CN111484806B - Epoxy thermosetting adhesive film with initial adhesiveness and preparation method and application thereof - Google Patents
Epoxy thermosetting adhesive film with initial adhesiveness and preparation method and application thereof Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers 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
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
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- 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
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- 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
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- C09J133/00—Adhesives 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
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
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- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
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- C09J2463/00—Presence of epoxy resin
Abstract
The invention relates to an epoxy thermosetting adhesive film with initial adhesiveness, a preparation method and application thereof, which is characterized in that the epoxy thermosetting adhesive film with initial adhesiveness comprises a first layer of acrylic acid modified epoxy resin thermosetting adhesive film, an epoxy resin thermosetting adhesive film and a second layer of acrylic acid modified epoxy resin thermosetting adhesive film; the first and second layers of acrylic modified epoxy resin thermosetting adhesive films both comprise a release film and a dried acrylic modified epoxy resin liquid mixture attached to the release film, one surface of the epoxy resin thermosetting adhesive film is attached to the acrylic modified epoxy resin liquid mixture on the first layer of acrylic modified epoxy resin thermosetting adhesive film, and the other surface of the epoxy resin thermosetting adhesive film is attached to the dried acrylic modified epoxy resin liquid mixture on the second layer of acrylic modified epoxy resin thermosetting adhesive film. The adhesive tape has initial viscosity, can be bonded and pre-fixed at room temperature, realizes high bonding strength through heating and curing, has the technical performance of the adhesive tape and the high bonding reliability of glue, is particularly suitable for the field of bonding and bonding of 3D memory chips, and has the advantages of simple processing technology, short flow and high yield.
Description
Technical Field
The invention relates to an epoxy thermosetting adhesive film with initial adhesiveness, a preparation method and application thereof.
Background
With the development of memory chips, the chips are designed to be stacked, the number of assembly structures is increased, 28 layers to 42 layers are stacked continuously, thermosetting epoxy resin adhesive films are not adopted for bonding between the chip assemblies, and the adhesive films are supplied by manufacturers such as Henkel, Hitach, NITTON, Threebond and the like in the industry. The thermosetting epoxy resin adhesive film has the characteristics of high bonding strength, high water resistance, high purity and controllable thickness.
The commercialized adhesive film disclosed by the company is a pure solid adhesive film, the surface of the adhesive film is in a solid state at room temperature, the surface of the adhesive film does not have any viscosity, and the adhesive film is not like a common double-sided adhesive tape, so that when the 3D memory chip is assembled and bonded, the chip is heated first, then the adhesive film is pasted, meanwhile, the other chip is pasted while the chip is heated, and finally, the adhesive film is put into a pressure oven to be integrally cured. That is to say, the epoxy thermosetting adhesive film without initial adhesion on the surface cannot perform 3D bonding on the chip at room temperature like a double-sided adhesive tape, and finally enters a pressure oven for curing again. The construction process of the thermosetting adhesive film without initial stickiness on the surface has the advantages of complex process scheme, longer process period, higher cost and lower yield.
As disclosed in patent 201510811364, the adhesive composition provided therein can form an encapsulating layer having good adhesive properties, impact resistance, thermal protection properties, and moisture barrier properties, and thus, an OED including components encapsulated with the adhesive composition can exhibit good life performance and durability, but no tackiness at room temperature. 201710590608.8 discloses a thermosetting pure glue film, which has a dielectric constant of 2.4-2.8, a dielectric loss value of 0.003-0.008, and a binding power of 1.2kgf/cm or more. But the surface is not tacky. 201811196482.7, specifically relates to a semi-solidified hot-melt method low-temperature epoxy adhesive film and a preparation and use method thereof, wherein a flexible chain segment is introduced into an epoxy resin molecular chain by a semi-solidified method, and then an epoxy adhesive film suitable for being applied to a low-temperature environment is prepared by a hot-melt method and a preparation and use method thereof. The low-temperature epoxy adhesive film is suitable for preparing an interlayer structure and a glue joint structure in a low-temperature environment. The low-temperature composite material can be applied to the fields of low-temperature wind tunnel blades, low-temperature composite material storage tanks, low-temperature superconduction and the like, the low temperature is below 150 ℃, and the surface of the low-temperature composite material storage tank is not sticky. Generally, the construction process of the thermosetting adhesive film without viscosity on the surface is complex, the process is long, and the yield is low.
