CN110922939A - Organosilicon gel with conductivity - Google Patents
Organosilicon gel with conductivity Download PDFInfo
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- CN110922939A CN110922939A CN201911289902.0A CN201911289902A CN110922939A CN 110922939 A CN110922939 A CN 110922939A CN 201911289902 A CN201911289902 A CN 201911289902A CN 110922939 A CN110922939 A CN 110922939A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0806—Silver
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
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Abstract
An electrically conductive silicone gel, characterized by being prepared by a mixing reaction of a component a and a component B, wherein: the component A comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-40 parts of vinyl silicone oil and 0.01-1 part of catalyst; the component B comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-30 parts of vinyl silicone oil, 0.1-5 parts of a hydrogen-containing cross-linking agent and 0.1-2 parts of an inhibitor. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, uniformly mixing and curing. The conductive silicone gel has low viscosity, good high and low temperature resistance and good pressure-sensitive adhesion with various base materials, and can be used for conductive interconnection in various fields.
Description
Technical Field
Relates to the technical field of organic silicon gel, in particular to an organic silicon gel compound with conductivity.
Background
With the wide application of intelligent electronic products, the conductive adhesive is continuously developed, so that the traditional lead-tin solder which is not environment-friendly is gradually replaced, and the conductive interconnection with fine size and spacing can be realized. These advantages make the conductive adhesive an important part essential for the assembly of new electronic products with miniaturized devices and integrated functions. Generally, a conductive paste is composed of a conductive filler and a resin matrix for adhesion, and the purpose of conductivity is achieved by mutual contact and tunneling of conductive particles. The conductive filler may be metal powder of silver, copper, nickel, gold, etc. Silver powders with different particle diameters become the mainstream conductive filler in the market at present due to proper cost performance and excellent conductivity.
However, most of the common conductive adhesives in the market currently use epoxy resin as matrix resin, and have excellent adhesive property. However, the cured epoxy resin has high crosslinking density and large volume shrinkage, so that the cured conductive adhesive is easy to have the defects of high internal stress, poor cold and hot shock resistance, low peel strength and the like, which may cause the problems of bonding failure, unreliable conduction and the like in the use process.
In recent years, addition-type silicone resins have been used as a resin matrix in conductive adhesives. Compared with epoxy resin, the silicone has higher temperature resistance, lower shrinkage stress and more excellent cold and hot shock resistance. But the disadvantage of low adhesiveness limits the application range of the organic silicon conductive adhesive.
Disclosure of Invention
In order to make up for the deficiencies of the prior art, the present invention provides a silicone gel having electrical conductivity. The organic silicon gel has the characteristics of low viscosity, good temperature resistance, good cold and hot shock resistance, extremely low volume shrinkage after curing and the like, particularly has excellent pressure-sensitive adhesion, and can form good adhesion on various base materials.
The technical scheme of the invention is as follows:
an electrically conductive silicone gel, characterized by being prepared by a mixing reaction of a component a and a component B, wherein: the component A comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-40 parts of vinyl silicone oil and 0.01-1 part of catalyst; the component B comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-30 parts of vinyl silicone oil, 0.1-5 parts of a hydrogen-containing cross-linking agent and 0.1-2 parts of an inhibitor. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, uniformly mixing and curing.
The molar ratio of the vinyl functional group to the silicon-hydrogen functional group in the component A and the component B is controlled to be 0.3-0.9: 1. preferably, the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is controlled to be 0.5-0.8: 1.
the vinyl silicone oil is silicone oil with vinyl groups at two ends, the vinyl content is 0.02-0.5 mmol/g, and the viscosity is 100-100000 cps. Preferably, the vinyl silicone oil is terminal vinyl silicone oil, the vinyl content of the vinyl silicone oil is 0.03-0.4 mmol/g, and the viscosity of the vinyl silicone oil is 100-10000 cps. More preferably, the vinyl silicone oil is terminal vinyl silicone oil, the vinyl content of the vinyl silicone oil is 0.05 to 0.3mmol/g, and the viscosity of the vinyl silicone oil is 500 to 5000 cps.
