CN110815968A - Composite graphite heat-conducting film and preparation process thereof - Google Patents
Composite graphite heat-conducting film and preparation process thereof Download PDFInfo
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Abstract
The composite graphite heat-conducting film disclosed by the invention comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, and the composite graphite heat-conducting film is characterized in that the adhesive layer comprises an adhesive component and a heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is (70: 30) - (40: 60). The invention solves the attenuation problem of double faced adhesive tape in the multilayer graphite laminating process, and the glue with low thickness by adopting the technology has high production efficiency and low cost, greatly improves the application range of products and meets the market demand.
Description
Technical Field
The invention relates to a heat dissipation material of a precise electronic product and a preparation process thereof, in particular to a composite graphite heat conduction film with low thermal resistance, high heat conduction and low cost and a preparation process thereof.
Background
The thermally conductive graphite film is also known as a thermally conductive graphite sheet, a heat dissipating graphite film, a graphite heat dissipating film, or the like. The heat-conducting graphite film is a novel heat-conducting and radiating material, has a very obvious heat-conducting and radiating effect, and is widely applied to electronic products such as PDP, LCDTV, Notebook PC, Flat Panel Display, MPU, Projector, Power Supply, LED and the like. Meanwhile, the adhesive film is one of popular heat dissipation adhesive films for mobile phones.
As shown in fig. 1, in the conventional multilayer graphite lamination process, a layer of artificially synthesized graphite heat-conducting film is coated with an ultrathin PET double-sided adhesive (generally 5 micrometers), and then another layer of artificially synthesized graphite heat-conducting film is coated on the double-sided adhesive, so as to obtain a double-layer graphite heat-conducting film material. By analogy, 3 layers and multilayer graphite heat-conducting film materials can be prepared. According to the traditional multilayer graphite laminating process, two layers of graphite films are bonded through ultrathin PET (polyethylene terephthalate) double faced adhesive tape (5 micrometers), the double faced adhesive tape is large in thermal resistance and generates large attenuation on heat conduction performance, and the attenuation is large when the number of layers is large.
Disclosure of Invention
In order to solve the problems, the composite graphite heat-conducting film disclosed by the invention solves the attenuation problem of double faced adhesive tapes in a multilayer graphite laminating process, is high in production efficiency and low in cost, greatly improves the application range of products, and meets the market demand. .
The invention discloses a composite graphite heat-conducting film, which comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is (70: 30) - (40: 60).
The invention discloses an improvement of a composite graphite heat-conducting film, wherein a heat-conducting filler in an adhesive layer comprises one or more of aluminum nitride, boron nitride, titanium dioxide, magnesium oxide, aluminum oxide, zinc oxide, silicon carbide and graphene.
The invention discloses an improvement of a composite graphite heat-conducting film, wherein a binder component in a glue layer is acrylic acid modified polyester resin.
The invention discloses an improvement of a composite graphite heat-conducting film, which is an acrylic acid modified polyester resin of a binder component in a glue layer, and comprises the following raw materials in parts by weight:
the invention discloses an improvement of a composite graphite heat-conducting film, wherein a solvent in raw materials of an adhesive component in an adhesive layer is ethyl acetate or toluene.
The invention discloses an improvement of a composite graphite heat-conducting film, wherein an initiator in raw materials of an adhesive component in an adhesive layer is one or a composition of dibenzoyl peroxide and azobisisobutyronitrile.
The invention discloses an improvement of a composite graphite heat-conducting film, wherein polyester resin in raw materials of adhesive components in an adhesive layer is obtained by putting terephthalic acid, isophthalic acid, adipic acid, sebacic acid, ethylene glycol, 1, 4-cyclohexanedimethanol, trimethylolpropane, neopentyl glycol and xylene into a reaction kettle and carrying out polycondensation. Here, it should be noted that the molar ratio of carboxyl group to hydroxyl group in the polybasic acid to the polyhydric alcohol is about 1: 1.
The invention discloses an improvement of a composite graphite heat-conducting film, wherein the polycondensation reaction temperature of polyester resin in raw materials of adhesive components in an adhesive layer is 150-250 ℃.
The invention discloses an improvement of a composite graphite heat-conducting membrane, wherein acrylic acid modified polyester resin in adhesive components in an adhesive layer is prepared by adding butyl acrylate, acrylic acid-2-ethylhexyl ester, methyl acrylate, acrylic acid-2-hydroxyethyl ester, acrylic acid-4-hydroxybutyl ester, polyester resin, an initiator and a solvent into a reaction kettle, heating to 75-85 ℃, and reacting for 6-9 hours. The reaction product can be prepared into a propylene-modified polyester resin solution.
The invention discloses an improvement of a composite graphite heat-conducting film, wherein the thickness of a glue layer is not more than 2 microns.
