CN115433424A - Low-oil-permeability phase-change heat conducting fin and preparation method thereof - Google Patents
Low-oil-permeability phase-change heat conducting fin and preparation method thereof Download PDFInfo
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- CN115433424A CN115433424A CN202211108299.3A CN202211108299A CN115433424A CN 115433424 A CN115433424 A CN 115433424A CN 202211108299 A CN202211108299 A CN 202211108299A CN 115433424 A CN115433424 A CN 115433424A
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- 238000002360 preparation method Methods 0.000 title abstract description 17
- 230000008859 change Effects 0.000 claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 37
- 239000010439 graphite Substances 0.000 claims abstract description 35
- 239000011347 resin Substances 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 28
- 239000000839 emulsion Substances 0.000 claims abstract description 26
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000012782 phase change material Substances 0.000 claims abstract description 21
- 239000007822 coupling agent Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 35
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 21
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 21
- HPEUJPJOZXNMSJ-UHFFFAOYSA-N Methyl stearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC HPEUJPJOZXNMSJ-UHFFFAOYSA-N 0.000 claims description 14
- 150000001875 compounds Chemical class 0.000 claims description 13
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 239000011231 conductive filler Substances 0.000 claims description 8
- CAMHHLOGFDZBBG-UHFFFAOYSA-N epoxidized methyl oleate Natural products CCCCCCCCC1OC1CCCCCCCC(=O)OC CAMHHLOGFDZBBG-UHFFFAOYSA-N 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
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- 238000002474 experimental method Methods 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
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- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 1
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- 238000011049 filling Methods 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C08J2325/00—Characterised by the use of 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 an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
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Abstract
The invention belongs to the field of heat conduction materials, and discloses a low-permeability oil phase change heat conduction sheet and a preparation method thereof, wherein the phase change heat conduction sheet is prepared from the following raw materials in parts by mass: 10 parts of resin emulsion, 80-120 parts of heat-conducting filler, 1.6-2.4 parts of coupling agent, 1-3 parts of phase change component and 0.5-1.5 parts of expanded graphite. The phase-change heat conducting fin obtained by controlling the detailed components and the proportion thereof for forming the phase-change heat conducting fin and integrally matching the resin matrix (corresponding to the resin emulsion in the raw materials), the heat conducting filler, the coupling agent, the phase-change component and the expanded graphite has the characteristic of low oil permeability while ensuring the compressible flow property of the phase-change material endowed with the heat conducting fin, and well solves the oil permeability problem caused by the solid-liquid transition of the phase-change material in the use process of the phase-change heat conducting fin.
Description
Technical Field
The invention belongs to the field of heat conduction materials, and particularly relates to a low-permeability oil phase change heat conduction sheet and a preparation method thereof.
Background
At present, electronic components's the degree of integrating is more and more high, and the device develops towards the orientation such as the quality is light, small, power density is big, so the heat of its inside production is more and more big, and the gathering of thermal a large amount of production is inside electronic components, can influence electronic components's life or directly make electronic components inefficacy to a great extent. Macroscopically, it appears that the heat generating source and the heat sink are in intimate contact, but microscopically, the solid-to-solid contact is not perfectly compliant, and air is present in these pores, which is highly detrimental to the removal of heat generated in the heat source from the electronic components.
The thermal interface material can well fill the air pores, so that the heat dissipation performance is improved. The phase-change thermal interface material has certain compressibility due to the solid-liquid transition of the phase-change material when the phase-change component reaches the phase-change temperature, so that the phase-change thermal interface material can better enter pores and realize more effective heat dissipation. But due to the presence of the phase change component, it often causes significant oil bleeding problems during solid-liquid conversion, reduces the reliability of the material, and may cause contamination of the device.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention aims to provide a low-permeability oil phase-change heat conducting fin and a preparation method thereof, wherein the phase-change heat conducting fin is obtained by controlling the detailed components and the proportion thereof for forming the phase-change heat conducting fin and integrally matching the resin matrix (corresponding to the resin emulsion in the raw materials), the heat conducting filler, the coupling agent, the phase-change component and the expanded graphite, and the oil permeability problem caused by solid-liquid transition of the phase-change material in the use process of the phase-change heat conducting fin is well solved.