Disclosure of Invention
In order to overcome the defects of the prior art, the first purpose of the invention is to provide an epoxy thermosetting adhesive film with initial adhesiveness, the second purpose is to provide a preparation method of the epoxy thermosetting adhesive film with initial adhesiveness, and the third purpose is to provide an application method of the epoxy thermosetting adhesive film with initial adhesiveness, so that the functions like double-sided adhesive tape are realized, 3D bonding can be performed on a chip at room temperature, the bonding process is simple, and the qualification rate of the chip is greatly improved.
In order to achieve the first object, the technical scheme of the epoxy thermosetting adhesive film with initial adhesiveness is realized by the following steps that the epoxy thermosetting adhesive film with initial adhesiveness is characterized by comprising a first layer of acrylic modified epoxy resin thermosetting adhesive film, an epoxy resin thermosetting adhesive film and a second layer of acrylic modified epoxy resin thermosetting adhesive film; the first and second layers of acrylic modified epoxy resin thermosetting adhesive films both comprise a release film and a dried acrylic modified epoxy resin liquid mixture attached to the release film, one surface of the epoxy resin thermosetting adhesive film is attached to the acrylic modified epoxy resin liquid mixture on the first layer of acrylic modified epoxy resin thermosetting adhesive film, and the other surface of the epoxy resin thermosetting adhesive film is attached to the dried acrylic modified epoxy resin liquid mixture on the second layer of acrylic modified epoxy resin thermosetting adhesive film;
the thickness of the epoxy resin thermosetting adhesive film is 10-200 μm, and the thickness of the first and second acrylic acid modified epoxy resin thermosetting adhesive films is 2-5 μm;
the epoxy resin thermosetting adhesive film is formed by drying an epoxy resin liquid mixture, wherein the epoxy resin liquid mixture comprises solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A, and the weight ratio of the solid epoxy resin to the solid epoxy accelerator to the stabilizer to the filler to the solvent A is as follows: 100: 10-30: 1-10: 10-200: 200-1500;
the liquid mixture of the acrylic modified epoxy resin comprises acrylic modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A, and the weight ratio of the acrylic modified alicyclic epoxy resin to the solid epoxy resin is as follows: 100: 20-80: 10-20: 1-10: 10-100: 200-1000.
In the technical scheme, the synthetic route of the acrylic acid modified alicyclic epoxy resin is as follows: adding an acrylate monomer with double bond alicyclic epoxy, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator A, reacting at the temperature of 40-80 ℃ for 2-5 hours, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylate monomer of the alicyclic epoxy with the double bonds is mainly one or a mixture of 3, 4-epoxy cyclohexyl methyl methacrylate and 3, 4-epoxy cyclohexyl methyl acrylate;
the acrylate monomer with hydroxyl is mainly one or a mixture of hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, hydroxyethyl acrylate, 2-hydroxypropyl acrylate or 4-hydroxybutyl acrylate;
the acrylic ester monomer containing carboxyl is one or a mixture of methacrylic acid or acrylic acid.
In the technical scheme, the initiator A is one or a mixture of more of benzoyl peroxide, benzoyl peroxide tert-butyl ester, methyl ethyl ketone peroxide, azobisisobutyronitrile, azobisisoheptonitrile or dimethyl azobisisobutyrate; the solvent B is one or a mixture of cyclohexanone, toluene, tetrahydrofuran, acetone, trichloromethane or dioxane.
In the technical scheme, the solvent A is one or a mixture of acetone, dichloromethane, trichloromethane, tetrahydrofuran or tetrachloromethane.
In the technical scheme, the solid epoxy resin is poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether (3:1), dicyclopentadiene phenol type epoxy resin, aralkyl phenol type epoxy resin, biphenyl type epoxy resin, condensed ring naphthalene type epoxy resin, o-cresol formaldehyde epoxy resin, dimer acid modified glycidyl ester type epoxy resin, one or a mixture of bisphenol A type novolac epoxy resin, and is commercialized as DPNE1501, PXNE2000, PXNE2002, BPNE3501, BPNE3502, NPTE4000, NPTE4002, EOCN6000 or BPANE8200 of Kainan Jiadesh company, and is commercially available as SQE-172, SQCN700 series, SQPN series, SQE series, SQXN series or TN series.
In the technical scheme, the solid epoxy resin accelerator is one or a mixture of more of modified amine, modified imidazole, nadic anhydride and 4, 4 '-diamino-3, 3' -diethyl diphenylmethane; commercially available PN-23, PN-40, PN-H, MY-24 or PN-50 from the company Aomoto Japan; FujicureFXR-1020, 1030, 1081, 1121 or 1090F of Fuji chemical Co., Ltd, Japan; NOVACURE HX-3722, 3088, 3742, 3721, 3748 or 3921 from asahi chemicals; 2P4MHZ, 2PHZ, 2MA-OK, C11Z-A or 2E4MZ formed in four countries; EH-4337S, EH-3293S or EH-4357S, Adecaco, Japan.
