CN116751533B - Non-post-curing epoxy adhesive tape and preparation method thereof - Google Patents

Non-post-curing epoxy adhesive tape and preparation method thereof Download PDF

Info

Publication number
CN116751533B
CN116751533B CN202311027432.7A CN202311027432A CN116751533B CN 116751533 B CN116751533 B CN 116751533B CN 202311027432 A CN202311027432 A CN 202311027432A CN 116751533 B CN116751533 B CN 116751533B
Authority
CN
China
Prior art keywords
parts
epoxy
curing
adhesive tape
post
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202311027432.7A
Other languages
Chinese (zh)
Other versions
CN116751533A (en
Inventor
周义博
吴书鹏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Suzhou Fineset Material Technology Co ltd
Original Assignee
Suzhou Fineset Material Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Suzhou Fineset Material Technology Co ltd filed Critical Suzhou Fineset Material Technology Co ltd
Priority to CN202311027432.7A priority Critical patent/CN116751533B/en
Publication of CN116751533A publication Critical patent/CN116751533A/en
Application granted granted Critical
Publication of CN116751533B publication Critical patent/CN116751533B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/30Adhesives in the form of films or foils characterised by the adhesive composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/4007Curing agents not provided for by the groups C08G59/42 - C08G59/66
    • C08G59/4014Nitrogen containing compounds
    • C08G59/4021Ureas; Thioureas; Guanidines; Dicyandiamides
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
    • C08G59/5026Amines cycloaliphatic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
    • C08G59/56Amines together with other curing agents
    • 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
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • 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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/20Adhesives in the form of films or foils characterised by their carriers
    • C09J7/22Plastics; Metallised plastics
    • C09J7/25Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
    • 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
    • C09J7/00Adhesives in the form of films or foils
    • C09J7/40Adhesives in the form of films or foils characterised by release liners
    • 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
    • C09J2301/00Additional features of adhesives in the form of films or foils
    • C09J2301/10Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
    • C09J2301/12Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
    • C09J2301/122Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
    • 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
    • C09J2479/00Presence of polyamine or polyimide
    • C09J2479/08Presence of polyamine or polyimide polyimide
    • C09J2479/086Presence of polyamine or polyimide polyimide in the substrate

Abstract

The invention relates to the technical field of adhesives, and discloses a non-post-curing epoxy adhesive tape and a preparation method thereof, wherein the epoxy adhesive tape sequentially comprises a substrate layer, an epoxy adhesive film layer and a release film layer from bottom to top along the thickness direction, and the epoxy adhesive film layer comprises the following raw materials in parts by weight: 70-100 parts of bisphenol A epoxy resin, 50-80 parts of dihydric alcohol diglycidyl ether, 0-20 parts of flexibilizer, 5-15 parts of curing agent, 50-100 parts of butanone and 15 parts of N, N-dimethylformamide, wherein the curing agent is formed by mixing alicyclic amine and dicyandiamide, and the dicyandiamide is mixed with the alicyclic amine after being dissolved by the N, N-dimethylformamide. The epoxy adhesive tape has the advantages of high adhesive strength and good temperature resistance, does not need post-curing in the preparation process, and has short preparation period and high adhesive speed.

