CN109705803B - Single-component organic silicon conductive adhesive and preparation method and application thereof - Google Patents
Single-component organic silicon conductive adhesive and preparation method and application thereof Download PDFInfo
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- CN109705803B CN109705803B CN201910027237.1A CN201910027237A CN109705803B CN 109705803 B CN109705803 B CN 109705803B CN 201910027237 A CN201910027237 A CN 201910027237A CN 109705803 B CN109705803 B CN 109705803B
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Abstract
The invention discloses a single-component organic silicon conductive adhesive which is prepared from the following components in parts by weight: 60-100 parts of vinyl-terminated silicone oil, 1-5 parts of hydrogen-containing silicone oil, 20-40 parts of silver powder, 5-10 parts of single-walled carbon nanotube, 0.2-5 parts of coupling agent, 0.2-1 part of catalyst and 0.5-3 parts of inhibitor. The invention also discloses a preparation method and application of the single-component organic silicon conductive adhesive. The single-component addition type organic silicon conductive adhesive has the advantages of good conductivity, low interface resistance and good toughness. The single-component addition type organic silicon conductive adhesive can be widely used for conductive bonding of photovoltaic laminated assembly battery pieces and conductive of electronic components and printed circuit boards.
Description
Technical Field
The invention belongs to the technical field of conductive adhesives, and particularly relates to a single-component organic silicon conductive adhesive as well as a preparation method and application thereof.
Background
The conductive adhesive is an adhesive with certain conductive performance after being cured, generally takes polymer resin and conductive filler as main components, and combines conductive particles together through the bonding action of the polymer resin to form a conductive path so as to realize the conductive connection of the bonded materials. Because the basic polymer of the conductive adhesive is an adhesive, the conductive adhesive can be cured and bonded at a proper curing temperature, and meanwhile, along with the development of high density and flexibility of electronic packaging, the requirement on connecting materials is higher and higher, electronic components and printed circuit boards directly generate stress due to thermal expansion coefficient mismatch in the temperature change process, the traditional tin/lead alloy welding points are difficult to bear to cause failure, and the conductive adhesive cannot be applied to the application field needing light, thin, short, small and low power consumption. The conductive adhesive has simple process and easy operation, and can improve the production efficiency, so the conductive adhesive is an ideal choice for replacing lead-tin welding to realize conductive connection.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a single-component organic silicon conductive adhesive.
The invention also aims to solve the technical problem of providing a preparation method of the single-component organic silicon conductive adhesive.
The invention finally solves the technical problem by applying the single-component organic silicon conductive adhesive.
The technical scheme is as follows: in order to solve the technical problems, the invention provides a single-component organic silicon conductive adhesive which is prepared from the following components in parts by weight: 60-100 parts of vinyl-terminated silicone oil, 1-5 parts of hydrogen-containing silicone oil, 20-40 parts of silver powder, 5-10 parts of single-walled carbon nanotube, 0.2-5 parts of coupling agent, 0.2-1 part of catalyst and 0.5-3 parts of inhibitor.
In order to keep the viscosity of the product to be low before curing and facilitate screen printing, the vinyl-terminated silicone oil has the vinyl content of 0.46-1.5% and the viscosity of 50-1000 mpa.s.
In order to ensure that the product keeps certain toughness after being cured, the hydrogen-containing silicone oil has the silicon-hydrogen content of 0.18-1.6%.
The silver powder is flake silver powder, the specific surface area of particles of the silver powder is relatively large, the stability is good, the oxidation degree and the oxidation tendency are low, and the particles are in surface contact or line contact, so that the resistance is relatively low and the conductivity is good; the average particle size of the flake silver powder is 1.5-10 mu m, and the proper particle size can ensure that the contact among conductive phase particles is denser and a more compact conductive network is formed.