In the technical scheme, the stabilizer is one or a mixture of more of barbituric acid, benzoic acid, fumaric acid, salicylic acid, citric acid, trihydroxybenzoic acid, ascorbic acid, parabanic acid, phenylboronic acid or tetrahydroxy-p-benzoquinone.
In the technical scheme, the filler is one or a mixture of more of calcium carbonate, talcum powder, magnesium oxide, spherical silicon dioxide, spherical aluminum oxide or spherical magnesium hydroxide, and the particle size is 10-2000 nm.
In order to achieve the second object, the second object of the present invention is achieved by a method for preparing an epoxy thermosetting adhesive film with initial adhesiveness, comprising the following four steps:
the first step is as follows: uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking in an oven at 40-80 ℃ for 20-60min to obtain an epoxy resin thermosetting adhesive film;
the second step is that: uniformly coating the acrylic modified epoxy resin liquid mixture on a release film, and baking in an oven at 40-80 ℃ for 20-60min to obtain an acrylic modified epoxy resin thermosetting adhesive film;
the third step: attaching the acrylic acid modified epoxy resin thermosetting adhesive film prepared in the second step on the epoxy resin thermosetting adhesive film prepared in the first step, and rolling for 5-20s by using the pressure of 0.05-0.5MPa to obtain an adhesive film with a four-layer structure;
the fourth step: removing the temporary release film of the epoxy resin thermosetting adhesive film on the four-layer structural adhesive film prepared in the third step, attaching a layer of the acrylic acid modified epoxy resin thermosetting adhesive film in the second step on the surface of the epoxy resin thermosetting adhesive film, and rolling for 5-20s by using the pressure of 0.05-0.5MPa to obtain the epoxy thermosetting adhesive film with the initial viscosity and the five-layer structure;
and (3) adhering the acrylic modified epoxy resin liquid mixture on the acrylic modified epoxy resin thermosetting adhesive film in the third step and the fourth step to the epoxy resin thermosetting adhesive film.
In order to achieve the third object, the third object of the present invention is achieved by the technical solution of the application method of the initially adhesive epoxy thermosetting adhesive film, which is characterized in that the release film on one side of the initially adhesive epoxy thermosetting adhesive film dedicated for chip assembly is torn off, the film is adhered to the surface to be adhered, air bubbles are removed by rolling with the pressure of 0.1-1MPa, the release film on the other side is torn off, another adhered object is adhered, air bubbles are removed by rolling with the pressure of 0.1-1MPa, and a pre-adhered assembly is obtained. And then placing the pre-bonding assembly into a pressure oven, curing for 30-60min at the temperature of 80-160 ℃ and the pressure of 0.1-1MPa, and thus completing the bonding of the adhesive film.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the traditional epoxy resin thermosetting adhesive film is of a sandwich structure, namely, the middle of two layers of release films is an epoxy thermosetting adhesive film without viscosity on the surface, the application discloses an epoxy thermosetting adhesive film with a five-layer structure, wherein the surface of the epoxy thermosetting adhesive film is provided with initial viscosity, namely, a first layer of acrylic acid modified epoxy resin thermosetting adhesive film, an epoxy resin thermosetting adhesive film and a second layer of acrylic acid modified epoxy resin thermosetting adhesive film, and the first layer and the second layer of acrylic acid modified epoxy resin thermosetting adhesive film comprise one layer of release film, as shown in figure 1.
2. The invention provides an acrylic acid modified epoxy resin adhesive film, wherein a hydroxyl-terminated acrylic monomer is a high polymer, the glass transition temperature is low, the synthesized polymerization surface has viscosity, and meanwhile, the added acrylic monomer contains carboxyl to ensure strong bonding performance with an interface, and the contained alicyclic epoxy monomer contains epoxy groups to ensure good compatibility with epoxy resin matrix resin.
3. The epoxy resin thermal curing adhesive has the surface with complementary viscosity, can be bonded and pre-fixed at room temperature, and realizes high bonding strength through heating and curing, and has the technical performance of an adhesive tape and the high bonding reliability of the adhesive.
4. The epoxy resin thermosetting adhesive provided by the invention replaces the existing thermosetting adhesive film process, 2 preheating steps are reduced, only the laminating at room temperature is needed, and then the curing is carried out at high temperature, so that the epoxy resin thermosetting adhesive has great advantages in both yield and cost.
