CN104858437A - Nano silver paste for printing conducting circuit and preparation method of nano silver paste - Google Patents
Nano silver paste for printing conducting circuit and preparation method of nano silver paste Download PDFInfo
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- CN104858437A CN104858437A CN201510198265.1A CN201510198265A CN104858437A CN 104858437 A CN104858437 A CN 104858437A CN 201510198265 A CN201510198265 A CN 201510198265A CN 104858437 A CN104858437 A CN 104858437A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000007639 printing Methods 0.000 title abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000006185 dispersion Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 11
- 230000000996 additive effect Effects 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 11
- 229910052709 silver Inorganic materials 0.000 claims description 57
- 239000004332 silver Substances 0.000 claims description 57
- 239000002270 dispersing agent Substances 0.000 claims description 19
- 238000009736 wetting Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 15
- 239000013008 thixotropic agent Substances 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 8
- 239000004925 Acrylic resin Substances 0.000 claims description 6
- 229920000178 Acrylic resin Polymers 0.000 claims description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000001856 Ethyl cellulose Substances 0.000 claims description 6
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 229920001249 ethyl cellulose Polymers 0.000 claims description 6
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims description 6
- 229940090181 propyl acetate Drugs 0.000 claims description 6
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims description 6
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 5
- 239000004952 Polyamide Substances 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 4
- WVYWICLMDOOCFB-UHFFFAOYSA-N 4-methyl-2-pentanol Chemical compound CC(C)CC(C)O WVYWICLMDOOCFB-UHFFFAOYSA-N 0.000 claims description 4
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 4
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 4
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 claims description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 2
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 claims description 2
- 125000002723 alicyclic group Chemical group 0.000 claims description 2
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 claims description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 2
- 239000000470 constituent Substances 0.000 claims description 2
- WZWSOGGTVQXXSN-UHFFFAOYSA-N cyclohexanone;toluene Chemical compound CC1=CC=CC=C1.O=C1CCCCC1 WZWSOGGTVQXXSN-UHFFFAOYSA-N 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 239000008096 xylene Substances 0.000 claims description 2
- 238000005452 bending Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 12
- 239000002002 slurry Substances 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 9
- 238000005245 sintering Methods 0.000 description 9
- 239000000758 substrate Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910021389 graphene Inorganic materials 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229920000728 polyester Polymers 0.000 description 5
- 229920000570 polyether Polymers 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 235000014113 dietary fatty acids Nutrition 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 229930195729 fatty acid Natural products 0.000 description 3
- 150000004665 fatty acids Chemical class 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 229920000768 polyamine Polymers 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 230000008602 contraction Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- -1 ethylene glycol monobutyl ether ester Chemical class 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- MRNHPUHPBOKKQT-UHFFFAOYSA-N indium;tin;hydrate Chemical compound O.[In].[Sn] MRNHPUHPBOKKQT-UHFFFAOYSA-N 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses nano silver paste for a high-precision printing conducting circuit. The nano silver paste comprises the following substances in percentage by mass: 70-85% of nano-silver particles, 5-15% of a solvent, 5-13% of a binder and 2-5% of an additive. A preparation method of the nano silver paste comprises the following steps: adding the solvent, binder and additive in a high-speed disperser to enable the solvent, binder and additive to be fully and uniformly mixed to form a binding carrier; adding the nano-silver particles, and adopting a high-speed dispersion method to uniformly disperse the nano-silver particles in the binding carrier so as to form the nano silver paste. The obtained nano silver paste can be widely applied to the printing conducting circuit by adopting the all-printed electronic technique to form a conducting circuit with high electroconductivity, high-precision and excellent bending resistance.
Description
Technical field
The invention belongs to nano material and printing technology, be specifically related to a kind of preparation method of high accuracy conductive circuit nanometer silver paste.
