CN108766619A - A kind of electronic component electrode slurry and preparation method thereof - Google Patents
A kind of electronic component electrode slurry and preparation method thereof Download PDFInfo
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- CN108766619A CN108766619A CN201810522353.6A CN201810522353A CN108766619A CN 108766619 A CN108766619 A CN 108766619A CN 201810522353 A CN201810522353 A CN 201810522353A CN 108766619 A CN108766619 A CN 108766619A
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- 239000011267 electrode slurry Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000011521 glass Substances 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 41
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 30
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 21
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 15
- 239000011858 nanopowder Substances 0.000 claims abstract description 15
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 15
- 238000007665 sagging Methods 0.000 claims abstract description 15
- 239000000080 wetting agent Substances 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 14
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical class CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 13
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims abstract description 12
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims abstract description 12
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 16
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 15
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 8
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 8
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- -1 methyl methacrylate Ester Chemical class 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 7
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 238000009826 distribution Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000008240 homogeneous mixture Substances 0.000 claims description 6
- 229910052573 porcelain Inorganic materials 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 229910052738 indium Inorganic materials 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims 2
- 229920005989 resin Polymers 0.000 claims 2
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims 1
- FEWFXBUNENSNBQ-UHFFFAOYSA-N 2-hydroxyacrylic acid Chemical compound OC(=C)C(O)=O FEWFXBUNENSNBQ-UHFFFAOYSA-N 0.000 claims 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims 1
- 150000001924 cycloalkanes Chemical group 0.000 claims 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims 1
- 239000011701 zinc Substances 0.000 claims 1
- 229910052725 zinc Inorganic materials 0.000 claims 1
- 230000005611 electricity Effects 0.000 abstract description 6
- 238000007639 printing Methods 0.000 abstract description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 229920002647 polyamide Polymers 0.000 description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- YPIFGDQKSSMYHQ-UHFFFAOYSA-N 7,7-dimethyloctanoic acid Chemical compound CC(C)(C)CCCCCC(O)=O YPIFGDQKSSMYHQ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- WSFQLUVWDKCYSW-UHFFFAOYSA-M sodium;2-hydroxy-3-morpholin-4-ylpropane-1-sulfonate Chemical group [Na+].[O-]S(=O)(=O)CC(O)CN1CCOCC1 WSFQLUVWDKCYSW-UHFFFAOYSA-M 0.000 description 3
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 3
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical class [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 description 2
- 238000003618 dip coating Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- YFDKVXNMRLLVSL-UHFFFAOYSA-N 2-dodecylbenzenesulfonic acid;sodium Chemical compound [Na].CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O YFDKVXNMRLLVSL-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- YENIOYBTCIZCBJ-UHFFFAOYSA-N acetic acid;1-methoxypropan-2-ol Chemical compound CC(O)=O.COCC(C)O YENIOYBTCIZCBJ-UHFFFAOYSA-N 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Manufacturing & Machinery (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Conductive Materials (AREA)
Abstract
The present invention provides a kind of electronic component electrode slurrys and preparation method thereof, are prepared by the raw material of following parts by weight:70-90 parts of denatured conductive nano powder, 8-15 parts of glass powder, 7-16 parts of bisphenol A epoxide resin E-20,10-18 parts of Hydroxylated acrylic resin, 3-6 parts of 3- aminopropyl triethoxysilanes, 2-5 parts of polyethylene glycol, 3-8 parts of methyl methacrylate, 5-10 parts of propylene glycol methyl ether acetate, 4-9 parts of neodecanoic glycidyl ether, 2-7 parts of dibutyl phthalate, 1-5 parts of wetting agent, 1-4 parts of sagging inhibitor, 1-3 parts of surfactant.Electrode slurry produced by the present invention has good conductive characteristic, and relatively low as resistance after the electrode print of electronic component, electricity conversion is higher, while electrode pulling force is not less than 6N.Therefore, it is of great significance the electrode slurry as printing electrode for electronic component.
