CN104157324B - A kind of green mud stone powder conductive silver paste and preparation method thereof - Google Patents
A kind of green mud stone powder conductive silver paste and preparation method thereof Download PDFInfo
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- CN104157324B CN104157324B CN201410368786.2A CN201410368786A CN104157324B CN 104157324 B CN104157324 B CN 104157324B CN 201410368786 A CN201410368786 A CN 201410368786A CN 104157324 B CN104157324 B CN 104157324B
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- stone powder
- mud stone
- green mud
- silver paste
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- 239000000843 powder Substances 0.000 title claims abstract description 23
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000004575 stone Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 8
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- -1 diocyl sodium sulfosuccinate Chemical compound 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 229910052580 B4C Inorganic materials 0.000 claims abstract description 7
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012964 benzotriazole Substances 0.000 claims abstract description 7
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004327 boric acid Substances 0.000 claims abstract description 7
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- 239000013078 crystal Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000011609 ammonium molybdate Substances 0.000 claims abstract description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims abstract description 5
- 229940010552 ammonium molybdate Drugs 0.000 claims abstract description 5
- 235000018660 ammonium molybdate Nutrition 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 7
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 6
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 6
- 229910052810 boron oxide Inorganic materials 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical group O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 6
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 6
- 238000004537 pulping Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000005476 soldering Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229910052793 cadmium Inorganic materials 0.000 description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
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- Parts Printed On Printed Circuit Boards (AREA)
Abstract
The invention discloses a kind of green mud stone powder conductive silver paste, it is characterized in that, be made up of the raw material of following weight portion: argentum powder 40-50, green mud stone powder 4-6, calcium carbonate crystal whisker 2-4, benzotriazole 2.1-3.5, ammonium molybdate 0.4-0.8, boric acid 1.2-3.2, citric acid 1.1-2.2, boron carbide 3-5, diocyl sodium sulfosuccinate 1.4-2.7, auxiliary agent 30-40, suitable quantity of water; The green mud stone powder conductive silver paste of the present invention, has the advantages such as resistance is little, soldering resistance is excellent, and can increase printed resolution, improves production efficiency, and cost is low, is conducive to carrying out of environmental protection work.
Description
Technical field
The present invention relates to conductive silver paste field, be specifically related to a kind of green mud stone powder conductive silver paste and preparation method thereof.
Background technology
Conductive silver paste refers to and is printed on conduction stock, so as to there is conduction electric current and get rid of the silver slurry of accumulation electrostatic charge ability, being usually on non-conductive stocks such as being imprinted on 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 existing conductive silver paste has disadvantages that in the market, do not contain only lead, cadmium etc. and poisonous, contaminated environment, and when being used on conduction stock, adhesive force is low, soldering resistance is not good, and sintering character is poor.
Summary of the invention
It is an object of the invention to provide a kind of green mud stone powder 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 green mud stone powder conductive silver paste, it is characterized in that, be made up of the raw material of following weight portion: argentum powder 40-50, green mud stone powder 4-6, calcium carbonate crystal whisker 2-4, benzotriazole 2.1-3.5, ammonium molybdate 0.4-0.8, boric acid 1.2-3.2, citric acid 1.1-2.2, boron carbide 3-5, diocyl sodium sulfosuccinate 1.4-2.7, auxiliary agent 30-40, suitable quantity of water.
Described auxiliary agent is made up of following raw materials in part 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 order slurry and get final product.
The preparation method of described a kind of green mud stone powder conductive silver paste, it is characterised in that comprise the following steps:
(1) take green mud stone powder, calcium carbonate crystal whisker adds suitable quantity of water and grinds pulping, pelletize, puts in calcining furnace and sinters 2-3 hour at 620-680 DEG C, takes out cooling, adds boric acid and grinds together 1-2 hour;
(2) citric acid, benzotriazole are added water and stir 10-20 minute, put into boron carbide and grind 2-3 hour pulping, spray drying;
(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 10-20 μm of slurry grain, to obtain final product.
The present invention has following beneficial effect: the green mud stone powder conductive silver paste of the present invention, has the advantages such as resistance is little, soldering resistance is excellent, and can increase printed resolution, improves production efficiency, and cost is low, is conducive to carrying out of environmental protection work.
Detailed description of the invention
Described a kind of green mud stone powder conductive silver paste, it is characterized in that, be made up of the raw material of following weight portion: argentum powder 42, green mud stone powder 4, calcium carbonate crystal whisker 3, benzotriazole 2.1, ammonium molybdate 0.8, boric acid 3.2, citric acid 1.1, boron carbide 3, diocyl sodium sulfosuccinate 2.7, auxiliary agent 33, suitable quantity of water.
