CN116769311A - Phase change material matrix for preparing thermal interface material, and preparation method and application thereof - Google Patents
Phase change material matrix for preparing thermal interface material, and preparation method and application thereof Download PDFInfo
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- CN116769311A CN116769311A CN202310694942.3A CN202310694942A CN116769311A CN 116769311 A CN116769311 A CN 116769311A CN 202310694942 A CN202310694942 A CN 202310694942A CN 116769311 A CN116769311 A CN 116769311A
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- 239000000463 material Substances 0.000 title claims abstract description 113
- 239000011159 matrix material Substances 0.000 title claims abstract description 43
- 239000012782 phase change material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 150000001336 alkenes Chemical class 0.000 claims abstract description 31
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229920000642 polymer Polymers 0.000 claims abstract description 29
- 230000008859 change Effects 0.000 claims abstract description 20
- 229920006037 cross link polymer Polymers 0.000 claims abstract description 19
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims description 20
- 229920002545 silicone oil Polymers 0.000 claims description 20
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 238000004132 cross linking Methods 0.000 claims description 10
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 7
- 229920000578 graft copolymer Polymers 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 7
- 238000007259 addition reaction Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims 1
- 239000000945 filler Substances 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000011231 conductive filler Substances 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- 239000002243 precursor Substances 0.000 description 4
- 229920002994 synthetic fiber Polymers 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 239000000017 hydrogel Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
The application provides a phase change material matrix for preparing a thermal interface material, a preparation method and application thereof, wherein the phase change material matrix for preparing the thermal interface material comprises the following raw materials in parts by weight: 0.1 to 99.9 parts of olefin material, 0 to 99.9 parts of graftable polymer prepolymer, 0.1 to 99.9 parts of crosslinked polymer prepolymer and 0.1 to 1 part of catalyst. Under the condition of the same filler part, compared with the thermal conductivity of the same type of thermal interface material prepared by using the polymer matrix with the phase change property, the thermal conductivity of the thermal interface material is improved by 28.6%, the contact thermal resistance is reduced by 46.1%, and the storage modulus is reduced by 93.33%. The preparation method is simple and is suitable for industrial production.
Description
Technical Field
The application relates to the technical field of materials, in particular to a phase change material matrix for preparing a thermal interface material, and a preparation method and application thereof.
Background
The thermal interface material plays a role of a thermal bridge in the thermal management technology of electronic devices such as packaging chips and equipment, and can fill the interface gap between a heat source and various thermal management components and establish a thermal transportation bridge, so that the packaging chips can dissipate heat in time, the high-efficiency operation of the packaging chips is ensured, and the service life of the packaging chips is prolonged. The key factor for measuring the heat transport efficiency of the thermal interface material is the effective total thermal resistance of the material, which is expressed as follows:
R total ＝R contact1 +R contact2 +d/k
wherein R is total Is the effective total thermal resistance; r is R contact1,2 The interface contact thermal resistance between the thermal interface material and the contact solid; k is the intrinsic thermal conductivity of the thermal interface material; d is the thermal interface material thickness. From the equation, it can be seen that the improvement of the thermal conductivity number (k) of the material and the reduction of the thermal contact resistance of the material are key to improving the thermal transport efficiency of the thermal interface material, i.e. enhancing the thermal conductivity. In recent years, many polymer composites have been designed as thermal interface materials to increase thermal conductivity and thereby reduce thermal resistance, and such thermal interface materials employ strategies such as increasing filler content to form a three-dimensional thermally conductive pathway network, filler hybridization, surface modification, and the like. In fact, an ideal thermal interface material has extremely strong heat conduction performance, good shape adaptability and interface compatibility, so that the material can be perfectly attached at an interface, the interface contact thermal resistance is reduced, and heat can be effectively transported across the boundary。
An effective way to improve the interfacial compatibility of thermal interface materials is to reduce the modulus of the material. The phase change material can be used as a thermal interface material matrix due to the characteristic of obvious change of modulus before and after phase change. When the thermal interface material is at high temperature, the matrix undergoes phase change, the modulus is reduced, and the interface compatibility is enhanced under the same pressure, so that the thermal conduction at the interface is improved. However, the traditional phase change material is solid-liquid phase change, which is extremely easy to cause liquefaction leakage of the phase change material during application, thereby affecting the heat conduction effect of the material and even damaging electronic devices. Preventing material liquefaction leakage is thus a great challenge for the development of phase change thermal interface materials.
