CN108943921A - A kind of multilayer insulation thermal interfacial material and preparation method thereof - Google Patents

A kind of multilayer insulation thermal interfacial material and preparation method thereof Download PDF

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CN108943921A
CN108943921A CN201810800172.5A CN201810800172A CN108943921A CN 108943921 A CN108943921 A CN 108943921A CN 201810800172 A CN201810800172 A CN 201810800172A CN 108943921 A CN108943921 A CN 108943921A
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layer
insulation
silicon rubber
thermal interfacial
rubber
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杨伟
冯昌平
白露
包睿莹
刘正英
杨鸣波
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Sichuan University
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Sichuan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B25/00—Layered products comprising a layer of natural or synthetic rubber
    • B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B25/042—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of natural rubber or synthetic rubber
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
    • C08L83/04—Polysiloxanes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/202—Conductive
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/20—Properties of the layers or laminate having particular electrical or magnetic properties, e.g. piezoelectric
    • B32B2307/206—Insulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/302—Conductive
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Fluid Mechanics (AREA)
  • Laminated Bodies (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention belongs to technical field of polymer materials, in particular to a kind of multilayer insulation thermal interfacial material and preparation method thereof.The present invention provides a kind of insulation thermal interfacial material, the insulation thermal interfacial material is by thermal insulation layer and thermally conductive layer by being alternately distributed the boundary material with multi-layer structure formed, wherein, thermal insulation layer is prepared by ceramic base heat filling filled silicon rubber, and thermally conductive layer is prepared by carbon-based heat filling filled silicon rubber；Multilayer in the multilayered structure is 2nLayer, n >=1.Gained insulation thermal interfacial material of the invention has a multilayered structure, and gained insulate, and (thermal coefficient up to 6~11W/mK), (volume resistivity is up to 10 for excellent electrical insulating property for thermal interfacial material thermal coefficient with higher11~1013Ω cm, breakdown strength are 5~9KV/mm) and excellent mechanical performance.

Description

A kind of multilayer insulation thermal interfacial material and preparation method thereof
Technical field
The invention belongs to technical field of polymer materials, in particular to a kind of multilayer insulation thermal interfacial material and its preparation sides Method.
Background technique
In the field of electronic component and integrated device, since various developments in science and technology are very rapid, various electronic components Integrated level is increasing, and the heat of required exclusion is consequently increased, and the requirement to heat-sinking capability is also just higher and higher.In electronics In appliance field, compared to nonisulated thermal interfacial material, the thermal interfacial material that insulate is more favored, because can effectively will be various The short circuit of equipment is not caused while heat transfer caused by electronic equipment is gone out.
Thermal interfacial material is usually to be added to the filler of high thermal conductivity to prepare in polymer, and heat filling presses insulation performance Insulating heat-conductive filler and nonisulated heat filling can be divided into.Insulating heat-conductive filler is mainly ceramic-like filler such as boron carbide, and Nonisulated heat filling includes carbon-based filler and metal packing.The thermal coefficient of common insulating heat-conductive filler is generally in 20- Within the scope of 300W/mK, and carbon-based filler then has higher thermal coefficient (500-5000W/mK).The thermal interfacial material that insulate is general It is to be filled to prepare by ceramic-like filler, but since filler itself has lower thermal coefficient, so the ceramic base heat of preparation The thermal coefficient of boundary material will be much smaller than carbon-based thermal interfacial material.The thermal coefficient of commercialization insulation thermal interfacial material is general Only 0.5-4W/mK.
The some methods that insulation thermal interfacial material is prepared using carbon-based heat filling of many document reports.Utilize insulation SiO2Silver nanowires and carbon nanotube (CNTs) are wrapped up remaining electrically isolated from property while improving epoxy resin thermally conductive coefficient, But the thermal coefficient of material only has 0.5-1.5W m-1K-1(Composites Science and Technology.2016； 128:207-214；Carbon.2011；49(2):495-500).Morishita reports a kind of side of Fillers selection distribution Method keeps the insulating properties of polymer material, and CNTs is selectively distributed in a phase-polymerization object to prevent building for conductive network Vertical, the thermal coefficient of composite material only has 0.43W m-1K-1(Journal of Materials Chemistry.2011；21 (15):5610).Although the thermal interfacial material of these methods preparation is with excellent insulating properties but all with poor thermal conductivity Can, thermal coefficient generally only has 0.5-1.5W m-1K-1, heat dissipation effect is unable to meet actual application.