Drawings
FIG. 1 is a schematic structural view of the present invention;
fig. 2 is a schematic structural view of the formation process of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example one
(1) Preparation of epoxy resin thermosetting adhesive film
Mixing solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required epoxy resin liquid mixture, uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking in an oven at 40 ℃ for 20min to obtain an epoxy resin thermosetting adhesive film on the release film, wherein the thickness of the epoxy resin thermosetting adhesive film is 100 mu m; wherein the weight ratio of the solid epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 10: 1: 10: 200 of a carrier;
the solvent A is acetone; the solid epoxy resin is poly [ (2-ethylene oxide) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propylene glycol ether (3: 1); the solid epoxy resin accelerator is nadic anhydride; the stabilizer is barbituric acid; the filler is calcium carbonate with the particle size of 10 nm.
(2) Synthesis of acrylic acid modified alicyclic epoxy resin
Adding an acrylate monomer with double bond alicyclic epoxy, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator A, reacting for 2 hours at the temperature of 40 ℃, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylic monomer of the alicyclic epoxy with double bonds is 3, 4-epoxy cyclohexyl methyl methacrylate; the acrylic ester monomer containing carboxyl is methacrylic acid; the acrylic monomer with hydroxyl is hydroxypropyl acrylate; the initiator A is benzoyl peroxide; the solvent B is dioxane.
(3) Preparation of acrylic acid modified epoxy thermosetting adhesive film
Mixing acrylic acid modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required acrylic acid modified epoxy resin liquid mixture, uniformly coating the acrylic acid modified epoxy resin liquid mixture on a release film, and baking in an oven at 40 ℃ for 20min to obtain an acrylic acid modified epoxy resin adhesive film, wherein the thickness of the acrylic acid ester modified epoxy resin adhesive film is 3 mu m; wherein the weight ratio of the acrylic acid modified alicyclic epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 20: 10: 1: 10: 200.
the solid epoxy resin is dicyclopentadiene phenol type epoxy resin; the solid epoxy resin accelerator is one of 4, 4 '-diamino-3, 3' -diethyl diphenylmethane; the stabilizer is benzoic acid; the filler is magnesium oxide, and the particle size is 2000 nm.
(4) Preparation of epoxy resin thermosetting adhesive film with initial adhesiveness
Covering the acrylic acid modified epoxy resin thermosetting adhesive film prepared in the step (3) on the epoxy resin thermosetting adhesive film prepared in the step (1), and rolling for 5 seconds by using the pressure of 0.05MPa to obtain the adhesive film with the four-layer structure. And (3) removing the temporary release film of the epoxy resin thermosetting adhesive film on the four-layer structural adhesive film, covering the surface of the epoxy resin thermosetting adhesive film with a layer of the acrylic acid modified epoxy resin thermosetting adhesive film obtained in the step (3), and rolling for 5 seconds by using the pressure of 0.05MPa to obtain the epoxy resin thermosetting adhesive film with the five-layer structure and the initial viscosity, as shown in figure 2.
The acrylic modified epoxy resin liquid mixture on the acrylic modified epoxy resin thermosetting adhesive film in the above steps is adhered to the epoxy resin thermosetting adhesive film.
(5) Application of epoxy thermosetting adhesive film
Tearing off the release film at room temperature, warm-sticking the epoxy resin thermosetting adhesive film with initial viscosity on the surface of the Die1, and rolling to remove air bubbles under the pressure of 0.1 MPa; tearing off the release film on the other side, sticking the Die2 on the adhesive film, and rolling to remove air bubbles under the pressure of 0.1 MPa; and curing for 30min at the temperature of 150 ℃ under the pressure of 0.5MPa to complete the bonding of the chip.
Example two
(1) Preparation of epoxy resin thermosetting adhesive film
Mixing solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required epoxy resin liquid mixture, uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking in an oven at 40 ℃ for 20min to obtain an epoxy resin thermosetting adhesive film on the release film, wherein the thickness of the epoxy resin thermosetting adhesive film is 10 mu m; wherein the weight ratio of the solid epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 10: 5: 100: 1000, parts by weight;
the solvent A is trichloromethane, and the solid epoxy resin is aralkyl phenol type epoxy resin; the solid epoxy resin accelerator is 4, 4 '-diamino-3, 3' -diethyl diphenylmethane; the stabilizer is phenylboronic acid; the filler is spherical silicon dioxide.