The invention discloses a preparation process of a composite graphite heat-conducting film, which comprises the following steps,
A. preparing glue, and preparing the prepared glue into a glue layer; preparing a graphite heat-conducting film;
B. b, attaching a graphite heat-conducting film to one side of the adhesive layer formed in the step A to form a single-layer composite film;
C. b, attaching a graphite heat-conducting film to the other side of the glue layer on the single-layer composite film formed in the step B to form a double-layer composite film;
D. c, attaching the double-layer composite film formed in the step C to the other side of the upper adhesive layer of the single-layer composite film formed in the step B to form a three-layer composite film;
E. and D, repeatedly attaching the other side of the upper adhesive layer of the single-layer composite film formed in the step B for n times to form a (n +3) layer composite film, wherein n is 0, 1, 2, 3 and 4.
The invention discloses an improvement of a preparation process of a composite graphite heat-conducting film, wherein the bonding pressure in the bonding process from step B to step E is 0.1-1 kilogram of force.
The invention discloses an improvement of a preparation process of a composite graphite heat-conducting film, wherein the thickness of a glue layer is not more than 2 microns.
The double-sided adhesive has high thermal resistance, can generate large attenuation on the heat conducting performance, and the more the layer number is, the larger the thickness is, and the larger the attenuation is. The technical scheme adopts the acrylic acid modified polyester resin, fully exerts the synergistic effect of the acrylic acid modified polyester resin and the acrylic acid modified polyester resin, and has excellent adhesive property and heat resistance and small heat shrinkage; the glue is matched with the heat-conducting filler to prepare the heat-conducting glue film, so that the heat-conducting effect is excellent.
Two layers of graphite films are directly bonded by using a double-sided adhesive tape without a base material and with the thickness of less than 2 microns, so that the thermal resistance is reduced to the minimum, and the heat-conducting performance of the product is basically not attenuated. Compared with the prior art (considering that the existing PET double-sided adhesive tape can provide better bonding effect only when the thickness reaches more than 5 microns), the adhesive layer structure of the invention keeps smaller thickness under the condition of adopting smaller thickness without influencing the bonding quality, thereby realizing no attenuation of heat conductivity.
And preparing a substrate-free high-thermal-conductivity double-sided adhesive tape, and mutually bonding two or more layers of artificially synthesized graphite heat-conducting films together to obtain the composite graphite heat-conducting material with the expected thickness. Due to the low thermal resistance of the glue and the coating thickness of only 2 microns, the problem of attenuation of the double-sided adhesive in the multilayer graphite laminating process is effectively solved, the production efficiency is high, the cost is low, the application range of the product is greatly improved, and the market demand is met.
The traditional multilayer graphite laminating process is to coat one layer of artificially synthesized graphite heat-conducting film with ultrathin PET double-sided adhesive (generally 5 μm), and then coat the other layer of artificially synthesized graphite heat-conducting film on the double-sided adhesive, so as to obtain the double-layer graphite heat-conducting film material. By analogy, 3 layers and multilayer graphite heat-conducting film materials can be prepared. According to the technical scheme, glue with the thickness of 2 microns is coated on one layer of the artificially synthesized graphite heat-conducting film, and then the other layer of the artificially synthesized graphite heat-conducting film is compounded on the glue, so that the double-layer composite graphite heat-conducting film is prepared. By analogy, 3 layers and multilayer composite graphite heat-conducting film materials can be prepared.
According to the traditional multilayer graphite laminating process, two layers of graphite films are bonded through ultrathin PET double-faced adhesive tape (5 microns), the double-faced adhesive tape is large in thermal resistance and can generate large attenuation on heat conduction performance, and the attenuation is large when the number of layers is large. According to the technical scheme, the two graphite films are directly bonded by the 2-micron double-sided adhesive tape without the base material, so that the thermal resistance is reduced to the minimum, and the attenuation of the thermal conductivity is basically avoided.
Drawings
FIG. 1 is a process flow of a multilayer graphite heat-conducting film lamination preparation process in the prior art, taking a 3-layer film as an example, in which the thickness of a PET double-sided adhesive is minimum 3 μm;
fig. 2 shows a process flow of the multilayer graphite heat-conducting film bonding preparation of the present invention, which takes a 3-layer film as an example, and the thickness of the double-sided adhesive in this example is 2 μm at the minimum.
Detailed Description
The present invention is further illustrated by the following specific embodiments, which are to be construed as merely illustrative, and not limitative of the remainder of the disclosure in any way whatsoever.
Example 1
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 70: 30.
Example 2
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 40: 60.
Example 3
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 60: 40.
Example 4
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 50: 50.
Example 5
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 50: 40.
Example 6
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 60: 30.