Description

Non-post-curing epoxy adhesive tape and preparation method thereof
Technical Field
The invention relates to the technical field of adhesives, in particular to a non-post-curing epoxy adhesive tape and a preparation method thereof.
Background
Epoxy adhesives have been attracting attention because of their high adhesive strength, low shrinkage, stable chemical properties, and excellent electrical insulation properties, and can be used for structural adhesion of common materials such as metals and plastics. The method is widely applied to industries such as electronic products, automobiles, buildings and the like. For example, in a new flexible circuit production process, copper foil is cut in advance according to the circuit layout requirement, and then PI substrate epoxy tapes are attached to two sides of the cut circuit, so that the flexible circuit is produced.
At present, the existing epoxy adhesive tape is usually required to be pre-bonded at a high temperature, the bonding strength after pre-bonding is generally not high, and meanwhile, due to the fact that a powder-form latent curing agent (such as dicyandiamide, anhydride and the like) is generally used for post-curing, the existing epoxy adhesive tape is required to undergo a post-curing process for 0.5-2 hours at a higher temperature so as to meet the requirements of sufficient bonding strength and high temperature resistance. This tends to severely reduce the productivity of the relevant product, resulting in a significant increase in production costs. Meanwhile, the use of the powdery curing agent also brings challenges and uncertainty to the dispersion uniformity, the coating uniformity, the appearance and the like in the production process of the adhesive tape. In addition, the existing epoxy adhesive tape often uses a latent curing agent, so that the epoxy adhesive tape is required to be stored at a low temperature below 10 ℃ in order to ensure stable performance, so that the transportation flexibility of the epoxy adhesive tape is greatly limited, and meanwhile, the cost is raised.
Therefore, there is a need to develop an epoxy adhesive tape that is simple to produce, does not require post-curing, and can be stored at normal temperature, so as to meet the increasingly urgent application requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a non-post-curing epoxy adhesive tape.
In order to achieve the above purpose, the invention adopts the following technical scheme: the non-post-curing type epoxy adhesive tape is characterized by comprising a substrate layer, an epoxy adhesive film layer and a release film layer from bottom to top in sequence along the thickness direction, wherein the epoxy adhesive film layer comprises the following raw materials in parts by weight: 70-100 parts of bisphenol A epoxy resin, 50-80 parts of dihydric alcohol diglycidyl ether, 0-20 parts of flexibilizer, 5-15 parts of curing agent, 50-100 parts of butanone and 15 parts of N, N-dimethylformamide, wherein the curing agent is formed by mixing alicyclic amine and dicyandiamide, and the dicyandiamide is mixed with the alicyclic amine after being dissolved by the N, N-dimethylformamide.
As a specific embodiment, the epoxy equivalent of the bisphenol a epoxy resin adopted in the raw materials is between 700 and 2500, and the epoxy equivalent of the dihydric alcohol diglycidyl ether is between 100 and 400, wherein the epoxy equivalent of the epoxy resin has a great influence on the final performance of the adhesive tape, and the poor flexibility of the adhesive film and poor adhesiveness of the substrate are caused by the excessively low epoxy equivalent, so that the risk of de-base is generated; too high an epoxy equivalent would cause difficulties in dissolving the epoxy resin, which is disadvantageous for coating.
As a specific embodiment, the toughening agent employs an epoxidized diene having an epoxide equivalent weight of between 100 and 300.
As a specific embodiment, the bisphenol A type epoxy resin is at least one of NPES-903H, NPES-907 and NPES-909 manufactured by Nanya plastics industry Co., ltd (hereinafter referred to as Nanya plastics).
As a specific embodiment, the glycol glycidyl ether is commercially available from the Japanese Sanyo chemical industry under the specific model number GLYCI-ALE PP-300P.
As a specific embodiment, the toughening agent is an epoxidized polybutadiene model DAICEL PB-3600 manufactured by Daicel trade (Shanghai) Inc.
As a specific embodiment, the curing agent is prepared from alicyclic amine and dicyandiamide according to a mass ratio of 1-5:1, wherein the alicyclic amine adopts at least one of menthane diamine and isophorone diamine, the alicyclic amine is liquid, and the dicyandiamide is powder.
Another object of the present invention is to provide a method for preparing a non-post-curable epoxy tape, for preparing the above-mentioned non-post-curable epoxy tape, comprising the steps of:
1) Mixing bisphenol A epoxy resin and butanone according to a proportion, rapidly stirring in a high-speed stirrer until the epoxy resin is completely dissolved, then sequentially adding dihydric alcohol diglycidyl ether and a toughening agent into the completely dissolved epoxy resin, and continuously stirring for 20min until the epoxy resin is uniformly mixed;