Described auxiliary agent is made up of following raw materials in part by weight: aluminium sesquioxide 2, boron oxide 4, polyvinyl alcohol 7, Colophonium 15,3-aminopropyl trimethoxysilane 1.5, polydimethylsiloxane 0.3, acetone 12, 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 order slurry and get final product.
Manufacture method comprises the following steps:
(1) take green mud stone powder, calcium carbonate crystal whisker adds suitable quantity of water and grinds pulping, pelletize, puts in calcining furnace and sinters 2-3 hour at 620-680 DEG C, takes out cooling, adds boric acid and grinds together 1-2 hour;
(2) citric acid, benzotriazole are added water and stir 10-20 minute, put into boron carbide and grind 2-3 hour pulping, spray drying;
(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 10-20 μm of slurry 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) sheet resistance: < 5m Ω/c;
(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. a green mud stone powder conductive silver paste, it is characterized in that, be made up of the raw material of following weight portion: argentum powder 40-50, green mud stone powder 4-6, calcium carbonate crystal whisker 2-4, benzotriazole 2.1-3.5, ammonium molybdate 0.4-0.8, boric acid 1.2-3.2, citric acid 1.1-2.2, boron carbide 3-5, diocyl sodium sulfosuccinate 1.4-2.7, auxiliary agent 30-40, suitable quantity of water; Described auxiliary agent is made up of following raw materials in part 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 order slurry and get final product.
2. the manufacture method of a green mud stone powder conductive silver paste as claimed in claim 1, it is characterised in that comprise the following steps:
(1) take green mud stone powder, calcium carbonate crystal whisker adds suitable quantity of water and grinds pulping, pelletize, puts in calcining furnace and sinters 2-3 hour at 620-680 DEG C, takes out cooling, adds boric acid and grinds together 1-2 hour;
(2) citric acid, benzotriazole are added water and stir 10-20 minute, put into boron carbide and grind 2-3 hour pulping, spray drying;
(3) reaction mass step (1), step (2) obtained and leftover materials ammonium molybdate, diocyl sodium sulfosuccinate and auxiliary agent mixing, be warming up to 100-120 DEG C, stirring reaction 1-2 hour, cooling, and grinding to form particle diameter is 10-20 μm of slurry grain, to obtain final product.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410368786.2A CN104157324B (en) | 2014-07-30 | 2014-07-30 | A kind of green mud stone powder conductive silver paste and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410368786.2A CN104157324B (en) | 2014-07-30 | 2014-07-30 | A kind of green mud stone powder conductive silver paste and preparation method thereof |
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| Publication Number | Publication Date |
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| CN104157324A CN104157324A (en) | 2014-11-19 |
| CN104157324B true CN104157324B (en) | 2016-06-15 |
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| CN106782743A (en) * | 2016-12-08 | 2017-05-31 | 姚均甫 | Compound conductive silver paste of a kind of wollastonite and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JPH10106349A (en) * | 1996-09-30 | 1998-04-24 | Tanaka Kikinzoku Kogyo Kk | Silver-based conductive paste |
| CN103177787A (en) * | 2011-12-26 | 2013-06-26 | 比亚迪股份有限公司 | Conductive powder used for preparing conductive silver paste and conductive silver paste |
| CN103559939A (en) * | 2013-09-22 | 2014-02-05 | 江苏瑞德新能源科技有限公司 | Solar cell positive silver paste suitable for high-temperature sintering |
| CN103903677A (en) * | 2014-03-18 | 2014-07-02 | 上海志感电子科技有限公司 | Medium temperature sintering type electro-conduction slurry with lead-free glass powder and preparation method of medium temperature sintering type electro-conduction slurry |
-
2014
- 2014-07-30 CN CN201410368786.2A patent/CN104157324B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JPH10106349A (en) * | 1996-09-30 | 1998-04-24 | Tanaka Kikinzoku Kogyo Kk | Silver-based conductive paste |
| CN103177787A (en) * | 2011-12-26 | 2013-06-26 | 比亚迪股份有限公司 | Conductive powder used for preparing conductive silver paste and conductive silver paste |
| CN103559939A (en) * | 2013-09-22 | 2014-02-05 | 江苏瑞德新能源科技有限公司 | Solar cell positive silver paste suitable for high-temperature sintering |
| CN103903677A (en) * | 2014-03-18 | 2014-07-02 | 上海志感电子科技有限公司 | Medium temperature sintering type electro-conduction slurry with lead-free glass powder and preparation method of medium temperature sintering type electro-conduction slurry |
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| CN104157324A (en) | 2014-11-19 |
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