Based on this, studies and develop and design a kind of multilayer insulation thermal interfacial material with high thermal conductivity and insulating properties then It is extremely important.
Summary of the invention
The object of the present invention is to provide a kind of insulation thermal interfacial materials, with multilayered structure, the hot interface material of gained insulation Expecting thermal coefficient with higher, (thermal coefficient up to 6~11W/mK), (volume resistivity is up to 10 for excellent electrical insulating property11~ 1013Ω cm, breakdown strength are 5~9KV/mm) and excellent mechanical performance.
Technical solution of the present invention:
The invention solves first technical problem be to provide a kind of insulation thermal interfacial material, the hot interface material of insulation Material is by thermal insulation layer and thermally conductive layer by being alternately distributed the boundary material with multi-layer structure formed, wherein absolutely Edge heat-conducting layer is prepared by ceramic base heat filling filled silicon rubber, and thermally conductive layer is by carbon-based heat filling filled silicon rubber It is prepared；Multilayer in the multilayered structure is 2nLayer, n >=1.
Further, the silicon rubber refers to carry out high temperature vulcanized the poly- of linear high polymerization degree by adding vulcanizing agent and have Organic siloxane (5000~10000 siloxane unit).
Further, the silicon rubber is selected from: methyl vinyl silicone rubber, dimethyl silicone rubber, methyl phenyl vinyl silicon Rubber or fluorine silicone rubber.Wherein the vinyl molar fraction of methyl vinyl silicone rubber is 0.05%~1%, when vinyl mole It is soft silicon rubber when score is 0.05%~0.15%, is low pressure when vinyl molar fraction is 0.15%~0.35% Compression permanent deformation silicon rubber is high-tear strength silicon rubber when vinyl molar fraction is 0.35%~1%.
Further, the ceramic base heat filling is selected from: in aluminium oxide, silicon carbide, boron nitride nanosheet or boron nitride It is at least one.
Further, the carbon-based heat filling is selected from: in graphene microchip, graphene, carbon fiber and carbon nanotube extremely Few one kind.
Further, in thermal insulation layer ceramics-based filler and silicon rubber ratio are as follows: 100 parts by weight of silicon rubber, ceramic base 20~300 parts by weight of heat filling.
Further, in thermal insulation layer carbon-based heat filling and silicon rubber ratio are as follows: 100 parts by weight of silicon rubber, it is carbon-based 20~300 parts by weight of heat filling.
Further, it is described insulation thermal interfacial material the number of plies be 2~128, each layer with a thickness of 0.001~2mm.Due to The breakdown voltage of final insulation thermal interfacial material can be reduced as the number of plies increases, and thermal coefficient then can be with every a layer thickness Reduce and increase, because heat filling orientation is more obvious；Therefore breakdown voltage and thermal coefficient in order to guarantee resulting materials In normal use scope, limit the number of plies of insulation thermal interfacial material as 2~128, each layer with a thickness of 0.001~2mm.
The invention solves second technical problem be to provide the preparation method of above-mentioned insulation thermal interfacial material, the system Preparation Method are as follows: be separately added into ceramics-based filler in silicon rubber and carbon-based filler is blended and the white material of Blend rubber and the black material of Blend rubber is made； The white material of Blend rubber and the black material of Blend rubber are pressed into sheet material again；Then a piece of white media sheet and a piece of black media sheet are pressed into tool There is the sheet material of double-layer structure, the sheet material with double-layer structure cuts, overlaps and suppress to obtain the sheet material with four-layer structure, tool There is the sheet material cutting of four-layer structure, overlap and suppress to obtain the sheet material with eight layers of structure；And so on, utilize identical system Preparation Method, which is made, has 2nThe sheet material of layer structure；To finally have 2nThe sheet material of layer structure is made 2 by vulcanizationnThe hot boundary of layer insulation Plane materiel material；Wherein, n >=1.
Further, in the above method, white media sheet and white media sheet are alternatively distributed when being overlapped after sheet material cutting.