2) Dissolving dicyandiamide in N, N-dimethylformamide, sequentially adding alicyclic amine and the dissolved dicyandiamide into the uniformly mixed glue solution, and stirring at a high speed for 10-15min;
3) Coating the glue solution prepared in the step 2) on a Polyimide (PI) substrate with the thickness of 50 mu m in a pot life through a scraper or a coater, putting the polyimide substrate into a high-temperature oven, baking the polyimide substrate for 5min at 135 ℃, removing the solvent, finishing the primary curing reaction, ensuring the thickness of the dry glue to be 30 mu m plus or minus 1 mu m, then attaching a release film, and standing the film for 72h at the temperature of 60 ℃ to ensure the complete reaction of the curing agent, thereby finishing the preparation of the epoxy adhesive tape.
The dicyandiamide of the latent powder curing agent is dissolved in the solvent in advance, so that the risks of poor appearance and adhesive property caused by uneven dispersion of glue solution are greatly reduced, the application period of the sufficient glue is ensured to ensure the coating stability, the reactivity of the related latent curing agent is improved, the curing reaction of the coated epoxy glue is ensured to be complete within a certain time, and the normal-temperature storage stability of the epoxy glue is improved.
As a specific embodiment, the substrate is a PI substrate.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1) Compared with the existing products, the epoxy adhesive tape adopting the formula does not need to carry out time-consuming post-curing process when in application, can achieve high bonding strength only at a certain temperature (150 ℃) and under a certain pressure (0.4 Mpa) for 5-8min, has no foaming and glue overflowing at 220 ℃ after bonding, and has good temperature resistance;
2) According to the invention, the curing agent adopts alicyclic amine and dicyandiamide to be used in a matched manner, so that the complex time-consuming process required by the dispersion of solid dicyandiamide powder is avoided, the application period is longer than 6 hours at normal temperature, the coating stability and the production feasibility are ensured, the thermal deformation temperature of the epoxy resin cured by the alicyclic amine system is relatively higher, the thermal deformation temperature of the epoxy resin can reach about 150 ℃, the epoxy resin has better temperature resistance, the epoxy resin cured by the dicyandiamide has relatively suitable application period at normal temperature, the thermal deformation temperature of the epoxy resin cured by the dicyandiamide is relatively lower, a certain bonding strength can be realized at relatively lower hot-pressing temperature and in shorter time, the dicyandiamide can be used as a latent curing agent when in powder form, the curing required temperature is higher (more than 180 ℃), the reactivity of the dicyandiamide is greatly increased, the latent effect is lost, the reaction curing can be completed at lower temperature and shorter time, the thermal deformation temperature after the curing of the two curing agent systems can be regulated and controlled, the bonding strength can be realized in a short time, and the bonding strength and the protection function can be realized for bonding materials;
3) The epoxy adhesive tape prepared by the invention does not need a post-curing process in the preparation process, does not exist a latent curing agent after complete reaction, does not need a conventional high-temperature post-curing process, and can still keep good adhesiveness and flexibility on a PI substrate when the thickness of the adhesive tape is 30 mu m through a reasonable toughening agent system.
Detailed Description
The technical scheme of the invention is further described below in conjunction with specific embodiments.
Example 1
In this example, a non-post-curing epoxy adhesive tape is provided, which is prepared as follows:
1) 100 parts of bisphenol A epoxy resin (NPES-909) is dissolved in 100 parts of butanone, a high-speed stirrer is used for stirring until the epoxy resin is completely dissolved, then 50 parts of GLYCI-ALE PP-300P and 15 parts of epoxidized polybutadiene are sequentially added, and stirring is continued for 20 minutes until uniform mixing is achieved;
2) Dissolving powdery dicyandiamide curing agent in 15 parts of N, N-dimethylformamide, sequentially adding 2.5 parts of dicyandiamide and 3.5 parts of solution-like menthane diamine into the mixed glue solution, and continuously stirring for 15-20min to ensure uniform mixing;
3) Coating the prepared virgin rubber on a 50 mu m PI substrate through a scraper, putting the PI substrate into a high-temperature oven, baking for 5min at 135 ℃, taking out the dried virgin rubber until the thickness reaches 30 mu m, cooling, attaching a release film, and putting the film into an 80 ℃ oven for 72h to ensure complete reaction.
In this example, bisphenol A type epoxy resin is available from Nanya plastics industry Co., ltd (hereinafter referred to as Nanya) NPES-909 having an epoxy equivalent of about 1800-2400; the dihydric alcohol diglycidyl is GLYCI-ALE PP-300 of the Sanyo chemical industry, and the epoxy equivalent is about 296; the toughening agent is DAICEL PB-3600 of Daxiaojia (Shanghai) limited company, the epoxy equivalent is about 196, and the toughening agent has excellent compatibility with bisphenol A epoxy resin.