Background technology
Printed electronics manufactures a new technology of electronic device based on traditional printing methods, can be widely used in large area, the various electronics of flexibility and low cost or photovoltaic.In " 13 " science and technology development forecasting that in August, 2014, the Ministry of Science and Technology promulgated, printed electronic material and technique lists one of prediction field first in.China in 2002 replaces the U.S. becomes the large wiring board producing country in third place in the world, China's production in 2003 and export amount all reach 6,000,000,000 U.S. dollars, 2007-2011 annual growth reaches 9.6%, be greater than 2.5% of the world, 2012 annual value of production reach 22,000,000,000 U.S. dollars, within 2013, China improves further in technology, management etc., and estimate that 2015 annual value of production reach 27,900,000,000 U.S. dollars, growth rate is stabilized in 5% thereafter.Existing 3000 many enterprises in the whole nation carry out printed substrate (PCB) and make, and larger enterprise focuses mostly in coastal area, and Shenzhen is more, and the enterprise of maximum-norm is Shenzhen Shennan Circuits Co., Ltd., and its profit reaches 2,600,000,000 yuan.Traditional etch process, equipment investment is high, production process reaches 26 steps, and discharging of waste liquid is large, and acidic etching waste liquid discharge capacity is about 2,560,000 tons/day, environment is made seriously polluted, production cost is high, and occupation area of equipment is large, and production efficiency is low, and the printed substrate obtained only plays support and the effect being connected electronic devices and components, i.e. conducting wire plate in the electronic device; The electronic circuit board that printed electronics obtains, owing to base material containing electronic component (as multi-layer sheet embedded set resistance, electric capacity, and embedding IC device etc.) and connection line, directly can form functional electronic circuit, the microminiaturization for electronic equipment is implemented to become possibility.
Existing conductive circuit is mainly based on silver-colored pulp material, the live width of traditional silver slurry silk-screen mode, line-spacing can not meet the demand of ultra-narrow frame, and adopt full printed electronics technology and nanometer silver paste technology to combine significantly to reduce live width, improve the high-accuracy property of conducting wire.Nano-silver powder prepares slurry as main functionality, the advantage that it substitutes traditional micro-silver powder is as follows: the silver paste that (1) produces with nano-silver powder is finer and smoother, finer and close conductive coating can be obtained by serigraphy, with the conduction live width <80 μm that nanometer silver paste is obtained, conductive film layer thickness G reatT.GreaT.GT3 μm; (2) few than micron order silver powder of the use amount of nano-silver powder, can reduce costs 5% ~ 10%; (3) traditional micron size conductive silver slurry sintering processing temperature is greater than 500 DEG C, and nanometer silver paste sintering temperature can be less than 300 DEG C, and sintering temperature reduces 40% ~ 60%, reduces the resistant to elevated temperatures requirement of substrate material.
At present, the patent about the preparation method of nanometer silver paste has a lot, but existing patent just simply relates to preparation method and nanometer silver paste for conductive circuit plate has no report.
" a kind of chip attachment nanometer silver paste preparation method " (201210426581.6), Li Mingyu etc. provide a kind of method preparing chip attachment nanometer silver paste, and preparation method is: stir in reducing agent and dispersant instillation liquor argenti nitratis ophthalmicus; The solution of gained is carried out centrifugation, and obtaining upper strata is mixed solution, and lower floor is the nano-Ag particles of precipitation; After isolated nano-Ag particles washed with de-ionized water, then with electrolyte solution flocculation, again separate out the nano-Ag particles that can carry out centrifugation; Nano-Ag particles carried out repeatedly clean, flocculate, repeatedly centrifugal, finally obtain water-soluble nano silver slurry; The nanometer silver paste obtained acts on chip and substrate surface interconnects, by adding thermosetting sintered joint in hot blast workbench or stove.
" a kind of low temperature-sintered nano silver paste preparation method " (201110104399.4), Wang Yong etc. disclose a kind of low temperature-sintered nano silver paste preparation method, and nanometer silver paste preparation method is: by ethanolic solution Heating Water, add component mixing, zero centigrade ultrasonic disperse, mechanical agitation and vacuum drying; The sintering temperature that this preparation method has silver slurry significantly reduces, and the feature that thermal conductivity is high, efficiently solves the heat dissipation problem of encapsulation.Be applicable to being applied to the Novel hot boundary material as power-type chip interconnects in Electronic Packaging field.