Wherein the single-walled carbon nanotubes are products with 10% solid content (purchased from OSICA). The single-walled carbon nanotube is a graphite tubular crystal, is formed by curling a single-layer graphite sheet around the center according to a certain spiral angle, has extremely high length-diameter ratio and electrical conductivity superior to most metals, and has high flexibility, so that the single-layer graphite sheet can be mutually connected to form a three-dimensional network, and the network structure can form uniform and permanent electrical conductivity. The addition of the single-walled carbon nanotube can reduce the addition proportion of the silver powder and reduce the cost.
The coupling agent is synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethylcyclotetrasiloxane as raw materials, and the coupling agent basically does not influence the hardness, viscosity and other properties of the addition type product.
Wherein the inhibitor is one or more of 1-ethynyl cyclohexanol, ether compounds or vinyl ring bodies. Among the ether compounds, isopropyl ether is preferable.
The catalyst is a chloroplatinic acid catalyst with the platinum content of 3000-5000 ppm, and has the advantages of high activity, high catalytic efficiency, good stability and strong toxicity resistance.
The invention also comprises a preparation method of the single-component organic silicon conductive adhesive, which comprises the following steps: adding end vinyl silicone oil and single-walled carbon nanotubes into a planetary dispersing stirrer, dispersing and stirring at a high speed, stirring for 0.5-1 h, and grinding; after grinding, adding hydrogen-containing silicone oil and silver powder into a stirrer, uniformly stirring, heating to 100-120 ℃, stirring for 1-1.5h in a vacuum state, and cooling at a stirring speed of 25-50 HZ; cooling to room temperature, adding coupling agent, inhibitor and catalyst, introducing water-removing compressed air, mixing, and removing bubbles under reduced pressure.
Wherein the rotating speed of the high-speed dispersion stirring is 100-1000 rm, and the grinding times are 4-8.
The invention also comprises the application of the single-component organic silicon conductive adhesive in the aspects of photovoltaic laminated assemblies, electronic components and printed circuit boards.
Has the advantages that: compared with the prior art, the invention has the advantages that: the single-component addition type organic silicon conductive adhesive prepared by the invention has the advantages of less than 10 after being cured-2Cm, lower interface resistance, and low cost and good toughness compared with the traditional conductive silver adhesive. The curing conditions of the single-component addition type organosilicon conductive adhesive are not particularly limited, the curing is preferably kept at the temperature of 60-150 ℃ for 0.1-150 min, secondary vulcanization can be selected after the forming, and the curing is preferably carried out at the temperature of 120-150 ℃ for 1-4 hours.
Detailed Description
The raw materials used are as follows:
example 1
Adding 100 parts of terminal vinyl silicone oil with the vinyl content of 0.46 percent and the viscosity of 500mpa.s and 10 parts of single-walled carbon nanotubes with the solid content of 10 percent into a planetary dispersion stirrer, dispersing and stirring at a high speed, wherein the stirring speed is 1000rpm, and grinding for 6 times by using a three-roll grinder after stirring for 0.5 h. And after grinding, adding 5 parts of hydrogen-containing silicone oil with the silicon-hydrogen content of 1.6 percent and 40 parts of flaky silver powder with the average particle size of 10 mu m into a stirrer, uniformly stirring, heating to 100 ℃, keeping the temperature under a vacuum state (less than-0.08 Mpa), stirring for 1h, cooling, and stirring at the rotating speed of 1000rpm to obtain the base material. Adding coupling agent V051 parts synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethylcyclotetrasiloxane as raw materials, 0.5 part of 1-alkynyl cyclohexanol and 0.2 part of chloroplatinic acid catalyst with the content of 5000ppm into the base material cooled to room temperature, introducing dehydrated compressed air, stirring and mixing, and reducing pressure and discharging bubbles after uniform mixing.