Example 2
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 1, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
20 parts of NPES-903H,80 parts of NPES-909, 70 parts of GLYCI-ALE PP-300P,15 parts of epoxidized butadiene, 3 parts of dicyandiamide, 6 parts of isophorone diamine, 90 parts of butanone and 15 parts of N, N-dimethylformamide.
In this example, the bisphenol A type epoxy resin adopts two types of Nanya NPES-903H and NPES-909, the epoxy equivalent of NPES-903H is 740-780, and the epoxy equivalent of NPES-909 is 1800-2400.
Example 3
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 1, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-907, 60 parts of GLYCI-ALE PP-300P,18 parts of epoxidized butadiene, 3 parts of dicyandiamide, 4.5 parts of menthane diamine, 80 parts of butanone and 15 parts of N, N-dimethylformamide.
In this example, the bisphenol A type epoxy resin is southern subunit epoxy resin NPES-907, and the epoxy equivalent is 1500-1800.
Example 4
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 1, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-907, 60 parts of GLYCI-ALE PP-300P,2.5 parts of dicyandiamide, 4 parts of isophorone diamine, 90 parts of butanone and 15 parts of N, N-dimethylformamide.
Example 5
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 1, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-903H,80 parts of GLYCI-ALE PP-300P,20 parts of epoxidized butadiene, 3 parts of dicyandiamide, 10 parts of menthane diamine, 50 parts of butanone and 15 parts of N, N-dimethylformamide.
Example 6
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 1, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-903H,80 parts of GLYCI-ALE PP-300P,5 parts of epoxidized butadiene, 3 parts of dicyandiamide, 10 parts of menthane diamine, 60 parts of butanone and 15 parts of N, N-dimethylformamide.
Comparative example 1
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as that of example 5, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-903H,45 parts of GLYCI-ALE PP-300P,20 parts of epoxidized butadiene, 3 parts of dicyandiamide, 10 parts of menthane diamine, 50 parts of butanone and 15 parts of N, N-dimethylformamide.
Comparative example 2
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as that of example 5, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of NPES-903H,80 parts of GLYCI-ALE PP-300P,20 parts of epoxidized butadiene, 13 parts of dicyandiamide, 70 parts of butanone and 15 parts of N, N-dimethylformamide.
Comparative example 3
In this example, a non-post-curing epoxy adhesive tape is provided, the main components and content of which are the same as those of example 5, and the preparation process is also substantially similar to that of example 5, and the difference between the preparation process and example 5 is that the step 2) of the preparation method is as follows: dicyandiamide is not required to be dissolved in N, N-dimethylformamide in advance, but is directly added into the mixed glue solution in the form of original powder.
Comparative example 4
In this example, a non-post-curing type epoxy adhesive tape was provided, and the preparation method thereof was the same as in example 5, except that the components and contents used for preparing the epoxy adhesive tape in this example were changed as follows:
100 parts of south Asia NPES-901, with the epoxy equivalent weight of 450-500, 80 parts of GLYCI-ALE PP-300P,20 parts of epoxidized butadiene, 3 parts of dicyandiamide, 10 parts of menthane diamine, 50 parts of butanone and 15 parts of N, N-dimethylformamide.
The following tests were performed on the epoxy tapes obtained in examples 1 to 6 and comparative examples 1 to 4:
1) Peel force and failure mode test
And (3) attaching the PI epoxy adhesive tape to a 30-micrometer copper foil, hot-pressing for 5min at 150 ℃ under 0.4Mpa by a hot press, taking out and cooling, testing the peeling force of the adhesive tape peeled from the copper foil by 180 degrees according to GB2792-2014, and recording the damage mode.
2) Flash and blister test
And (3) attaching the PI epoxy adhesive tape to the copper foil in the same way, fixing two ends by using a clamp, placing in a 220 ℃ oven for 30min, cooling, taking out, and observing whether glue overflow and foaming occur.
3) Appearance and flexibility test of adhesive film on surface of PI substrate
Cutting the prepared epoxy adhesive tape into blocks with the length of 5cm x 5cm, tearing off the release film, fully doubling the release film towards one side of the PI substrate, and observing whether the adhesive film has cracks or not and is separated from the substrate or not.
The test results are shown in Table 1.
Table 1:
as can be seen from Table 1, the examples of the present invention have high peel strength, good high temperature resistance, and good flexibility and adhesion properties on PI substrates.
The above embodiments are provided to illustrate the technical concept and features of the present invention and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention should be construed to be included in the scope of the present invention.