Disclosure of Invention
The application provides a phase change material matrix for preparing a thermal interface material, and a preparation method and application thereof. The method aims to solve the problem of interface compatibility between the thermal interface material and the contact object, so that the thermal interface material is more attached to the interface, thereby reducing interface contact thermal resistance and improving heat conduction efficiency.
In order to achieve the above purpose, the technical scheme adopted by the application is as follows:
the application provides a phase change material matrix for preparing a thermal interface material, which comprises the following raw materials in parts by weight: 0.1 to 99.9 parts of olefin material, 0 to 99.9 parts of graftable polymer prepolymer, 0.1 to 99.9 parts of crosslinked polymer prepolymer and 0.1 to 1 part of catalyst.
Further, the olefin material is hexadecene and/or octadecene material with phase change property.
Further, the grafted polymer prepolymer is hydrogen-containing silicone oil which can perform addition reaction with olefin materials.
Further, the crosslinked polymer prepolymer is a polydimethylsiloxane prepolymer.
Further, the catalyst is at least one selected from chloroplatinic acid, chloroplatinic acid-isopropanol complex and chloroplatinic acid-divinyl tetramethyl disiloxane complex.
The application also provides a preparation method of the phase change material matrix for preparing the thermal interface material, which comprises the following steps: uniformly mixing and stirring an olefin material, a graftable polymer prepolymer, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix for preparing a thermal interface material; in the method, after the olefin material is grafted with the grafted polymer prepolymer, the olefin material is crosslinked with the crosslinked polymer prepolymer to form a covalent bond network; or after grafting the olefin material and the graftable polymer prepolymer, dissolving the olefin material in the crosslinked polymer prepolymer for self crosslinking to form a covalent bond network.
Further, the macromolecular prepolymer after the olefin material is grafted exists in a matrix: crosslinking with other polymer prepolymers or dispersing in a polymer crosslinked network or both.
The application also provides a preparation method of the phase change material matrix for preparing the thermal interface material, which comprises the following steps: uniformly mixing and stirring an olefin material, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix which can be used for preparing a thermal interface material; wherein in the method the olefinic material is directly crosslinked with the crosslinked polymeric prepolymer.
The application also provides application of the phase change material matrix for preparing the thermal interface material in the field of preparing the thermal interface material.
Further, the thermal conductivity coefficient of the thermal interface material is between 0.1W/mK and 100.0W/mK, and the contact thermal group is 10 - 7 m 2 K/W～10 -4 m 2 K/W, modulus is in the range of 0.001 KPa-1000 MPa.
Compared with the prior art, the technical scheme provided by the application has at least the following advantages:
the application provides a phase change material matrix for preparing a thermal interface material, a preparation method and application thereof, and the thermal conductivity of the thermal interface material compounded by the polymer matrix with the phase change characteristic is improved by 28.6%, the contact thermal resistance is reduced by 46.1% and the storage modulus is reduced by 93.33% compared with the thermal interface material which is of the same type but not prepared by the matrix under the condition of the same filler part. The preparation method is simple and is suitable for industrial production.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, which are not to be construed as limiting the embodiments unless specifically indicated otherwise.
FIG. 1 shows a polymer matrix prepared by different modes according to the embodiment of the application;
FIG. 2 shows polymer matrices prepared in various ways according to an embodiment of the present application;
FIG. 3 shows polymer matrices prepared in various ways according to an embodiment of the present application;
FIG. 4 is a state diagram of the matrix before and after phase transition after crosslinking observed by an Olympic polarization microscope in an embodiment of the present application.