Example 7
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 40: 50.
Example 8
The composite graphite heat-conducting film in the embodiment comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 45: 55.
In the above embodiments, corresponding to embodiments 1 to 8, the thermal conductive filler in the adhesive layer may be aluminum nitride; boron nitride; boron nitride, titanium dioxide mixture (the mixing mass ratio can be 1: 6 or 7: 3 or 2: 3, etc. and other arbitrary ratios); magnesium oxide; aluminum oxide; zinc oxide, silicon carbide; graphene; aluminum oxide, zinc oxide, silicon carbide mixture (the mixing mass ratio can be 1: 6: 3, 1: 7: 3, 2: 3 and the like, and any other ratio).
In the above examples, corresponding to examples 1 to 8 and modified examples thereof, the adhesive component in the adhesive layer was an acrylic modified polyester resin.
Preferably, the following schemes I to VIII can be adopted for the acrylic modified polyester resin corresponding to examples 1 to 8 and modified examples thereof:
I. the acrylic acid modified polyester resin comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 80 ℃, and reacting for 8 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
II. The acrylic acid modified polyester resin comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 81 ℃, and reacting for 6 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
III, acrylic acid modified polyester resin, which comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 83 ℃, and reacting for 7 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
IV, acrylic acid modified polyester resin, which comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 73 ℃, and reacting for 7 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
V, acrylic acid modified polyester resin, which comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding all the raw materials into a reaction kettle, heating to 80 ℃, and reacting for 8 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
VI, the acrylic acid modified polyester resin comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 75 ℃, and reacting for 9 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
VII, acrylic acid modified polyester resin, which comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 85 ℃, and reacting for 6 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
VIII, acrylic acid modified polyester resin, which comprises the following raw materials in parts by weight:
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 85 ℃, and reacting for 6 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
Preferably, the following scheme can be adopted for the polyester resin: the polyester resin is prepared by putting terephthalic acid, isophthalic acid, adipic acid, sebacic acid, ethylene glycol, 1, 4-cyclohexanedimethanol, trimethylolpropane, neopentyl glycol and xylene into a reaction kettle and carrying out polycondensation at the temperature of 250 ℃ at 150-. It should be noted that the molar ratio of carboxyl groups to hydroxyl groups in the polyacid and polyol starting materials should be ensured to be about 1: 1 when the starting materials are introduced. The polycondensation reaction temperature can be 150 ℃, 200 ℃, 250 ℃, 175 ℃, 230 ℃, 210 ℃ and any other temperature within the range, which can meet the reaction requirement and the product quality requirement of the fully mixed raw materials
Preferably, the thickness of the glue layer can be adopted correspondingly to the embodiments 1-8 and the modified embodiments thereof: 2 microns, 1 micron, 0.5 microns, 1.7 microns, 1.5 microns, 0.3 microns, 0.1 microns, 0.7 microns.
The following description will be given by taking a specific embodiment as an example.
As shown in fig. 2, taking 3-layer composite graphite as an example:
in the scheme, the composite graphite heat-conducting film is adopted and comprises the graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the graphite heat-conducting film is arranged at intervals, the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is 70: 30; the heat conducting filler is aluminum nitride.
The adhesive component in the adhesive layer is acrylic acid modified polyester resin,
the preparation method comprises the steps of adding the raw materials into a reaction kettle, heating to 85 ℃, and reacting for 6 hours to obtain the catalyst. The reaction product can be prepared into a propylene-modified polyester resin solution.
The polyester resin is prepared by putting 0.1M terephthalic acid, 0.1M isophthalic acid, 0.1M adipic acid, 0.15M sebacic acid, 0.1M ethylene glycol, 0.1M1, 4-cyclohexanedimethanol, 0.1M trimethylolpropane, 0.1M neopentyl glycol and 500mL xylene into a reaction kettle and carrying out polycondensation at the temperature of 240 ℃.
And uniformly stirring the prepared glue, and preparing the double-sided adhesive without the base material by using a coating machine, wherein the thickness is controlled within 2 mu m.
And (3) mounting the rolled graphite heat-conducting film coil material obtained in the step (1) on a tail unwinding shaft of a coating machine, penetrating through a guide roller according to requirements, compounding the rolled graphite heat-conducting film coil material with the substrate-free double-faced adhesive tape prepared in the step (1) on line (the pressure of a compression roller is 0.5kg), and then winding the rolled graphite heat-conducting film coil material on a tail winding shaft of the coating machine.
And (3) taking 2 rolls of the material prepared in the step (2) and 1 roll of the material to be synthesized into the graphite heat-conducting film coiled material, and performing post-processing on the coiled material on a laminating machine.