Further, above-mentioned insulation thermal interfacial material the preparation method comprises the following steps:
Work as n=1, when the number of plies for the thermal interfacial material that insulate is 2 layers, the preparation method is that: first by silicon rubber and ceramic base The white material of Blend rubber is blended to obtain in filler, and the black material of Blend rubber is blended to obtain in silicon rubber with carbon-based filler；Again by the white material of Blend rubber and Blend rubber Black material is pressed into white media sheet and black media sheet respectively；Then a piece of white media sheet and a piece of black media sheet are obtained by cold compaction White media sheet and the alternatively distributed unvulcanized two sheets of cold pressing of black media sheet；Finally two sheets are made two layers by vulcanization Insulate thermal interfacial material；
Work as n > 1, the number of plies for the thermal interfacial material that insulate is 2nWhen layer, the preparation method is that: by above-mentioned cold pressing unvulcanized two Layer of sheet material (the i.e. white media sheet and black tablet being prepared by a piece of white media sheet and a piece of black media sheet by cold pressing when n=1 The unvulcanized two sheets of the alternatively distributed cold pressing of material) it is cut into the identical two panels of size, it is then overlapped and is cold-pressed white tablet is made Material and the alternatively distributed four layer of sheet material material of black media sheet；Four layer of sheet material materials are cut into the identical two panels of size again, then It is overlapped and is cold-pressed and white media sheet and the alternatively distributed eight layer of sheet material material of black media sheet is made；And so on, utilize identical side Legal system obtains 2nLayer of sheet material material；2nLayer of sheet material material is made 2 finally by vulcanizationnLayer insulation thermal interfacial material.
Further, in the above method, silicon rubber be blended with ceramics-based filler the white material of Blend rubber method are as follows: first by silicon rubber Glue, vulcanizing agent, fumed silica and dimethylsiloxane oligomer two-roll mill be uniformly mixed to obtain Blend rubber, then plus Enter ceramics-based filler to be uniformly mixed.
Further, in the above method, silicon rubber be blended with carbon-based filler the black material of Blend rubber method are as follows: first by silicon rubber Glue, vulcanizing agent, fumed silica and dimethylsiloxane oligomer two-roll mill be uniformly mixed to obtain Blend rubber, then plus Enter carbon-based filler to be uniformly mixed.
Further, in the above method, the vulcanizing agent is bis- (tert-butyl peroxide) hexanes of 2,5- dimethyl -2,5-, mistake Aoxidize diethyl propyl benzene, one of di-t-butyl peroxide and peroxidized t-butyl perbenzoate.
Further, in the above method, silicon rubber, vulcanizing agent, fumed silica and dimethylsiloxane oligomer ratio Example are as follows: 100 parts by weight of silicon rubber, 0.2~5 parts by weight of vulcanizing agent, 0~20 parts by weight of fumed silica, dimethyl siloxane Oligomer: 0~15 parts by weight.
Further, in above-mentioned preparation method, the cold pressing of unvulcanized silicon rubber sheet material is that mold is utilized in vulcanizing press It is made, in the cold-press process, cold pressing pressure is 2~10MPa, and the cold pressing time is 0.5~5 minute；The length and width of mold die cavity and Thickness distribution is 50~1000mm, 50~1000mm and 0.5~5mm, and mold die cavity is sized at unvulcanized silica gel sheet material Size.
Further, in above-mentioned preparation method, sulfuration process is divided into primary vulcanization and post-cure, the temperature once vulcanized, Time and pressure are respectively 120~180 DEG C, 5~30 minutes and 5~20MPa；Post-cure is carried out in high temperature oven, The temperature and time of vulcanization is respectively 160~220 DEG C and 2~8 hours.
Compared with prior art, the present invention having the following advantages and benefits:
(1) the insulation thermal interfacial material of preparation of the present invention is to utilize the method repeatedly suppressed for thermal insulation layer and lead Conductance thermosphere is pressed into multilayered structure, in multilayer thermal interface material thermal insulation layer and thermally conductive layer be it is alternatively distributed at Zebra stripes structure, this structure then assign material excellent electrical insulating property in vertical sheet material direction；Along being parallel to sheet material side Then assign material excellent heating conduction to the heat filling of orientation.
(2) multilayer insulation method of preparing heat interfacial material of the present invention has equipment simple, simple process and low cost, It is pollution-free and be easy to the advantages that industrializing.
(3) in the present invention, in the multiple pressing process of unvulcanized silica gel, the heat filling of sheet can be along being parallel to piece Material direction orientation, the degree of orientation of filler are improved with the increase of the number of plies, and the orientation of filler is conducive to the raising of thermal coefficient.
Detailed description of the invention
Fig. 1 is the preparation process schematic diagram of multilayer insulation thermal interfacial material of the present invention；Wherein, process flow 1 is high temperature sulphur The mixing of SiClx glue and heat filling, process flow 2 are the pressing process of unvulcanized multilayer silicon rubber film material, process flow 3 be sulfidation, and process flow 4 is the application of thermal interfacial material, and 5 be ceramics-based filler, and 6 be carbon-based filler, and 7 is mixed for silicon rubber Refining glue, 8 be radiator, and 9 be insulation thermal interfacial material, and 10 be chip.
