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CN108659747A - A kind of pressure sensitive conductive adhesive and preparation method thereof - Google Patents

A kind of pressure sensitive conductive adhesive and preparation method thereof Download PDF

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Publication number
CN108659747A
CN108659747A CN201810337644.8A CN201810337644A CN108659747A CN 108659747 A CN108659747 A CN 108659747A CN 201810337644 A CN201810337644 A CN 201810337644A CN 108659747 A CN108659747 A CN 108659747A
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CN
China
Prior art keywords
parts
pressure sensitive
conductive adhesive
sensitive conductive
silver
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Pending
Application number
CN201810337644.8A
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Chinese (zh)
Inventor
赵志云
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Huzhou China Mdt Infotech Ltd
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Huzhou China Mdt Infotech Ltd
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Priority to CN201810337644.8A priority Critical patent/CN108659747A/en
Publication of CN108659747A publication Critical patent/CN108659747A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J133/00Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04Homopolymers or copolymers of esters
    • C09J133/06Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/08Homopolymers or copolymers of acrylic acid esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/46Polymerisation initiated by wave energy or particle radiation
    • C08F2/48Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J9/00Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02Electrically-conducting adhesives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Conductive Materials (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention relates to adhesive technical fields.A kind of pressure sensitive conductive adhesive of the present invention, includes the raw material of following components:10 20 parts of acrylic acid, 10 20 parts of methyl acrylate, 20 30 parts of butyl acrylate, 10 20 parts of conductive filler, 5 10 parts of photoinitiator, 23 parts of crosslinking agent, 67 parts of poly- second butyl ester, 5 10 parts of accelerating agent.The present invention also provides a kind of preparation methods of pressure sensitive conductive adhesive, include the following steps:First the acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 85 90 DEG C, 15 20min, crosslinking agent is added, after reacting 20 30min, remaining acrylic acid is added dropwise, surplus stock is added, continues to heat 4 5h, is cooled to room temperature.The present invention has a kind of hardening time short, the good advantage of bond effect, and has good mechanical strength.