In order to achieve the above object, according to one aspect of the present invention, there is provided a phase change thermally conductive sheet, which is characterized by being prepared from the following raw materials in parts by mass:
in a further preferred embodiment of the present invention, the resin emulsion is an acrylic emulsion, preferably one of a styrene-acrylic emulsion and an acrylic emulsion; the solid content in the resin emulsion is more than or equal to 50wt%.
As a further preferred of the present invention, the heat conductive filler is one or more of alumina, silicon carbide, and aluminum nitride; preferably, the mass portion of the heat-conducting filler is 80 parts, 100 parts or 120 parts.
In a further preferred aspect of the present invention, the alumina is spherical alumina, and the spherical alumina preferably has a particle size of 2 μm to 40 μm;
the silicon carbide is blocky silicon carbide with the grain diameter of 10 mu m;
the aluminum nitride is spherical aluminum nitride, and the particle size is preferably 40 mu m.
As a further preferred aspect of the present invention, the heat conductive filler is a composite alumina, and the composite alumina is a spherical alumina with a particle size of 40 μm, 10 μm, 5 μm, and 2 μm, respectively, in a mass ratio of 18 to 22:10 to 14:14 to 18: 50-54 are mixed;
or the heat conducting filler is preferably compound alumina and massive silicon carbide according to a mass ratio of 4:1 obtained by mixing; wherein the compound alumina is spherical alumina with the grain diameters of 40 mu m, 10 mu m, 5 mu m and 2 mu m respectively according to the mass ratio of 18-22: 10 to 14:14 to 18: 50-54, wherein the particle size of the massive silicon carbide is 10 mu m;
or the heat conducting filler is preferably compound alumina and spherical aluminum nitride according to the mass ratio of 3:2 mixing to obtain; wherein the compound alumina is spherical alumina with the grain diameters of 40 mu m, 10 mu m, 5 mu m and 2 mu m respectively according to the mass ratio of 18-22: 10 to 14:14 to 18: 50-54, and the grain diameter of the spherical aluminum nitride is 40 mu m.
As a further preferred aspect of the present invention, the coupling agent is a titanate coupling agent.
As a further preferable aspect of the present invention, the mass ratio of the thermally conductive filler to the coupling agent is 50:1.
in a further preferred embodiment of the present invention, the phase transition component is one of methyl stearate and paraffin, and the phase transition temperature is 37 ℃ to 45 ℃.
In a further preferred embodiment of the present invention, the expanded graphite is 80-mesh expanded graphite.
According to another aspect of the present invention, there is provided a method for producing the above-mentioned phase-change thermally conductive sheet, comprising the steps of:
a) Mixing expanded graphite and a phase change component in water bath for 1-2 h at the temperature which is at least 20 ℃ higher than the phase change temperature of the phase change component to obtain a phase change material/expanded graphite mixture;
b) Mixing resin emulsion, heat-conducting filler, coupling agent and the phase-change material/expanded graphite mixture, heating to 100-120 ℃, stirring at 800-1500 rpm for 0.5-1 h, volatilizing solvent components in the resin emulsion to obtain a uniformly mixed melt material;
c) Placing the melt material in a vacuum environment with the negative pressure not higher than-0.1 MPa for 3-5 min;
d) Pressing the material obtained in the step c) to obtain a phase change heat conducting strip; wherein the pressure applied by the tabletting treatment is 5-10 MPa.
Compared with the prior art, the phase-change heat conducting fin obtained by utilizing the resin matrix (corresponding to the resin emulsion in the raw materials), the heat conducting filler, the coupling agent, the phase-change component and the expanded graphite and controlling the proportion among the five components has the characteristic of low oil seepage while ensuring the compressibility of the heat conducting fin endowed by the phase-change material, and well solves the oil seepage problem caused by solid-liquid transformation of the phase-change material in the use process of the phase-change heat conducting fin.