Description
Technical field
The present invention relates to a kind of electrode slurrys, and in particular to a kind of electronic component electrode slurry and preparation method thereof.
Background technology
Electrode slurry is the electronic functional material for integrating material, metallurgy, chemical industry, electronic technology, is hybrid integrated electricity
The basic material of road, sensing element, surface installation technique, resistor network, display and various electronic discrete elements etc..Through
The techniques such as silk-screen printing, levelling, drying, sintering are crossed, electrode slurry can be formed by curing conductive film on the substrates such as ceramics, can make
At thick film integrated circuit, resistor, resistor network, capacitor, multilayer ceramic capacitor, conductor ink, electrode of solar battery,
LED cold light sources, organic light emitting display, printing and high-resolution electric conductor, thin film switch/flexible circuit, conducting resinl, sensitive member
Device and other electronic components.
Electrode slurry is mainly made of function phase, Binder Phase, organic carrier three parts, and the raw material composition of electrode slurry is to determine
The key factor of fixed electrode performance.However the function of existing electrode slurry is mainly mutually silver powder, silver powder has good conduction
Performance, however silver powder is expensive and is easy to happen migration and is constantly carried with the continuous improvement to electronic component performance requirement
The performance of high electronic component and its manufacturing cost of reduction, are the key that production high-performance electric subcomponents.Therefore, it is necessary to electricity
Pole slurry is further studied.
Invention content
Above of the existing technology in order to solve the problems, such as, the purpose of the present invention is to provide a kind of electronic component electricity consumptions
Pole slurry and preparation method thereof.
To achieve the goals above, the present invention provides following technical scheme:
A kind of electronic component electrode slurry, is prepared by the raw material of following parts by weight:The silver that lauryl mercaptan is modified
70-90 parts of copper-clad nano powder, 8-15 parts of glass powder, 7-16 parts of bisphenol A epoxide resin E-20, Hydroxylated acrylic resin 10-18
Part, 3-6 parts of 3- aminopropyl triethoxysilanes, 2-5 parts of polyethylene glycol, 3-8 parts of methyl methacrylate, propylene glycol monomethyl ether acetic acid
5-10 parts of ester, 4-9 parts of neodecanoic glycidyl ether, 2-7 parts of dibutyl phthalate, 1-5 parts of wetting agent, sagging inhibitor 1-4
Part, 1-3 parts of surfactant,
The modified composite conducting nano powder is the wicker copper nano powder that lauryl mercaptan is modified;
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio are(3-10):(8-15):(15-
30):(10-20):(2-6).
Preferably, a kind of electronic component electrode slurry of the present invention, by the raw material preparation of following parts by weight
At:80 parts of denatured conductive nano powder, 12 parts of glass powder, 11 parts of bisphenol A epoxide resin E-20,14 parts of Hydroxylated acrylic resin, 3-
4.5 parts of aminopropyl triethoxysilane, 3.5 parts of polyethylene glycol, 6 parts of methyl methacrylate, propylene glycol methyl ether acetate 7.5
Part, 6.5 parts of neodecanoic glycidyl ether, 5 parts of dibutyl phthalate, 3 parts of wetting agent, 2.5 parts of sagging inhibitor, surface-active
2 parts of agent,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 6:11:23:15:4.
Preferably, one kind that the average molecular weight of the polyethylene glycol is 300,600,1000,1500 or 2000.
Preferably, the wetting agent is zinc naphthenate or Sucker plucker polyoxyethylene ether.
Preferably, the sagging inhibitor is polyamide wax.
Preferably, it is 1 that the surfactant, which is mass ratio,:(1-3)Cetab and dodecyl
Phenylbenzimidazole sulfonic acid sodium.