(2) Synthesis of acrylic acid modified alicyclic epoxy resin
The synthetic route of the acrylic acid modified alicyclic epoxy resin is as follows: adding an acrylate monomer with double bond alicyclic epoxy, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator A, reacting for 5 hours at the temperature of 80 ℃, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylic monomer of the alicyclic epoxy with double bonds is 1, 2-epoxy-4-vinyl cyclohexane; the acrylic ester monomer containing carboxyl is acrylic acid; the acrylic monomer with hydroxyl is hydroxypropyl acrylate; the initiator A is azobisisoheptonitrile; and the solvent B is trichloromethane.
(3) Preparation of acrylic acid modified epoxy thermosetting adhesive film
Mixing acrylic acid modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required acrylic acid modified epoxy resin liquid mixture, uniformly coating the acrylic acid modified epoxy resin liquid mixture on a release film, and baking the release film in an oven at 70 ℃ for 40min to obtain an acrylic acid modified epoxy resin adhesive film, wherein the thickness of the acrylic acid ester modified epoxy resin adhesive film is 4 microns; wherein the weight ratio of the acrylic acid modified alicyclic epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 70: 15: 6: 70: 800;
the solid epoxy resin is o-cresol formaldehyde epoxy resin; the solid epoxy resin accelerator is NOVACURE HX-3722; the stabilizer is parabanic acid; the filler is spherical aluminum oxide, and the particle size is 1000 nm.
(4) Preparation of epoxy resin thermosetting adhesive film with initial adhesiveness
Covering the acrylic acid modified epoxy resin thermosetting adhesive film prepared in the step (3) on the epoxy resin thermosetting adhesive film prepared in the step (1), and rolling for 20s by using the pressure of 0.1MPa to obtain the adhesive film with the four-layer structure. And (3) removing the temporary release film of the epoxy resin thermosetting adhesive film on the four-layer structural adhesive film, covering the surface of the epoxy resin thermosetting adhesive film with a layer of the acrylic acid modified epoxy resin thermosetting adhesive film obtained in the step (3), and rolling for 20s by using the pressure of 0.1MPa to obtain the epoxy resin thermosetting adhesive film with the five-layer structure and the initial viscosity, as shown in figure 2.
The acrylic modified epoxy resin liquid mixture on the acrylic modified epoxy resin thermosetting adhesive film in the above steps is adhered to the epoxy resin thermosetting adhesive film.
(5) Application of epoxy thermosetting adhesive film
Tearing off the release film on one side of the epoxy resin thermosetting adhesive film with initial viscosity at room temperature, pasting the epoxy resin thermosetting adhesive film with initial viscosity on the surface of the Die1, and rolling to remove air bubbles, wherein the pressure is 0.2 MPa; tearing off the release film on the other side, sticking the Die2 on the adhesive film, and rolling to remove air bubbles under the pressure of 0.2 MPa; and curing for 30min at the temperature of 120 ℃ under the pressure of 0.6MPa to complete the bonding of the chip.
EXAMPLE III
(1) Preparation of epoxy resin thermosetting adhesive film
Mixing solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required epoxy resin liquid mixture, uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking the temporary release film in an oven at 70 ℃ for 40min to obtain an epoxy resin thermosetting adhesive film on the release film, wherein the thickness of the epoxy resin thermosetting adhesive film is 80 mu m; wherein the weight ratio of the solid epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 20: 5: 100: 600, preparing a mixture;
the solvent A is tetrahydrofuran; the solid epoxy resin is EOCN 6000; the solid epoxy resin accelerator is 2P4MHZ formed by four countries; the stabilizer is ascorbic acid; the filler is magnesium oxide, and the particle size is 100 nm.
(2) Synthesis of acrylic acid modified alicyclic epoxy resin
Adding an acrylate monomer of alicyclic epoxy with double bonds, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator, reacting for 4 hours at the temperature of 60 ℃, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylic monomer of the alicyclic epoxy with double bonds is 3, 4-epoxy cyclohexyl methacrylate; the acrylic ester monomer containing carboxyl is acrylic acid; the acrylic monomer with hydroxyl is hydroxyethyl acrylate; the free radical initiator A is azobisisobutyronitrile; and the solvent B is cyclohexanone.
(3) Preparation of acrylic acid modified epoxy thermosetting adhesive film
Mixing acrylic acid modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required acrylic acid modified epoxy resin liquid mixture, uniformly coating the acrylic acid modified epoxy resin liquid mixture on a release film, and baking in an oven at 60 ℃ for 30min to obtain an acrylic acid modified epoxy resin adhesive film, wherein the thickness of the acrylic acid ester modified epoxy resin adhesive film is 3 mu m; wherein the weight ratio of the acrylic acid modified alicyclic epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 40: 12: 5: 40: 500, a step of;
the solid epoxy resin is BPANE 8200; the solid epoxy resin accelerator is PN-40; the stabilizing agent is citric acid; the filler is spherical silicon dioxide, and the particle size is 160 nm.