Based on the invention, during preparation, the resin emulsion, the heat-conducting filler, the coupling agent, the phase-change material and the expanded graphite are mixed according to a certain proportion, and the low-permeability oil phase-change heat-conducting sheet is prepared in a cold press molding mode. The invention can especially take styrene-acrylic emulsion and acrylate emulsion as raw materials, the use of the emulsion simplifies the process, the crosslinking molding can be realized through subsequent heating and vacuum pumping treatment, and the addition proportion of the heat-conducting filler can be increased by using the emulsion, thereby realizing high heat conductivity. The addition of the coupling agent can well perform organic modification on the surface of the filler, realize better combination with a resin matrix, and increase the addition of the heat-conducting filler, thereby finally improving the heat conductivity of the material; and the phase-change material is added, and when the phase-change temperature is reached, the material has certain compressibility, so that air gaps are filled better, and a better heat dissipation effect is realized. The phase-change material has low addition proportion (the mass ratio of the heat-conducting filler to the phase-change component is 80-120: 1-3), and has small influence on the final heat conductivity of the phase-change heat-conducting sheet. When the using temperature reaches the phase-change temperature, the phase-change material is changed from a solid state to a liquid state, and has high flowing property; the single resin matrix and the phase-change material are mixed, the coating effect of the resin on the liquid phase-change material is limited, and although the resin has good compressibility, the phase-change material can seep out; assuming that only the mixture of expanded graphite and phase change material, and the mixture of expanded graphite and phase change material alone, the resulting material does not have flexibility and compressibility (compressibility is the key to the function of the phase change thermally conductive sheet as a thermal interface material, which is why the prior art often does not contemplate the use of expanded graphite). The invention disperses the expanded graphite in the resin matrix to form a new carrier, and the combination of the expanded graphite and the resin can reduce the damage of the expanded graphite to the compressibility of the material on one hand, and can reduce the oil leakage problem when the expanded graphite is used as the barrier point of an oily substance on the other hand. The novel carrier with the resin matrix structure dispersed with the expanded graphite has good compressibility and low oil permeability due to the adsorption and barrier effects of the expanded graphite dispersed in the carrier, and the balance between high compressibility fluidity and low oil permeability of the phase change heat conducting sheet is realized.
Taking the use of acrylic emulsion as an example, the addition of the compound heat-conducting filler establishes a more effective heat-conducting path, and the heat conductivity of the material is improved; the phase change component is added, so that the heat dissipation plate has certain compression fluidity at the use temperature and pressure, air gaps can be well filled, and the heat dissipation effect is improved; the novel carrier formed by the resin matrix dispersed with the expanded graphite has good compressibility and low oil permeability due to the adsorption and barrier effects of the expanded graphite dispersed in the carrier, and the balance between high compressibility fluidity and low oil permeability of the phase change heat conducting fin is realized.
The invention can especially use the compound alumina obtained by compounding 4 kinds of spherical alumina with different grain diameters as the heat conducting filler, the 4 kinds of spherical alumina with different grain diameters are calculated according to the spherical closest stacking model to obtain the mass ratio of the spherical alumina with the grain diameters of 40 mu m, 10 mu m, 5 mu m and 2 mu m according to the mass ratio of 18-22: 10 to 14:14 to 18: 50-54, thereby better realizing the construction of the heat conduction path. Of course, the use of the mixture of spherical alumina and massive silicon carbide is beneficial to increasing the contact area of the heat-conducting filler and is beneficial to further improving the heat conductivity of the material.
The hypotonic oil phase change heat conducting fin obtained by the invention has certain compressibility under the use temperature and pressure, so that the contact thermal resistance is reduced, and more efficient heat dissipation is realized. The existing phase change heat conducting fin is used for pursuing better flowing performance, and the oil leakage problem caused by the better flowing performance is ignored; the novel carrier formed by combining the expanded graphite and the resin matrix is beneficial to improving the thermal conductivity of the material, is more beneficial to preventing the leakage of the phase change material, and realizes the balance between the compressible flowability and the low oil permeability of the phase change heat conducting fin.
Drawings
FIG. 1 is a graph comparing the oil-bleeding performance test of example 6 with that of comparative example 1 and a commercial phase-change thermally conductive sheet (Honeywell PTM 7950); wherein (a) in fig. 1 corresponds to before testing of each sample, and (b) in fig. 1 corresponds to after testing of each sample.
FIG. 2 is a DSC chart of examples 1 to 3.