Claims (6)

1. The non-post-curing type epoxy adhesive tape is characterized by comprising a substrate layer, an epoxy adhesive film layer and a release film layer from bottom to top in sequence along the thickness direction, wherein the epoxy adhesive film layer comprises the following raw materials in parts by weight: 70-100 parts of bisphenol A epoxy resin, 50-80 parts of dihydric alcohol diglycidyl ether, 0-20 parts of flexibilizer, 5-15 parts of curing agent, 50-100 parts of butanone and 15 parts of N, N-dimethylformamide, wherein the curing agent is formed by mixing alicyclic amine and dicyandiamide, the dicyandiamide is mixed with the alicyclic amine after being dissolved by the N, N-dimethylformamide,
wherein the epoxy equivalent of the bisphenol A type epoxy resin adopted in the raw materials is between 700 and 2500;
the toughening agent adopts epoxy diene, and the epoxy equivalent is between 100 and 300;
the glycol glycidyl ether is purchased from the Japanese Sanyo chemical industry, and the specific model is GLYCI-ALE PP-300P.
2. The non-post-curing epoxy tape of claim 1, wherein the bisphenol a type epoxy resin is at least one of NPES-903H, NPES-907 and NPES-909 manufactured by south asia plastic industries, inc.
3. The non-post cure epoxy tape of claim 1, wherein the toughening agent is an epoxidized polybutadiene of model DAICEL PB-3600 manufactured by large cellophane trade (Shanghai) limited.
4. The non-post-curing epoxy adhesive tape according to claim 1, wherein the curing agent is prepared from alicyclic amine and dicyandiamide according to a mass ratio of 1-5:1, and the alicyclic amine adopts at least one of menthanediamine and isophorone diamine.
5. A method for preparing the non-post-curing epoxy adhesive tape according to any one of claims 1 to 4, comprising the steps of:
1) Mixing bisphenol A epoxy resin and butanone according to a proportion, rapidly stirring in a high-speed stirrer until the epoxy resin is completely dissolved, then sequentially adding dihydric alcohol diglycidyl ether and a toughening agent into the completely dissolved epoxy resin according to a proportion, and continuously stirring for 20min until the epoxy resin is uniformly mixed;
2) Dissolving dicyandiamide in N, N-dimethylformamide, sequentially adding alicyclic amine and the dissolved dicyandiamide into the uniformly mixed glue solution, and stirring at a high speed for 10-15min;
3) Coating the glue solution prepared in the step 2) on a 50 mu m base material in a pot life through a scraper or a coating machine, putting the base material into a high-temperature oven, baking for 5min at 135 ℃, removing the solvent, finishing the primary curing reaction, ensuring that the thickness of the dry glue is 30 mu m plus or minus 1 mu m, then attaching a release film, and standing for 72h at the temperature of 80 ℃ to ensure that the curing agent is completely reacted, thereby finishing the preparation of the epoxy adhesive tape.
6. The method for producing a non-post-curable epoxy tape according to claim 5, wherein the substrate is a PI substrate.
CN202311027432.7A 2023-08-16 2023-08-16 Non-post-curing epoxy adhesive tape and preparation method thereof Active CN116751533B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311027432.7A CN116751533B (en) 2023-08-16 2023-08-16 Non-post-curing epoxy adhesive tape and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311027432.7A CN116751533B (en) 2023-08-16 2023-08-16 Non-post-curing epoxy adhesive tape and preparation method thereof

Publications (2)

Publication Number Publication Date
CN116751533A CN116751533A (en) 2023-09-15
CN116751533B true CN116751533B (en) 2023-11-07

