CN106098147B - A kind of oiliness conductive silver paste and preparation method thereof - Google Patents
A kind of oiliness conductive silver paste and preparation method thereof Download PDFInfo
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- CN106098147B CN106098147B CN201610538531.5A CN201610538531A CN106098147B CN 106098147 B CN106098147 B CN 106098147B CN 201610538531 A CN201610538531 A CN 201610538531A CN 106098147 B CN106098147 B CN 106098147B
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- silver powder
- silver
- silver paste
- conductive silver
- oiliness
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- 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
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- 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
Abstract
The invention discloses a kind of oiliness conductive silver paste and preparation method thereof, its each raw material is by the composition of mass parts：It is 1 in mass ratio by flake silver powder and spherical silver powder that 10~30 parts of silver powder, 5~15 parts of nano silver wire, 20~40 parts of epoxy resin, 20~40 parts of dibasic ester, 10~20 parts of polyurethane, 0.1~2 part of dispersant, 0.1~2 part of acid anhydride type curing agent, wherein silver powder, which are,:1~5 mixing is formed.The conductive silver paste of the present invention is reduced the usage amount of conductive filler, improves the electric conductivity of material, while reduced the usage amount of silver, reduce production cost by the compounding of silver powder and nano silver wire.
Description
Technical field
The present invention relates to conductive silver paste technical field, and in particular to a kind of oiliness conductive silver paste and preparation method thereof.
Background technology
In Information Technology Development, conductive silver paste has vital role status.It is main in general conductive silver paste
Contain various functions filler such as conductive filler (such as copper, aluminium, silver metal powder), inorganic filler glass dust, oxide powder, organic viscous
Agent, curing agent etc. are tied, silver content is 80~90%.Consider from theory significance, the conductive effect of the more highly conductive silver paste of silver content
It is better；But from actual production, because silver is precious metal, the silver content in filler is fewer, and production cost is lower.
Containing 28~32wt% conductive silver wires, 25 in nano-silver thread conductive silver paste disclosed in Chinese patent CN104464887A
~40wt% resin, 20~30wt% organic solvents, 1~10wt% glass dust and 1~10wt% additives, it is being prepared
When in need heating water bath to stir, and the volume resistance of gained silver paste is bigger than normal.
Chinese patent CN103059767A discloses a kind of high temperature resistant, the production method of low-resistance conductive silver paste, its
Also need to add 5% nano-silver powder while micro-silver powder content reaches more than 45%, can be only achieved preferable electric conductivity.
Therefore, good conductive silver paste should have higher electric conductivity and relatively low production cost, so could be big
Width increases the competitiveness of product.Take into account electric conductivity and production cost be silver paste coating industry development trend.
The content of the invention
The present invention is to avoid above-mentioned the deficiencies in the prior art part, there is provided a kind of oiliness conductive silver paste and its preparation side
Method, it is intended to mention silver paste interlayer electrical conductivity, reduce cost.
The present invention solves technical problem, adopts the following technical scheme that：
Each raw material is by the composition of mass parts in the oiliness conductive silver paste of the present invention：
Wherein, it is 1 in mass ratio by flake silver powder and spherical silver powder that the silver powder, which is,:1~5 mixing is formed.The sheet
The particle diameter of silver powder is in 80~200nm, and the particle diameter of the spherical silver powder is at 0.2~4 μm.
A diameter of 40~200nm of the nano silver wire, length are 10~500 μm.
Preferably, the dispersant is selected from lauryl sodium sulfate, cetyl benzenesulfonic acid sodium, carboxymethyl propyl cellulose
At least one of with sodium carboxymethylcellulose.
Preferably, the epoxy resin is solid-state bisphenol A type epoxy resin fat.
Preferably, the acid anhydride type curing agent is aromatic anhydride (such as phthalic anhydride, trimellitic anhydride, equal benzene
Tetracarboxylic acid dianhydride, benzophenone tetracarboxylic dianhydride), alicyclic acid anhydrides (such as maleic anhydride, tung oil acid anhydride, alkylene succinic anhydride,
THPA, HHPA, methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, carbic anhydride, methylnadic anhydride, glutaric acid
Acid anhydride, terpenes acid anhydrides, methyl cyclohexene tetracarboxylic dianhydride, dodecenylsuccinic acid acid anhydride), long-chain fat race acid anhydrides (such as poly- azelaic acid
Acid anhydride, poly- SA acid anhydride), acid anhydrides containing halogen (such as PHT4, tetrachlorophthalic anhydride), acid anhydride adduct (such as trimellitic anhydride second two
Alcohol, glyceride, diphenyl sulfone tetracarboxylic dianhydride).