FIG. 3 is a heat dissipation performance test chart of LED lamps of example 4, example 6 and comparative example 2.
FIG. 4 is a graph showing the cycle performance test of example 6.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
In the examples and comparative examples below, isopropyl tris (dioctylpyrophosphate) titanate was used as the coupling agent (although other coupling agents, such as other titanate coupling agents, can be used). In addition, among the heat conductive fillers used hereinafter, heat conductive fillers of each particle size class (e.g., spherical alumina, massive silicon carbide, spherical aluminum nitride) are commercially available.
Example 1
1. The raw material formula is as follows:
2. preparation:
firstly, placing the expanded graphite and the methyl stearate in a beaker, heating in water bath at 60 ℃, and mixing for 1h to obtain the expanded graphite/methyl stearate composite material. Adding acrylate emulsion, compound alumina, titanate coupling agent and expanded graphite/methyl stearate composite material in proportion at the rotating speed of 1000rpm at 100 ℃, and stirring for 1h; vacuumizing the obtained mixture for 3min, wherein the vacuum degree is-0.1 MPa (of course, other vacuum degree settings can be used, and the closer the vacuum environment is to the vacuum, the better); finally, the hypotonic oil phase change heat conducting sheet is obtained through hydraulic tabletting, the pressure is 5MPa, and the time is 5min.
Example 2
1. The raw material formula comprises:
2. preparation: the same as in example 1.
Example 3
1. The raw material formula is as follows:
2. preparation: the same as in example 1.
Example 4
1. The raw material formula comprises:
wherein the grain diameter of the spherical aluminum nitride is 40 μm, and the mass ratio of the compound aluminum oxide to the aluminum nitride is 60:40.
2. preparation: the same as in example 1.
Example 5
1. The raw material formula is as follows:
2. preparation: the same as in example 1.
Example 6
1. The raw material formula is as follows:
the grain diameter of the silicon carbide is 10 mu m, and the mass ratio of the compound aluminum oxide to the silicon carbide is 80:20.
2. preparation: the same as in example 1.
Example 7
1. The raw material formula is as follows:
the phase transition temperature of the paraffin is 40 ℃.
2. Preparation: the same as in example 1.
Example 8
1. The raw material formula comprises:
2. preparation: the same as in example 1.
The material properties of this example are similar to example 2.
Example 9
1. The raw material formula comprises:
2. preparation: the same as in example 1.
The material properties of this example are similar to example 2.
Comparative example 1
1. The raw material formula is as follows:
the grain diameter of the silicon carbide is 10 mu m, and the mass ratio of the compound alumina to the silicon carbide is 80:20.
2. preparation: the same as in example 1. There is no mixing process of the expanded graphite and the methyl stearate.
Comparative example 2
1. The raw material formula comprises:
10 portions of styrene-acrylic emulsion (solid content 57 percent by weight)
100 portions of heat-conducting filler (compounded aluminum oxide and silicon carbide)
(wherein, aluminum oxide (m) is compounded 40μm :m 10μm :m 5μm :m 2μm ＝20:12:16:52))
The grain diameter of the silicon carbide is 10 mu m, and the mass ratio of the compound alumina to the silicon carbide is 80:20.
2. preparation: the same as in example 1. There is no mixing process of the expanded graphite and the methyl stearate.
Performance testing
The above examples and comparative examples were subjected to performance tests, and the results are shown in Table 1. The specific test process is as follows:
and (3) oil seepage performance test: the plate was placed in an oven at 120 ℃ for 24 hours, and the front and rear changes of the heat-conducting sheet were observed. Leakage rate x = (m) 1 -m 2 )/m 1 ,m 1 M is the mass of the heat-conducting strip before being put into the oven 2 The quality of the heat conducting fin after the test is carried out.
And (3) testing the compressible property: and (3) placing the phase-change heat-conducting strip at 55 ℃ and under the pressure of 10psi for 5min, and measuring the thickness change of the phase-change heat-conducting strip with the same size under the test condition. Compression ratio = (h) 1 -h 2 /h 1 )h 1 The original thickness of the phase-change heat-conducting fin is h 2 The thickness of the phase change heat conducting fin after the test.