Description

A kind of pressure sensitive conductive adhesive and preparation method thereof
Technical field
The present invention relates to adhesive technical fields, in particular to a kind of pressure sensitive conductive adhesive and preparation method thereof.
Background technology
Conductivity type adhesive be one kind can effectively be glued a variety of materials but also adhesive.It is conductive Glue can be divided into structural type and filled-type two major classes by base composition.Structural type refers to the high molecular material itself as conducting resinl matrix I.e. conductive conducting resinl;Filled-type refers to usual adhesive as matrix, and addition electroconductive stuffing is relied on to make glue Conducting resinl with electric action.At present conducting polymer composite prepare it is sufficiently complex, from practical application also have it is larger away from From, therefore widely used is filled conductive glue.
And now with electronic device towards miniaturization, current conducting resinl gradually develops to filming, therefore mesh Preceding conducting resinl is long there are hardening time, bond effect difference the problem of, therefore need a kind of hardening time short at present, bond The good conductive adhesive of effect.
Invention content
To solve the above-mentioned problems, provide that a kind of hardening time is short, the good conductive adhesive of bond effect.The present invention uses Following technical scheme:
A kind of pressure sensitive conductive adhesive, which is characterized in that the raw material including following components:
10-20 parts of acrylic acid, 10-20 parts of methyl acrylate, 20-30 parts of butyl acrylate, 10-20 parts of conductive filler are light-initiated 5-10 parts of agent, 2-3 parts of crosslinking agent, 6-7 parts of poly- second butyl ester, 5-10 parts of accelerating agent.
Present invention employs photoinitiators to close the coefficient scheme of latent curing agent, can be auxiliary by ultraviolet light Carry out curing reaction is helped, the cured efficiency of adhesive is accelerated, and the present invention additionally uses poly- second butyl ester, contributes to the present invention non- Component is sufficiently mixed, and improves the mechanical strength of the present invention.
Preferably, the conductive filler uses silver-coated copper powder.
Present invention employs silver-coated copper powders as conductive filler, and silver-coated copper powder is as conductive filler compared to using the silver powder to have Help reduce cost, and add silver-coated copper powder help to improve the present invention machine capability, and silver-coated copper powder compared to There is higher conductive capability using copper powder, enhance the toughness and abrasive resistance of the present invention.
Preferably, the silver-coated copper powder granularity is 300-450 mesh.
Using the silver-coated copper powder that mesh number is larger in the present invention program, copper powder is contributed to be well dispersed in adhesive system It is interior, it on the one hand can enhance the conductive capability of adhesive, on the other hand can enhance the toughness of adhesive, improve the machinery of product Performance helps to improve the adhesive property of product.
Preferably, the silver-coated copper powder is prepared using following methods:By copper-bath and polyvinylpyrrolidone Mixing so that a concentration of 1-3mol/L of copper sulphate is passed through nitrogen as protective atmosphere, then under the conditions of 50-60 DEG C, is added It is 6-7 that citric acid solution, which adjusts system pH, reacts 20-30min, obtains copper powder, and 20-30 parts are dissipated in water, ammonia is then added dropwise Water, adjustment pH are 8-9, and enuatrol is added, forms suspension, stirs 10-20 minutes, then 5-6 parts of silver nitrates are dissolved in water, It is gradually added drop-wise in the time of 20-30min in the suspension, is filtered after reaction, washed, it is dry.
First, present invention employs the scheme that copper-bath and polyvinylpyrrolidone produce copper powder, help to obtain The smaller copper powder of particle, and nitrogen protection and citric acid are added in preparation process, help to prevent in preparation process Copper powder is aoxidized, and has then used the scheme of ammonium hydroxide and enuatrol again, and the copper oxide of Copper Powder Surface is destroyed by ammonium hydroxide, is then led to It crosses and silver nitrate solution is slowly added dropwise so that copper and silver nitrate are reacted on the contact surface, protect copper will not be because of by enuatrol The oxidation of air forms copper oxide, covers silver-colored effect to improve Copper Powder Surface, improves the electrical efficiency of the present invention.
Preferably, temperature dry in the drying process is 65-70 DEG C.
The present invention contributes to prevent copper powder is heated from quick oxidation occurs using lower drying temperature, prevents conduction Rate reduces.
Preferably, the photoinitiator uses α, α-diethoxy acetophenone, alpha-hydroxyalkyl benzophenone, α-amine alkylbenzene One or more of ketone combines.
Preferably, the crosslinking agent uses N, N- methylene-bisacrylamides, the accelerating agent to use N, N- bis- Ethyl aniline.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 85-90 DEG C, 15-20min adds crosslinking agent, after reacting 20-30min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 4-5h, is cooled to room temperature.
The present invention first by the acrylic acid hybrid reaction of butyl acrylate, methyl acrylate and a part, is crosslinked, so After add surplus stock, contribute to reinforce raw material mixed effect, while also contribute to improve the present invention cementitiousness.
Specific implementation mode
The present invention is further expalined with reference to specific implementation case:
Embodiment 1
A kind of pressure sensitive conductive adhesive includes the raw material of following components:
10 parts of acrylic acid, 10 parts of methyl acrylate, 20 parts of butyl acrylate, 10 parts, α of silver-coated copper powder, α-diethoxy acetophenone 5 Part, N, 2 parts of N- methylene-bisacrylamides, 6 parts, N of poly- second butyl ester, 5 parts of N- diethylanilines.
Wherein, the silver-coated copper powder granularity is 300 mesh.
