CN106883786A - A kind of preparation method of comprehensive thermal setting conductive glue - Google Patents
A kind of preparation method of comprehensive thermal setting conductive glue Download PDFInfo
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- CN106883786A CN106883786A CN201710102258.6A CN201710102258A CN106883786A CN 106883786 A CN106883786 A CN 106883786A CN 201710102258 A CN201710102258 A CN 201710102258A CN 106883786 A CN106883786 A CN 106883786A
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- thermal setting
- setting conductive
- conductive glue
- glue
- comprehensive thermal
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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
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention discloses a kind of preparation method of comprehensive thermal setting conductive glue, comprise the following steps：S1：Prepare the raw material of following percentage by weight：Conducting particles 10% 20%, Graphene 0.5% 1.5%, epoxy resin 20% 35%, ethylene-vinyl acetate PUR 5% 12%, sagging inhibitor 0.5% 1%, latent curing agent 2% 4%, curing accelerator 0% 1%, antioxidant 0.2% 0.5%, diluent 30% 50%；S2：Conducting particles, Graphene, epoxy resin, ethylene-vinyl acetate PUR, sagging inhibitor, antioxidant and diluent are mixed, is then stirred, mixture A is obtained, mixture A addition three-rollers are ground；S3：Addition latent curing agent and curing accelerator, are then stirred, and mixture B is obtained, and mixture B is ground with three-roller then, and control temperature is obtained material below 35 DEG C；S4：Material is carried out into froth in vacuum, conducting resinl glue is obtained；S5：By conducting resinl glue-coating in drying tunnel temperature on the transparent mould release membrances of PET, is controlled for 90 100 DEG C, coating speed is 8 12m/min, and glue thickness is 30 60 μm after drying.After the completion of coating, comprehensive thermal setting conductive glue is obtained.The prepared comprehensive thermal setting conductive glue of the present invention is ultra-thin, and possesses excellent adhesion strength and electric conductivity, and compatibility is good, prepares simple, low cost.
Description
Technical field
The present invention relates to a kind of thermal setting conductive glue, more particularly to a kind of preparation method of comprehensive thermal setting conductive glue.The heat
Gu conducting resinl is applied to the fields such as flexible printed-circuit board (FPC), Rigid Flex, belong to conductive adhesive field.
Background technology
Thermal setting conductive glue is widely used in fields such as flexible printed-circuit board (FPC), Rigid Flexs, mainly passes through
Electrical connection is obtained with FPC circuit boards, electromagnetic shielding and reinforcing earthing effect is played.It is particularly applicable in smart mobile phone mainboard mould
Group, digital photo camera module etc..
The existing most adhesion strength of thermal setting conductive glue is relatively low, easily cracking, causes circuit board service life to shorten；And
Thickness is thicker, it is impossible to be applicable the trend of circuit board ultrathin now.Therefore, led we have proposed a kind of novel omnibearing thermosetting
The preparation method of electric glue is used to solve the above problems.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes a kind of preparation side of comprehensive thermal setting conductive glue
Method.
A kind of preparation method of comprehensive thermal setting conductive glue proposed by the present invention, comprises the following steps：
S1：Prepare the raw material of following percentage by weight：Conducting particles 10%-20%, Graphene 0.5%-1.5%, epoxy
Resin 20%-35%, ethene-vinyl acetate PUR 5%-12%, sagging inhibitor 0.5%-1%, latent curing agent 2%-
4%, curing accelerator 0%-1%, antioxidant 0.2%-0.5%, diluent 30%-50%；
S2：By conducting particles, Graphene, epoxy resin, ethene-vinyl acetate PUR, sagging inhibitor, antioxidant and
Diluent mixes, and then stirs, and mixture A is obtained, and mixture A addition three-rollers are ground；
S3：Addition latent curing agent and curing accelerator, then stir, and mixture B is obtained, and then use three-roller
Mixture B is ground, control temperature is obtained material below 35 DEG C；
S4：Material is carried out into froth in vacuum, conducting resinl glue is obtained；
S5：By conducting resinl glue-coating on the transparent mould release membrances of PET, controlling drying tunnel temperature for 90-100 DEG C, coating speed
It is 8-12m/min, glue thickness is 30-60 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
Preferably, in the S1, epoxy resin is solid epoxy, and the softening point of epoxy resin is 80-105 DEG C；Second
The softening point of alkene-vinyl acetate PUR is 80-90 DEG C.