And (3) testing heat dissipation performance: the three-layer structure of the LED lamp, the phase change heat conducting fin and the radiator is adopted, and the surface temperature difference of the LED lamp before and after the heat conducting fin is added is measured.
And (3) testing the cycling stability: the LED lamp is started for 5min, and the LED lamp is closed and cooled for 90s to form a cycle, the cycle is performed for 100 times, and the surface temperature change curve of the LED lamp is recorded.
Table 1: properties of the products obtained in examples and comparative examples
As can be seen from the test results in Table 1, the oil permeability of the products of examples 1 to 6 of the present invention is 0.18% or less, the thermal conductivity is 4W/(m.K) or more, the compression ratio is 16% or more, and the LED can generate a temperature difference of 14 ℃ or more before and after the use of the thermal conductive pad. Comparative example 1 no expanded graphite was added, and it was found that the oil permeability was increased, demonstrating that in the phase change thermally conductive sheet obtained according to the present invention, the addition of expanded graphite in a certain proportion and the resin matrix form a new carrier, which is beneficial to preventing leakage of the phase change material, and achieving a balance between high compressibility fluidity and low oil permeability of the phase change thermally conductive sheet. Comparative example 2, in which no phase change component and no expanded graphite were added, was observed to show a significant decrease in compressibility, a deterioration in surface bonding with the device, and a relatively significant decrease in heat dissipation properties. Comparing example 5 with example 6, it can be seen that, under the condition that the total filling amount of the heat-conducting filler is not changed, part of the spherical alumina is replaced by part of the massive silicon carbide, the contact area between the fillers is increased by adding the massive silicon carbide, more heat-conducting paths are formed, and the heat conductivity of the phase-change heat-conducting strip is improved.
The phase-change thermally conductive sheet obtained in example 6 was subjected to an oil-bleeding performance test with the phase-change thermally conductive sheet obtained in comparative example 1 and a commercial product (Honeywell PTM 7950) under the test conditions of being left in an oven at 120 ℃ for 24 hours, and the change of the thermally conductive sheet was observed. As shown in fig. 1, it can be seen that the phase-change thermal conductive gasket obtained in example 6 has substantially no oil leakage, the sample in comparative example 1 has a small amount of oil leakage, and the commercial product of the phase-change thermal conductive sheet has a large amount of oil leakage, so that a certain amount of expanded graphite is combined with the resin matrix to form a new carrier, which can solve the oil leakage problem during the phase change process.
The phase-change thermal conductive sheets obtained in example 1, example 2 and example 3 were subjected to DSC experiments, and the results are shown in fig. 2, from which it can be seen that the phase-change thermal conductive pad has a distinct phase-change behavior at 38 ℃.
The heat dissipation performance test experiments of the embodiment 4, the embodiment 6 and the comparative example 2 are carried out, wherein the experimental conditions specifically adopt a three-layer structure of an LED lamp, a phase change heat conducting fin and a radiator, and the surface temperature difference of the LED lamp before and after the heat conducting fin is added is measured. As shown in fig. 3, it can be seen that, when no gasket is added (i.e., when no phase-change heat-conducting sheet is added), the LED lamp operates at a stable surface temperature of about 70 degrees celsius, when the phase-change heat-conducting gasket of example 4 is added between the LED lamp and the heat sink, the LED lamp operates at a stable surface temperature of about 50 degrees celsius, when the phase-change heat-conducting gasket of example 6 is added between the LED lamp and the heat sink, the LED lamp operates at a stable surface temperature of about 55 degrees celsius, and when the phase-change heat-conducting gasket of comparative example 2 is added between the LED lamp and the heat sink, the LED lamp operates at a stable surface temperature of about 60 degrees celsius. Therefore, the surface temperature of the LED during operation can be well reduced by adding the heat conduction gasket, and the compressible performance of the phase-change heat conduction gasket can bring better interface contact and further reduce the surface temperature of the LED lamp through the comparative example 2 and the embodiment 6.
The experimental conditions of the cycle stability experiment of the embodiment 6 are that a three-layer structure of an LED lamp, a phase change heat conducting fin and a radiator is adopted, the LED lamp is started for 5min, the cooling is turned off for 90s to form a cycle, the cycle is carried out for 100 times, and the surface temperature change curve of the LED lamp is recorded. The result is shown in fig. 4, from which it can be seen that the phase-change heat-conducting gasket has stable performance during recycling.
