefral 0.4, lecithin 0.3, polysiloxanes 0.3, terpinol 24, its preparation method is bismuth oxide and boron oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds ethyl cellulose to grind 20-40 minute; Repefral, terpinol are stirred and evenly mixed, at 140-190 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add lecithin, polysiloxanes, lauryl sodium sulfate, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
Manufacture method comprises the following steps:
(1) get ethylenediamine, conduction anaerobic ceramic powder mixed grinding makes 200-300 order slurry for 2-3 hour, adds aluminium oxide, boron oxide to continue to grind 3-4 hour, spraying is dry, dries, and sends in calciner sintering 1-2 hour at 450-510 DEG C;
(2) taking polyethylene glycol is put into reactor and is heated to 55-65 DEG C, adds polyvinyl butyral resin, keeps temperature to stir 2-3 hour, dissolve completely to polyvinyl butyral resin, add calcium nitrate, citric acid, nano-graphite, insulation 30-50 minute, grinds pulping again;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
The technical indicator of processing the conductive silver paste obtaining by above-described embodiment is as follows:
(1) viscosity: 50-100PaS(Brookfield, 10RPM);
(2) adhesive force: > 10N/mm
2;
(3) plumbous cadmium content: < 100ppm;
(4) solderability excellent, burnt in a heap easily separated, printing adaptability good and solvent resistance is excellent.
Claims (2)
1. one kind conducts electricity the compound conductive silver paste of anaerobic ceramic powder/nano-graphite, it is characterized in that, made by the raw material of following weight portion: silver powder 40-50, aluminium oxide 1.5-2.6, boron oxide 2.1-3.2, citric acid 1.2-2.9, polyvinyl butyral resin 0.7-1.5, nano-graphite 2-3, polyethylene glycol 2-4, calcium nitrate 0.4-0.8, ethylenediamine 1-3, conduction anaerobic ceramic powder 2-5, auxiliary agent 30-40; Described auxiliary agent is made up of following raw materials in part by weight: bismuth oxide 2-3, boron oxide 3-4, ethyl cellulose 0.8-1.4, lauryl sodium sulfate 0.3-0.4, repefral 0.2-0.4, lecithin 0.3-0.5, polysiloxanes 0.2-0.3, terpinol 20-25, its preparation method is bismuth oxide and boron oxide to be put into calciner at 520-610 DEG C, calcine 1-2 hour, taking-up is cooled to room temperature, adds ethyl cellulose to grind 20-40 minute; Repefral, terpinol are stirred and evenly mixed, at 140-190 DEG C, react 2-3 hour, be cooled to 80-100 DEG C, add lecithin, polysiloxanes, lauryl sodium sulfate, keep temperature to stir 3-4 hour; Above each product is mixed, grind and make 300-400 order slurry and get final product for 2-4 hour.
2. a kind of manufacture method of conducting electricity the compound conductive silver paste of anaerobic ceramic powder/nano-graphite according to claim 1, is characterized in that comprising the following steps:
(1) get ethylenediamine, conduction anaerobic ceramic powder mixed grinding makes 200-300 order slurry for 2-3 hour, adds aluminium oxide, boron oxide to continue to grind 3-4 hour, spraying is dry, dries, and sends in calciner sintering 1-2 hour at 450-510 DEG C;
(2) taking polyethylene glycol is put into reactor and is heated to 55-65 DEG C, adds polyvinyl butyral resin, keeps temperature to stir 2-3 hour, dissolve completely to polyvinyl butyral resin, add calcium nitrate, citric acid, nano-graphite, insulation 30-50 minute, grinds pulping again;
(3) step (1), (2) reaction mass and other leftover materials are mixed, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, grinding to form particle diameter is 10-20 μ m slurry grain, to obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410303512.5A CN104078095A (en) | 2014-06-30 | 2014-06-30 | Conductive oxygen-free ceramic powder/nano-graphite composite conductive silver paste and preparing method thereof |
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| CN201410303512.5A CN104078095A (en) | 2014-06-30 | 2014-06-30 | Conductive oxygen-free ceramic powder/nano-graphite composite conductive silver paste and preparing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104392764A (en) * | 2014-10-17 | 2015-03-04 | 阜阳市节源照明电器有限责任公司 | Wear-resistant conductive silver paste and manufacturing method thereof |
| 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 |
| CN105810288A (en) * | 2016-04-26 | 2016-07-27 | 江阴市天邦涂料股份有限公司 | Silver-aluminum paste easy to sinter for solar cell |
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| JPH0770362A (en) * | 1993-09-07 | 1995-03-14 | Sumitomo Metal Mining Co Ltd | Conductive paste composition, boron-coated silver powder used in said composition and production of said powder |
| CN101872653A (en) * | 2010-06-28 | 2010-10-27 | 彩虹集团公司 | Nano silver conductive paste and preparation method thereof |
| CN102751000A (en) * | 2012-06-16 | 2012-10-24 | 华东微电子技术研究所合肥圣达实业公司 | Lead-free and cadmium-free electrode silver slurry for piezoelectric ceramics and preparation method thereof |
| CN102768464A (en) * | 2011-05-04 | 2012-11-07 | 上海鑫力新材料科技有限公司 | Photosensitive conductive aluminium paste and preparation method |
| CN102831952A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Conductive silver paste for environmental-friendly lead-free silicon solar cell front electrode and preparation method of conductive silver paste |
| CN103021505A (en) * | 2012-12-10 | 2013-04-03 | 滁州恒恩光电科技有限公司 | Conducting silver aluminum slurry containing dicyclohexyl phthalate |
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2014
- 2014-06-30 CN CN201410303512.5A patent/CN104078095A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0770362A (en) * | 1993-09-07 | 1995-03-14 | Sumitomo Metal Mining Co Ltd | Conductive paste composition, boron-coated silver powder used in said composition and production of said powder |
| CN101872653A (en) * | 2010-06-28 | 2010-10-27 | 彩虹集团公司 | Nano silver conductive paste and preparation method thereof |
| CN102768464A (en) * | 2011-05-04 | 2012-11-07 | 上海鑫力新材料科技有限公司 | Photosensitive conductive aluminium paste and preparation method |
| CN102751000A (en) * | 2012-06-16 | 2012-10-24 | 华东微电子技术研究所合肥圣达实业公司 | Lead-free and cadmium-free electrode silver slurry for piezoelectric ceramics and preparation method thereof |
| CN102831952A (en) * | 2012-08-24 | 2012-12-19 | 合肥中南光电有限公司 | Conductive silver paste for environmental-friendly lead-free silicon solar cell front electrode and preparation method of conductive silver paste |
| CN103021505A (en) * | 2012-12-10 | 2013-04-03 | 滁州恒恩光电科技有限公司 | Conducting silver aluminum slurry containing dicyclohexyl phthalate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104392764A (en) * | 2014-10-17 | 2015-03-04 | 阜阳市节源照明电器有限责任公司 | Wear-resistant conductive silver paste and manufacturing method thereof |
| 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 |
| CN105810288A (en) * | 2016-04-26 | 2016-07-27 | 江阴市天邦涂料股份有限公司 | Silver-aluminum paste easy to sinter for solar cell |
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Application publication date: 20141001 |