CN110054998B - Graphene directional heat conduction double-sided adhesive tape - Google Patents
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- CN110054998B CN110054998B CN201910109601.9A CN201910109601A CN110054998B CN 110054998 B CN110054998 B CN 110054998B CN 201910109601 A CN201910109601 A CN 201910109601A CN 110054998 B CN110054998 B CN 110054998B
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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
- 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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- 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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/21—Paper; Textile fabrics
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- 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
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
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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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional 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
- C09J2301/122—Additional 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
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
Abstract
The invention discloses a graphene directional heat-conducting double-sided adhesive tape which comprises a glass fiber cloth substrate layer, heat-conducting adhesive layers coated on two sides of the glass fiber cloth substrate layer and a release film layer attached to one side, opposite to the glass fiber cloth substrate layer, of the heat-conducting adhesive layer, wherein the heat-conducting adhesive layer comprises the following components in parts by weight: 30-45 parts of hydroxyl-terminated polysiloxane, 10-18 parts of epoxy resin, 30-40 parts of MQ resin, 2-5 parts of tetraethoxysilane, 1-3 parts of isobutyl triethoxysilane, 0.1-1 part of isopropyl titanate, 25-40 parts of graphene powder, 5-10 parts of nano boron nitride, 2-6 parts of vinyl toluene, 5-10 parts of 3-mercaptopropyl triethoxysilane, 0.1-1 part of ethoxy propargyl glycol, 0.1-3 parts of an organic tin catalyst and 55-70 parts of an organic solvent; the graphene directional heat conduction double-sided adhesive tape disclosed by the invention is high in heat conductivity coefficient, free of obvious adhesive residue after being subjected to damp-heat aging, and good in removability.
Description
Technical Field
The invention relates to an adhesive tape, in particular to a graphene directional heat conduction double-sided adhesive tape.
Background
With the rapid development of the electronic industry, electronic products tend to be light and small, so the integration level of electronic components is higher and higher, and the requirement on the heat conduction and dissipation performance of electronic components is higher and higher. The heat conductive tape has a function of heat conduction and bonding, is widely used, and has characteristics of flexibility, compressibility, conformability, a wide temperature range and the like, thereby occupying a large heat conductive material market.
The existing method for preparing the heat-conducting adhesive tape is to add a heat-conducting filler into a colloid to achieve the purpose of heat conduction, but the heat conductivity coefficient of the existing heat-conducting double-sided adhesive tape is generally lower, and the situation that the adhesive is easy to remain when the colloid is removed after working in a high-temperature environment for a long time. Therefore, how to provide the graphene oriented heat conduction double-sided tape which has good heat conduction performance and no obvious adhesive residue after damp and hot aging becomes the direction of efforts of the technicians in the field.
Disclosure of Invention
The invention aims to provide a graphene directional heat conduction double-sided adhesive tape which is good in heat conduction performance, free of obvious adhesive residue after damp and hot aging and good in removability.
In order to achieve the purpose, the invention adopts the technical scheme that: a graphene directional heat-conducting double-sided adhesive tape comprises a glass fiber cloth substrate layer, heat-conducting adhesive layers coated on two sides of the glass fiber cloth substrate layer, and a release film layer adhered to one side of the heat-conducting adhesive layer opposite to the glass fiber cloth substrate layer,
the heat-conducting adhesive layer comprises the following components in parts by weight:
30-45 parts of hydroxyl-terminated polysiloxane,
10-18 parts of epoxy resin,
30-40 parts of MQ resin,
2-5 parts of tetraethoxysilane,
1-3 parts of isobutyl triethoxy silane,
0.1 to 1 part of isopropyl titanate,
25-40 parts of graphene powder,
5-10 parts of nano boron nitride,
2-6 parts of vinyl toluene,
5-10 parts of 3-mercaptopropyltriethoxysilane,
0.1 to 1 part of ethoxy alkynediol,
0.1 to 3 parts of organic tin catalyst,
55-70 parts of an organic solvent.
The technical scheme of further improvement in the technical scheme is as follows:
1. in the scheme, the molecular weight of the hydroxyl-terminated polysiloxane is 20-30 ten thousand, and the hydroxyl content of the hydroxyl-terminated polysiloxane is 0.3-1.5%.
