CN109705803A - A kind of single-component organic silicon conducting resinl and its preparation method and application - Google Patents

A kind of single-component organic silicon conducting resinl and its preparation method and application Download PDF

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CN109705803A
CN109705803A CN201910027237.1A CN201910027237A CN109705803A CN 109705803 A CN109705803 A CN 109705803A CN 201910027237 A CN201910027237 A CN 201910027237A CN 109705803 A CN109705803 A CN 109705803A
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organic silicon
conducting resinl
component
silicon conducting
component organic
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CN109705803B (en
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蔡琴
李军明
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Zhenjiang Boshen New Materials Co Ltd
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Zhenjiang Boshen New Materials Co Ltd
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Abstract

The invention discloses a kind of single-component organic silicon conducting resinls, the single-component organic silicon conducting resinl includes that following component is made in parts by weight: 60 ~ 100 parts of vinyl-terminated silicone fluid, 1 ~ 5 part of containing hydrogen silicone oil, 20 ~ 40 parts of silver powder, 5 ~ 10 parts of single-walled carbon nanotube, 0.2 ~ 5 part of coupling agent, 0.2 ~ 1 part of catalyst, 0.5 ~ 3 part of inhibitor.The invention also discloses a kind of preparation method and application of single-component organic silicon conducting resinl.It is of the invention to be advantageous in that one-component additional organosilicon conducting resinl prepared by the present invention has preferable conductivity, lower interface resistance, preferable toughness.It is conductive that one-component additional organosilicon conducting resinl of the invention can be widely used for photovoltaic imbrication component cell piece conductive adhesive, electronic component and printed circuit board.