The preparation method of electronic component electrode slurry of the present invention, includes the following steps:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
It is warming up to 650-800 DEG C, keeps the temperature 1h, 1100-1250 DEG C of melting 1-2h is then warming up to again, the glass water quenching after melting is obtained
Glass grit is used in combination ball milling that glass powder average grain diameter is made to be≤8 μm;
(2)Glass powder is mixed, it is molten to be added to the ethyl alcohol that 5-10 times of parts by weight polyethylene glycol mass fraction is 10-20wt%
In liquid, reaction 20-40min is stirred at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 90-120 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 1-2h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
Further, the viscosity of electrocondution slurry obtained is 40-70Pas.
Advantageous effect:The present invention provides a kind of electronic component electrode slurrys and preparation method thereof, are tied by testing
Fruit is it is found that electrode slurry produced by the present invention has good conductive characteristic, as resistance after the electrode print of electronic component
Relatively low, electricity conversion is higher, and wicker copper nano powder is modified through lauryl mercaptan, and the dispersibility in system obtains
Great raising, to further improve the uniformity that conductive powder body after slurry brushing is distributed in substrate, to electrode
The raising of slurry electric conductivity plays an important role.Organic carrier in the application raw material is through 3- aminopropyl triethoxysilanes
It is crosslinked so that cross-linking system forms fine and close reticular structure, so as to improve electrical-conductive nanometer powder and glass powder in organism
Adhesive force, prevent powder from being migrated in system, show that electrode pulling force is not less than by the tensile test result to electrode
6N.Therefore, it is of great significance the electrode slurry as printing electrode for electronic component.
Specific implementation mode
The invention will now be further described with reference to specific embodiments, but examples are merely exemplary, not to this hair
Bright range constitutes any restrictions.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
Can the details and form of technical solution of the present invention be modified or be replaced, but these modifications and replacement each fall within the present invention's
In protection domain.
The preparation method of the wicker copper nano powder is:
8g copper acetates (II) hydrate is added in the ammonium hydroxide of 3mL 25wt% and the solution of 7mL water to form blue solution, so
Afterwards, 0.5mL 10M NaOH solutions are added to form light blue precipitate slurry;Then the hydrazine hydrate solution of 5mL 50wt% is added
Into reaction system, 30min is vigorously stirred in nitrogen atmosphere at room temperature, forms nano-particle of copper solution;It is micro- to copper nanometer
Grain solution in be added silver nitrate make its final concentration of 10%, then into solution be added 2mL mass fractions be 1% ascorbic acid it is molten
Liquid, is stirred at room temperature reaction 1h, and supernatant collection lower sediment particle is removed by centrifugation;
1g lauryl mercaptans are added in 2mL methanol solutions, mixture A is formed, mixture A is added in precipitation particle will
Particle is resuspended, and 1h is vigorously stirred in the environment of nitrogen, and upper solution is removed by centrifugation, and 2- is cleaned using deionized water
It 3 times, is finally cleaned once with 10mL methanol, by the way that precipitation particle is collected by centrifugation, is then placed in the precipitation particle of collection very again
Altitude dries the wicker copper nano powder being modified to get lauryl mercaptan.
Embodiment 1
A kind of electronic component electrode slurry, is prepared by the raw material of following parts by weight:The silver that lauryl mercaptan is modified
80 parts of copper-clad nano powder, 12 parts of glass powder, 11 parts of bisphenol A epoxide resin E-20,14 parts of Hydroxylated acrylic resin, 3- aminopropyls
4.5 parts of triethoxysilane, 3.5 parts of polyethylene glycol, 6 parts of methyl methacrylate, 7.5 parts of propylene glycol methyl ether acetate, the new last of the ten Heavenly stems
6.5 parts of acid glycidyl ether, 5 parts of dibutyl phthalate, 3 parts of wetting agent, 2.5 parts of sagging inhibitor, 2 parts of surfactant,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 6:11:23:15:4.
The average molecular weight of the polyethylene glycol is 1000.
The wetting agent is zinc naphthenate.
The sagging inhibitor is polyamide wax.