2. In the above embodiment, the organic tin catalyst is at least one selected from dibutyltin dilaurate, dioctyltin dilaurate, dibutyltin dilaurate, and stannous octoate.
3. In the above scheme, the organic solvent is ethyl acetate.
4. In the scheme, the thickness of the glass fiber cloth substrate layer is 20-50 microns.
5. In the scheme, the thickness of the heat-conducting adhesive layer is 5-20 microns.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. according to the graphene oriented heat conduction double-sided tape, a heat conduction adhesive layer of the graphene oriented heat conduction double-sided tape forms a composite heat conduction system by adopting 25-40 parts of graphene powder and 5-10 parts of nano boron nitride, 0.1-1 part of ethoxy propargyl glycol and 5-10 parts of 3-mercaptopropyl triethoxysilane are added to be dispersed together with a heat conduction filler, so that the heat conduction performance of the tape is further improved, the effect that the addition amount of the heat conduction filler is as small as possible reaches a higher heat conduction coefficient is achieved, the heat conduction coefficient of the prepared adhesive layer reaches more than 3W/(m.K), and the problem that the physical performance and the insulating performance of the tape are influenced by excessive addition of the heat conduction filler is avoided.
2. According to the graphene oriented heat conduction double-sided tape, a heat conduction adhesive layer formula uses 30-45 parts of hydroxyl-terminated polysiloxane as a base resin, 10-18 parts of epoxy resin is introduced, on the basis, 2-5 parts of tetraethoxysilane, 1-3 parts of isobutyl triethoxysilane and 2-6 parts of vinyl toluene are added, and a mixed catalytic system of 0.1-1 part of isopropyl titanate and 0.1-3 parts of organic tin catalysts is adopted, so that the prepared adhesive layer is high in crosslinking density and high in cohesive force, and therefore the graphene oriented heat conduction double-sided tape is free of obvious residual adhesive after being subjected to wet heat aging and good in removability.
Drawings
Fig. 1 is a schematic diagram of a graphene oriented heat-conducting double-sided adhesive tape structure of the invention.
Detailed Description
The invention is further described below with reference to the following examples:
examples 1 to 4: a graphene directional heat-conducting double-sided tape comprises a glass fiber cloth substrate layer, heat-conducting adhesive layers coated on two sides of the glass fiber cloth substrate layer, and a release film layer attached to one side, opposite to the glass fiber cloth substrate layer, of the heat-conducting adhesive layer;
the thickness of the glass fiber cloth substrate layer is 30 micrometers, and the thickness of the heat-conducting adhesive layer is 15 micrometers;
the heat-conducting adhesive layer comprises the following components in parts by weight:
TABLE 1
The molecular weight of the hydroxyl-terminated polysiloxane is 20-30 ten thousand, and the hydroxyl content of the hydroxyl-terminated polysiloxane is 0.3-1.5%.
The organotin catalyst in example 1 was dibutyltin dilaurate, the organotin catalyst in example 2 was dioctyltin dilaurate, the organotin catalyst in example 3 was dibutyltin dilaurate, and the organotin catalyst in example 4 was stannous octoate.
The organic solvent is ethyl acetate.
The preparation method of the graphene oriented heat conduction double-sided adhesive tape comprises the following steps:
s1, adding 30-45 parts of hydroxyl-terminated polysiloxane, 10-18 parts of epoxy resin, 30-40 parts of MQ resin, 2-5 parts of tetraethoxysilane, 1-3 parts of isobutyltriethoxysilane, 2-6 parts of vinyl toluene and 30-40 parts of organic solvent into a reaction kettle, heating to 130-135 ℃, adding 0.1-1 part of isopropyl titanate and 0.1-3 parts of organic tin catalyst, reacting for 2-3 hours at 140-150 ℃, and cooling to obtain an organic silicon pressure-sensitive adhesive solution;
s2, adding 25-40 parts of graphene powder, 5-10 parts of nano boron nitride, 5-10 parts of 3-mercaptopropyltriethoxysilane, 0.1-1 part of ethoxy propargyl glycol and the rest of organic solvent into a stirring kettle, dispersing at high speed for 40-60 minutes, slowly adding the organic silicon pressure-sensitive adhesive solution prepared in the step S1 into the stirring kettle, and stirring for 30-40 minutes to prepare a heat-conducting adhesive;
s3, coating the heat-conducting adhesive prepared in the S2 on two sides of a glass fiber cloth substrate layer, drying and curing to form a heat-conducting adhesive layer;
and S4, attaching the release film layer to one surface of the heat-conducting adhesive layer opposite to the glass fiber cloth substrate layer, and rolling and slitting to obtain the graphene directional heat-conducting double-sided adhesive tape.