" a kind of technique adopting nanometer silver paste to make touch-screen " (201310394497.5), Bai Axiang etc. provide a kind of technique adopting nanometer silver paste to make touch-screen, adopt this technique, decrease manufacturing procedure, overcome tin indium oxide cost high, the shortcomings such as complex process; Have that equipment investment is few, technique be simple, be easy to the advantages such as control, and due to the touch-screen pliability adopting this technique to make good, the touch-control of final touch-screen Realization of Product is effective.
" a kind of redox graphene Nano Silver slurry, preparation method and application thereof " (201410484093.X), Huang Qiaoyin etc. provide a kind of redox graphene Nano Silver slurry, preparation method and application thereof, belong to solar cell and manufacture field.Wherein redox graphene Nano Silver slurry is mixed redox graphene nano-silver thread compound, glass dust and organic bond, utilizes three-high mill to roll below fineness to 15 μm and make; The redox graphene Nano Silver slurry with light transmission provided by the invention can reduce the impact of electrode shading, and its low resistance, high connductivity density help the conversion efficiency improving solar cell; Realize this material of graphene nano silver as the anode silver paste of solar cell, reduce the component of silver in existing anode silver paste, greatly reduce production cost, help universal this green energy resource further.
" low-temperature sintering silver nanoparticle composition and the electronic article using said composition and formed " (201080039335.4), Gregory be originally provided between low-temperature short-time sinter, the good and making of low-resistance silver-colored conductive film and wiring with the adaptation of substrate, with the use of the combination and article thereof that realize Nano silver grain.The principal component of silver nanoparticle composition solvent is water; the pH of composition is in the scope of 5.3 ~ 8.0; Nano silver grain contained in said composition is protected by organic acid or derivatives thereof, the content of this organic acid or derivatives thereof relative to silver in the scope of 2 ~ 20%.
Summary of the invention
The object of the invention is to provide a kind of high accuracy conductive circuit nanometer silver paste, and its constituent and mass percent are nano-Ag particles 70% ~ 85%, solvent 5% ~ 15%, binding agent 5% ~ 13%, additive 2% ~ 5%.
Described nano-Ag particles average grain diameter is 10 ~ 30nm.
Described solvent is one or more mixtures in aromatic hydrocarbon, aliphatic hydrocarbon, alicyclic, ester, diol, derivatives, alcohol.
Described solvent is one or more mixtures in benzene,toluene,xylene, pentane, hexane, octane, cyclohexane, cyclohexanone, toluene cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, 1-Methoxy-2-propyl acetate, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethanol, isopropyl alcohol, methyl isobutyl carbinol.
Described binding agent is the mixture of one or more in polyvinyl alcohol, acrylic resin, ethyl cellulose.
Described additive is one or more mixtures in wetting dispersing agent, thixotropic agent, and wherein wetting dispersing agent is 1. fatty acid wetting dispersing agent: BYK-130, BYK-192 etc.; 2. polyester and polyether polymer class wetting dispersing agent: BYK-110, BYK-180 etc.; 3. modified high-molecular amount polyamines class wetting dispersing agent: BYK-140, BYK-142 etc.; 4. polyurethanes wetting dispersing agent: BYK-163, BYK-174 etc.; Thixotropic agent is aerosil, rilanit special, polyamide wax etc.
Another object of the present invention is to provide the preparation method of above-mentioned conductive circuit nanometer silver paste, and concrete operations are as follows:
(1) add in high speed dispersor by solvent, binding agent and additive, under normal temperature, normal pressure, 9000 ~ 20000 rpm high-speed stirred 10 ~ 60s, make solvent, binding agent and additive fully mix and form bonding carrier;
(2) adopted by nano-Ag particles high speed dispersion process to be dispersed in bonding carrier, namely form nanometer silver paste, wherein dispersion condition is under normal temperature, normal pressure, 9000 ~ 20000 rpm high-speed stirred 10 ~ 60s.