The surfactant is that mass ratio is 1:2 cetab and sodium dodecylbenzenesulfonate.
The preparation method of electronic component electrode slurry of the present invention, includes the following steps:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
720 DEG C are warming up to, 1h is kept the temperature, 1180 DEG C of melting 1.5h is then warming up to again, the glass water quenching after melting is obtained into glass grit,
Ball milling be used in combination that glass powder average grain diameter is made to be≤8 μm;
(2)Glass powder is mixed, is added in the ethanol solution that 8 times of parts by weight polyethylene glycol mass fractions are 15wt%,
It is stirred to react 30min at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 105 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 1.5h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
Embodiment 2
A kind of electronic component electrode slurry, is prepared by the raw material of following parts by weight:The silver that lauryl mercaptan is modified
70 parts of copper-clad nano powder, 8 parts of glass powder, 7 parts of bisphenol A epoxide resin E-20,10 parts of Hydroxylated acrylic resin, 3- aminopropyls three
3 parts of Ethoxysilane, 2 parts of polyethylene glycol, 3 parts of methyl methacrylate, 5 parts of propylene glycol methyl ether acetate, neodecanoic acid shrink sweet
4 parts of oily ether, 2 parts of dibutyl phthalate, 1 part of wetting agent, 1 part of sagging inhibitor, 1 part of surfactant,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 3:8:15:10:2.
The average molecular weight of the polyethylene glycol is 300.
The wetting agent is zinc naphthenate.
The sagging inhibitor is polyamide wax.
The surfactant is that mass ratio is 1:1 cetab and sodium dodecylbenzenesulfonate.
The preparation method of electronic component electrode slurry of the present invention, includes the following steps:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
650 DEG C are warming up to, 1h is kept the temperature, 1100 DEG C of melting 1h is then warming up to again, the glass water quenching after melting is obtained into glass grit, and
Glass powder average grain diameter is set to be≤8 μm with ball milling;
(2)Glass powder is mixed, is added in the ethanol solution that 5 times of parts by weight polyethylene glycol mass fractions are 10wt%,
It is stirred to react 20min at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 90 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 1h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
Embodiment 3
A kind of electronic component electrode slurry, is prepared by the raw material of following parts by weight:The silver that lauryl mercaptan is modified
75 parts of copper-clad nano powder, 10 parts of glass powder, 10 parts of bisphenol A epoxide resin E-20,12 parts of Hydroxylated acrylic resin, 3- aminopropyls
4 parts of triethoxysilane, 3 parts of polyethylene glycol, 4 parts of methyl methacrylate, 6 parts of propylene glycol methyl ether acetate, neodecanoic acid shrink
5 parts of glycerin ether, 4 parts of dibutyl phthalate, 2 parts of wetting agent, 2 parts of sagging inhibitor, 1.5 parts of surfactant,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 4:10:20:12:3.
The average molecular weight of the polyethylene glycol is 600.
The wetting agent is Sucker plucker polyoxyethylene ether.
The sagging inhibitor is polyamide wax.
The surfactant is that mass ratio is 1:1.5 cetab and dodecylbenzene sulfonic acid
Sodium.
The preparation method of electronic component electrode slurry of the present invention, includes the following steps:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
700 DEG C are warming up to, 1h is kept the temperature, 1120 DEG C of melting 1.3h is then warming up to again, the glass water quenching after melting is obtained into glass grit,
Ball milling be used in combination that glass powder average grain diameter is made to be≤8 μm;
(2)Glass powder is mixed, the ethanol solution that 6 times of parts by weight polyethylene glycol mass fractions are 10-20wt% is added to
In, reaction 25min is stirred at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 100 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 1.3h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
Embodiment 4
A kind of electronic component electrode slurry, is prepared by the raw material of following parts by weight:The silver that lauryl mercaptan is modified
90 parts of copper-clad nano powder, 15 parts of glass powder, 16 parts of bisphenol A epoxide resin E-20,18 parts of Hydroxylated acrylic resin, 3- aminopropyls
6 parts of triethoxysilane, 5 parts of polyethylene glycol, 8 parts of methyl methacrylate, 10 parts of propylene glycol methyl ether acetate, neodecanoic acid shrink
9 parts of glycerin ether, 7 parts of dibutyl phthalate, 5 parts of wetting agent, 4 parts of sagging inhibitor, 3 parts of surfactant,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 10:15:30:20:6.