Preferably, in the S1, conducting particles is one or more in bronze, silver powder, silver-coated copper powder, copper powder and nickel powder
Combination, particle shape is spherical and piece shape, and two kinds of form ratios are 0.2-2, and granularity is 1.5-40 μm；Antioxidant is antioxygen
Agent 1010；Diluent is the combination of one or more in acetone, ethyl acetate, cyclohexanone and toluene.
Preferably, in the S1, the latent curing agent is dicyandiamide and its derivative, and particle diameter is 1-5 μm；Solidification
Accelerator is imidazoles accelerator；Graphene is less than 5 layers (content >=90%) Graphenes；Sagging inhibitor is that polyamide wax is gentle
One kind in aerosil, and granularity is 1-2 μm.
Preferably, in the S1, the raw material of following percentage by weight is prepared：Conducting particles 12%-19%, Graphene
0.6%-1%, epoxy resin 23%-31%, ethene-vinyl acetate PUR 5%-10%, sagging inhibitor 0.5%-0.8%,
Latent curing agent 3%-4%, curing accelerator 0.5%-1%, antioxidant 0.2%-0.5%, diluent 35%-45%.
Preferably, in the S5, by conducting resinl glue-coating on the transparent mould release membrances of PET, control drying tunnel temperature be 92-98
DEG C, coating speed is 9-11m/min, and glue thickness is 30-40 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
Preferably, in the S5, the thickness of the transparent mould release membrances of PET is 50 μm, and off-type force is 15g/inch.
In the present invention, a kind of preparation method of comprehensive thermal setting conductive glue possesses advantages below：
1st, it is ultra-thin：Domestic thermal setting conductive glue mostly can only accomplish 40-60 μ m thicks, and the present invention can accomplish the same of 30 μ m-thicks
When, adhesion strength does not weaken；
2nd, Graphene is added, excellent electric conductivity greatly reduces the addition of metal dust, reduces cost simultaneously,
Resin obtains ratio lifting, and adhesion strength has reached general thermal setting conductive glue more than 1.3 times；
3rd, compatibility is good, is applicable various welding procedures；
4th, room temperature working life be more than 30 days, common product was at 15 days or so.
The prepared comprehensive thermal setting conductive glue of the present invention is ultra-thin, and possesses excellent adhesion strength and electric conductivity, and compatibility is good,
Prepare simple, low cost.
Brief description of the drawings
Fig. 1 be a kind of comprehensive thermal setting conductive glue proposed by the present invention preparation method obtained in thermal setting conductive glue structure
Schematic diagram；
Fig. 2 be a kind of comprehensive thermal setting conductive glue proposed by the present invention preparation method obtained in thermal setting conductive glue application
Case structure schematic diagram；
Fig. 3 be a kind of comprehensive thermal setting conductive glue proposed by the present invention preparation method obtained in thermal setting conductive glue use
Process chart.
In figure：1 conductive glue surface, the transparent mould release membrances of 2 PET, 3 metallic plates, 4 polyimide films, 5 FPC wiring boards.
Specific embodiment
The present invention is made with reference to specific embodiment further explain.
Embodiment one
Reference picture 1, the present embodiment proposes a kind of preparation method of comprehensive thermal setting conductive glue, comprises the following steps：
S1：Prepare the raw material of following percentage by weight：Silver-coated copper powder 18.5%, Graphene 0.6%, epoxy resin
28.7%, ethene-vinyl acetate PUR 8.6%, cyanoguanidine derivative 3.2%, 2-methylimidazole 0.6%, polyamide wax
0.7%, antioxidant 1010 0.3%, diluent 38.8%；
S2：By conducting particles, Graphene, epoxy resin, ethene-vinyl acetate PUR, sagging inhibitor, antioxidant and
Diluent mixes, and then stirs, and mixture A is obtained, and mixture A addition three-rollers are ground；
S3：Addition latent curing agent and curing accelerator, then stir, and mixture B is obtained, and then use three-roller
Mixture B is ground, control temperature is obtained material below 35 DEG C；
S4：Material is carried out into froth in vacuum, conducting resinl glue is obtained；
S5：By conducting resinl glue-coating on the transparent mould release membrances of PET, controlling drying tunnel temperature for 90 DEG C, coating speed is
10m/min, glue thickness is 30 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
Embodiment two
Reference picture 1, the present embodiment proposes a kind of preparation method of comprehensive thermal setting conductive glue, comprises the following steps：
S1：Prepare the raw material of following percentage by weight：Copper powder 13.5%, silver-coated copper powder 6.5%, Graphene 0.8%, epoxy
Resin 30.4%, ethene-vinyl acetate PUR 6.5%, cyanoguanidine derivative 3.3%, 2-methylimidazole 0.6%, polyamide
Wax 0.5%, antioxidant 1010 0.5%, diluent 37.4%；
S2：By conducting particles, Graphene, epoxy resin, ethene-vinyl acetate PUR, sagging inhibitor, antioxidant and
Diluent mixes, and then stirs, and mixture A is obtained, and mixture A addition three-rollers are ground；
S3：Addition latent curing agent and curing accelerator, then stir, and mixture B is obtained, and then use three-roller
Mixture B is ground, control temperature is obtained material below 35 DEG C；
S4：Material is carried out into froth in vacuum, conducting resinl glue is obtained；
S5：By conducting resinl glue-coating on the transparent mould release membrances of PET, controlling drying tunnel temperature for 100 DEG C, coating speed is
12m/min, glue thickness is 30 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
Storage condition：
Thermal setting conductive glue condition of storage must is fulfilled for following condition：In 3 DEG C -8 DEG C of temperature, relative humidity (RH)≤60%
Preserved in environment.