(4) Preparation of epoxy resin thermosetting adhesive film with initial adhesiveness
Covering the acrylic modified epoxy resin thermosetting adhesive film prepared in the step (3) on the epoxy resin thermosetting adhesive film prepared in the step (1), rolling for 10s by using the pressure of 0.3MPa to obtain an adhesive film with a four-layer structure, removing the temporary release film of the epoxy resin thermosetting adhesive film on the adhesive film with the four-layer structure, covering the surface of the epoxy resin thermosetting adhesive film with a layer of the acrylic modified epoxy resin thermosetting adhesive film prepared in the step (3), and rolling for 10s by using the pressure of 0.3MPa to obtain the epoxy resin thermosetting adhesive film with the initial viscosity and the five-layer structure, as shown in figure 2.
The acrylic modified epoxy resin liquid mixture on the acrylic modified epoxy resin thermosetting adhesive film in the above steps is adhered to the epoxy resin thermosetting adhesive film.
(5) Application of epoxy thermosetting adhesive film
Tearing off a release film on one side of the epoxy resin thermosetting adhesive film with initial viscosity at room temperature, pasting the epoxy resin thermosetting adhesive film with initial viscosity on the surface of the Die1, and rolling to remove air bubbles, wherein the pressure is 0.3 MPa; tearing off the release film on the other side, sticking the Die2 on the adhesive film, and rolling to remove air bubbles under the pressure of 0.1 MPa; and curing for 40min at the temperature of 140 ℃ under the pressure of 0.3MPa to complete the bonding of the chip.
Example four
(1) Preparation of epoxy resin thermosetting adhesive film
Mixing solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required epoxy resin liquid mixture, uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking the temporary release film in an oven at 75 ℃ for 55min to obtain an epoxy resin thermosetting adhesive film on the release film, wherein the thickness of the epoxy resin thermosetting adhesive film is 200 mu m; wherein the weight ratio of the solid epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 14: 6: 50: 700 of the base material;
the solvent A is tetrahydrofuran; the solid epoxy resin is the JUNNAN Shengquan epoxy resin SQE-172; the solid epoxy resin accelerator is 2E4MZ formed by four countries; the stabilizer is fumaric acid; the filler is spherical silicon dioxide, and the particle size is 1200 nm.
(2) Synthesis of acrylic acid modified alicyclic epoxy resin
The synthetic route of the acrylic acid modified alicyclic epoxy resin is as follows: adding an acrylate monomer with double bond alicyclic epoxy, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator A, reacting for 3 hours at the temperature of 60 ℃, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylic monomer of the alicyclic epoxy with double bonds is 1, 2-epoxy-4-vinyl cyclohexane; the acrylic ester monomer containing carboxyl is methacrylic acid; the acrylic monomer with hydroxyl is hydroxypropyl methacrylate; the free radical initiator A is dimethyl azodiisobutyrate; and the solvent B is trichloromethane.
(3) Preparation of acrylic acid modified epoxy thermosetting adhesive film
Mixing acrylic acid modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A to obtain a required acrylic acid modified epoxy resin liquid mixture, uniformly coating the acrylic acid modified epoxy resin liquid mixture on a release film, and baking in an oven at 50 ℃ for 50min to obtain an acrylic acid modified epoxy resin adhesive film, wherein the thickness of the acrylic acid ester modified epoxy resin adhesive film is 2 microns; wherein the weight ratio of the acrylic acid modified alicyclic epoxy resin, the solid epoxy accelerator, the stabilizer, the filler and the solvent A is as follows: 100: 40: 12: 5: 50: 600, preparing a mixture;
the solid epoxy resin is a Jinan Shengquan epoxy resin SQCN 700; the solid epoxy resin accelerator is NOVACURE 3088 from asahi chemical company; the stabilizer is ascorbic acid; the filler is talcum powder, and the particle size is 260 nm.
(4) Preparation of epoxy resin thermosetting adhesive film with initial adhesiveness
Covering the acrylic acid modified epoxy resin thermosetting adhesive film prepared in the step (3) on the epoxy resin thermosetting adhesive film prepared in the step (1), and rolling for 10s by using the pressure of 0.4MPa to obtain the adhesive film with the four-layer structure. And (3) removing the temporary release film of the epoxy resin thermosetting adhesive film on the four-layer structural adhesive film, covering the surface of the epoxy resin thermosetting adhesive film with a layer of the acrylic acid modified epoxy resin thermosetting adhesive film obtained in the step (3), and rolling for 10s by using the pressure of 0.4MPa to obtain the epoxy resin thermosetting adhesive film with the initial viscosity and the five-layer structure, wherein the epoxy resin thermosetting adhesive film is shown in figure 2.