Detailed Description
The inventors found that material interface compatibility was improved by improving the thermal interface material modulus; the modulus of the thermal interface material can be effectively regulated by selecting a proper polymer matrix; the phase change material can be used as a matrix to prepare a thermal interface material because of obvious change of modulus before and after phase change; however, pure phase-change materials such as paraffin can exhibit liquefaction after phase change, resulting in leakage of the material.
Based on the method, an olefin material with phase change characteristics is connected with side chain hydrogen-containing silicone oil to synthesize the silicone oil with phase change characteristics, and the synthesized silicone oil is used as a high molecular monomer to be crosslinked with other high molecular prepolymers such as dimethyl siloxane and the like through covalent bonds to jointly form a crosslinked network, so that a high molecular colloid with solid-solid phase change characteristics and obvious change of modulus is obtained; or the synthesized phase-change silicone oil and other silicone oil high polymer prepolymers capable of being crosslinked mutually by themselves are mixed and crosslinked to form a covalent bond network, and the phase-change silicone oil can be well locked by the covalent bond network of the crosslinked silicone oil according to the similar phase-change silicone oil structure and the crosslinked silicone oil structure, so that leakage is prevented. The uncrosslinked raw materials are uniformly mixed with high heat conduction filler according to different component ratios, and then are subjected to heating, curing and crosslinking treatment, so that the thermal interface material with solid-solid phase change characteristics, improved material modulus and improved interface compatibility can be obtained.
The application provides a phase change material matrix for preparing a thermal interface material, which comprises the following raw materials in parts by weight: 0.1 to 99.9 parts of olefin material, 0 to 99.9 parts of graftable polymer prepolymer, 0.1 to 99.9 parts of crosslinked polymer prepolymer and 0.1 to 1 part of catalyst.
The application also provides a preparation method of the phase change material matrix for preparing the thermal interface material, as shown in fig. 1 and 3, wherein the method comprises the following steps: uniformly mixing and stirring an olefin material, a graftable polymer prepolymer, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix for preparing a thermal interface material; in the method, after the olefin material is grafted with the grafted polymer prepolymer, the olefin material is crosslinked with the crosslinked polymer prepolymer to form a covalent bond network; or, after the olefin material is grafted with the grafted polymer prepolymer, the olefin material is dispersed in a covalent bond network formed by self-crosslinking of the crosslinked polymer prepolymer, and the green area in fig. 3 is the position where the grafted polymer prepolymer may be dispersed.
In the present application, as shown in fig. 1, the polymer prepolymer grafted with the olefin material reacts with the crosslinked polymer prepolymer to form a polymer crosslinked network, that is, the grafted polymer prepolymer is a part of the polymer crosslinked structure; in another form, the term "soluble" means that the grafting precursor is not crosslinked by reaction with the crosslinking precursor, and is dispersed in the form of a monomer solution in a polymer crosslinked network formed by crosslinking the crosslinked polymer precursor. The analogy here is that hydrogels, in which water is dispersed in the gel network, i.e. dissolved therein. The grafting precursor is dispersed in the crosslinked network, i.e., dissolved therein, as shown in the green region of FIG. 3.
The present application also provides a method for preparing the phase change material matrix for preparing the thermal interface material, as shown in fig. 2, which comprises: uniformly mixing and stirring an olefin material, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix which can be used for preparing a thermal interface material; wherein in the method the olefinic material is directly crosslinked with the crosslinked polymeric prepolymer.
The application also provides application of the phase change material matrix for preparing the thermal interface material in the field of preparing the thermal interface material.
The present application will be described in detail with reference to the following embodiments. In the following examples, the unit "part" is referred to, and "part by mass" unless otherwise indicated.
Example 1
(A) 4.4 parts by mass of side chain hydrogen-containing silicone oil and 11.6 parts of hexadecene are subjected to a progressive addition reaction to obtain 16 parts of grafted hexadecene side chain hydrogen-containing silicone oil, and the synthesis operation is a well-known part and is not repeated.