The above embodiments are merely examples, and the hypotonic oil phase change thermal conductive sheet in the present invention may further include a sixth component, such as carbonyl iron, etc., in addition to the five components of the resin matrix, the thermal conductive filler, the coupling agent, the phase change component, and the expanded graphite, according to actual requirements for the properties of the phase change thermal conductive sheet, when the phase change thermal conductive sheet is manufactured, the raw material may further include the sixth component (the carbonyl iron may be added to make the material have a certain electromagnetic shielding function).
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The phase change heat conducting sheet is characterized by being prepared from the following raw materials in parts by mass:
2. the phase-change heat conducting sheet according to claim 1, wherein the resin emulsion is an acrylic emulsion, preferably one of a styrene-acrylic emulsion and an acrylic emulsion; the solid content in the resin emulsion is more than or equal to 50wt%.
3. The phase-change thermally conductive sheet according to claim 1, wherein the thermally conductive filler is one or more of alumina, silicon carbide, and aluminum nitride; preferably, the mass part of the heat-conducting filler is 80 parts, 100 parts or 120 parts.
4. The phase-change thermally conductive sheet according to claim 3, wherein the alumina is spherical alumina, and the particle size of the spherical alumina is preferably 2 μm to 40 μm;
the silicon carbide is blocky silicon carbide with the grain diameter of 10 mu m;
the aluminum nitride is spherical aluminum nitride, and the particle size is preferably 40 mu m.
5. The phase-change heat conducting sheet according to claim 1, wherein the heat conducting filler is a composite alumina made of spherical alumina having particle diameters of 40 μm, 10 μm, 5 μm and 2 μm, in a mass ratio of 18 to 22:10 to 14:14 to 18: 50-54 are mixed;
or the heat-conducting filler is preferably a mixture of compound alumina and massive silicon carbide according to a mass ratio of 4:1 obtained by mixing; wherein the compound alumina is spherical alumina with the grain diameters of 40 μm, 10 μm, 5 μm and 2 μm respectively according to the mass ratio of 18-22: 10 to 14:14 to 18: 50-54, wherein the particle size of the massive silicon carbide is 10 mu m;
or the heat conducting filler is preferably compound alumina and spherical aluminum nitride according to the mass ratio of 3:2 mixing to obtain; wherein the compound alumina is spherical alumina with the grain diameters of 40 μm, 10 μm, 5 μm and 2 μm respectively according to the mass ratio of 18-22: 10 to 14:14 to 18: 50-54, and the grain diameter of the spherical aluminum nitride is 40 mu m.
6. The phase-change thermally conductive sheet according to claim 1, wherein the coupling agent is a titanate coupling agent.
7. The phase-change thermally conductive sheet as claimed in claim 1, wherein the mass ratio of the thermally conductive filler to the coupling agent is 50:1.
8. the phase-change thermally conductive sheet as claimed in claim 1, wherein the phase-change component is one of methyl stearate and paraffin, and the phase-change temperature is 37 ℃ to 45 ℃.
9. The phase-change thermally conductive sheet according to claim 1, wherein the expanded graphite is 80-mesh expanded graphite.
10. The method for producing a phase-change thermally conductive sheet as claimed in any one of claims 1 to 9, comprising the steps of:
a) Mixing expanded graphite and a phase change component in water bath for 1-2 h at the temperature which is at least 20 ℃ higher than the phase change temperature of the phase change component to obtain a phase change material/expanded graphite mixture;
b) Mixing resin emulsion, heat-conducting filler, coupling agent and the phase-change material/expanded graphite mixture, heating to 100-120 ℃, stirring at 800-1500 rpm for 0.5-1 h, volatilizing solvent components in the resin emulsion, and obtaining a uniformly mixed melt material;
c) Placing the melt material in a vacuum environment with the negative pressure not higher than-0.1 MPa for 3-5 min;
d) Pressing the material obtained in the step c) into sheets to obtain phase change heat conducting sheets; wherein the pressure applied by the tabletting treatment is 5-10 MPa.
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