(5) Application of epoxy thermosetting adhesive film
Tearing off a release film on one side of the epoxy resin thermosetting adhesive film with initial viscosity at room temperature, pasting the epoxy resin thermosetting adhesive film with initial viscosity on the surface of the Die1, and rolling to remove air bubbles, wherein the pressure is 0.8 MPa; tearing off the release film on the other side, sticking the Die2 on the adhesive film, and rolling to remove air bubbles under the pressure of 0.8 MPa; and curing for 60min at the temperature of 100 ℃ under the pressure of 0.8MPa to complete the bonding of the chip.
The epoxy resin thermosetting adhesive films with initial adhesiveness prepared in examples one to four were subjected to performance tests as shown in table 1:
testing of adhesive strength: and testing the thrust of the cured chip on the embodiment by adopting DAGE3800 after curing, wherein the thrust speed is 300mm/min, and the bonding strength can be obtained after testing.
And (3) testing the glass transition temperature Tg by adopting a DSC method, putting 0.5mg of a sample into equipment, controlling the temperature to be 20-200 ℃ and the temperature rise speed to be 10 ℃/min, and analyzing the obtained curve to obtain Tg data.
The CTE test method refers to the standard JISK7197 method, the detection temperature range is-50-600 ℃, the temperature is controlled to be 0.01-100min, and the TMA range (sensitivity) is as follows: 5 mm-0.02 m, sample size: 100mm 25 mm. The test instrument references two data of CTE obtained from the curve obtained using TMA 4000 SE, one above and one below the Tg point.
The modulus testing method adopts a DMA8000 dynamic thermomechanical analyzer and a stretching method, the frequency is set to be 500HZ, the temperature rising speed is 20-200 ℃, and the modulus data at 25 ℃ can be obtained by analyzing and testing the curve.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. An epoxy thermosetting adhesive film with initial adhesiveness is characterized by comprising a first layer of acrylic modified epoxy thermosetting adhesive film, an epoxy thermosetting adhesive film and a second layer of acrylic modified epoxy thermosetting adhesive film; the first and second layers of acrylic modified epoxy resin thermosetting adhesive films both comprise a release film and a dried acrylic modified epoxy resin liquid mixture attached to the release film, one surface of the epoxy resin thermosetting adhesive film is attached to the acrylic modified epoxy resin liquid mixture on the first layer of acrylic modified epoxy resin thermosetting adhesive film, and the other surface of the epoxy resin thermosetting adhesive film is attached to the dried acrylic modified epoxy resin liquid mixture on the second layer of acrylic modified epoxy resin thermosetting adhesive film;
the thickness of the epoxy resin thermosetting adhesive film is 10-200 μm, and the thickness of the first and second acrylic acid modified epoxy resin thermosetting adhesive films is 2-5 μm;
the epoxy resin thermosetting adhesive film is formed by drying an epoxy resin liquid mixture, wherein the epoxy resin liquid mixture comprises solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A, and the weight ratio of the solid epoxy resin to the solid epoxy accelerator to the stabilizer to the filler to the solvent A is as follows: 100: 10-30: 1-10: 10-200: 200-1500;
the liquid mixture of the acrylic modified epoxy resin comprises acrylic modified alicyclic epoxy resin, solid epoxy resin, a solid epoxy accelerator, a stabilizer, a filler and a solvent A, and the weight ratio of the acrylic modified alicyclic epoxy resin to the solid epoxy resin is as follows: 100: 20-80: 10-20: 1-10: 10-100: 200-1000.
2. The epoxy thermosetting adhesive film with initial adhesiveness according to claim 1, wherein the acrylic modified alicyclic epoxy resin is synthesized by the following route: adding an acrylate monomer with double bond alicyclic epoxy, an acrylate monomer with hydroxyl and an acrylate monomer containing carboxyl into a solvent B, adding an initiator A, reacting at the temperature of 40-80 ℃ for 2-5 hours, and purifying to obtain viscous acrylic modified alicyclic epoxy resin;
the acrylate monomer of the alicyclic epoxy with the double bonds is one or a mixture of 3, 4-epoxy cyclohexyl methyl acrylate and 3, 4-epoxy cyclohexyl methyl acrylate;
the acrylate monomer with hydroxyl is one or a mixture of hydroxypropyl acrylate, hydroxyethyl methacrylate, hydroxypropyl methacrylate, hydroxyethyl acrylate, 2-hydroxypropyl acrylate or 4-hydroxybutyl acrylate;
the acrylic ester monomer containing carboxyl is one or a mixture of methacrylic acid or acrylic acid.