The inventive method reduces nano-Ag particles sintering temperature, reduces the resistant to elevated temperatures requirement of substrate material simultaneously, improves coating quality and production efficiency, have consumption silver low, cost is low; Whole production process is pollution-free, has the feature without open interface; The nanometer silver paste that the present invention obtains can be uniformly dispersed in bonding carrier due to nano-Ag particles, and in sintering process, the volume contraction of slurry is even, effectively can solve the contraction broken string phenomenon of slug type silver slurry, improve the adhesion of conductive silver wire and substrate; Nano-Ag particles sintering temperature is low, and the sintering temperature of Nano Silver reduces along with the reduction of its particle diameter, its this characteristic not only reduces the resistant to elevated temperatures requirement of substrate material, be conducive to improving coating quality and production efficiency, silver consumption and cost are reduced, silver powder is also made to be easy to form continuous print conducting circuit in sintering process, not only good conductivity, and oxidation resistance is strong.The nanometer silver paste that the present invention obtains adopts full printed electronics technology can be widely used in conductive circuit, forms the conducting wire of high conductivity, high accuracy and good buckle resistance.
Detailed description of the invention
Below by embodiment, the present invention is described in further detail, but protection scope of the present invention is not limited to described content.
embodiment 1:this high accuracy conductive circuit nanometer silver paste, its component and mass percent as follows:
Average grain diameter is the nano-Ag particles 70% of 10nm
Ethylene glycol monobutyl ether 8%
Cyclohexanone 7%
Acrylic resin 13%
Polyester and polyether polymer class wetting dispersing agent BYK-110 2%;
The preparation method of above-mentioned nanometer silver paste, step is as follows:
1) 70g cyclohexanone, 80g ethylene glycol monobutyl ether, 130g acrylic resin and 20g polyester and polyether polymer class wetting dispersing agent BYK-110 are added in high speed dispersor, each component 9000rpm high-speed stirred 35s under normal temperature and pressure conditions is fully mixed, forms bonding carrier;
2) by 700g average grain diameter be 10nm nano-Ag particles adopt high speed dispersion process be dispersed in bonding carrier in, can nanometer silver paste be formed, wherein dispersion condition: normal temperature, normal pressure, high-speed stirred: 9000 rpm, mixing time: 35s.
embodiment 2:this high accuracy conductive circuit nanometer silver paste, its component and mass percent as follows:
Average grain diameter is the nano-Ag particles 85% of 20nm
Methyl isobutyl carbinol 5%
Polyvinyl alcohol 5%
Modified high-molecular amount polyamines class wetting dispersing agent BYK-140 3.5%
Polyamide wax thixotropic agent BYK-410 1.5%;
The preparation method of above-mentioned nanometer silver paste, step is as follows:
1) 50g methyl isobutyl carbinol, 50g polyvinyl alcohol, 35g modified high-molecular amount polyamines class wetting dispersing agent BYK-140 and 15g polyamide wax thixotropic agent BYK-410 are added in high speed dispersor, each component 20000rpm high-speed stirred 10s under normal temperature and pressure conditions is fully mixed, forms bonding carrier;
2) by 850g average grain diameter be 20nm nano-Ag particles adopt high speed dispersion process be dispersed in bonding carrier in, can nanometer silver paste be formed, wherein dispersion condition: normal temperature, normal pressure, high-speed stirred: 20000 rpm, mixing time: 10s.