(B) 80 parts of heat-conducting filler, 16 parts of grafted hexadecene side chain hydrogen-containing silicone oil and 4 parts of polydimethylsiloxane prepolymer are added into a high-speed mixing stirrer to be stirred at normal temperature and high speed, and specific parameters can be set to 1000rpm for 60 seconds, 1200rpm for 45 seconds, 1500rpm for 30 seconds and 1800rpm for 15 seconds.
(C) After stirring well, chloroplatinic acid-divinyl tetramethyl disiloxane complex (0.1 part) was added.
(D) Stirring was continued at 1000rpm for 45 seconds, followed by 1200rpm for 30 seconds and 1500rpm for 15 seconds at 20℃vacuum-90.0 kPa.
(E) The mixture was taken out and rolled to different thicknesses.
(F) And (5) testing for standby after heating and curing.
Example 2
The procedure of example 1 was substantially identical, except that the parts of the synthetic material were changed to 80 parts by mass of the heat-conductive filler, 14 parts of the side-chain hydrogen silicone oil grafted with hexadecene (3.8 parts of side-chain hydrogen silicone oil, 10.2 parts of hexadecene), and 6 parts of the polydimethylsiloxane prepolymer.
Example 3
The procedure of example 1 was substantially identical, except that the parts of the synthetic material were changed to 80 parts by mass of the heat-conductive filler, 12 parts of the side-chain hydrogen silicone oil grafted with hexadecene (3.3 parts of side-chain hydrogen silicone oil, 8.7 parts of hexadecene), and 8 parts of the polydimethylsiloxane prepolymer.
Example 4
The procedure of example 1 was substantially identical, except that the parts of the synthetic material were changed to 80 parts by mass of the heat-conductive filler, 10 parts of the grafted hexadecene side chain hydrogen-containing silicone oil (2.7 parts of side chain hydrogen-containing silicone oil, 7.3 parts of hexadecene), and 10 parts of the polydimethylsiloxane prepolymer.
Comparative example 1
Substantially the same procedure as in example 1 was conducted, except that the parts of the synthetic material was changed to 80 parts by mass of the heat conductive filler and 20 parts by mass of the polydimethylsiloxane prepolymer.
(1) Thermal interface material conduction test:
the intrinsic thermal conductivity and the thermal contact resistance of the material are tested by using a Rayleigh thermal conductivity coefficient testing device (LW 9389). The test is in accordance with ASTM D5470, a standard which is a well known part and need not be described in detail herein.
Examples 1 to 4 and comparative example 1 were tested according to the above method, and the thermal conductivity and thermal contact resistance of the resulting thermal interface material were measured as shown in the following table:
(2) And (3) testing mechanical strength of the material:
the materials were tested at high and low temperatures (room temperature, 75 ℃) using a universal stretcher (Shimadzu, model AG-X plus 10N-10 kN). The testing method is a well-known part and need not be described here. The stretching rate was set at 3mm/min.
The tensile strength and elongation at break of examples 1 to 4 were tested according to the methods described above, and the test summary results are shown in the following table:
(3) Leak rate test:
the leakage rate is determined by setting the initial mass to M 0 Is carried out on a filter paper held in an oven at 60 ℃. After one hour, the sample was removed, weighed with an analytical balance, and the filter paper was replaced after each weighing. The mass of the sample after heating n times in an oven is defined as M n The material leakage rate is calculated according to the following formula:
L＝(M 0 -M n )/M 0 ×100％
| final leakage rate after 24 hours (%) | |
| Example 4 | 0.754 |
| Example 3 | 0.837 |
| Example 2 | 0.885 |
| Example 1 | 0.916 |
(4) Material modulus test:
and (3) testing the storage modulus of the material by adopting a dynamic thermal mechanical analyzer (DMA), wherein the testing temperature range is 0-80 ℃ and the heating rate is 2 ℃ per minute.
Further to the above-described changes in the temperature rise modulus according to the above-described method, examples 1 to 4 were tested, and the test results are summarized in the following table:
(5) As shown in FIG. 4, it can be seen from FIG. 4 that the olefin molecular chain undergoes phase change in situ after crosslinking by using an Olympic polarization microscope, and the olefin molecular chain is in a non-free state due to the limitation of covalent bonds, so that the olefin molecular chain does not undergo convergence and precipitation before and after phase change, and repeated heating and cooling operations prove the characteristics, thereby further proving that the polymer matrix has stable solid-solid phase change characteristics.
It will be understood by those of ordinary skill in the art that the foregoing embodiments are specific examples of carrying out the application and that various changes in form and details may be made therein without departing from the spirit and scope of the application. Various changes and modifications may be made by one skilled in the art without departing from the spirit and scope of the application, and the scope of the application is therefore intended to be limited only by the appended claims.
Claims (10)
1. A phase change material matrix useful for preparing a thermal interface material, comprising, in parts by weight: 0.1 to 99.9 parts of olefin material, 0 to 99.9 parts of graftable polymer prepolymer, 0.1 to 99.9 parts of crosslinked polymer prepolymer and 0.1 to 1 part of catalyst.
2. The phase change material matrix useful for preparing a thermal interface material according to claim 1, wherein the olefinic material is a hexadecene and/or octadecene material having phase change properties.
3. The phase change material matrix useful for preparing a thermal interface material according to claim 1, wherein the graftable polymer prepolymer is a hydrogen containing silicone oil capable of undergoing an addition reaction with an olefinic material.
4. The phase change material matrix useful for preparing a thermal interface material according to claim 1, wherein the crosslinked polymeric polymer is a polydimethylsiloxane prepolymer.
5. The phase change material matrix useful for preparing a thermal interface material according to claim 1, wherein the catalyst is selected from at least one of chloroplatinic acid, chloroplatinic acid-isopropanol complexes, chloroplatinic acid-divinyl tetramethyl disiloxane complexes.
6. A method of preparing a phase change material matrix useful for preparing a thermal interface material according to any one of claims 1 to 5, comprising:
uniformly mixing and stirring an olefin material, a graftable polymer prepolymer, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix for preparing a thermal interface material;
in the method, after the olefin material is grafted with the grafted polymer prepolymer, the olefin material is crosslinked with the crosslinked polymer prepolymer to form a covalent bond network;
or after grafting the olefin material and the graftable polymer prepolymer, dissolving the olefin material in the crosslinked polymer prepolymer for self crosslinking to form a covalent bond network.
7. The method for preparing a phase change material matrix useful for preparing a thermal interface material according to claim 6, wherein the polymer pre-polymer after grafting the olefin material exists in the matrix in the form of: crosslinking with other polymer prepolymers or dispersing in a polymer crosslinked network or both.
8. A method of preparing a phase change material matrix useful for preparing a thermal interface material according to any one of claims 1 to 5, comprising:
uniformly mixing and stirring an olefin material, a crosslinked polymer prepolymer and a catalyst to obtain a phase change material matrix which can be used for preparing a thermal interface material;
wherein in the method the olefinic material is directly crosslinked with the crosslinked polymeric prepolymer.
9. Use of a phase change material matrix according to any of claims 1 to 5 for the preparation of a thermal interface material in the field of the preparation of thermal interface materials.
10. The use of a phase change material matrix for the preparation of a thermal interface material according to any one of claims 1 to 5, wherein the thermal interface material has a thermal conductivity of 0.1W/mK to 100.0W/mK and a contact heat group of 10 -7 m 2 K/W～10 -4 m 2 K/W, modulus is in the range of 0.001 KPa-1000 MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310694942.3A CN116769311A (en) | 2023-06-13 | 2023-06-13 | Phase change material matrix for preparing thermal interface material, and preparation method and application thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310694942.3A CN116769311A (en) | 2023-06-13 | 2023-06-13 | Phase change material matrix for preparing thermal interface material, and preparation method and application thereof |
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| Country | Link |
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