3. The epoxy thermosetting adhesive film with initial adhesiveness according to claim 2, wherein said initiator A is one or a mixture of more of benzoyl peroxide, benzoyl tert-butyl peroxide, methyl ethyl ketone peroxide, azobisisobutyronitrile, azobisisoheptonitrile or dimethyl azobisisobutyrate; the solvent B is one or a mixture of cyclohexanone, toluene, tetrahydrofuran, acetone, trichloromethane or dioxane.
4. The epoxy thermosetting adhesive film with initial adhesiveness of claim 1, wherein the solvent A is one or more of acetone, dichloromethane, chloroform, tetrahydrofuran or tetrachloromethane.
5. The epoxy thermosetting adhesive film with initial adhesiveness according to claim 1, wherein said solid epoxy resin is one or a mixture of several of poly [ (2-oxiranyl) -1, 2-cyclohexanediol ] 2-ethyl-2- (hydroxymethyl) -1, 3-propanediol ether, dicyclopentadiene phenol type epoxy resin, aralkyl phenol type epoxy resin, biphenyl type epoxy resin, condensed ring naphthalene type epoxy resin, o-cresol novolac epoxy resin, dimer acid modified glycidyl ester type epoxy resin, bisphenol a type novolac epoxy resin.
6. The epoxy thermosetting adhesive film with initial adhesiveness as claimed in claim 1, wherein said solid epoxy resin accelerator is one or more selected from modified amines, modified imidazoles, nadic anhydride, and 4, 4 '-diamino-3, 3' -diethyldiphenylmethane.
7. The epoxy thermosetting adhesive film with initial adhesiveness according to claim 1, wherein said stabilizer is one or more of barbituric acid, benzoic acid, fumaric acid, salicylic acid, citric acid, trihydroxybenzoic acid, ascorbic acid, parabanic acid, phenylboronic acid, and tetrahydroxy-p-benzoquinone.
8. The epoxy thermosetting adhesive film with initial adhesion of claim 1, wherein the filler is one or more of calcium carbonate, talc, magnesium oxide, spherical silica, spherical alumina or spherical magnesium hydroxide, and has a particle size of 10-2000 nm.
9. The method for preparing the epoxy thermosetting adhesive film with initial adhesiveness as claimed in claim 1, comprising four steps of:
the first step is as follows: uniformly coating the epoxy resin liquid mixture on a temporary release film, and baking in an oven at 40-80 ℃ for 20-60min to obtain an epoxy resin thermosetting adhesive film;
the second step is that: uniformly coating the acrylic modified epoxy resin liquid mixture on a release film, and baking in an oven at 40-80 ℃ for 20-60min to obtain an acrylic modified epoxy resin thermosetting adhesive film;
the third step: attaching the acrylic acid modified epoxy resin thermosetting adhesive film prepared in the second step on the epoxy resin thermosetting adhesive film prepared in the first step, and rolling for 5-20s by using the pressure of 0.05-0.5MPa to obtain an adhesive film with a four-layer structure;
the fourth step: removing the temporary release film of the epoxy resin thermosetting adhesive film on the four-layer structural adhesive film prepared in the third step, adhering a layer of the acrylic acid modified epoxy resin thermosetting adhesive film in the second step on the surface of the epoxy resin thermosetting adhesive film, and rolling for 5-20s by using the pressure of 0.05-0.5MPa to obtain the epoxy thermosetting adhesive film with the initial viscosity and the five-layer structure;
and (3) adhering the acrylic modified epoxy resin liquid mixture on the acrylic modified epoxy resin thermosetting adhesive film in the third step and the fourth step to the epoxy resin thermosetting adhesive film.
10. The method of claim 1, wherein the first-mentioned adhesive epoxy thermosetting adhesive film is removed from a release film on one side, and then adhered to a surface to be adhered, and then rolled to remove air bubbles under a pressure of 0.1-1MPa, and the second-mentioned release film is removed from the other side, and then another object to be adhered is adhered, and then rolled to remove air bubbles under a pressure of 0.1-1MPa to obtain a pre-adhered assembly, and then the pre-adhered assembly is placed in a pressure oven at a temperature of 80-160 ℃ and a pressure of 0.1-1MPa and cured for 30-60min to complete the adhesion of the adhesive film.
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