Description

A kind of single-component organic silicon conducting resinl and its preparation method and application
Technical field
The invention belongs to conducting resinl technical fields, and in particular to a kind of single-component organic silicon conducting resinl and preparation method thereof and Using.
Background technique
Conducting resinl is the adhesive with certain electric conductivity after a kind of solidification, it is usually filled out with fluoropolymer resin and conduction Material is chief component, is combined together conducting particles by the bonding effect of fluoropolymer resin, forms conductive path, real Now glued the conductive connection of material.Since the base polymer of conducting resinl is a kind of adhesive, suitable solidification temperature can choose Degree carries out solidification bonding, while the development with Electronic Packaging to high density and flexibility, and the requirement to connecting material is increasingly Height, electronic component and printed circuit board directly can generate stress due to coefficient of thermal expansion mismatch in temperature changing process, Traditional tin/metal solder joint is difficult to bear and cause to fail, and can not be applicable to light and short answering compared with low power consumption Use field.Conducting resinl simple process, it is easily operated, production efficiency can be improved, so conducting resinl is substitution slicker solder welding, realize The ideal chose of conductive connection.
Summary of the invention
Goal of the invention: technical problem to be solved by the invention is to provide a kind of single-component organic silicon conducting resinls.
Also there is provided a kind of preparation methods of single-component organic silicon conducting resinl for technical problems to be solved by the present invention.
The last technical problems to be solved of the present invention are to have passed through the application of the single-component organic silicon conducting resinl.
Technical solution: described in order to solve the above-mentioned technical problems, the present invention provides a kind of single-component organic silicon conducting resinl Single-component organic silicon conducting resinl includes that following component is made in parts by weight: 60~100 parts of vinyl-terminated silicone fluid, containing hydrogen silicone oil 1 ~5 parts, 20~40 parts of silver powder, 5~10 parts of single-walled carbon nanotube, 0.2~5 part of coupling agent, 0.2~1 part of catalyst, inhibitor 0.5~3 part.
Wherein, in order to make product keep facilitating carry out silk-screen printing, the end-vinyl silicon compared with low viscosity before curing For the contents of ethylene of oil 0.46~1.5%, viscosity is 50~1000mpa.s.
Wherein, in order to guarantee that product keeps certain toughness after hardening, the containing hydrogen silicone oil is silicon hydrogen content 0.18 ~1.6%.
Wherein, the silver powder is flake silver powder, and the specific surface area of particle is relatively large, and stability is good, oxidizability and oxygen Change trend is lower, is face contact or line contact between particle, so resistance is relatively low, good conductivity;Flake silver powder average grain diameter It 1.5~10 μm, selects lucky partial size that the contact between conductive phase particle can be made closeer, forms finer and close conductive mesh Network.
Wherein, the single-walled carbon nanotube is the product of solid content 10% (purchase is in OSICA company).Single-walled carbon nanotube It is graphite tubular crystal, is that mono-layer graphite piece is crimped around center by certain helical angle, has high draw ratio, lead Electrically it is better than most metals, and the high-flexibility of its own can be interconnected to form a three-dimensional network, the network knot Structure can form uniform permanent electric conductivity, and compared with conventional conductive elargol, this material improves the connections of component, reduce metal The mobility of particle can also increase wearability.Addition single-walled carbon nanotube can reduce the adding proportion of silver powder, reduce at This.
Wherein, it is that raw material closes that the coupling agent, which is allyl glycidyl ether and tetramethyl-ring tetrasiloxane containing epoxy group, At the coupling agent does not have an impact the performances such as hardness, the viscosity of add-on type product substantially.
Wherein, the inhibitor is one or more of 1- ethynylcyclohexanol, ether compound or vinyl ring body. It wherein, is preferably isopropyl ether in ether compound.
Wherein, the catalyst is the chloroplatinic acid catalyst that platinum content is 3000~5000ppm, high activity, height catalysis effect Rate, stability is good, and mithridatism is strong.
The invention also includes the preparation methods of the single-component organic silicon conducting resinl, comprising the following steps: in planet point It dissipates high speed dispersion after vinyl-terminated silicone fluid, single-walled carbon nanotube are added in blender to stir, be ground after stirring 0.5~1h;Grinding Containing hydrogen silicone oil, silver powder is added in blender afterwards, is warming up to 100 DEG C -120 DEG C after mixing evenly, stirs 1- under vacuum state It is cooling after 1.5h, 25~50HZ of stirring rate;Coupling agent, inhibitor and catalyst are added after being cooled to room temperature and is passed through except hydraulic pressure Contracting air, decompression row steeps after mixing to obtain the final product.
Wherein, 100~1000rm of revolving speed of the high speed dispersion stirring, the grinding number are 4~8 times.
The content of present invention further includes a kind of single-component organic silicon conducting resinl in photovoltaic imbrication component, electronic component and printing Application in terms of circuit board.