Comparative examples 1-3, a heat-conducting double-sided tape, comprising a glass fiber cloth substrate layer, heat-conducting adhesive layers coated on two sides of the glass fiber cloth substrate layer, and a release film layer attached to one side of the heat-conducting adhesive layer opposite to the glass fiber cloth substrate layer;
the thickness of the glass fiber cloth substrate layer is 30 micrometers, and the thickness of the heat-conducting adhesive layer is 15 micrometers;
the heat-conducting adhesive layer comprises the following components in parts by weight:
TABLE 2
The molecular weight of the hydroxyl-terminated polysiloxane is 20-30 ten thousand, and the hydroxyl content of the hydroxyl-terminated polysiloxane is 0.3-1.5%.
The organic tin catalyst of comparative example 1 was dibutyltin dilaurate, the organic tin catalyst of comparative example 2 was dibutyltin dilaurate, and the organic tin catalyst of comparative example 3 was stannous octoate.
The organic solvent is ethyl acetate.
The preparation process is the same as the embodiment.
The heat-conducting adhesive layer properties of the heat-conducting double-sided tapes prepared in the above examples 1 to 4 and comparative examples 1 to 3 are shown in table 3:
TABLE 3
In table 3, "×" indicates clear residual glue, "Δ" indicates slight residual glue, and ". smallcircle" indicates no residual glue.
As shown in the evaluation results in table 3, the thermal conductivity of the thermal conductive adhesive layer of the graphene oriented thermal conductive double-sided tape in each embodiment of the invention is higher than that of each proportion, and no significant residual adhesive is generated after the thermal and humidity aging, so that the prepared tape has good removability.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (6)
1. The utility model provides a directional heat conduction double-sided sticky tape of graphite alkene which characterized in that: comprises a glass fiber cloth substrate layer, heat-conducting adhesive layers coated on two sides of the glass fiber cloth substrate layer, and a release film layer adhered on one side of the heat-conducting adhesive layer opposite to the glass fiber cloth substrate layer,
the heat-conducting adhesive layer comprises the following components in parts by weight:
30-45 parts of hydroxyl-terminated polysiloxane,
10-18 parts of epoxy resin,
30-40 parts of MQ resin,
2-5 parts of tetraethoxysilane,
1-3 parts of isobutyl triethoxy silane,
0.1 to 1 part of isopropyl titanate,
25-40 parts of graphene powder,
5-10 parts of nano boron nitride,
2-6 parts of vinyl toluene,
5-10 parts of 3-mercaptopropyltriethoxysilane,
0.1 to 1 part of ethoxy alkynediol,
0.1 to 3 parts of organic tin catalyst,
55-70 parts of an organic solvent.
2. The graphene oriented thermal conductive double-sided tape according to claim 1, wherein: the molecular weight of the hydroxyl-terminated polysiloxane is 20-30 ten thousand, and the hydroxyl content of the hydroxyl-terminated polysiloxane is 0.3-1.5%.
3. The graphene oriented thermal conductive double-sided tape according to claim 1, wherein: the organic tin catalyst is at least one of dibutyltin dilaurate, dioctyltin dilaurate, dibutyltin dilaurate or stannous octoate.
4. The graphene oriented thermal conductive double-sided tape according to claim 1, wherein: the organic solvent is ethyl acetate.
5. The graphene oriented thermal conductive double-sided tape according to claim 1, wherein: the thickness of the glass fiber cloth substrate layer is 20-50 mu m.
6. The graphene oriented thermal conductive double-sided tape according to claim 1, wherein: the thickness of the heat-conducting adhesive layer is 5-20 mu m.
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| CN115710472A (en) * | 2022-10-31 | 2023-02-24 | 福建友谊胶粘带集团有限公司 | High-thermal-conductivity adhesive tape with good heat dissipation effect and preparation method thereof |
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