embodiment 3:this high accuracy conductive circuit nanometer silver paste, its component and mass percent as follows:
Average grain diameter is the nano-Ag particles 75% of 15nm
1-Methoxy-2-propyl acetate 5%
Propyl acetate 7%
Ethyl cellulose 5%
Polyvinyl alcohol 5%
Polyurethanes wetting dispersing agent BYK-163 2%
Polyamide wax thixotropic agent BYK-R605 1%;
The preparation method of above-mentioned nanometer silver paste, step is as follows:
1) 50g 1-Methoxy-2-propyl acetate, 70g propyl acetate, 50g ethyl cellulose, 50g polyvinyl alcohol, 20g wetting dispersing agent BYK-163 and 10g thixotropic agent BYK-R605 are added in high speed dispersor, each component 14000rpm high-speed stirred 15s under normal temperature and pressure conditions is fully mixed, forms bonding carrier;
2) by 750g average grain diameter be 15nm nano-Ag particles adopt high speed dispersion process be dispersed in bonding carrier in, can form nanometer silver paste, wherein dispersion condition is normal temperature, normal pressure, high-speed stirred: 14000 rpm, mixing time: 15s.
embodiment 4:this high accuracy conductive circuit nanometer silver paste, its component and mass percent as follows:
Average grain diameter is the nano-Ag particles 80% of 30nm
Dimethylbenzene 3%
Ethylene glycol monobutyl ether 6%
Acrylic resin 4%
Polyvinyl alcohol 3%
Fatty acid wetting dispersing agent BYK-130 3%
Thixotropic agent aerosil 1%;
The preparation method of above-mentioned nanometer silver paste, step is as follows:
1) 30g dimethylbenzene, 60g ethylene glycol monobutyl ether ester, 40g acrylic resin, 30g polyvinyl alcohol, 30g fatty acid wetting dispersing agent BYK-130 and 10g aerosil thixotropic agent are added in high speed dispersor, each component 10000rpm high-speed stirred 30s under normal temperature and pressure conditions is fully mixed, forms bonding carrier;
2) by 800g average grain diameter be 30nm nano-Ag particles adopt high speed dispersion process be dispersed in bonding carrier in, can nanometer silver paste be formed; Wherein dispersion condition: normal temperature, normal pressure, high-speed stirred: 10000 rpm, mixing time: 30s.
embodiment 5:this high accuracy conductive circuit nanometer silver paste, its component and mass percent as follows:
Average grain diameter is the nano-Ag particles 72% of 25nm
Octane 5%
Propyl acetate 10%
Ethyl cellulose 7%
Polyvinyl alcohol 3%
Polyester and polyether polymer class wetting dispersing agent BYK-180 2%
Thixotropic agent rilanit special 1%;
The preparation method of above-mentioned nanometer silver paste, step is as follows:
1) 50g octane, 100g propyl acetate, 70g ethyl cellulose, 30g polyvinyl alcohol, 20g polyester and polyether polymer class wetting dispersing agent BYK-180 and 10g rilanit special thixotropic agent are added in high speed dispersor, each component 16000rpm high-speed stirred 12s under normal temperature and pressure conditions is fully mixed, forms bonding carrier;
2) by 720g average grain diameter be 25nm nano-Ag particles adopt high speed dispersion process be dispersed in bonding carrier in, can nanometer silver paste be formed, wherein dispersion condition: normal temperature, normal pressure, high-speed stirred: 16000 rpm, mixing time: 12s.
performance test is tested:
Nanometer silver paste obtained in above-described embodiment 1 to embodiment 5 is carried out performance test.
Table 1: nanometer silver paste the performance test results
。
Claims (9)
1. a conductive circuit nanometer silver paste, is characterized in that constituent and mass percent are: nano-Ag particles 70% ~ 85%, solvent 5% ~ 15%, binding agent 5% ~ 13%, additive 2% ~ 5%.
2. conductive circuit nanometer silver paste according to claim 1, is characterized in that: nano-Ag particles average grain diameter is 10 ~ 30nm.
3. conductive circuit nanometer silver paste according to claim 1 and 2, is characterized in that: solvent is one or more mixtures in aromatic hydrocarbon, aliphatic hydrocarbon, alicyclic, ester, diol, derivatives, alcohol.