The preparation method of oiliness conductive silver paste of the present invention, comprises the following steps：
A, epoxy resin and dibasic ester are mixed into 20~40min on high shear machine, obtains mixed liquor A；
B, nano silver wire and dispersant are added in the mixed liquor A, vacuum defoamation is carried out in de-airing mixer and is mixed
Close, obtain mixed liquid B；
C, silver powder and polyurethane resin are added in the mixed liquid B, it is stirred under vacuum 30 in de-airing mixer~
40min, obtain mixed liquor C；
D, acid anhydride type curing agent is added in the mixed liquor C, 30~40min is stirred under vacuum in de-airing mixer, so
Filtered by 250 mesh screen cloths, that is, obtain oiliness conductive silver paste.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, oiliness conductive silver paste of the invention reduces the use of conductive filler by the compounding of silver powder and nano silver wire
Amount, improves the electric conductivity of material, while reduces the usage amount of silver, reduces production cost.
2nd, oiliness conductive silver paste of the invention uses acid anhydride type curing agent, and its volatility is small, toxicity is low, general validity period
It is long, favorably and technological operation, easily coordinate with epoxy resin, it is big to add amount of filler, can reduce product cost.
Embodiment
Clearly elaboration explanation is done to technical scheme below by embodiment.
Epoxy resin used in following embodiments is solid-state bisphenol A type epoxy resin fat, trade mark E-21；Polyurethane resin used
The trade mark is AH-0201D, purchased from Anhui Anda-Huatai New Material Co., Ltd..
Embodiment 1
The oiliness conductive silver paste of the present embodiment is prepared as follows：
A, 40g epoxy resin and 20g dibasic esters are obtained into mixed liquor A in high shear machine mixing 30min；
B, 10g nano silver wires and 2g are disperseed into agent carboxymethyl propyl cellulose to add in mixed liquor A, in de-airing mixer
Vacuum defoamation and mixing are carried out, obtains mixed liquid B；
C, by 30g silver powder and 20g polyurethane resins, 30min is stirred under vacuum in de-airing mixer, obtains mixed liquor C；Its
Middle silver powder is mixed by 10g flake silver powders and the spherical silver powder of 20g.
D, 1g phthalic anhydrides are added in mixed liquor C, 30min are stirred under vacuum in de-airing mixer, then through 250
Mesh screen cloth filters, that is, obtains oiliness conductive silver paste.
Embodiment 2~7
After being adjusted by table 1 to the raw material in embodiment 1 and its quality, embodiment 2~7 is carried out by identical method.
Wherein, curing agent used in embodiment 2~6 is phthalic anhydride, and curing agent used in embodiment 7 is trimellitic acid
Acid anhydride.
The raw material composition of each embodiment conductive silver paste of table 1
Conductive silver paste prepared by above-described embodiment carries out performance test：
Electric performance test：Using sheet resistance instrument test resistance；
Adhesive force is tested：Vertically drawn using 3M600 adhesive tapes, draw nothing to come off twice in succession；
Hardness test；
Ageing-resistant test：Setting temperature is 65 DEG C, humidity is 90 parts of RH, and retention time 96h, ageing-resistant front and rear test is electric
Resistive is defined as well in the range of 10%, poor beyond being then defined as.
Test result is shown in Table 2：
The performance test results of 2 each embodiment of table
Comparative example 1,2,3, it can be seen that using nano silver wire filler best results, and with nano silver wire content
Increase electric conductivity is improving, but obscission occurs in adhesive force test after too high levels.
Comparative example 2,4,5, it can be seen that reduce the content of silver powder or change flaky nanometer silver powder and spherical in silver powder
The ratio of silver powder can cause the change of conductance, but to adhesive force, hardness, ageing-resistant do not impact.
Finally it should be noted that：Obviously, above-described embodiment is only intended to clearly illustrate example of the present invention, and simultaneously
The non-restriction to embodiment.For those of ordinary skill in the field, can also do on the basis of the above description
Go out other various forms of changes or variation.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn
Among the obvious changes or variations that Shen goes out is still in protection scope of the present invention.