Example 2
Adding 60 parts of vinyl-terminated silicone oil with the vinyl content of 1.5 percent and the viscosity of 50mpa.s and 5 parts of single-walled carbon nanotubes with the solid content of 10 percent into a planetary dispersion stirrer, dispersing and stirring at a high speed, wherein the stirring speed is 100rpm, and grinding for 4 times by using a three-roll grinder after stirring for 1 h. Adding 1 part of hydrogen-containing silicone oil with 1.6 percent of silicon hydrogen content and 20 parts of flake silver powder with the average particle size of 10 mu m into a stirrer after grinding, uniformly stirring, heating to 120 ℃, keeping the temperature under vacuum state (-0.08 Mpa), stirring for 1h, cooling, and stirring at the rotating speed of 100rpm to obtain the base material. Adding 050.2 parts of coupling agent V synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethylcyclotetrasiloxane as raw materials, 1.5 parts of 1-alkynyl cyclohexanol and 0.5 part of chloroplatinic acid catalyst with the content of 3000ppm into the base material cooled to room temperature, introducing dehydrated compressed air, stirring and mixing, and reducing pressure and discharging bubbles after uniform mixing.
Example 3
Adding 80 parts of terminal vinyl silicone oil with the vinyl content of 1 percent and the viscosity of 500mpa.s and 8 parts of single-walled carbon nano tubes with the solid content of 10 percent into a planetary dispersion stirrer, dispersing and stirring at a high speed of 500rpm, stirring for 0.5h, and grinding for 8 times by using a three-roll grinder. And after grinding, adding 3 parts of hydrogen-containing silicone oil with the silicon-hydrogen content of 1.6 percent and 30 parts of flaky silver powder with the average particle size of 10 mu m into a stirrer, uniformly stirring, heating to 110 ℃, keeping the temperature under vacuum state (less than-0.08 Mpa), stirring for 1h, cooling, and stirring at the rotating speed of 500rpm to obtain the base material. Adding 052.5 parts of coupling agent V synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethylcyclotetrasiloxane as raw materials, 3 parts of 1-alkynyl cyclohexanol and 1 part of chloroplatinic acid catalyst with the content of 4000ppm into the base material cooled to room temperature, introducing water-removing compressed air, stirring and mixing, and reducing pressure and removing bubbles after mixing uniformly.
Example 4
Adding 60 parts of terminal vinyl silicone oil with the vinyl content of 1.5 percent and the viscosity of 50mpa.s and 5 parts of single-walled carbon nanotubes with the solid content of 10 percent into a planetary dispersion stirrer, dispersing and stirring at a high speed, wherein the stirring speed is 100rpm, and grinding for six times by using a three-roll grinder after stirring for 0.5 h. Adding 1 part of hydrogen-containing silicone oil with 1.6 percent of silicon hydrogen content and 20 parts of flake silver powder with the average particle size of 10 mu m into a stirrer after grinding, uniformly stirring, heating to 100 ℃, keeping the temperature under vacuum state (-0.08 Mpa), stirring for 1h, cooling, and stirring at the rotating speed of 100rpm to obtain the base material. Adding 050.2 parts of coupling agent V synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethylcyclotetrasiloxane as raw materials, 1.5 parts of 1-alkynyl cyclohexanol and 0.5 part of chloroplatinic acid catalyst with the content of 3000ppm into the base material cooled to room temperature, introducing dehydrated compressed air, stirring and mixing, and reducing pressure and discharging bubbles after uniform mixing.
Example 5
Essentially in accordance with example 1, except that the inhibitor is isopropyl ether.
Comparative example 1
In this comparative example, the weight portion of the single-walled carbon nanotube having a solid content of 10% was 15 parts, and the rest is the same as that described in example 1.
Comparative example 2
In this comparative example, no single-walled carbon nanotubes were added, as described for example 1.
The curing conditions of the single-component addition type organosilicon conductive adhesive in the embodiments 1-5 of the invention are not particularly limited, and preferably the curing conditions are kept at the temperature of 60-150 ℃ for 0.1-150 min, and secondary vulcanization can be selected after the forming, preferably the curing conditions are carried out at the temperature of 120-150 ℃ for 1-4 hours.