The average molecular weight of the polyethylene glycol is 2000.
The wetting agent is Sucker plucker polyoxyethylene ether.
The sagging inhibitor is polyamide wax.
The surfactant is that mass ratio is 1:3 cetab and sodium dodecylbenzenesulfonate.
The preparation method of electronic component electrode slurry of the present invention, includes the following steps:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
800 DEG C are warming up to, 1h is kept the temperature, 1250 DEG C of melting 2h is then warming up to again, the glass water quenching after melting is obtained into glass grit, and
Glass powder average grain diameter is set to be≤8 μm with ball milling;
(2)Glass powder is mixed, is added in the ethanol solution that 10 times of parts by weight polyethylene glycol mass fractions are 20wt%,
Reaction 40min is stirred at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 120 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 2h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
Comparative example 1
Difference lies in what is added in comparative example 1 is unmodified electrical-conductive nanometer powder to comparative example 1 with embodiment 1.
Comparative example 2
Difference lies in be not added with 3- aminopropyl triethoxysilanes to comparative example 2 with embodiment 1 in comparative example 2.
The technical solution of embodiment 1-4 and comparative example 1-2 is subjected to following performance test, test result is as shown in table 1:
Solderability:1cm x 1cm areas, after sintering, the rosin alcoholic solution of surface dip-coating 2% are printed on silicon chip
It as scaling powder, is dipped vertically into 220 DEG C of Sn62Pb36Ag2 tin pots 1-3 seconds, calculates 1cm2The area of tin accounts for total face in upper leaching
Product ratio >=95%.
Soldering resistance:By burned 1cm2After solderability testing piece dip-coating alcohol rosin flux, 220 DEG C are immersed
In Sn62Pb36Ag2 tin pots, the time > that is corroded completely of observation sinter layer 10 seconds.
Adhesive force:Conductive silver slurry is printed on the front of semi-finished product crystal silicon solar batteries and is burnt through standard manufacturing process
As positive silver electrode 45° angle peeling force, electrocondution slurry of the present invention are tested with puller system with standard tin-coated copper strip automatic welding
The electrode adhesion of firing(Mean value)> 8.64N.
By test result as it can be seen that the electrocondution slurry of the present invention has good conductive characteristic, as electronic component
Resistance is relatively low after electrode print, and electricity conversion is higher, while lauryl mercaptan is modified wicker copper nano powder to electrode slurry
The raising of the electric conductivity of material plays an important role.Show that electrode pulling force is not less than by the tensile test result to electrode
6N is of great significance the electrode slurry as printing electrode for electronic component.
Table 1
Claims (8)
1. a kind of electronic component electrode slurry, which is characterized in that be prepared by the raw material of following parts by weight:Dodecyl
Mercaptan modified 70-90 parts of wicker copper nano powder, 8-15 parts of glass powder, 7-16 parts of bisphenol A epoxide resin E-20, hydroxy
10-18 parts of acid resin, 3-6 parts of 3- aminopropyl triethoxysilanes, 2-5 parts of polyethylene glycol, 3-8 parts of methyl methacrylate, third
5-10 parts of glycol methyl ether acetate, 4-9 parts of neodecanoic glycidyl ether, 2-7 parts of dibutyl phthalate, 1-5 parts of wetting agent,
1-4 parts of sagging inhibitor, 1-3 parts of surfactant;
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio are(3-10):(8-15):(15-
30):(10-20):(2-6).