The utility model has the advantages that compared with the existing technology, of the invention to be advantageous in that: one-component add-on type prepared by the present invention has There is < 10 after machine silicon conduction adhesive curing-2The volume resistivity of ohm.cm, lower interface resistance, with conventional conductive elargol phase Than at low cost, good toughness.One-component additional organosilicon conducting resinl condition of cure of the invention is not particularly limited, and preferably 60~150 DEG C at a temperature of keep 0.1~150min, after molding may be selected post-cure, preferably 1 at 120~150 DEG C~ It is carried out within the scope of 4 hours.
Specific embodiment
The raw material used:
Embodiment 1
The vinyl-terminated silicone fluid 100 of contents of ethylene 0.46%, viscosity 500mpa.s are added in planet dispersator Part, 10 parts of the single-walled carbon nanotube of solid content 10%, high speed dispersion stirs, speed of agitator 1000rpm, with three after stirring 0.5h Roller mill is ground 6 times.5 parts of containing hydrogen silicone oil of silicon hydrogen content 1.6% are added after grinding in blender, average grain diameter 10 μm 40 parts of flake silver powder, be warming up to 100 DEG C after mixing evenly, keep under vacuum state (< -0.08Mpa), stir cold after 1h But, speed of agitator 1000rpm obtains base-material.It is sweet that the allyl glycidyl containing epoxy group is added in the base-material being cooled to room temperature Oily ether and tetramethyl-ring tetrasiloxane are that 1 part of the coupling agent V05,0.5 part of 1- alkynyl cyclohexanol, content of Material synthesis exist 0.2 part of the chloroplatinic acid catalyst of 5000ppm, is passed through water removal compressed air, is stirred, after mixing decompression row bubble.
Embodiment 2
Contents of ethylene 1.5%, 60 parts of vinyl-terminated silicone fluid of viscosity 50mpa.s are added in planet dispersator, 5 parts of the single-walled carbon nanotube of solid content 10%, high speed dispersion stirring, speed of agitator 100rpm are ground after stirring 1h with three rollers Machine is ground 4 times.1 part of containing hydrogen silicone oil of silicon hydrogen content 1.6% is added after grinding in blender, the piece that 10 μm of average grain diameter 20 parts of shape silver powder, it is warming up to 120 DEG C after mixing evenly, keeps under vacuum state (< -0.08Mpa), stirs cooling, stirring after 1h Revolving speed is 100rpm, obtains base-material.The allyl glycidyl ether and four containing epoxy group is added in the base-material being cooled to room temperature Methyl cyclotetrasiloxane is the chlorine of 0.2 part of coupling agent V05,1.5 parts of 1- alkynyl cyclohexanol, content in 3000ppm of Material synthesis 0.5 part of platinic acid catalyst, it is passed through water removal compressed air, is stirred, after mixing decompression row bubble.
Embodiment 3
Contents of ethylene 1%, 80 parts of vinyl-terminated silicone fluid of viscosity 500mpa.s are added in planet dispersator, Gu 8 parts of the single-walled carbon nanotube of content 10%, high speed dispersion stirring, speed of agitator 500rpm are ground after stirring 0.5h with three rollers Machine is ground 8 times.3 parts of containing hydrogen silicone oil of silicon hydrogen content 1.6% are added after grinding in blender, the piece that 10 μm of average grain diameter 30 parts of shape silver powder, it is warming up to 110 DEG C after mixing evenly, keeps under vacuum state (< -0.08Mpa), stirs cooling, stirring after 1h Revolving speed is 500rpm, obtains base-material.The allyl glycidyl ether and four containing epoxy group is added in the base-material being cooled to room temperature Methyl cyclotetrasiloxane is the chlorine platinum of 2.5 parts of coupling agent V05,3 parts of 1- alkynyl cyclohexanol, content in 4000ppm of Material synthesis 1 part of acid catalyst, it is passed through water removal compressed air, is stirred, after mixing decompression row bubble.
Embodiment 4
Contents of ethylene 1.5%, 60 parts of vinyl-terminated silicone fluid of viscosity 50mpa.s are added in planet dispersator, 5 parts of the single-walled carbon nanotube of solid content 10%, high speed dispersion stirring, speed of agitator 100rpm are ground after stirring 0.5h with three rollers Grinding machine is ground six times.1 part of containing hydrogen silicone oil, 10 μm of average grain diameter of silicon hydrogen content 1.6% is added after grinding in blender 20 parts of flake silver powder, be warming up to 100 DEG C after mixing evenly, keep under vacuum state (< -0.08Mpa), stir it is cooling after 1h, Speed of agitator is 100rpm, obtains base-material.The allyl glycidyl ether containing epoxy group is added in the base-material being cooled to room temperature It is 0.2 part of the coupling agent V05 of Material synthesis, 1.5 parts of 1- alkynyl cyclohexanol, content in 3000ppm with tetramethyl-ring tetrasiloxane 0.5 part of chloroplatinic acid catalyst, be passed through water removal compressed air, be stirred, after mixing decompression row bubble.
Embodiment 5
Almost the same with embodiment 1, different is, inhibitor is isopropyl ether.
Comparative example 1
In this comparative example, 10% single-walled carbon nanotube parts by weight of solid content are 15 parts, remaining is the same as to embodiment 1 Description.
Comparative example 2
In this comparative example, single-walled carbon nanotube is not added, remaining is the same as the description to embodiment 1.
1~5 one-component additional organosilicon conducting resinl condition of cure of the embodiment of the present invention is not particularly limited, and preferably 60~150 DEG C at a temperature of keep 0.1~150min, after molding may be selected post-cure, preferably 1 at 120~150 DEG C~ It is carried out within the scope of 4 hours.
One-component additional organosilicon conducting resinl prepared by Examples 1 to 5 and comparative example 1,2 tests its solidification speed As a result degree, volume resistivity, thixotropy, tensile strength, elongation at break are indicated by table 1:
Table 1
Various embodiments of the present invention are described above, above description is exemplary, and non-exclusive, and It is not limited to disclosed each embodiment.Without departing from the scope and spirit of illustrated each embodiment, for this skill Many modifications and changes are obvious for the those of ordinary skill in art field.