Claims (2)
- A kind of 1. oiliness conductive silver paste, it is characterised in that：Each raw material is by the composition of mass parts in the oiliness conductive silver paste：Wherein, it is 1 in mass ratio by flake silver powder and spherical silver powder that the silver powder, which is,:1~5 mixing is formed；The epoxy resin is solid-state bisphenol A type epoxy resin fat；The acid anhydride type curing agent is selected from aromatic anhydride, aliphatic anhydride, long-chain fat race acid anhydrides, acid anhydrides containing halogen or acid anhydrides Addition product；The particle diameter of the flake silver powder is in 80~200nm, and the particle diameter of the spherical silver powder is at 0.2~4 μm；A diameter of 40~200nm of the nano silver wire, length are 10~500 μm；It is fine that the dispersant is selected from lauryl sodium sulfate, cetyl benzenesulfonic acid sodium, carboxymethyl propyl cellulose and carboxymethyl Tie up at least one of plain sodium.
- 2. the preparation method of the oiliness conductive silver paste described in a kind of claim 1, it is characterised in that comprise the following steps：A, epoxy resin and dibasic ester are mixed into 20~40min on high shear machine, obtains mixed liquor A；B, nano silver wire and dispersant are added in the mixed liquor A, vacuum defoamation and mixing is carried out in de-airing mixer, is obtained To mixed liquid B；C, silver powder and polyurethane resin are added in the mixed liquid B, 30~40min is stirred under vacuum in de-airing mixer, is obtained To mixed liquor C；D, acid anhydride type curing agent is added in the mixed liquor C, 30~40min, Ran Houjing is stirred under vacuum in de-airing mixer 250 mesh screen cloths filter, that is, obtain oiliness conductive silver paste.
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| CN201610538531.5A CN106098147B (en) | 2016-07-08 | 2016-07-08 | A kind of oiliness conductive silver paste and preparation method thereof |
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| CN201610538531.5A CN106098147B (en) | 2016-07-08 | 2016-07-08 | A kind of oiliness conductive silver paste and preparation method thereof |
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| CN106098147B true CN106098147B (en) | 2018-04-10 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106675434B (en) * | 2017-01-09 | 2019-09-20 | 成都科愿慧希科技有限公司 | One kind can rapid curing conductive silver glue |
| CN107129752B (en) * | 2017-06-29 | 2019-08-30 | 合肥微晶材料科技有限公司 | A kind of graphene silver nanowires composite mortar and preparation method thereof |
| CN114023486A (en) * | 2021-10-20 | 2022-02-08 | 西安理工大学 | Environment-friendly micro-nano composite waterborne conductive silver paste and preparation method thereof |
| CN114023491A (en) * | 2021-11-12 | 2022-02-08 | 福建江夏学院 | High-performance conductive paste with low silver content and preparation method thereof |
| CN114283962B (en) * | 2021-11-19 | 2024-01-30 | 安徽中科元贞科技有限责任公司 | Silver plating microsphere-based conductive silver paste and preparation method thereof |
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| JP2005267859A (en) * | 2004-03-16 | 2005-09-29 | Toyobo Co Ltd | Conductive paste |
| CN102676102A (en) * | 2011-03-16 | 2012-09-19 | 上海富信新能源科技有限公司 | Silver nanowire doped conductive silver colloid and preparation method thereof |
| CN102766426A (en) * | 2012-07-03 | 2012-11-07 | 烟台德邦科技有限公司 | Conductive adhesive for encapsulating semiconductor chip and preparation method thereof |
| 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 |
| CN105131882A (en) * | 2015-10-09 | 2015-12-09 | 重庆文理学院 | Conductive silver adhesive doped with conductive polymers |
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- 2016-07-08 CN CN201610538531.5A patent/CN106098147B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005267859A (en) * | 2004-03-16 | 2005-09-29 | Toyobo Co Ltd | Conductive paste |
| CN102676102A (en) * | 2011-03-16 | 2012-09-19 | 上海富信新能源科技有限公司 | Silver nanowire doped conductive silver colloid and preparation method thereof |
| CN102766426A (en) * | 2012-07-03 | 2012-11-07 | 烟台德邦科技有限公司 | Conductive adhesive for encapsulating semiconductor chip and preparation method thereof |
| 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 |
| CN105131882A (en) * | 2015-10-09 | 2015-12-09 | 重庆文理学院 | Conductive silver adhesive doped with conductive polymers |
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