CN115572439B - Aluminum-based flexible thermal interface material and preparation method and application thereof - Google Patents
Aluminum-based flexible thermal interface material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of heat conducting materials, in particular to an aluminum-based flexible thermal interface material, the heat-conducting material comprises a polymer of formula 1, ethylene propylene diene monomer rubber and a heat-conducting filler; the heat conducting filler comprises aluminum powder and metal oxide. The invention also provides the preparation and application of the material. The aluminum-based flexible thermal interface material of the invention, through the combination of the polymer of the formula 1, ethylene propylene diene monomer rubber and heat conducting filler, can realize cooperation, can improve its heat conductivility and flexibility, make it can effectively compromise good heat conduction and flexibility.
Description
Technical Field
The invention belongs to a thermal interface the technical field of the preparation of materials, in particular to an aluminum-based flexible thermal interface material.
Background
In recent years, with the rapid development of 5G and very large scale integrated circuits (VSLI), power consumption of electronic products is gradually increasing, and thermal management has been regarded as a key issue. Thermal management is typically achieved by removing excessive heat using a heat sink, however, perfect contact between the electronic chip and the heat sink is difficult to form, resulting in a large thermal resistance and reduced thermal diffusivity. To address this problem, some soft and deformable thermal interface materials are used to fill the gap between the electronic chip and the heat sink to improve heat transfer, keep the electronic chip within a suitable temperature range, improve the performance and lifetime of the electronic chip.
Polymers are commonly used as substrates for thermal interface materials due to their excellent insulating and mechanical properties. However, the intrinsic thermal conductivity of the polymer is very low<0.5W m -1 K -1 ) The requirements of the practical application of the thermal interface material cannot be met. Inorganic fillers having high thermal conductivity are thus widely used in combination with polymer matrices to improve their thermal conductivity.
The rapid development of emerging technologies places higher demands on thermal interface materials in order to be suitable for higher power as well as wearable electronics. At the same time as the thermal conductivity is high, new demands are placed on its flexibility. Because higher power and wearable electronics make warpage between the heat spreader and the chip due to different coefficients of thermal expansion and human activity more pronounced, the thermal interface material requires proper adhesion and excellent thermal conductivity and flexibility to enable the thermal interface material to accommodate the heat spreader and chip warpage. However, most of the current thermal interface materials are focused on the aspects of heat conduction performance, stability, reworkability and the like. This is because the thermal conductivity and flexibility of the thermal interface material are a pair of contradictors. The thermal conductivity of the thermal interface material can be increased by adding more thermally conductive filler content, but the thermal interface material tends to be less flexible due to the decreasing polymer matrix content.
Disclosure of Invention
The first aim of the invention is to provide an aluminum-based flexible thermal interface material, aiming at solving the problem that the heat conductivity and the flexibility of the existing interface material are difficult to be combined, so that the aluminum-based flexible thermal interface material is good in both flexibility and heat conductivity.
The second object of the invention is to provide a preparation method of the aluminum-based flexible thermal interface material.
The third object of the invention is to provide the application of the aluminum-based flexible thermal interface material.
An aluminum-based flexible thermal interface material comprises a polymer of formula 1, ethylene propylene diene monomer rubber and a heat conducting filler;
in the formula 1, the total molecular weight is 5000-8500; vinyl content 20-25%;
the heat conducting filler comprises aluminum powder and metal oxide.
According to the aluminum-based flexible thermal interface material, the cooperation can be realized through the combination of the polymer of the formula 1, the ethylene propylene diene monomer and the heat conducting filler, the heat conducting performance and the flexibility of the aluminum-based flexible thermal interface material can be improved, and the aluminum-based flexible thermal interface material can effectively take good heat conduction and flexibility into consideration.
In the invention, the polymer of formula 1 and ethylene propylene diene monomer are taken as matrixes, and the heat conducting filler is uniformly dispersed in the polymer matrixes. The research of the invention shows that the combination of the polymer of the formula 1 and the ethylene propylene diene monomer can realize synergy, can realize solidification under the condition of high filler addition, and can synchronously improve the heat conduction performance and the flexibility, so that the heat conduction performance and the flexibility are both excellent.
In the invention, in the formula 1, the single graft chain of the ester group
The molecular weight of the (C) is 1000-2500, and the vinyl content is 20-35%.
In the invention, the polymer of the formula 1 is obtained by esterification grafting reaction of a polymer of the formula 1-A and a polymer of the formula 1-B:
as preferable: the molecular weight of the polymer of the formula 1-A is 3000-3500, vinyl content is 20-35%; further preferably, the molecular weight of the polymer of formula 1-A is 3050-3150.
Preferably, the polymers of formula 1-B have a molecular weight of from 1000 to 2500 and a vinyl content of from 20 to 35%; it is further preferred that the polymer of formula 1-B has a molecular weight of 1450-1550.
Preferably, formula 1-A: the weight ratio of the formula 1-B is 0.5-1.5:0.5-1.5; further preferably 1 to 1.2:1. That is, the formula 1-A: the molar ratio of the formula 1-B is 1:1.5-2.5. The mole number is the weight of formula 1 or formula 2 divided by the total weight of each component.
In the invention, the ethylene propylene diene monomer rubber is at least one of T612 and T612A, A1016, and the thickening capacity is not less than (greater than or equal to) 5.5mm 2 s -1 。
Preferably, the ethylene propylene diene monomer rubber is T612A and A1016. Preferably, the weight ratio of T612A to A1016 is 1-2:1. According to the invention, the research shows that the ethylene propylene diene monomer rubber combined with the polymer of the formula 1 can be further cooperated unexpectedly, so that the interface material with better heat conduction and flexibility can be obtained.
In the heat-conducting filler, the metal oxide is at least one of aluminum oxide and zinc oxide;
in the invention, the following components are added: the grain diameter of the aluminum powder is 10-20 mu m; the particle size of the metal oxide is 10-500 nm. According to the invention, under the polymer system, the heat conduction particles and the grading of the particle size are further matched, so that the heat conduction and the flexibility of the interface material can be further improved by further cooperation.
In the invention, the heat conducting filler can be subjected to hydrophilic modification treatment in advance.
Preferably, the mass ratio of the aluminum powder to the metal oxide is 80-95:5-20; preferably 85-90:10-15; more preferably 4 to 7:1.
In the invention, the aluminum-based flexible thermal interface material has the polymer content of formula 1 of 0.5-6%; the content of the ethylene propylene diene monomer is 2-8%; the balance is heat conductive filler. Preferably, the content of the polymer of formula 1 is 0.5 to 1%; the content of ethylene propylene diene monomer is 4-6%; the balance is heat conductive filler. In the invention, due to the combination of the polymer network of the formula 1 and the ethylene propylene diene monomer, the interface material can be still formed by solidification under the condition of high heat conduction filler doping amount, and the flexibility and the heat conductivity can be synchronously improved.
In the invention, an auxiliary agent is also allowed to be added into the aluminum-based flexible thermal interface material, wherein the auxiliary agent is one of antioxidants BHT264, 1035 and EDTA disodium;
preferably, the content of the auxiliary agent is less than or equal to 0.2%, preferably 0.01-0.05%.
The invention also provides a preparation method of the aluminum-based flexible thermal interface material, which is obtained by mixing the components.
For example, the polymer of the formula 1, ethylene propylene diene monomer rubber, a heat-conducting filler and optionally an additive are mixed.
Another preferred preparation scheme of the invention: gradient mixing the polymer of formula 1-A, the polymer of formula 1-B, the heat conducting filler and the antioxidant in a high-speed mixer, and then continuously carrying out gradient mixing under negative pressure to obtain a mixture;
uniformly coating the mixture in a release film, uniformly calendaring, and curing at 140-160 ℃ to obtain an aluminum-based flexible thermal interface material;
preferably, the rotating speed of each section in the gradient mixing process is 750-850 rpm, 950-1050 rpm, 1150-1250 rpm, 1450-1550 rpm and 1750-1850 rpm respectively;
preferably, the temperature of the gradient mixing stage is 10-60 ℃;
the treatment time of each section is 2-5 min;
preferably, the curing time is 1 to 3 hours.
The invention relates to a preparation method of a more specific aluminum-based flexible thermal interface material, which comprises the following steps:
step one
Taking the formula 1-A, the formula 1-B, ethylene propylene diene monomer rubber, an antioxidant and a heat conducting filler according to the designed components; the dispensed material is first added to a high speed mixer. Setting rotational speed gradient mixing stirring at 800rpm, 1000rpm, 1200rpm, 1500rpm and 1800rpm for 2.45min each time; heating and stirring at 10-60deg.C for 2.45min, preferably 20-30deg.C.
Step two
Firstly, placing the sample prepared in the first step into a high-speed mixer, and continuously stirring under a vacuum condition to obtain a prepolymer; when vacuum stirring is carried out, the temperature is controlled to be 20-60 ℃.
Step three
The polymer is coated in a release film, uniformly calendered by a double-roller gate, cured for 2 hours at 150 ℃ to obtain the aluminum-based flexible thermal interface material, and can be stored at room temperature. Preferably, in the third step, the prepolymer prepared in the second step is coated between two release films, the obtained sample is uniformly rolled through a double-roller gate with the set thickness of 0.5-2mm, preferably 1mm, the rolled sample is solidified for 2 hours at 150 ℃, and the aluminium-based flexible thermal interface material is obtained after being taken out and cooled.
The invention also provides application of the aluminum-based flexible thermal interface material as a heat dissipation material for preparing at least one of electronic devices, wearing equipment and battery packs.
The application of the invention, for example, the material is applied to the heat dissipation of the electronic device, so that the heat generated by the operation of the electronic device is conducted out as soon as possible, and the influence of heat accumulation on the service life and the working efficiency of the instrument is avoided. Or the material is applied to heat dissipation of the flexible wearable equipment, and the low modulus enables the flexible wearable equipment to have better flexibility, so that the flexible wearable equipment can be better attached to the surface curve of a human body, and the negative influence of the working temperature of the wearable equipment on the human body is avoided. Or the material is applied to the thermal management of the battery pack, so that the internal temperature uniformity of the battery pack is improved, the battery pack works in an optimal temperature range, and the working efficiency and the stability are improved.
Principle and advantages
The invention provides a brand new aluminum-based flexible thermal interface material, which is prepared by combining the polymer of formula 1 and ethylene propylene diene monomer rubber as a substrate and combining with the combined control of a heat conducting filler, so that the synergy can be realized, the problem that the filler is difficult to cure due to large addition can be solved, and the heat conducting property and the flexibility of the material can be synchronously and effectively improved.
According to the invention, according to the hydrogel principle, ethylene propylene diene monomer rubber is used for replacing water of the traditional hydrogel, organic gel is constructed, a polymer network of formula 1 and aluminum-containing filler such as aluminum powder are added into the organic gel, a heat conduction path is constructed through the aluminum powder with high filler content, the heat conduction performance of the material is improved, and the flexibility of the material is improved through a polymer matrix and the organic gel. By changing the content of the filler and the polymer, the adjustable heat conducting property and mechanical property are realized.
According to the invention, the aluminum-based thermal interface material with adjustable heat conducting property and mechanical property is prepared by synthesizing the heat conducting filler-polymer matrix-organic gel composite materials with different mass ratios and regulating and controlling the heat conducting property and mechanical property of the composite materials. In the invention, polybutadiene added with maleic anhydride and hydroxyl-terminated polybutadiene are reacted to form a polymer network, so that the mechanical property of a matrix is provided; the proportion of the polymer network in the whole is regulated by ethylene propylene diene monomer, so that the material has the property of hydrogel, and the mechanical property of a polymer matrix is regulated, thereby realizing the regulation from hard to soft. Finally, the heat conducting property is greatly regulated and controlled by the addition amount of the heat conducting filler, so that the requirements of more occasions are met. Meanwhile, the invention can greatly regulate and control the heat conduction and mechanical properties by selecting a small amount of polymers, and has simple process, thereby providing necessary conditions for reducing the application cost.
In conclusion, the processing technology is simple, and the heat conduction and mechanical properties of the material can be regulated and controlled; effectively improves the comprehensive capacity and meets the use requirements of more occasions.
Drawings
FIG. 1 is a graph of the thermal conductivity of the finished products obtained in examples 1-4;
FIG. 2 is a graph showing the thermal conductivity of the finished products obtained in comparative examples 1-5;
FIG. 3 is a graph of Young's modulus of the final products obtained in examples 1-4;
FIG. 4 is a graph showing Young's modulus of the final products obtained in comparative examples 1 and 2;
Detailed Description
The following examples are provided to further illustrate the invention and are not intended to limit the invention. The invention may be embodied in any of the ways described in the summary of the invention.
Formula 1-A: HTPB (Poly bd R45V) was purchased from Soda corporation, japan.
Formula 1-B: MLPB (Ricon 130MA 8) was purchased from French Cray Valley Hydrocarbon Specialty Chemicals.
Ethylene propylene diene monomer rubber (A-1016, T612) was purchased from Peng petroleum additive Inc. in Hongze, china.
The antioxidant is antioxidant BHT264.
The grain diameter of the aluminum powder is 10-20 mu m; the particle size of the metal oxide is 10-500 nm.
Measurement method of thermal conductivity and flexibility and test standard:
(1) And (3) heat conduction coefficient test:
the standard test method for measuring the heat conduction in the vertical direction by a steady state method comprises the following specific steps of: placing the thermal interface composite material between the instrument bars, and establishing stable heat flow through the assembly; then monitoring the temperature in the meter bar at two or more locations along its length; the temperature difference across the interface is calculated from the temperature readings obtained and used to determine the thermal conductivity of the interface.
(2) Flexible test
The flexibility of the sample is reflected by Young's modulus, and the tensile property of the thermal interface composite material is tested by using an Shimadzu universal electronic tester AGX-10 kNVD. Test conditions and parameters: the temperature was 25℃and the stretching speed was 5mm/min. The test sample is to cut the thermal interface composite material into 50mm lengths respectively, carry out a tensile experiment on the composite material, record stress-strain curves of the composite material, and obtain the slope of the stress-strain curves as Young's modulus.
Example 1:
a maleic anhydride-added polybutadiene (MLPB; 0.16 g) having a molecular weight of 3100 and a vinyl content of 20-35%, a hydroxyl-terminated polybutadiene (HTPB; 0.14 g) having a molecular weight of 1500 and a vinyl content of 20%, an ethylene propylene diene monomer T612A (2.7 g), aluminum (38.39 g), zinc oxide (8.55 g) and an antioxidant (0.02 g) were fed into a high-speed mixer. The rotational speed gradient mixing stirring at 800rpm, 1000rpm, 1200rpm, 1500rpm, 1800rpm was set twice, each for 2.45min. Stirring was continued for 2.45min at 20℃under vacuum-90.0 kPa at the same rotational speed gradient. And uniformly coating the mixture in a release film, curing for 2 hours at 150 ℃ to obtain the high-heat-conductivity flexible thermal interface material, and storing at room temperature.
Example 2:
a maleic anhydride-added polybutadiene (0.16 g) having a molecular weight of 3100 and a vinyl content of 20 to 35%, a hydroxyl-terminated polybutadiene (0.14 g) having a molecular weight of 1500 and a vinyl content of 20%, an ethylene propylene diene monomer A1016 (2.7 g), aluminum (40.39 g), zinc oxide (6.55 g) and an antioxidant (0.02 g) were added to a high-speed mixer. The rotational speed gradient mixing stirring at 800rpm, 1000rpm, 1200rpm, 1500rpm, 1800rpm was set twice, each for 2.45min. Stirring was continued for 2.45min at 20℃under vacuum-90.0 kPa at the same rotational speed gradient. And uniformly coating the mixture in a release film, curing for 2 hours at 150 ℃ to obtain the high-heat-conductivity flexible thermal interface material, and storing at room temperature.
Example 3:
a maleic anhydride-added polybutadiene (0.16 g) having a molecular weight of 3100 and a vinyl content of 20 to 35%, a hydroxyl-terminated polybutadiene (0.14 g) having a molecular weight of 1500 and a vinyl content of 20%, an ethylene propylene diene monomer rubber T612 (1.35 g), A1016 (1.35 g), aluminum (40.39 g), zinc oxide (6.55 g) and an antioxidant (0.02 g) were added to a high-speed mixer. The rotational speed gradient mixing stirring at 800rpm, 1000rpm, 1200rpm, 1500rpm, 1800rpm was set twice, each for 2.45min. Stirring was continued for 2.45min at 20℃under vacuum-90.0 kPa at the same rotational speed gradient. And uniformly coating the mixture in a release film, curing for 2 hours at 150 ℃ to obtain the high-heat-conductivity flexible thermal interface material, and storing at room temperature.
Example 4:
a maleic anhydride-added polybutadiene (0.3 g) having a molecular weight of 3100 and a vinyl content of 20 to 35%, a hydroxyl-terminated polybutadiene (0.3 g) having a molecular weight of 1500 and a vinyl content of 20%, an ethylene propylene diene monomer A1016 (2.4 g), aluminum (40.39 g), zinc oxide (6.55 g) and an antioxidant (0.02 g) were added to a high-speed mixer. The rotational speed gradient mixing stirring at 800rpm, 1000rpm, 1200rpm, 1500rpm, 1800rpm was set twice, each for 2.45min. Stirring was continued for 2.45min at 20℃under vacuum-90.0 kPa at the same rotational speed gradient. And uniformly coating the mixture in a release film, curing for 2 hours at 150 ℃ to obtain the high-heat-conductivity flexible thermal interface material, and storing at room temperature.
Comparative example 1:
substantially the same as in example 2, except that the amount of the heat conductive filler added was halved, that is, the different heat conductive fillers include aluminum and zinc oxide in amounts of 20.20g and 3.3g, respectively.
Comparative example 2
The same formulation as in example 2 was used except that no ethylene propylene diene monomer was added and the mass fraction was filled with the same ratio of polybutadiene-added maleic anhydride to hydroxyl-terminated polybutadiene, i.e., maleic anhydride-added polybutadiene (1.6 g, hydroxyl-terminated polybutadiene (1.4 g), other operations and parameters were the same as in example 2.
Comparative example 3
The same formulation as in example 1 was used except that no MLPB and HTPB were added, and the contents of both were filled with ethylene propylene diene monomer a1016, i.e., the amount of ethylene propylene diene monomer a1016 added was 3g, and other operations and parameters were the same as in example 2.
Comparative example 4
The formulation of example 1 was identical except that no MLPB was added and the weight was filled with HTPB, i.e., HTPB was added and pulled in to 0.3g, with the other operations and parameters being the same as in example 2.
Comparative example 5
The formulation of example 1 was identical except that no HTPB was added and the weight was filled with MLPB, i.e., 0.3g of MLPB was added, and the other operations and parameters were the same as in example 2.
Test results:
as is clear from a comparison of example 2 and comparative examples 1 to 3, the combination of MLPB and HTPB can be used to polymerize the polymer of formula 1, and the combination of the polymer with the ethylene propylene diene monomer and the filler can realize synergy, and a material having both good thermal conductivity and flexibility can be obtained. In addition, based on comparison of the embodiment 2 and the embodiment 3, on the basis of the combination of the MLPB and HTPB combined polymerization and the ethylene propylene diene monomer, further combined ethylene propylene diene monomer (such as T612 and A1016 combined) can further realize synergy, and further improve the heat conduction performance and the flexibility of the interface material. It is also evident from a comparison of example 2 and comparative examples 3 to 5 that the single MLPB and HTPB cannot be polymerized to form the polymer of formula 1, which affects the effect of combining the ethylene propylene diene monomer and the filler, and affects the heat conduction of the interface material, and that comparative examples 3, 4 and 5 cannot be cured and molded, and remain liquid all the time, so that the Young's modulus cannot be obtained.
Claims (19)
1. An aluminum-based flexible thermal interface material, characterized in that: comprises a polymer of formula 1, ethylene propylene diene monomer rubber and a heat-conducting filler;
In the formula 1, the total molecular weight is 5000-8500, and the vinyl content is 20-25%;
the polymer of the formula 1 is obtained through an esterification grafting reaction of a polymer A and a polymer B, wherein the polymer A is an MLPB polymer with the brand of Ricon 130MA 8;
the polymer B is HTPB polymer with the brand of Polybd R45V;
the heat conducting filler comprises aluminum powder and metal oxide.
2. The aluminum-based flexible thermal interface material of claim 1, wherein: polymer A: the weight ratio of the polymer B is 0.5-1.5:0.5-1.5.
3. The aluminum-based flexible thermal interface material of claim 2, wherein: polymer A: the weight ratio of the polymer B is 1-1.2:1.
4. The aluminum-based flexible thermal interface material of claim 1, wherein: the ethylene propylene diene monomer is at least one of T612 and T612A, A1016, and the thickening capacity is not less than 5.5mm 2 s -1 。
5. The aluminum-based flexible thermal interface material of claim 4, wherein: the ethylene propylene diene monomer rubber is T612A and A1016.
6. The aluminum-based flexible thermal interface material of claim 5, wherein: in the ethylene propylene diene monomer, the weight ratio of T612A to A1016 is 1-2:1.
7. The aluminum-based flexible thermal interface material of claim 1, wherein: in the heat conducting filler, the metal oxide is at least one of aluminum oxide and zinc oxide.
8. The aluminum-based flexible thermal interface material of claim 7, wherein: the mass ratio of the aluminum powder to the metal oxide is 80-95:5-20.
9. The aluminum-based flexible thermal interface material of claim 8, wherein: the particle size of the aluminum powder is 10-20 mu m; the particle size of the metal oxide is 10-500 nm.
10. The aluminum-based flexible thermal interface material of any of claims 1-9, wherein: the content of the polymer in the formula 1 is 0.5-6%; the content of ethylene propylene diene monomer is 2-8%; the balance is heat conductive filler.
11. The aluminum-based flexible thermal interface material of claim 10, wherein: an auxiliary agent is also added, and the auxiliary agent is one of antioxidant BHT264, antioxidant 1035 and EDTA disodium.
12. The aluminum-based flexible thermal interface material of claim 11, wherein: the content of the auxiliary agent is less than or equal to 0.2 percent.
13. The aluminum-based flexible thermal interface material of claim 12, wherein: the content of the auxiliary agent is 0.01-0.05%.
14. A method for preparing the aluminum-based flexible thermal interface material according to any one of claims 1 to 13, which is characterized in that: mixing the above materials.
15. A method for preparing the aluminum-based flexible thermal interface material according to any one of claims 1 to 9, which is characterized in that: the polymer A, the polymer B, the ethylene propylene diene monomer rubber, the heat conducting filler and the antioxidant are mixed in a gradient manner in a high-speed mixer, and then the gradient mixing is carried out continuously under negative pressure to obtain a mixture;
and uniformly coating the mixture in a release film, uniformly calendaring, and curing at 140-160 ℃ to obtain the aluminum-based flexible thermal interface material.
16. The method of preparing an aluminum-based flexible thermal interface material of claim 15, wherein: the rotating speeds of the sections in the gradient mixing process are 750-850 rpm, 950-1050 rpm, 1150-1250 rpm, 1450-1550 rpm and 1750-1850 rpm respectively.
17. The method of preparing an aluminum-based flexible thermal interface material of claim 16, wherein: the temperature of the gradient mixing stage is 10-60 ℃;
the treatment time of each section is 2-5 min.
18. The method of preparing an aluminum-based flexible thermal interface material of claim 16, wherein: the curing time is 1-3 h.
19. Use of the aluminum-based flexible thermal interface material according to any one of claims 1 to 13, characterized in that: the heat dissipation material is used as a heat dissipation material for preparing at least one of electronic devices, wearable equipment and battery packs.
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| US6238596B1 (en) * | 1999-03-09 | 2001-05-29 | Johnson Matthey Electronics, Inc. | Compliant and crosslinkable thermal interface materials |
| US20060228542A1 (en) * | 2005-04-08 | 2006-10-12 | Saint-Gobain Performance Plastics Corporation | Thermal interface material having spheroidal particulate filler |
| CN106433035B (en) * | 2016-10-18 | 2018-11-20 | 中国科学院深圳先进技术研究院 | A kind of hot interface composites of aluminum-based filler and the preparation method and application thereof |
| CN112679798B (en) * | 2020-12-10 | 2023-04-18 | 中国科学院深圳先进技术研究院 | Polyolefin-based graphite oriented thermal interface material and preparation method thereof |
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