The single-component addition type organosilicon conductive adhesive prepared in examples 1-5 and comparative examples 1 and 2 is tested for curing speed, volume resistivity, thixotropy, tensile strength and elongation at break, and the results are shown in table 1:
TABLE 1
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (4)
1. The single-component organic silicon conductive adhesive is characterized by being prepared from the following components in parts by weight: 60-100 parts of vinyl-terminated silicone oil, 1-5 parts of hydrogen-containing silicone oil, 20-40 parts of silver powder, 5-10 parts of single-walled carbon nanotubes, 0.2-5 parts of a coupling agent, 0.2-1 part of a catalyst and 0.5-3 parts of an inhibitor, wherein the vinyl-terminated silicone oil has a vinyl content of 0.46-1.5% and a viscosity of 50-1000 mpa.s, the hydrogen-containing silicone oil has a silicon hydrogen content of 0.18-1.6%, the silver powder is sheet silver powder and has an average particle size of 1.5-10 mu m, the coupling agent is synthesized by taking allyl glycidyl ether containing epoxy groups and tetramethyl-cyclotetrasiloxane as raw materials, the inhibitor is one or more of 1-ethynyl cyclohexanol ether compounds or vinyl ring bodies, and the catalyst is a chloroplatinic acid catalyst with a platinum content of 3000-5000 ppm.
2. The preparation method of the single-component organic silicon conductive adhesive as claimed in claim 1, which is characterized by comprising the following steps: adding end vinyl silicone oil and single-walled carbon nanotubes into a planetary dispersing stirrer, dispersing and stirring at a high speed, stirring for 0.5-1 h, and grinding; after grinding, adding hydrogen-containing silicone oil and silver powder into a stirrer, uniformly stirring, heating to 100-120 ℃, stirring for 1-1.5h under a vacuum state, and cooling; cooling to room temperature, adding coupling agent, inhibitor and catalyst, introducing water-removing compressed air, mixing, and removing bubbles under reduced pressure.
3. The preparation method of the single-component organosilicon conductive adhesive according to claim 2, wherein the rotation speed of the high-speed dispersion stirring is 100-1000 rpm, and the grinding times are 4-8 times.
4. The use of the single-component silicone conductive adhesive of claim 1 in photovoltaic laminated assemblies, electronic components, and printed circuit boards.
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| CN110144190B (en) * | 2019-05-29 | 2021-10-22 | 东莞市泰亚电子科技有限公司 | Preparation method of addition type high-thermal-conductivity organic silicon electronic pouring sealant |
| 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 |
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| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
| CN103160049A (en) * | 2012-12-07 | 2013-06-19 | 河南城建学院 | Preparation method for nano-silver/carbon nano-tube (CNT)/polyvinyl alcohol (PVA) composite electroconductive film |
| CN104854176A (en) * | 2012-12-20 | 2015-08-19 | 道康宁公司 | Curable silicone compositions, electrically conductive silicone adhesives, methods of making and using same, and electrical devices containing same |
| CN108977168A (en) * | 2018-07-11 | 2018-12-11 | 上海锐朗光电材料有限公司 | High temperature rapid curing high conductivity organic silica gel is bonded agent |
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| KR20090047328A (en) * | 2007-11-07 | 2009-05-12 | 삼성전기주식회사 | Conductive paste and printed circuit board using the same |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102408858A (en) * | 2011-10-24 | 2012-04-11 | 上海大学 | Stable type conductive adhesive and preparation method thereof |
| CN103160049A (en) * | 2012-12-07 | 2013-06-19 | 河南城建学院 | Preparation method for nano-silver/carbon nano-tube (CNT)/polyvinyl alcohol (PVA) composite electroconductive film |
| CN104854176A (en) * | 2012-12-20 | 2015-08-19 | 道康宁公司 | Curable silicone compositions, electrically conductive silicone adhesives, methods of making and using same, and electrical devices containing same |
| CN108977168A (en) * | 2018-07-11 | 2018-12-11 | 上海锐朗光电材料有限公司 | High temperature rapid curing high conductivity organic silica gel is bonded agent |
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