Wherein, the silver-coated copper powder is prepared using following methods:Copper-bath and polyvinylpyrrolidone are mixed, So that a concentration of 1mol/L of copper sulphate, is passed through nitrogen as protective atmosphere, then under the conditions of 50 DEG C, citric acid solution is added Adjustment system pH is 6-7, reacts 20min, obtains copper powder, and 20 parts are dissipated in water, and ammonium hydroxide is then added dropwise, and adjustment pH is 8, is added Enuatrol forms suspension, stirs 10 minutes, then 5 parts of silver nitrates are dissolved in water, and institute is gradually added drop-wise within the time of 20min It in the suspension stated, filters, washs, 65 DEG C of dryings after reaction.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 85 DEG C, 15min adds crosslinking agent, after reacting 20min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 4h, is cooled to room temperature.
Embodiment 2
A kind of pressure sensitive conductive adhesive includes the raw material of following components:
20 parts of acrylic acid, 20 parts of methyl acrylate, 30 parts of butyl acrylate, 20 parts, α, α-diethoxy acetophenone of silver-coated copper powder 10 parts, N, 3 parts of N- methylene-bisacrylamides, 7 parts, N of poly- second butyl ester, 10 parts of N- diethylanilines.
Wherein, the silver-coated copper powder granularity is 450 mesh.
Wherein, the silver-coated copper powder is prepared using following methods:Copper-bath and polyvinylpyrrolidone are mixed, So that a concentration of 3mol/L of copper sulphate, is passed through nitrogen as protective atmosphere, then under the conditions of 60 DEG C, citric acid solution is added Adjustment system pH is 7, reacts 30min, obtains copper powder, and 30 parts are dissipated in water, and ammonium hydroxide is then added dropwise, and adjustment pH is 9, and oil is added Sour sodium forms suspension, stirs 20 minutes, then 6 parts of silver nitrates are dissolved in water, and is gradually added drop-wise within the time of 30min described Suspension in, filtered after reaction, wash, 70 DEG C of dryings.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 90 DEG C, 20min adds crosslinking agent, after reacting 30min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 5h, is cooled to room temperature.
Embodiment 3
A kind of pressure sensitive conductive adhesive includes the raw material of following components:
15 parts of acrylic acid, 15 parts of methyl acrylate, 25 parts of butyl acrylate, 15 parts, α of silver-coated copper powder, α-diethoxy acetophenone 7 Part, N, 2 parts of N- methylene-bisacrylamides, 6 parts, N of poly- second butyl ester, 7 parts of N- diethylanilines.
Wherein, the silver-coated copper powder granularity is 400 mesh.
Wherein, the silver-coated copper powder is prepared using following methods:Copper-bath and polyvinylpyrrolidone are mixed, So that a concentration of 2mol/L of copper sulphate, is passed through nitrogen as protective atmosphere, then under the conditions of 55 DEG C, citric acid solution is added Adjustment system pH is 4, reacts 25min, obtains copper powder, and 25 parts are dissipated in water, and ammonium hydroxide is then added dropwise, and adjustment pH is 8, and oil is added Sour sodium forms suspension, stirs 15 minutes, then 5 parts of silver nitrates are dissolved in water, and is gradually added drop-wise within the time of 25min described Suspension in, filtered after reaction, wash, 70 DEG C of dryings.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 90 DEG C, 15min adds crosslinking agent, after reacting 25min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 5h, is cooled to room temperature.
Embodiment 4
A kind of pressure sensitive conductive adhesive includes the raw material of following components:
12 parts of acrylic acid, 12 parts of methyl acrylate, 23 parts of butyl acrylate, 13 parts, α of silver-coated copper powder, α-diethoxy acetophenone 7 Part, N, 2 parts of N- methylene-bisacrylamides, 7 parts, N of poly- second butyl ester, 6 parts of N- diethylanilines.
Wherein, the silver-coated copper powder granularity is 320 mesh.
Wherein, the silver-coated copper powder is prepared using following methods:Copper-bath and polyvinylpyrrolidone are mixed, So that a concentration of 1mol/L of copper sulphate, is passed through nitrogen as protective atmosphere, then under the conditions of 52 DEG C, citric acid solution is added Adjustment system pH is 6, reacts 22min, obtains copper powder, and 22 parts are dissipated in water, and ammonium hydroxide is then added dropwise, and adjustment pH is 8, and oil is added Sour sodium forms suspension, stirs 10 minutes, then 5-6 parts of silver nitrates are dissolved in water, and institute is gradually added drop-wise within the time of 20min It in the suspension stated, filters, washs, 65 DEG C of dryings after reaction.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 85 DEG C, 15min adds crosslinking agent, after reacting 22min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 4h, is cooled to room temperature.
Embodiment 5
A kind of pressure sensitive conductive adhesive includes the raw material of following components:
19 parts of acrylic acid, 18 parts of methyl acrylate, 28 parts of butyl acrylate, 17 parts, α of silver-coated copper powder, α-diethoxy acetophenone 8 Part, N, 2 parts of N- methylene-bisacrylamides, 7 parts, N of poly- second butyl ester, 7 parts of N- diethylanilines.
Wherein, the silver-coated copper powder granularity is 300 mesh.
Wherein, the silver-coated copper powder is prepared using following methods:Copper-bath and polyvinylpyrrolidone are mixed, So that a concentration of 1mol/L of copper sulphate, is passed through nitrogen as protective atmosphere, then under the conditions of 50 DEG C, citric acid solution is added Adjustment system pH is 6, reacts 30min, obtains copper powder, and 20 parts are dissipated in water, and ammonium hydroxide is then added dropwise, and adjustment pH is 8, and oil is added Sour sodium forms suspension, stirs 20 minutes, then 6 parts of silver nitrates are dissolved in water, and is gradually added drop-wise within the time of 30min described Suspension in, filtered after reaction, wash, 70 DEG C of dryings.
A kind of preparation method of pressure sensitive conductive adhesive, which is characterized in that include the following steps:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 88 DEG C, 18min adds crosslinking agent, after reacting 24min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 5h, is cooled to room temperature.