The hydrogen-containing cross-linking agent is silicone oil with more than 2 silicon-hydrogen bonds on one molecular chain, and the content of the silicon-hydrogen bonds is 1-16 mmol/g. Preferably, the hydrogen-containing cross-linking agent is silicone oil with two ends free of silicon-hydrogen bonds and more than 2 silicon-hydrogen bonds in one molecular chain, and the content of the silicon-hydrogen bonds is 1-8 mmol/g. More preferably, the hydrogen-containing cross-linking agent is silicone oil with two ends free of silicon-hydrogen bonds and more than 2 silicon-hydrogen bonds in one molecular chain, and the content of the silicon-hydrogen bonds is 1-4 mmol/g.
The catalyst is a complex catalyst containing platinum. Preferably, the catalyst is a platinum-gold containing vinyl siloxane complex.
The inhibitor is an alkynol compound. Preferably, the inhibitor is one or more of 3-methyl-1-butyn-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3-phenyl-1-butyn-3-ol.
The conductive silver powder is micron silver powder, and the average particle size of the micron silver powder is 1-10 mu m; preferably, the average particle size of the conductive silver powder is 3-8 mu m. More preferably, the conductive silver powder includes flake and spherical silver powder having an average particle size of 3 to 8 μm.
Compared with the prior conductive adhesive technology, the conductive adhesive has the following beneficial effects: the viscosity is low, and the method is suitable for technologies such as screen printing, dispensing and the like, and is beneficial to conductive connection with fine pitches; the high and low temperature resistance is good, and the long-term use requirement of minus 50-200 ℃ can be met; based on good pressure-sensitive adhesion, the conductive adhesive can be used for conductive interconnection of different substrates and various fields.
Detailed Description
The present invention is described in detail below with reference to specific examples, which are provided only for illustrating the present invention and are not to be construed as limiting the scope of the present invention.
Example 1
Accurately weighing 20 parts of terminal vinyl silicone oil with the vinyl content of 0.11mmol/g, 80 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the components into a double-planet high-speed dispersion kettle, fully stirring for 1hr at room temperature to obtain a component A, and packaging for later use; accurately weighing 19 parts of terminal vinyl silicone oil with the vinyl content of 0.11mmol/g, 80 parts of conductive silver powder, 1 part of hydrogen-containing cross-linking agent with the hydrogen content of 3mmol/g and 0.02 part of 3-methyl-1-butyn-3-ol as a stabilizing agent, sequentially adding the components into a double-planet high-speed dispersion kettle, fully stirring the components for 1 hour at room temperature to obtain a component B, and packaging the component B for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is 0.7: 1.
the volume resistivity of the conductive silica gel (tested by GB/T1410-2006) is 1.1 x 10-4Omega. cm, 1/4 cone penetration (tested using GB/T269) was 60.
Example 2
Accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.11mmol/g, 90 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the materials into a double-planet high-speed dispersion kettle, fully stirring the materials at room temperature for 1 hour to obtain a component A, and packaging the component A for later use; accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.11mmol/g, 90 parts of conductive silver powder, 0.4 part of hydrogen-containing cross-linking agent with the hydrogen content of 3mmol/g and 0.02 part of stabilizer 3-methyl-1-butyn-3-ol, sequentially adding into a double-planet high-speed dispersion kettle, fully stirring at room temperature for 1hr to obtain a component B, and packaging for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is 0.5: 1.
the volume resistivity of the conductive silicone gel (tested by GB/T1410-2006) is 6.5 x 10-3Omega. cm, 1/4 cone penetration (tested using GB/T269) was 45.