Reference picture 2-3, uses technique：
1st, before using the gluing knot FPC wiring boards 5 of thermal setting conductive and metallic plate 3, first cleaning circuit plate polyimide film (PI) 4
Face and the adhesive surface of metallic plate 3, are dried with after alkali cleaning pickling；
2nd, conductive glue surface 1 is engaged with the face of polyimide film (PI) 4 of FPC wiring boards 5, in 100 DEG C or so of heating
Pre- laminating is carried out on platform, the transparent mould release membrances 2 of PET are thrown off, metallic plate 3 of being fitted on warm table, then hot-press solidifying, presses condition
170-180 DEG C, pressing time 3-5min, pressure 3-4MPa take out after the completion of hot pressing and are positioned in 140-160 DEG C of baking oven；
3rd, 140-160 DEG C of solidify afterwards × 1h in an oven.
Performance test is contrasted：
Comparative example 1 is domestic thermal setting conductive glue, and comparative example 2 is import thermal setting conductive glue；
Resistance change rate is the electricity before (resistance before resistance-conducting resinl soldering after conducting resinl soldering)/conducting resinl soldering
Resistance；
Peel strength according to IPC-TM-650 2.4.9 chapters method of testing；
Resistance to tin-welding according to IPC-TM-650 2.4.139 chapters method of testing.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (7)
1. a kind of preparation method of comprehensive thermal setting conductive glue, it is characterised in that comprise the following steps：
S1：Prepare the raw material of following percentage by weight：Conducting particles 10%-20%, Graphene 0.5%-1.5%, epoxy resin
20%-35%, ethene-vinyl acetate PUR 5%-12%, sagging inhibitor 0.5%-1%, latent curing agent 2%-4%,
Curing accelerator 0%-1%, antioxidant 0.2%-0.5%, diluent 30%-50%；S2：By conducting particles, Graphene, ring
The mixing of oxygen tree fat, ethene-vinyl acetate PUR, sagging inhibitor, antioxidant and diluent, then stirs, and is obtained mixed
Compound A, mixture A addition three-rollers are ground；
S3：Addition latent curing agent and curing accelerator, then stir, and mixture B is obtained, then with three-roller to mixed
Compound B is ground, and control temperature is obtained material below 35 DEG C；
S4：Material is carried out into froth in vacuum, conducting resinl glue is obtained；
S5：By conducting resinl glue-coating on the transparent mould release membrances of PET, controlling drying tunnel temperature for 90-100 DEG C, coating speed is 8-
12m/min, glue thickness is 30-60 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
2. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S1,
Epoxy resin is solid epoxy, and the softening point of epoxy resin is 80-105 DEG C；The softening point of ethene-vinyl acetate PUR
It is 80-90 DEG C.
3. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S1,
Conducting particles is one or more of combination in bronze, silver powder, silver-coated copper powder, copper powder and nickel powder, particle shape for spherical and
Piece shape, two kinds of form ratios are 0.2-2, and granularity is 1.5-40 μm；Antioxidant is antioxidant 1010；Diluent be acetone,
One or more in ethyl acetate, cyclohexanone and toluene of combination.
4. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S1,
The latent curing agent is dicyandiamide and its derivative, and particle diameter is 1-5 μm；Curing accelerator is imidazoles accelerator；Stone
Black alkene is less than 5 layers (content >=90%) Graphenes；Sagging inhibitor is the one kind in polyamide wax and aerosil, and grain
Spend is 1-2 μm.
5. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S1,
Prepare the raw material of following percentage by weight：Conducting particles 12%-19%, Graphene 0.6%-1%, epoxy resin 23%-31%,
Ethene-vinyl acetate PUR 5%-10%, sagging inhibitor 0.5%-0.8%, latent curing agent 3%-4%, solidification promote
Agent 0.5%-1%, antioxidant 0.2%-0.5%, diluent 35%-45%.
6. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S5,
By conducting resinl glue-coating on the transparent mould release membrances of PET, controlling drying tunnel temperature for 92-98 DEG C, coating speed is 9-11m/min,
Glue thickness is 30-40 μm after drying；After the completion of coating, comprehensive thermal setting conductive glue is obtained.
7. the preparation method of a kind of comprehensive thermal setting conductive glue according to claim 1, it is characterised in that in the S5,
The thickness of the transparent mould release membrances of PET is 50 μm, and off-type force is 15g/inch.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710102258.6A CN106883786A (en) | 2017-02-24 | 2017-02-24 | A kind of preparation method of comprehensive thermal setting conductive glue |
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| CN201710102258.6A CN106883786A (en) | 2017-02-24 | 2017-02-24 | A kind of preparation method of comprehensive thermal setting conductive glue |
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| CN201710102258.6A Pending CN106883786A (en) | 2017-02-24 | 2017-02-24 | A kind of preparation method of comprehensive thermal setting conductive glue |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502276A (en) * | 2017-08-25 | 2017-12-22 | 安徽省鸿鑫生物科技有限公司 | A kind of LED encapsulation electrically conductive polyamide PUR and preparation method thereof |
| CN107698998A (en) * | 2017-09-25 | 2018-02-16 | 江苏时瑞电子科技有限公司 | A kind of electrocondution slurry organic carrier and preparation method thereof |
| CN112457798A (en) * | 2020-11-25 | 2021-03-09 | 山东金鼎电子材料有限公司 | High-thermal-conductivity low-resistance graphene conductive adhesive and preparation method thereof |
| CN113185931A (en) * | 2021-03-31 | 2021-07-30 | 浙江中科玖源新材料有限公司 | Transparent conductive film and preparation method thereof |
| CN115678473A (en) * | 2022-11-09 | 2023-02-03 | 宁夏中色新材料有限公司 | Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof |
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| CN105086873A (en) * | 2015-08-07 | 2015-11-25 | 华烁科技股份有限公司 | Isotropous thermosetting conductive adhesive film and preparation method thereof |
| CN106147665A (en) * | 2016-07-01 | 2016-11-23 | 深圳市烯世传奇科技有限公司 | A kind of durability heat-conducting glue based on graphene powder and preparation method thereof |
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| CN104877611A (en) * | 2009-11-17 | 2015-09-02 | 日立化成工业株式会社 | Circuit Connection Material, Connection Structure Using Same, And Temporary Pressure-bonding Method |
| CN104017511A (en) * | 2014-06-20 | 2014-09-03 | 莱芜金鼎电子材料有限公司 | Preparation method of epoxy resin conductive adhesive film and conductive adhesive layer of epoxy resin conductive adhesive film |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107502276A (en) * | 2017-08-25 | 2017-12-22 | 安徽省鸿鑫生物科技有限公司 | A kind of LED encapsulation electrically conductive polyamide PUR and preparation method thereof |
| CN107698998A (en) * | 2017-09-25 | 2018-02-16 | 江苏时瑞电子科技有限公司 | A kind of electrocondution slurry organic carrier and preparation method thereof |
| CN112457798A (en) * | 2020-11-25 | 2021-03-09 | 山东金鼎电子材料有限公司 | High-thermal-conductivity low-resistance graphene conductive adhesive and preparation method thereof |
| CN113185931A (en) * | 2021-03-31 | 2021-07-30 | 浙江中科玖源新材料有限公司 | Transparent conductive film and preparation method thereof |
| CN115678473A (en) * | 2022-11-09 | 2023-02-03 | 宁夏中色新材料有限公司 | Single-component silver conductive adhesive suitable for normal-temperature storage and preparation method thereof |
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Application publication date: 20170623 |