Claims (8)

1. a kind of pressure sensitive conductive adhesive, which is characterized in that the raw material including following components:
10-20 parts of acrylic acid, 10-20 parts of methyl acrylate, 20-30 parts of butyl acrylate, 10-20 parts of conductive filler are light-initiated 5-10 parts of agent, 2-3 parts of crosslinking agent, 6-7 parts of poly- second butyl ester, 5-10 parts of accelerating agent.
2. a kind of pressure sensitive conductive adhesive according to claim 1, it is characterised in that:The conductive filler is wrapped using silver Copper powder.
3. a kind of pressure sensitive conductive adhesive according to claim 2, it is characterised in that:The silver-coated copper powder granularity is 300-450 mesh.
4. a kind of pressure sensitive conductive adhesive according to claim 3, which is characterized in that the silver-coated copper powder is using following It is prepared by method:Copper-bath and polyvinylpyrrolidone are mixed so that a concentration of 1-3mol/L of copper sulphate is passed through nitrogen As protective atmosphere, then under the conditions of 50-60 DEG C, citric acid solution is added and adjusts system pH between 6-7, reacts 20- 30min obtains copper powder, and 20-30 parts are dissipated in water, ammonium hydroxide is then added dropwise, pH is between 8-9 for adjustment, and enuatrol is added, and is formed Suspension stirs 10-20 minute, then 5-6 parts of silver nitrates are dissolved in water, be gradually added drop-wise within the time of 20-30min described in It in suspension, filters, washs after reaction, it is dry.
5. a kind of pressure sensitive conductive adhesive according to claim 4, it is characterised in that:Drying in the drying process Temperature is 65-70 DEG C.
6. a kind of pressure sensitive conductive adhesive according to claim 1, it is characterised in that:The photoinitiator uses α, α- One or more of diethoxy acetophenone, alpha-hydroxyalkyl benzophenone, α-amine alkyl phenones combine.
7. a kind of pressure sensitive conductive adhesive according to claim 1, it is characterised in that:The crosslinking agent uses N, N- sub- Bisacrylamide, the accelerating agent use N, N- diethylanilines.
8. a kind of preparation method of pressure sensitive conductive adhesive according to one of claim 1-7, which is characterized in that including with Lower step:
(1)The acrylic acid of butyl acrylate, methyl acrylate and a part is mixed, stirs evenly, is heated to 85-90 DEG C, 15-20min adds crosslinking agent, after reacting 20-30min;
(2)Remaining acrylic acid is added dropwise, adds surplus stock, continues to heat 4-5h, is cooled to room temperature.
CN201810337644.8A 2018-04-16 2018-04-16 A kind of pressure sensitive conductive adhesive and preparation method thereof Pending CN108659747A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111500215A (en) * 2020-04-30 2020-08-07 张家港保税区汇英聚福材料科技合伙企业(有限合伙) Pressure-sensitive conductive adhesive and preparation method thereof
IT201900015794A1 (en) * 2019-09-06 2021-03-06 Jianqiang Zhao Fast setting conductive adhesive at room temperature

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698784A (en) * 2009-09-22 2010-04-28 北京高盟化工有限公司 Pressure sensitive conductive adhesive composite and preparation method thereof
CN105219315A (en) * 2015-11-09 2016-01-06 深圳德邦界面材料有限公司 A kind of sedimentation-prevention type pressure-sensitive conductive glue and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101698784A (en) * 2009-09-22 2010-04-28 北京高盟化工有限公司 Pressure sensitive conductive adhesive composite and preparation method thereof
CN105219315A (en) * 2015-11-09 2016-01-06 深圳德邦界面材料有限公司 A kind of sedimentation-prevention type pressure-sensitive conductive glue and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IT201900015794A1 (en) * 2019-09-06 2021-03-06 Jianqiang Zhao Fast setting conductive adhesive at room temperature
CN111500215A (en) * 2020-04-30 2020-08-07 张家港保税区汇英聚福材料科技合伙企业(有限合伙) Pressure-sensitive conductive adhesive and preparation method thereof
CN111500215B (en) * 2020-04-30 2021-11-26 张家港保税区汇英聚福材料科技合伙企业(有限合伙) Pressure-sensitive conductive adhesive and preparation method thereof

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