Example 3
Accurately weighing 10 parts of vinyl-terminated silicone oil with the vinyl content of 0.06mmol/g, 90 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the materials into a double-planet high-speed dispersion kettle, fully stirring the materials at room temperature for 1 hour to obtain a component A, and packaging the component A for later use; accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.06mmol/g, 90 parts of conductive silver powder, 0.15 part of hydrogen-containing cross-linking agent with the hydrogen content of 4.3mmol/g and 0.02 part of stabilizer 3-phenyl-1-butyn-3-ol, sequentially adding the components into a double-planet high-speed dispersion kettle, fully stirring the components for 1 hour at room temperature to obtain a component B, and packaging the component B for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the A component and the B component is 0.54: 1.
the volume resistivity of the conductive silicone gel (tested by GB/T1410-2006) is 5.8 x 10-3Omega. cm, 1/4 cone penetration (tested using GB/T269) was 50.
Example 4
Accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.25mmol/g, 90 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the materials into a double-planet high-speed dispersion kettle, fully stirring the materials at room temperature for 1 hour to obtain a component A, and packaging the component A for later use; accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.25mmol/g, 90 parts of conductive silver powder, 1.5 parts of hydrogen-containing cross-linking agent with the hydrogen content of 1.95mmol/g and 0.02 part of stabilizer 3-phenyl-1-butyn-3-ol, sequentially adding the components into a double-planet high-speed dispersion kettle, fully stirring the components for 1 hour at room temperature to obtain a component B, and packaging the component B for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is 0.6: 1.
volume of the conductive silicone gelThe resistivity (tested by GB/T1410--3Omega. cm, 1/4 cone penetration (tested using GB/T269) was 36.
Comparative example 1
Accurately weighing 15 parts of vinyl-terminated silicone oil with the vinyl content of 0.11mmol/g, 85 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the materials into a double-planet high-speed dispersion kettle, fully stirring the materials at room temperature for 1 hour to obtain a component A, and packaging the component A for later use; accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.11mmol/g, 89 parts of conductive silver powder, 1 part of hydrogen-containing cross-linking agent with the hydrogen content of 4.3mmol/g and 0.02 part of stabilizer 3-phenyl-1-butyn-3-ol, sequentially adding into a double-planet high-speed dispersion kettle, fully stirring at room temperature for 1hr to obtain a component B, and packaging for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is 1.6: 1.
the volume resistivity of the conductive silicone gel (tested by GB/T1410-2006) is 7.8 x 10-3Omega. cm, 1/4 cone penetration (using GB/T269 test) is greater than 100 and no pressure sensitive adhesion.
Comparative example 2
Accurately weighing 15 parts of vinyl-terminated silicone oil with the vinyl content of 0.06mmol/g, 85 parts of conductive silver powder and 0.2 part of chloroplatinic acid-vinyl siloxane complex with the platinum content of 5000ppm, sequentially adding the materials into a double-planet high-speed dispersion kettle, fully stirring the materials at room temperature for 1 hour to obtain a component A, and packaging the component A for later use; accurately weighing 10 parts of terminal vinyl silicone oil with the vinyl content of 0.06mmol/g, 89 parts of conductive silver powder, 1 part of hydrogen-containing cross-linking agent with the hydrogen content of 3.8mmol/g and 0.02 part of stabilizer 3-phenyl-1-butyn-3-ol, sequentially adding the components into a double-planet high-speed dispersion kettle, fully stirring the components for 1 hour at room temperature to obtain a component B, and packaging the component B for later use. When in use, the component A and the component B are mixed according to the weight ratio of 1: 1, mixing uniformly and defoaming in vacuum. Curing at 150 ℃ for 1 h.
Wherein the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is 2.5: 1.
the volume resistivity of the conductive silicone gel (tested by GB/T1410-2006) is 6.3 x 10-3Omega. cm, 1/4 cone penetration (using GB/T269 test) is greater than 100 and no pressure sensitive adhesion.