Claims (10)

1. a kind of single-component organic silicon conducting resinl, which is characterized in that the single-component organic silicon conducting resinl includes in parts by weight Following component is made: 60 ~ 100 parts of vinyl-terminated silicone fluid, 1 ~ 5 part of containing hydrogen silicone oil, and 20 ~ 40 parts of silver powder, single-walled carbon nanotube 5 ~ 10 Part, 0.2 ~ 5 part of coupling agent, 0.2 ~ 1 part of catalyst, 0.5 ~ 3 part of inhibitor.
2. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the second of the vinyl-terminated silicone fluid For amount vinyl content 0.46 ~ 1.5%, viscosity is 50 ~ 1000mpa.s.
3. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the containing hydrogen silicone oil is silicon hydrogen content 0.18 ~ 1.6%.
4. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the silver powder is flake silver powder, is put down Equal 1.5 ~ 10 μm of partial size.
5. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the coupling agent is containing epoxy group Allyl glycidyl ether and tetramethyl-ring tetrasiloxane are Material synthesis.
6. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the inhibitor is 1- acetylene basic ring One or more of hexanol, ether compound or vinyl ring body.
7. single-component organic silicon conducting resinl according to claim 1, which is characterized in that the catalyst is that platinum content is The chloroplatinic acid catalyst of 3000 ~ 5000ppm.
8. the preparation method of the described in any item single-component organic silicon conducting resinls of claim 1 ~ 8, which is characterized in that including following Step: high speed dispersion stirs after vinyl-terminated silicone fluid, single-walled carbon nanotube are added in planet dispersator, stirs 0.5 ~ 1h After grind;Containing hydrogen silicone oil, silver powder is added after grinding in blender, is warming up to 100 DEG C -120 DEG C after mixing evenly, vacuum state It is cooling after lower stirring 1-1.5h;Coupling agent, inhibitor and catalyst are added after being cooled to room temperature and is passed through water removal compressed air, mixes Decompression row steeps after closing uniformly to obtain the final product.
9. the preparation method of single-component organic silicon conducting resinl according to claim 8, which is characterized in that the high speed dispersion The revolving speed of stirring is 100 ~ 1000rpm, and the grinding number is 4 ~ 8 times.
10. a kind of single-component organic silicon conducting resinl described in claim 1 ~ 7 is in photovoltaic imbrication component, electronic component and printing Application in terms of circuit board.
CN201910027237.1A 2019-01-11 2019-01-11 Single-component organic silicon conductive adhesive and preparation method and application thereof Active CN109705803B (en)

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Cited By (6)

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CN110144190A (en) * 2019-05-29 2019-08-20 罗青菊 A kind of add-on type high heat conduction organosilicon electronic seal glue preparation method
CN110157375A (en) * 2019-06-21 2019-08-23 上海本诺电子材料有限公司 A kind of conductive and heat-conductive Silica hydrogel adhesive and preparation method thereof
CN111139026A (en) * 2020-01-14 2020-05-12 深圳市华天河科技有限公司 Double-component addition type anti-settling conductive adhesive and preparation method thereof
CN113185838A (en) * 2021-04-16 2021-07-30 镇江博慎新材料有限公司 High-strength high-transparency silicone RTV material
CN114479758A (en) * 2022-03-22 2022-05-13 江苏天辰新材料股份有限公司 High-thermal-conductivity single-component organosilicon sealant and preparation method and application thereof
CN116218460A (en) * 2022-12-20 2023-06-06 广州市儒兴科技股份有限公司 Organic silicon conductive adhesive and preparation method and application thereof

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110144190A (en) * 2019-05-29 2019-08-20 罗青菊 A kind of add-on type high heat conduction organosilicon electronic seal glue preparation method
CN110157375A (en) * 2019-06-21 2019-08-23 上海本诺电子材料有限公司 A kind of conductive and heat-conductive Silica hydrogel adhesive and preparation method thereof
CN111139026A (en) * 2020-01-14 2020-05-12 深圳市华天河科技有限公司 Double-component addition type anti-settling conductive adhesive and preparation method thereof
CN113185838A (en) * 2021-04-16 2021-07-30 镇江博慎新材料有限公司 High-strength high-transparency silicone RTV material
CN114479758A (en) * 2022-03-22 2022-05-13 江苏天辰新材料股份有限公司 High-thermal-conductivity single-component organosilicon sealant and preparation method and application thereof
CN116218460A (en) * 2022-12-20 2023-06-06 广州市儒兴科技股份有限公司 Organic silicon conductive adhesive and preparation method and application thereof

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