And (3) rolling the composite graphite heat-conducting film prepared in the step (1) upwards, unreeling the composite graphite heat-conducting film with the glue surface upwards, then compounding the synthetic graphite heat-conducting film roll material on the glue surface, and effectively bonding the two layers of materials together through the pressure of a rubber roller.
And (3) continuously unreeling the double-layer composite graphite heat-conducting film prepared in the step (4) forwards, unreeling the composite graphite heat-conducting film prepared in the step (2) downwards in the other step (1), and effectively bonding the double-layer composite graphite heat-conducting film and the composite graphite heat-conducting film together through another rubber roller of a laminating machine to prepare the 3-layer composite graphite heat-conducting film.
And (3) peeling off the release film on the 3 layers of graphite heat-conducting films compounded in the step (5), and then rolling the release film on the PE tube core through a rolling shaft to form the 3 layers of composite graphite heat-conducting film material.
By the method, the composite graphite heat-conducting membrane material with 4 layers or more can be prepared.
Remarking:
1. the laminating machine requires the minimum configuration to be 3 receiving and 3 releasing.
2. The thermal conductivity of the different materials is given in the following table:
in the scheme of the invention, including but not limited to the embodiment, the product is sampled by 10 pieces for testing, the average value of the performance is satisfied, the heat conductivity coefficient is 1000-1500 w/m.k, and the density is 1.8-2.1 g/cm3。
The technical range of the embodiment of the invention is not exhaustive, and a new technical scheme formed by equivalent replacement of single or multiple technical features of the cloud system/server by the remote control system in the technical scheme of the embodiment is also within the technical range of the invention; in all the embodiments of the present invention, which are listed or not listed, each parameter in the same embodiment only represents an example (i.e., a feasible embodiment) of the technical solution, and there is no strict matching and limiting relationship between the parameters, wherein the parameters may be replaced with each other without departing from the axiom and the requirements of the present invention, unless otherwise specified.
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and the technical scheme also comprises the technical scheme formed by any combination of the technical characteristics. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.
Claims (10)
1. The composite graphite heat-conducting film comprises a graphite heat-conducting film, an adhesive layer and a multilayer laminated structure, wherein the multilayer laminated structure is formed by arranging the graphite heat-conducting film at intervals, and is characterized in that the adhesive layer comprises an adhesive component and heat-conducting filler, and the mass ratio of the adhesive component to the heat-conducting filler is (70: 30) - (40: 60).
2. The composite graphite heat-conducting film according to claim 1, wherein the heat-conducting filler in the adhesive layer comprises one or more of aluminum nitride, boron nitride, titanium dioxide, magnesium oxide, aluminum oxide, zinc oxide, silicon carbide and graphene.
3. The composite graphite heat transfer film of claim 1, wherein the binder component of the glue layer is an acrylic modified polyester resin.
4. The composite graphite heat-conducting film according to claim 3, wherein the acrylic modified polyester resin of the adhesive component in the adhesive layer comprises the following raw materials in parts by weight:
5. the composite graphite heat-conducting film according to claim 4, wherein the solvent in the raw material of the binder component in the glue layer is ethyl acetate or toluene.
6. The composite graphite heat-conducting film according to claim 4, wherein the initiator in the raw material of the adhesive component in the adhesive layer is one of dibenzoyl peroxide and azobisisobutyronitrile or a combination thereof.
7. The composite graphite heat-conducting film according to claim 4, wherein the polyester resin in the raw material of the binder component in the adhesive layer is obtained by polycondensation of terephthalic acid, isophthalic acid, adipic acid, sebacic acid, ethylene glycol, 1, 4-cyclohexanedimethanol, trimethylolpropane, neopentyl glycol and xylene.
8. The composite graphite heat-conducting film as claimed in claim 7, wherein the polycondensation reaction temperature of the polyester resin in the raw material of the binder component in the glue layer is 150-250 ℃.
9. The composite graphite thermal film according to any one of claims 1 to 8, wherein the thickness of the subbing layer is not greater than 2 μm.
10. The preparation process of the composite graphite heat-conducting film comprises the following steps,
A. preparing glue, and preparing the prepared glue into a glue layer; preparing a graphite heat-conducting film;
B. b, attaching a graphite heat-conducting film to one side of the adhesive layer formed in the step A to form a single-layer composite film;
C. b, attaching a graphite heat-conducting film to the other side of the glue layer on the single-layer composite film formed in the step B to form a double-layer composite film;
D. c, attaching the double-layer composite film formed in the step C to the other side of the upper adhesive layer of the single-layer composite film formed in the step B to form a three-layer composite film;
E. and D, repeatedly attaching the other side of the upper adhesive layer of the single-layer composite film formed in the step B for n times to form a (n +3) layer composite film, wherein n is 0, 1, 2, 3 and 4.
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