Family

ID=87948133

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311027432.7A Active CN116751533B (en) 2023-08-16 2023-08-16 Non-post-curing epoxy adhesive tape and preparation method thereof

Country Status (1)

Country Link
CN (1) CN116751533B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2180012A1 (en) * 2008-10-23 2010-04-28 Hexion Specialty Chemicals Research Belgium S.A. Curable epoxy resin and dicyandiamide solution
CN108047982A (en) * 2017-11-14 2018-05-18 浙江元集新材料科技股份有限公司 A kind of preparation method of special heat-resistant bonded of the height of aluminum-based copper-clad plate
CN109554149A (en) * 2018-10-18 2019-04-02 哈尔滨工业大学无锡新材料研究院 A kind of flexible circuit board epoxy adhesive and the preparation method and application thereof
CN114395346A (en) * 2021-12-21 2022-04-26 苏州赛伍应用技术股份有限公司 Adhesive, polyimide adhesive film, polyimide heating film and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2180012A1 (en) * 2008-10-23 2010-04-28 Hexion Specialty Chemicals Research Belgium S.A. Curable epoxy resin and dicyandiamide solution
CN108047982A (en) * 2017-11-14 2018-05-18 浙江元集新材料科技股份有限公司 A kind of preparation method of special heat-resistant bonded of the height of aluminum-based copper-clad plate
CN109554149A (en) * 2018-10-18 2019-04-02 哈尔滨工业大学无锡新材料研究院 A kind of flexible circuit board epoxy adhesive and the preparation method and application thereof
CN114395346A (en) * 2021-12-21 2022-04-26 苏州赛伍应用技术股份有限公司 Adhesive, polyimide adhesive film, polyimide heating film and preparation method thereof

Also Published As

Publication number Publication date
CN116751533A (en) 2023-09-15

Similar Documents

Publication Publication Date Title
CN100432144C (en) Resin composition and its uses in adhesive sheet and copper-cladded plate
JP4798803B2 (en) Reactive adhesive composition for fixing electronic parts and adhesive sheet thereof
JP2010505978A (en) Especially heat-activatable adhesive tape for attaching electronic parts and conductor paths
KR20070114702A (en) Adhesive strip that can be activated by heat and is based on nitrile rubber and polyvinyl butyral for sticking together electronic components and strip conductors
JP4849654B2 (en) Adhesive composition and adhesive sheet
JP3621351B2 (en) Thermally reactive adhesive composition and thermally reactive adhesive film
JP4994743B2 (en) Film adhesive and method of manufacturing semiconductor package using the same
JP5771988B2 (en) Thermosetting resin composition
TW201105766A (en) Application of heat-activated adhesive tape for gluing flexible printed circuit board
WO2002055626A1 (en) Removable adhesive compositions and process for producing the same
WO1999009101A1 (en) Conductive epoxy resin compositions, anisotropically conductive adhesive films and electrical connecting methods
CN116751533B (en) Non-post-curing epoxy adhesive tape and preparation method thereof
WO2012073672A1 (en) Heat-curing resin composition, heat-curing adhesive sheet, and method for producing heat-curing adhesive sheet
CN109554149B (en) Epoxy adhesive for flexible circuit board and preparation method and application thereof
TWI417357B (en) Resin composition for adhesive sheet and adhesive sheet using the composition for flexible printed circuit board
JP2007515496A (en) Bonding method of FPCB
JP3727155B2 (en) Conductive epoxy resin composition, anisotropic conductive adhesive film, and electrical connection method between conductors
JPS61211016A (en) Bonding of flexible print base and reinforcing plate
JP4086279B2 (en) Reactive adhesive composition and adhesive sheet thereof
JP3319650B2 (en) Copper foil for copper clad laminates
JP4086278B2 (en) Reactive adhesive composition and adhesive sheet thereof
JPH10168400A (en) Sheetlike tacky body and its production
CN116042125A (en) Quick-reaction type epoxy adhesive film and preparation method and application thereof
CN115926707A (en) Adhesive, preparation method and application thereof
JPS60141873A (en) Adhesive agent composition for chemical plating

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant