CN112778562A - Efficient heat-conducting interface material and preparation method and application thereof - Google Patents
Efficient heat-conducting interface material and preparation method and application thereof Download PDFInfo
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- CN112778562A CN112778562A CN202011627598.9A CN202011627598A CN112778562A CN 112778562 A CN112778562 A CN 112778562A CN 202011627598 A CN202011627598 A CN 202011627598A CN 112778562 A CN112778562 A CN 112778562A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D123/00—Coating compositions based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Coating compositions based on derivatives of such polymers
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
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Abstract
The invention provides a heat-conducting interface material, which has a layered structure; includes a first resin layer; the heat conducting film layer is compounded on the first resin layer; and the second resin layer is compounded on the heat conduction film layer. According to the invention, the high-thermal-conductivity film layer is compounded on the middle layer of the thermal-conductivity resin gasket, and thermal-conductivity filler is used, so that vertical thermal conductivity is ensured, and horizontal soaking can be carried out, and the highest comprehensive thermal conductivity can reach 50w/mk under the condition that the hardness is less than 60 degrees of shore oo. The heat-conducting interface material provided by the invention can be widely applied to the field of electronics/automobiles, and with the development of household appliances/automobiles towards the direction of high power, light weight and small volume of chips/batteries, the appearance of the heat-conducting interface material represents the future development direction, and an effective heat treatment scheme is provided for the intelligent development of automobile electronics.
Description
Technical Field
The invention belongs to the technical field of heat-conducting interface materials, relates to a heat-conducting interface material, and a preparation method and application thereof, and particularly relates to a high-efficiency heat-conducting interface material, and a preparation method and application thereof.
Background
With the rapid development of modern electronic technology, the integration degree and the assembly density of electronic components are continuously improved, and the working power consumption and the heat productivity of the electronic components are increased sharply while providing strong use functions. High temperatures can have detrimental effects on the stability, reliability and lifetime of electronic components, such as excessive temperatures that can compromise semiconductor junctions, damage the circuit connection interfaces, increase the resistance of the conductors and cause mechanical stress damage. Therefore, ensuring that the heat generated by the heat-generating electronic components can be discharged in time has become an important aspect of the system assembly of microelectronic products. For portable electronic products (such as notebook computers) with high integration degree and assembly density, heat dissipation even becomes a technical bottleneck problem of the whole product. Thermal interface (interface) materials play a very critical role in thermal management, and are an important research branch in heat conduction. The use principle is as follows: there are very fine asperity gaps between the microelectronic material surface and the heat sink, and if they are mounted directly together, the actual contact area between them is only about 10% of the area of the heat sink base, and the rest is air gaps. Air is a poor thermal conductor, which causes a very large thermal contact resistance between the electronic component and the heat sink, seriously hampering the heat conduction, and finally causing the low efficiency of the heat sink. Therefore, the gaps are filled with the thermal interface material with high thermal conductivity, air in the gaps is removed, an effective heat conduction channel is established between the electronic element and the radiator, the contact thermal resistance can be greatly reduced, the effect of the radiator is fully exerted, the electronic device can work in a proper temperature range, and the normal performance of the electronic device is ensured.
A heat-conducting interface material, also called an interface heat-conducting material, is a heat-conducting material acting between a heating device and a heat sink, and is commonly used for IC packaging and electronic heat dissipation. The heat-conducting interface material seamlessly butts the surface of the heating device and the radiator through the elasticity and flexibility of the heat-conducting interface material, so that micro gaps and uneven surfaces generated when the two materials are contacted are filled, the thermal resistance is reduced, efficient heat dissipation is realized, and the heat dissipation performance of the device is improved. The traditional heat-conducting interface material is usually silicone resin, acrylic resin or polyurethane resin, and heat-conducting fillers, curing agents and other auxiliaries are added into the silicone resin, acrylic resin or polyurethane resin, and the soft heat-conducting gasket/gel/phase change and other heat interface materials are formed through heating and curing, so that heat transfer between a heating surface and a radiator is realized. However, with the continuous increase of the computing power and power consumption of devices, higher requirements are put forward on heat-conducting interface materials in the field, and the heat conductivity coefficient of conventional heat-conducting interface materials in the current market can only reach 10w/mk at most, even if some heat-conducting interface materials appearing in the market include two major mainstream products of foreign manufacturers (Fuji poly, denka, hangao, laird and the like) and domestic manufacturers (ternary electronics, hongfucheng, medium stone and the like), the heat-conducting interface materials also generally exist: the heat conduction power is not enough under the flexible condition of shore oo below 60 degrees, the quality such as poor environmental weatherability is poor, and the increasing heat treatment requirements of intelligent products cannot be met.
Therefore, how to find a more suitable thermal interface material, which has both a flexible property satisfying the condition and a higher thermal conductivity coefficient, has become one of the problems to be solved by many researchers in the field.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a thermal interface material, a preparation method and an application thereof, and particularly to a high efficiency thermal interface material. The heat-conducting interface material prepared by the company can be uniformly heated in the horizontal direction while ensuring vertical heat conduction, has the highest comprehensive heat-conducting property of 50w/mk under the condition that the hardness is less than shore oo60 degrees, and has excellent heat-conducting property.
The invention provides a heat-conducting interface material, which has a layered structure;
includes a first resin layer;
the heat conducting film layer is compounded on the first resin layer;
and the second resin layer is compounded on the heat conduction film layer.
Preferably, the first resin layer includes one or more of a silicone resin layer, an acrylic resin layer, and a urethane resin layer;
the thickness of the first resin layer is 0.1-10 mm;
the second resin layer comprises one or more of a silicone resin layer, an acrylic resin layer and a polyurethane resin layer;
the thickness of the second resin layer is 0.1-10 mm.
Preferably, the heat conducting film layer comprises a heat conducting nitride film layer and/or a heat conducting carbon film layer;
the material of the heat conducting film layer comprises one or more of graphene, aluminum nitride, metal and boron nitride;
the thickness of the heat conducting film layer is 0.1-100 mu m;
the form of the heat-conducting interface material comprises a heat-conducting adhesive material, a heat-conducting gel material, a heat-conducting resin material or a heat-conducting gasket;
the thermally conductive interface material has a shore00 hardness of 60 ° or less.
Preferably, the resin layer comprises the following raw materials in percentage by mass:
2-20 parts by weight of resin and a curing agent;
50-95 parts by weight of a heat conductive filler;
0.1-5 parts by weight of an auxiliary agent;
the heat-conducting interface material is a heat-conducting material used between the heating device and the heat sink.
Preferably, the addition amount of the curing agent is that the molar weight of resin reaction groups consumed by the curing agent is 0.3-0.8 of the molar weight of the total resin reaction groups;
the thermally conductive filler comprises one or more of alumina, boron nitride, and silicon nitride;
the auxiliary agent comprises a dispersing agent;
the dispersant comprises dispersant triton and/or dispersant peg;
the heat-conducting interface material is used for electronic products and/or automobiles.
The invention provides a preparation method of a heat-conducting interface material, which comprises the following steps:
1) mixing the resin, the curing agent and the auxiliary agent, and then adding the heat-conducting filler for vacuum mixing to obtain a semi-finished heat-conducting glue;
2) forming and curing the semi-finished product of the heat-conducting glue obtained in the step to obtain a heat-conducting gasket;
3) and compounding a heat conduction film on the surface of the heat conduction gasket obtained in the step, coating the heat conduction adhesive semi-finished product obtained in the step on the heat conduction film, and curing to obtain the heat conduction interface material.
Preferably, the viscosity of the mixed solution is 1000-10000 pas;
the vacuum mixing method for adding the heat-conducting filler comprises the following specific steps:
adding the heat-conducting filler for vacuum mixing for multiple times, vacuumizing, and adding the heat-conducting filler again for vacuum mixing:
the temperature of the vacuum mixing is 20-200 ℃;
the single time of the vacuum mixing is 1-200 min;
the vacuum degree of the vacuum mixing is less than or equal to 0.2 Pa.
Preferably, the times of the multiple times are 2-5 times;
the viscosity of the viscous liquid after the heat-conducting filler is added for the first time and vacuum mixing is carried out is 1000-30000 pas;
heating for vacuum defoaming after the vacuum mixing;
the temperature after heating is 20-100 ℃;
and the vacuum defoaming time is 1-200 min.
Preferably, the viscosity of the semi-finished product of the heat-conducting glue is 100000-300000 pas;
the forming mode comprises film forming;
the thickness of the coating formed by coating is 0.1-10 mm;
the curing temperature in the step 2) and the curing temperature in the step 3) are respectively 100-200 ℃;
the curing time in the step 2) and the step 3) is 2-100 min respectively;
the mode of the composite heat-conducting film comprises vacuum coating.
The invention provides application of the heat-conducting interface material prepared by any one of the above technical schemes or the heat-conducting interface material prepared by the preparation method of any one of the above technical schemes in the fields of electronic products and/or automobiles.
The invention provides a heat-conducting interface material, which has a layered structure; includes a first resin layer; the heat conducting film layer is compounded on the first resin layer; and the second resin layer is compounded on the heat conduction film layer. Compared with the prior art, the invention aims at the problem that the heat-conducting property of the existing heat-conducting interface material can not meet the requirement, and even a product with slightly high heat-conducting property is ubiquitous: and the defects of insufficient heat conduction power, poor environmental weather resistance and the like under the flexible condition of ensuring that the Shore oo is below 60 degrees are limited.
The research of the invention considers that the heat conducting interface material in the conventional technology can only realize vertical heat transfer, and the heat conducting particles in the horizontal direction are basically not contacted and do not contribute to the heat transfer. The invention provides a heat-conducting interface material with a specific composite layer structure, which comprises a three-layer structure, wherein a high-efficiency heat-conducting film layer is compounded between resin layers. According to the invention, the high-thermal-conductivity film layer is compounded on the middle layer of the thermal-conductivity resin gasket, and thermal-conductivity filler is used, so that vertical thermal conductivity is ensured, and horizontal soaking can be carried out, and the highest comprehensive thermal conductivity can reach 50w/mk under the condition that the hardness is less than 60 degrees of shore oo.
The invention further prepares the heat-conducting rubber material by the curing agent and the resin in a specific proportion, so that the hardness of the heat-conducting rubber material can still be ensured within 60 degrees of shore oo after the heat-conducting filler is added, and the comprehensive heat-conducting property is excellent. The novel heat-conducting interface material provided by the invention can be widely applied to the field of electronics/automobiles, and with the development of household appliances/automobiles towards the direction of high power, light weight and small size of chips/batteries, the appearance of the heat-conducting interface material represents the future development direction, and an effective heat treatment scheme is provided for the intelligent development of automobile electronics.
The experimental results show that: the heat conductivity coefficient of the heat-conducting glue and the gasket made of the material can reach 50w/mk to the maximum, the hardness is less than shore oo60 degrees, the strength is higher than 1Mpa, and the loss of each performance is within 10 percent after double 85 testing for 1000 hours.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
All of the starting materials of the present invention, without particular limitation as to their source, may be purchased commercially or prepared according to conventional methods well known to those skilled in the art.
All of the starting materials of the present invention are not particularly limited in their purity, and the present invention preferably employs the purity conventionally employed in the art of analytically pure or thermally conductive interface materials.
The invention provides a heat-conducting interface material, which has a layered structure;
includes a first resin layer;
the heat conducting film layer is compounded on the first resin layer;
and the second resin layer is compounded on the heat conduction film layer.
The heat-conducting interface material has a layered structure and comprises a first resin layer.
In the present invention, the first resin layer preferably includes one or more of a silicone resin layer, an acrylic resin layer, and a urethane resin layer, and more preferably a silicone resin layer, an acrylic resin layer, or a urethane resin layer.
In the present invention, the thickness of the first resin layer is preferably 0.1 to 10mm, more preferably 0.5 to 8mm, more preferably 1 to 6mm, and more preferably 2 to 5 mm.
The heat-conducting interface material comprises a heat-conducting film layer compounded on the first resin layer.
In the present invention, the heat conducting film layer preferably includes a heat conducting nitride film layer and/or a heat conducting carbon film layer, and more preferably includes a heat conducting nitride film layer or a heat conducting carbon film layer.
In the present invention, the material of the heat conducting film layer preferably includes one or more of graphene, aluminum nitride, metal and boron nitride, more preferably graphene, aluminum nitride, metal or boron nitride, and more preferably graphene, aluminum nitride, silver or boron nitride.
In the invention, the thickness of the heat conducting film layer is preferably 0.1-100 μm, more preferably 1-50 μm, more preferably 5-40 μm, and more preferably 15-30 μm.
The heat-conducting interface material also comprises a second resin layer compounded on the heat-conducting film layer.
In the present invention, the second resin layer preferably includes one or more of a silicone resin layer, an acrylic resin layer, and a urethane resin layer, and more preferably a silicone resin layer, an acrylic resin layer, or a urethane resin layer.
In the present invention, the thickness of the second resin layer is preferably 0.1 to 10mm, more preferably 0.5 to 8mm, more preferably 1 to 6mm, and more preferably 2 to 5 mm.
In the present invention, the form of the thermal interface material preferably includes a thermal conductive adhesive material, a thermal conductive gel material, a thermal conductive resin material, or a thermal conductive gasket.
In the present invention, the heat conductive interface material is preferably a heat conductive material used between the heat generating device and the heat sink.
In the present invention, the shore00 hardness of the thermal interface material is preferably 60 ° or less.
In the present invention, the thermal interface material is preferably a thermal interface material for electronic products and/or automobiles, and more preferably a thermal interface material for electronic products or automobiles.
According to the heat-conducting interface material, the resin layer preferably comprises the following raw materials in percentage by mass:
2-20 parts by weight of resin and a curing agent;
50-95 parts by weight of a heat conductive filler;
0.1-5 parts by weight of an auxiliary agent.
In the present invention, the resin and the curing agent are preferably added in an amount of 2 to 20 parts by weight, more preferably 6 to 16 parts by weight, and still more preferably 10 to 12 parts by weight. The addition amount of the heat-conducting filler is preferably 50 to 95 parts by weight, more preferably 60 to 85 parts by weight, and still more preferably 70 to 75 parts by weight. The addition amount of the auxiliary agent is preferably 0.1-5 parts by weight, more preferably 1-4 parts by weight, and more preferably 2-3 parts by weight.
In the invention, the addition amount of the curing agent is preferably 0.3 to 0.8, more preferably 0.4 to 0.7, and more preferably 0.5 to 0.6 of the molar amount of the resin reaction groups consumed by the curing agent based on the total molar amount of the resin reaction groups.
In the present invention, the thermally conductive filler preferably includes one or more of alumina, boron nitride, and silicon nitride, and more preferably alumina, boron nitride, or silicon nitride.
In the present invention, the auxiliary agent preferably comprises a dispersant, more specifically, the dispersant preferably comprises a dispersant triton and/or a dispersant peg, more preferably a dispersant triton or a dispersant peg.
The invention provides a preparation method of a heat-conducting interface material, which preferably comprises the following steps:
1) mixing the resin, the curing agent and the auxiliary agent, and then adding the heat-conducting filler for vacuum mixing to obtain a semi-finished heat-conducting glue;
2) forming and curing the semi-finished product of the heat-conducting glue obtained in the step to obtain a heat-conducting gasket;
3) and compounding a heat conduction film on the surface of the heat conduction gasket obtained in the step, coating the heat conduction adhesive semi-finished product obtained in the step on the heat conduction film, and curing to obtain the heat conduction interface material.
In the present invention, parameters, selections and compositions of the raw materials, processes and synthesized products required in the preparation process of the thermal interface material, and corresponding preferred principles, may correspond to parameters, selections and compositions of the raw materials, processes and synthesized products corresponding to the thermal interface material in the application, and corresponding preferred principles, and are not described in detail herein.
Firstly, mixing resin, a curing agent and an auxiliary agent, and then adding a heat-conducting filler for vacuum mixing to obtain a semi-finished product of the heat-conducting glue.
In the invention, the viscosity of the mixed liquid is preferably 1000-10000 pas, more preferably 3000-8000 pas, and more preferably 5000-6000 pas.
In the present invention, the specific steps of adding the heat conductive filler and vacuum mixing are preferably as follows:
and adding the heat-conducting filler for vacuum mixing for multiple times, vacuumizing, and adding the heat-conducting filler again for vacuum mixing.
In the invention, the temperature of the vacuum mixing is preferably 20-200 ℃, more preferably 60-160 ℃, and more preferably 100-120 ℃.
In the invention, the single time of the vacuum mixing is preferably 1-200 min, more preferably 40-160 min, and more preferably 80-120 min.
In the present invention, the degree of vacuum in the vacuum kneading is preferably 0.2Pa or less.
In the invention, the number of times of the multiple times is preferably 2-5 times, more preferably 2.5-4.5 times, and more preferably 3-4 times.
In the invention, the viscosity of the viscous liquid after the first addition of the heat-conducting filler and the vacuum mixing is preferably 1000-30000pas, more preferably 6000-25000 pas, and more preferably 11000-20000 pas.
In the present invention, the vacuum kneading preferably includes a step of heating to defoam in vacuum.
In the invention, the temperature after heating is preferably 20-100 ℃, more preferably 30-90 ℃, more preferably 40-80 ℃, and more preferably 50-70 ℃.
In the invention, the time for vacuum defoaming is preferably 1-200 min, more preferably 40-160 min, and more preferably 80-120 min.
In the invention, the viscosity of the semi-finished product of the heat-conducting glue is preferably 100000-300000 pas, more preferably 140000-260000 pas, and more preferably 180000-220000 pas.
The heat-conducting gasket is obtained by molding and curing the semi-finished product of the heat-conducting adhesive obtained in the step.
In the present invention, the molding preferably includes film molding.
In the invention, the thickness of the coating formed by coating is preferably 0.1-10 mm, more preferably 2-8 mm, and more preferably 4-6 mm.
In the invention, the curing temperature is preferably 100-200 ℃, more preferably 120-180 ℃, and more preferably 140-160 ℃.
In the invention, the curing time is preferably 2-100 min, more preferably 10-80 min, and more preferably 30-60 min.
And finally, compounding a heat-conducting film on the surface of the heat-conducting gasket obtained in the step, coating the heat-conducting film with the semi-finished heat-conducting adhesive obtained in the step, and curing to obtain the heat-conducting interface material.
In the invention, the curing temperature is preferably 100-200 ℃, more preferably 120-180 ℃, and more preferably 140-160 ℃. I.e. cured again.
In the invention, the curing time is preferably 2-100 min, more preferably 10-80 min, and more preferably 30-60 min. I.e. cured again.
In the present invention, the manner of the composite heat conductive film preferably includes vacuum plating.
The invention is a complete and detailed integral technical scheme, and the preparation method specifically comprises the following steps:
the heat-conducting interface material provided by the invention sequentially comprises the working procedures of mixing, vacuum stirring, mixing, tabletting, coating and curing;
wherein the raw materials of the thermal interface material comprise the following components:
resin/curing agent, heat-conducting filler and auxiliary agent;
the resin can directly contain a curing agent component or the curing agent is added additionally, and the resin system comprises silicon resin, acrylic resin, polyurethane resin and the like with good elastic property;
the addition of curing agents requires between 30% and 80% free radical cure for the selected resin.
More specific steps may be:
adding an auxiliary agent into a resin/curing agent system, uniformly mixing, then adding 1/3 of a heat-conducting filler, mixing and dispersing at a high speed, sequentially adding the rest two 1/3, continuously mixing and dispersing at a high speed, after the micromolecules are pumped out, stirring at a constant speed for 30min in a vacuum environment, stopping stirring, discharging, tabletting and curing; and coating a high-thermal-conductivity coating such as graphene, aluminum nitride, metal, boron nitride and the like on the upper surface of the cured heat-conducting gasket in a vacuum coating manner, then coating the coating on the surface of the coating, performing secondary tabletting and curing, and thus obtaining the required product.
Compared with the heat conducting gasket on the market, the heat conducting interface material provided by the invention is a composite layer structure, and a high heat conducting coating is arranged in the middle. Wherein, the raw materials of the material layer comprise the following components: the heat-conducting filler is characterized by comprising a resin/curing agent system, a heat-conducting filler and an auxiliary agent, wherein the molar ratio of resin reaction groups consumed by a curing agent in the resin/curing agent system is 1: 0.3-0.8; the middle plated heat conducting layer comprises graphene, boron nitride, metal, aluminum nitride and the like. The present invention is not particularly limited with respect to the source and type of the resin/curing agent system, and any silicone/acrylic/polyurethane known to those skilled in the art may be used, as may commercially available products thereof. According to the invention, the heat-conducting rubber material is prepared from the curing agent and the resin in a specific ratio, so that the hardness of the rubber material can still be ensured within 60 ℃ of the shoreoo after the filler is added, and the comprehensive heat-conducting property is excellent.
The invention also provides application of the heat-conducting interface material prepared by any one of the technical schemes or the preparation method of any one of the technical schemes in the field of electronic products and/or automobiles.
The invention provides a high-efficiency heat-conducting interface material, a preparation method and application thereof. The heat-conducting interface material with the specific composite layer structure comprises a three-layer structure, wherein an efficient heat-conducting film layer is compounded between resin layers. According to the invention, a layer of high-heat-conductivity film material such as aluminum, silver, boron nitride, silicon carbide, aluminum nitride and the like is plated in the conventional heat-conducting gasket in a vacuum coating mode, and then the effect of comprehensive heat conduction of the whole heat-conducting interface material in horizontal and vertical multi-directions is realized by virtue of the heat-conducting filler in the heat-conducting adhesive, namely the heat-conducting particles in the vertical direction, so that the heat-conducting efficiency of the interface material is greatly improved. The invention can ensure vertical heat conduction and horizontal heat soaking, and the comprehensive heat conduction performance can reach 50w/mk at the highest under the condition of ensuring that the hardness is less than 60 DEG shore.
The invention further prepares the heat-conducting rubber material by the curing agent and the resin in a specific proportion, so that the hardness of the heat-conducting rubber material can still be ensured within 60 degrees of shore oo after the heat-conducting filler is added, and the comprehensive heat-conducting property is excellent. The novel heat-conducting interface material provided by the invention can be widely applied to the field of electronics/automobiles, and with the development of household appliances/automobiles towards the direction of high power, light weight and small size of chips/batteries, the appearance of the heat-conducting interface material represents the future development direction, and an effective heat treatment scheme is provided for the intelligent development of automobile electronics.
The experimental results show that: the heat conductivity coefficient of the heat-conducting glue and the gasket made of the material can reach 50w/mk to the maximum, the hardness is less than shore oo60 degrees, the strength is higher than 1Mpa, and the loss of each performance is within 10 percent after double 85 testing for 1000 hours.
For further illustration of the present invention, the following detailed description of a thermal interface material, a method for making the same, and applications of the same is provided in connection with the following examples, but it should be understood that the examples are implemented on the premise of the technical solution of the present invention, and the detailed embodiments and specific procedures are given only for further illustration of the features and advantages of the present invention, not for limitation of the claims of the present invention, and the scope of the present invention is not limited to the following examples.
The invention tests the heat-conducting interface material, and the method comprises the following steps:
coefficient of thermal conductivity: the test standard of ISO-22007-2 is met;
thermal resistance: the test standard of ASTMD5470 is met;
hardness: shoreoo;
reliability: 85% RH, 85 deg.C, 1000H
Example 1
Weighing 20 parts of SH-9608 (purchased from New Sihai chemical Co., Ltd., Hubei) in a planetary stirrer by 100 parts by weight, adding 1 part of triton x100 dispersant, dispersing for 10min at high speed together to obtain mixed solution with the viscosity of 1000-10000 pas, adding 23 parts of alumina heat-conducting powder vkl18 (purchased from New Crystal Material Co., Ltd., Anhui), carrying out vacuum mixing for 20min to obtain viscous liquid with the viscosity of 1000-30000pas, carrying out vacuum discharge, adding 23 parts of vkl16, repeatedly carrying out vacuum mixing for 20min, carrying out vacuum discharge, adding 23 parts of vk-l15, carrying out mixing for 5min, then heating to 50 ℃, and continuing vacuum mixing and defoaming for 30min to obtain semi-finished product of heat-conducting glue with the viscosity of 100000pas to 30000 pas.
Coating the semi-finished heat-conducting glue on the surface of release paper by blade coating equipment, wherein the thickness of the coating is 0.5mm, drying and curing the semi-finished heat-conducting glue for 10min at 130 ℃, rolling the semi-finished heat-conducting glue, and transferring the semi-finished heat-conducting glue to a vacuum coating chamber for vacuum coating of a layer of aluminum nitride film with the thickness of 0.2 um;
and (3) winding the silica gel gasket plated with the aluminum nitride film to a coating line, coating a layer of the stirred heat-conducting adhesive semi-finished product with the thickness of 0.5mm on the surface of the coating layer, drying and curing at the temperature of 130 ℃/10min, and winding to obtain a finished product.
Example 2
Weighing 15 parts of JY8742 (purchased from Junyi chemical technology Co., Ltd., Dongguan) by 100 parts by weight in a planetary stirrer, adding 1 part of triton x100 dispersant, dispersing for 10min at high speed to obtain mixed liquor with the viscosity of 1000-10000 pas, adding 23 parts of boron nitride (purchased from Shanghai lane field nanometer material Co., Ltd.) with the particle size of 45um, mixing for 20min in vacuum to obtain viscous liquid with the viscosity of 1000-30000pas, vacuumizing, adding 23 parts of boron nitride, mixing for 20min in vacuum repeatedly, vacuumizing, adding 23 parts of boron nitride, mixing and defoaming for 30min continuously to obtain a semi-finished product of the heat-conducting glue with the viscosity of 100000pas to 30000 pas. Extruding the semi-finished product of the heat-conducting adhesive into a heat-conducting gasket with the thickness of 1mm by using a three-roller calender, drying and curing, winding, and transferring to a vacuum coating chamber for vacuum coating of a silver film with the thickness of 0.1 um;
and (3) winding the silica gel gasket plated with the silver film to a film coating line, coating a layer of the stirred heat-conducting adhesive semi-finished product with the thickness of 1mm on the surface of the film coating layer, drying and curing at the temperature of 130 ℃/10min, and winding to obtain a finished product.
Example 3
Weighing 20 parts by weight of UE 638-04 (purchased from Camphor wood Xinwang plastic raw material Ming Hui of Dongguan city) in a planetary stirrer, adding 1 part of F410 (purchased from Olympic Polymer Co., Ltd., Foshan city), dispersing at high speed for 10min, heating to 50 ℃ to obtain mixed liquid with the viscosity of 1000-10000 pas, adding 23 parts of alumina heat-conducting powder vkl18 (purchased from Olympic New Material Co., Ltd.), performing vacuum mixing for 20min to obtain viscous liquid with the viscosity of 1000-30000pas, performing vacuum discharging, adding 23 parts of vkl16, performing vacuum mixing for 20min repeatedly, performing vacuum discharging, adding the last 23 parts of vk-115, and performing vacuum mixing and defoaming for 30min to obtain semi-finished heat-conducting adhesive with the viscosity of 100000pas to 30000 pas.
Coating a heat-conducting gasket with the thickness of 1.5mm on the semi-finished product of the heat-conducting adhesive by using a coating line, drying and curing, winding, and transferring to a vacuum coating chamber for evaporating and coating an aluminum nitride film with the thickness of 0.5 um;
and (3) winding the silica gel gasket coated with the aluminum nitride film by evaporation to a coating line, coating the surface of the coating layer with a layer of the stirred heat-conducting adhesive semi-finished product with the thickness of 1.5mm, drying and curing at the temperature of 130 ℃/10min, and winding to obtain a finished product.
Comparative example 1
Preparing a semi-finished product of the heat-conducting glue by the method in the embodiment 1, coating the semi-finished product of the heat-conducting glue on the surface of release paper by blade coating equipment, wherein the thickness of the coating is 0.5mm, and drying and curing at 130 ℃ for 10min to prepare the heat-conducting gasket.
Comparative example 2
The semi-finished product of the heat-conducting adhesive is prepared by the method in the embodiment 2, and is extruded by a three-roller calender to have the thickness of 1mm, and is dried and cured to prepare the heat-conducting gasket.
The heat-conducting interface materials prepared in the examples and the comparative examples of the present invention were subjected to performance tests.
TABLE 1 Performance test results of thermal interface materials prepared in examples 1 to 3 of the present invention and comparative examples 1 to 2
The embodiment shows that the heat-conducting interface material provided by the invention has good heat conductivity coefficient, thermal resistance and lower hardness, and the core performance of the heat-conducting interface material is reduced and controlled within 10 percent after a 1000-hour double 85 reliability test.
The above detailed description of the present invention provides a high efficiency thermal interface material, and its preparation method and application, and the present invention is described in the context of specific embodiments, which are only used to help understand the method and its core ideas of the present invention, including the best mode, and also to enable any person skilled in the art to practice the present invention, including making and using any devices or systems and implementing any combination of methods. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention. The scope of the invention is defined by the claims and may include other embodiments that occur to those skilled in the art. Such other embodiments are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims.