The above description is only a part of the preferred embodiments of the present invention, and the present invention is not limited to the contents of the embodiments. It will be apparent to those skilled in the art that various changes and modifications can be made within the spirit of the invention, and any changes and modifications made are within the scope of the invention.
Claims (9)
1. An electrically conductive silicone gel, characterized by being prepared by a mixing reaction of a component a and a component B, wherein: the component A comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-40 parts of vinyl silicone oil and 0.01-1 part of catalyst; the component B comprises the following components in parts by weight: 60-90 parts of conductive silver powder, 10-30 parts of vinyl silicone oil, 0.5-1 part of hydrogen-containing cross-linking agent and 0.1-2 parts of inhibitor, wherein when the conductive silver powder is used, the component A and the component B are mixed according to the weight ratio of 1: 1, uniformly mixing and curing.
2. An electrically conductive silicone gel according to claim 1, characterized in that: the molar ratio of the vinyl functional group to the silicon-hydrogen functional group in the component A and the component B is controlled to be 0.3-0.9; preferably, the molar ratio of the vinyl functional groups to the silicon-hydrogen functional groups in the component A and the component B is controlled to be 0.5-0.8.
3. An electrically conductive silicone gel according to claim 1, characterized in that: the vinyl silicone oil is silicone oil with vinyl groups at two ends, the vinyl content is 0.02-0.5 mmol/g, and the viscosity is 100-100000 cps.
4. The vinyl-terminated silicone oil according to claim 3, characterized in that: the content of vinyl is 0.03-0.4 mmol/g, and the viscosity is 100-10000 cps; more preferably, the vinyl silicone oil is terminal vinyl silicone oil, the vinyl content of the vinyl silicone oil is 0.05 to 0.3mmol/g, and the viscosity of the vinyl silicone oil is 500 to 5000 cps.
5. An electrically conductive silicone gel according to claim 1, characterized in that: the hydrogen-containing cross-linking agent is silicone oil with more than 2 silicon-hydrogen bonds on one molecular chain, and the content of the silicon-hydrogen bonds is 1-16 mmol/g.
6. The hydrogen-containing crosslinking agent according to claim 5, characterized in that: the hydrogen-containing cross-linking agent is silicone oil with two ends free of silicon-hydrogen bonds and more than 2 silicon-hydrogen bonds on one molecular chain, and the content of the silicon-hydrogen bonds is 1-8 mmol/g; more preferably, the hydrogen-containing cross-linking agent is silicone oil with two ends free of silicon-hydrogen bonds and more than 2 silicon-hydrogen bonds in one molecular chain, and the content of the silicon-hydrogen bonds is 1-4 mmol/g.
7. An electrically conductive silicone gel according to claim 1, characterized in that: the catalyst is a complex catalyst containing platinum; preferably, the catalyst is a platinum-gold containing vinyl siloxane complex.
8. An electrically conductive silicone gel according to claim 1, characterized in that: the inhibitor is an alkynol compound; preferably, the inhibitor is one or more of 3-methyl-1-butyn-ol, 3, 5-dimethyl-1-hexyn-3-ol, 3-phenyl-1-butyn-3-ol.
9. The conductive silver powder is micron silver powder, and the average particle size of the micron silver powder is 1-10 mu m; preferably, the average particle size of the conductive silver powder is 3-8 mu m; more preferably, the conductive silver powder includes flake and spherical silver powder having an average particle size of 3 to 8 μm.
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Cited By (2)
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CN112341989A (en) * | 2020-11-30 | 2021-02-09 | 矽时代材料科技股份有限公司 | Heat-conducting silver adhesive and preparation method thereof |
CN115109562A (en) * | 2022-08-09 | 2022-09-27 | 广州市白云化工实业有限公司 | Bi-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
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CN115109562A (en) * | 2022-08-09 | 2022-09-27 | 广州市白云化工实业有限公司 | Bi-component high-heat-dissipation high-conductivity organic silicon pouring sealant and preparation method thereof |
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