2. a kind of electronic component electrode slurry according to claim 1, which is characterized in that by following parts by weight
Raw material is prepared:80 parts of denatured conductive nano powder, 12 parts of glass powder, 11 parts of bisphenol A epoxide resin E-20, hydroxy acrylic acid
14 parts of resin, 4.5 parts of 3- aminopropyl triethoxysilanes, 3.5 parts of polyethylene glycol, 6 parts of methyl methacrylate, propylene glycol monomethyl ether
7.5 parts of acetate, 6.5 parts of neodecanoic glycidyl ether, 5 parts of dibutyl phthalate, 3 parts of wetting agent, sagging inhibitor 2.5
Part, 2 parts of surfactant,
The group of the glass powder becomes:Bi2O3、Sb2O3、SiO2、ZnO、Na2O, mass ratio 6:11:23:15:4.
3. a kind of electronic component electrode slurry according to claim 1, which is characterized in that the polyethylene glycol is put down
One kind that average molecular weight is 300,600,1000,1500 or 2000.
4. a kind of electronic component electrode slurry according to claim 1, which is characterized in that the wetting agent is cycloalkanes
Sour zinc or Sucker plucker polyoxyethylene ether.
5. a kind of electronic component electrode slurry according to claim 1, which is characterized in that the sagging inhibitor is poly-
Amide waxe.
6. a kind of electronic component electrode slurry according to claim 1, which is characterized in that the surfactant is
Mass ratio is 1:(1-3)Cetab and sodium dodecylbenzenesulfonate.
7. the preparation method of claim 1-6 any one of them electronic component electrode slurrys, which is characterized in that including with
Lower step:
(1)The preparation of glass powder:Each raw material is weighed by weight, is uniformly mixed in porcelain crucible, is melted in Muffle furnace, first
It is warming up to 650-800 DEG C, keeps the temperature 1h, 1100-1250 DEG C of melting 1-2h is then warming up to again, the glass water quenching after melting is obtained
Glass grit is used in combination ball milling that glass powder average grain diameter is made to be≤8 μm;
(2)Glass powder is mixed, it is molten to be added to the ethyl alcohol that 5-10 times of parts by weight polyethylene glycol mass fraction is 10-20wt%
In liquid, reaction 20-40min is stirred at room temperature, obtains mixture A;
(3)By bisphenol A epoxide resin E-20, Hydroxylated acrylic resin, 3- aminopropyl triethoxysilanes, methyl methacrylate
Ester, propylene glycol methyl ether acetate, neodecanoic glycidyl ether, dibutyl phthalate are mixed according to corresponding parts by weight,
It is heated to 90-120 DEG C in the state of stirring, this temperature is kept to continue to be stirred to react 1-2h, mixture B is made;
(4)Denatured conductive nano powder, mixture A, mixture B and remaining remaining raw material are added in de-airing mixer and stir 2h,
Homogeneous mixture is formed, then through three-high mill grinding distribution, is ground into homogeneous slurry, control scraper plate fineness≤10 μm, then pass through
500 mesh silk screen filters obtain electronic component electrode slurry.
8. the preparation method of electronic component electrode slurry according to claim 7, which is characterized in that conduction obtained
The viscosity of slurry is 40-70Pas.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN112951482A (en) * | 2021-02-26 | 2021-06-11 | 无锡帝科电子材料股份有限公司 | Electronic component slurry and processing technology |
CN114093551A (en) * | 2020-08-24 | 2022-02-25 | 日油株式会社 | Conductive composition |
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CN105788758A (en) * | 2016-03-21 | 2016-07-20 | 江苏时空涂料有限公司 | Method for preparing low-cost lead-free photosensitive electrode paste |
CN107614423A (en) * | 2015-05-15 | 2018-01-19 | 富士胶片株式会社 | Core-shell particles, the manufacture method of core-shell particles and film |
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CN104036876A (en) * | 2014-06-12 | 2014-09-10 | 西安工程大学 | Preparation method of high-temperature copper electronic paste |
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