Claims (10)
1. A thermally conductive interface material, wherein said thermally conductive interface material has a layered structure;
includes a first resin layer;
the heat conducting film layer is compounded on the first resin layer;
and the second resin layer is compounded on the heat conduction film layer.
2. The thermal interface material of claim 1, wherein the first resin layer comprises one or more of a silicone layer, an acrylic resin layer, and a polyurethane resin layer;
the thickness of the first resin layer is 0.1-10 mm;
the second resin layer comprises one or more of a silicone resin layer, an acrylic resin layer and a polyurethane resin layer;
the thickness of the second resin layer is 0.1-10 mm.
3. The thermal interface material of claim 1, wherein the thermally conductive film layer comprises a thermally conductive nitride film layer and/or a thermally conductive carbon film layer;
the material of the heat conducting film layer comprises one or more of graphene, aluminum nitride, metal and boron nitride;
the thickness of the heat conducting film layer is 0.1-100 mu m;
the form of the heat-conducting interface material comprises a heat-conducting adhesive material, a heat-conducting gel material, a heat-conducting resin material or a heat-conducting gasket;
the thermally conductive interface material has a shore00 hardness of 60 ° or less.
4. The thermal interface material as claimed in claim 1, wherein the resin layer comprises, in mass percent, the following raw materials:
2-20 parts by weight of resin and a curing agent;
50-95 parts by weight of a heat conductive filler;
0.1-5 parts by weight of an auxiliary agent;
the heat-conducting interface material is a heat-conducting material used between the heating device and the heat sink.
5. The thermal interface material as claimed in claim 4, wherein the curing agent is added in an amount of 0.3 to 0.8 mol per mol of resin reactive groups consumed by the curing agent;
the thermally conductive filler comprises one or more of alumina, boron nitride, and silicon nitride;
the auxiliary agent comprises a dispersing agent;
the dispersant comprises dispersant triton and/or dispersant peg;
the heat-conducting interface material is used for electronic products and/or automobiles.
6. A preparation method of a heat conduction interface material is characterized by comprising the following steps:
1) mixing the resin, the curing agent and the auxiliary agent, and then adding the heat-conducting filler for vacuum mixing to obtain a semi-finished heat-conducting glue;
2) forming and curing the semi-finished product of the heat-conducting glue obtained in the step to obtain a heat-conducting gasket;
3) and compounding a heat conduction film on the surface of the heat conduction gasket obtained in the step, coating the heat conduction adhesive semi-finished product obtained in the step on the heat conduction film, and curing to obtain the heat conduction interface material.
7. The preparation method according to claim 1, wherein the viscosity of the mixed solution is 1000 to 10000 pas;
the vacuum mixing method for adding the heat-conducting filler comprises the following specific steps:
adding the heat-conducting filler for vacuum mixing for multiple times, vacuumizing, and adding the heat-conducting filler again for vacuum mixing:
the temperature of the vacuum mixing is 20-200 ℃;
the single time of the vacuum mixing is 1-200 min;
the vacuum degree of the vacuum mixing is less than or equal to 0.2 Pa.
8. The method according to claim 7, wherein the plurality of times is 2 to 5 times;
the viscosity of the viscous liquid after the heat-conducting filler is added for the first time and vacuum mixing is carried out is 1000-30000 pas;
heating for vacuum defoaming after the vacuum mixing;
the temperature after heating is 20-100 ℃;
and the vacuum defoaming time is 1-200 min.
9. The preparation method according to claim 1, wherein the viscosity of the semi-finished product of the heat-conducting glue is 100000-300000 pas;
the forming mode comprises film forming;
the thickness of the coating formed by coating is 0.1-10 mm;
the curing temperature in the step 2) and the curing temperature in the step 3) are respectively 100-200 ℃;
the curing time in the step 2) and the step 3) is 2-100 min respectively;
the mode of the composite heat-conducting film comprises vacuum coating.
10. Use of the thermal interface material according to any one of claims 1 to 5 or the thermal interface material prepared by the preparation method according to any one of claims 6 to 8 in the fields of electronic products and/or automobiles.
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| CN114163673A (en) * | 2021-12-14 | 2022-03-11 | 广东思泉新材料股份有限公司 | Low-dielectric high-thermal-conductivity interface film and preparation method thereof |
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