4. conductive circuit nanometer silver paste according to claim 3, is characterized in that: solvent is one or more mixtures in benzene,toluene,xylene, pentane, hexane, octane, cyclohexane, cyclohexanone, toluene cyclohexanone, methyl acetate, ethyl acetate, propyl acetate, 1-Methoxy-2-propyl acetate, glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethanol, isopropyl alcohol, methyl isobutyl carbinol.
5. conductive circuit nanometer silver paste according to claim 1 and 2, is characterized in that: binding agent is the mixture of one or more in polyvinyl alcohol, acrylic resin, ethyl cellulose.
6. conductive circuit nanometer silver paste according to claim 1 and 2, is characterized in that: additive is one or more mixtures in wetting dispersing agent, thixotropic agent.
7. conductive circuit nanometer silver paste according to claim 6, is characterized in that: wetting dispersing agent is BYK-130, BYK-192, BYK-110, BYK-180, BYK-140, BYK-142, BYK-163 or BYK-174.
8. conductive circuit nanometer silver paste according to claim 6, is characterized in that: thixotropic agent is aerosil, rilanit special or polyamide wax.
9. the preparation method of the conductive circuit nanometer silver paste described in any one of claim 1-8, is characterized in that concrete operations are as follows:
Add in high speed dispersor by solvent, binding agent and additive, under normal temperature, normal pressure, 9000 ~ 20000 rpm high-speed stirred 10 ~ 60s, make solvent, binding agent and additive fully mix and form bonding carrier;
Adopted by nano-Ag particles high speed dispersion process to be dispersed in bonding carrier, namely form nanometer silver paste, wherein dispersion condition is under normal temperature, normal pressure, 9000 ~ 20000 rpm high-speed stirred 10 ~ 60s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510198265.1A CN104858437A (en) | 2015-04-24 | 2015-04-24 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510198265.1A CN104858437A (en) | 2015-04-24 | 2015-04-24 | Nano silver paste for printing conducting circuit and preparation method of nano silver paste |
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| CN104858437A true CN104858437A (en) | 2015-08-26 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN105528962A (en) * | 2016-01-13 | 2016-04-27 | 江苏银晶光电科技发展有限公司 | Nano silver paste printed glass display screen and manufacturing process thereof |
| CN109277723A (en) * | 2018-10-06 | 2019-01-29 | 天津大学 | The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste |
| WO2019114048A1 (en) * | 2017-12-14 | 2019-06-20 | 中国科学院深圳先进技术研究院 | Self-heat-release pressureless sintered conductive silver paste and preparation method therefor |
| CN109935984A (en) * | 2017-12-18 | 2019-06-25 | 泰科电子(上海)有限公司 | Elastic conduction terminal and its manufacturing method |
| CN118315103A (en) * | 2024-06-11 | 2024-07-09 | 芯体素(杭州)科技发展有限公司 | Improved silver paste, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105427919A (en) * | 2015-11-23 | 2016-03-23 | 广东银研高新材料股份有限公司 | Self-antibacterial nano conductive silver paste and preparation method and application thereof |
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| CN105528962A (en) * | 2016-01-13 | 2016-04-27 | 江苏银晶光电科技发展有限公司 | Nano silver paste printed glass display screen and manufacturing process thereof |
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| CN109935984A (en) * | 2017-12-18 | 2019-06-25 | 泰科电子(上海)有限公司 | Elastic conduction terminal and its manufacturing method |
| CN109935984B (en) * | 2017-12-18 | 2021-01-22 | 泰科电子(上海)有限公司 | Elastic conductive terminal and manufacturing method thereof |
| CN109277723A (en) * | 2018-10-06 | 2019-01-29 | 天津大学 | The Ag-SiO of resistance to silver-colored electromigration under a kind of hot environment2The preparation method of nano-solder paste |
| CN118315103A (en) * | 2024-06-11 | 2024-07-09 | 芯体素(杭州)科技发展有限公司 | Improved silver paste, preparation method and application thereof |
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