Fig. 2 is silicon rubber/boron nitride/graphene nanometer sheet thermal interfacial material optical picture in Examples 1 to 4；White Layer is boron carbide filled high-temperature vulcanization silica gel, and black layer is graphene nanometer sheet filled high-temperature vulcanization silica gel, can clearly be seen Zebra stripes structure is observed, each layer of thickness is all relatively uniform and is not broken；This clearly zebra stripes structure is protected Electrical insulating property in vertical direction is demonstrate,proved.
Fig. 3 is the structural schematic diagram that the present invention prepares material during multilayer insulation thermal interfacial material；Wherein, 1 is silicon rubber Ceramics-based filler in matrix body, 2 be the carbon-based filler in silicone rubber matrix, by schematic diagram it is found that with thermal interface material layer The orientation of several increase laminal filters in the base is more and more obvious.
Specific embodiment
The present invention thermal insulation layer and thermally conductive layer is prepared by multiple compression moulding with multi-layer structure Insulate thermal interfacial material；Thermal insulation layer and thermally conductive layer are alternatively distributed in zebra stripes in multilayer thermal interface material Structure, thermal insulation layer are prepared by ceramics-based filler filled silicon rubber, and thermally conductive layer is filled by carbon-based heat filling Silicon rubber preparation.
The present invention provides a kind of preparation method of multilayer insulation thermal interfacial material, first with two-roll mill by silicon rubber Glue, vulcanizing agent, fumed silica and dimethylsiloxane oligomer are uniformly mixed to obtain rubber compound, are then respectively adding ceramic base The white material of Blend rubber and the black material of Blend rubber is made in filler or carbon-based filler, and cold-press process is recycled to be pressed into white material and black material respectively A piece of white media sheet and a piece of black media sheet must finally be had two layers of sheet material by sheet material by cold compaction, will be with two layers Sheet material is cut into the identical two panels of size from centre, two panels overlap it is re-compacted there is four layers of sheet material, utilization is identical Preparation method utilize and can suppress to have eight layers of sheet material with four layers of sheet material, may finally obtain with 2nThe number of plies Sheet material, n are the number of cold pressing；The final hot boundary of multilayer insulation is made by high temperature vulcanized in the unvulcanized silica gel sheet material of the multilayer of acquisition Plane materiel material.
To make the object, technical solutions and advantages of the present invention clearer, the technical solution below in the present invention carries out clear Chu is fully described by, it is clear that described embodiments are some of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
Examples 1 to 4:
A kind of multilayer insulation silica gel/boron nitride/graphene nanometer sheet insulation thermal interfacial material, preparation is in accordance with the following steps It carries out:
(1) by 100g silicon rubber and 2g cumyl peroxide amine, 5g fumed silica and 2g dimethyl siloxane are low Polymers uniformly mixes to obtain rubber compound by two-roll mill at room temperature, and wherein silicon rubber selection vinyl molar fraction is 0.25% low compression set silicon rubber；Then it weighs 50g boron nitride and 50g graphene nanometer sheet is added separately to be kneaded The white material of Blend rubber and the black material of Blend rubber are made in glue；
(2) it takes appropriate rubber compound in being put into vulcanizing press on mold according to mold size, is first cold-pressed at room temperature 10MPa It 1 minute, is vented three times, in case there is bubble in sample interior；Utilize the preparation process point of multilayer insulation thermal interfacial material shown in Fig. 1 Zhi get be with 2 layers, 4 layers, 8 layers and 16 layers of the unvulcanized multi-layer sheet of cold pressing, the size of unvulcanized multi-layer sheet 2mm × 60mm×60mm；Wherein, 2 layer of sheet material materials the preparation method comprises the following steps: first the white material of Blend rubber and the black material of Blend rubber are pressed into respectively Then a piece of white media sheet and a piece of black media sheet are obtained white media sheet and black material by cold compaction by white media sheet and black media sheet The alternatively distributed unvulcanized two sheets material of cold pressing of sheet material；The unvulcanized two sheets of gained are cut into size phase from centre again Same two panels, then overlapping and cold compaction obtain white media sheet and the alternatively distributed unvulcanized four layer of sheet material material of cold pressing of black media sheet Material；Then unvulcanized four layer of sheet material material will be cold-pressed and be cut into the identical two panels of size from centre, pass through cold pressing after being then overlapped White media sheet and the alternatively distributed unvulcanized eight layer of sheet material material of cold pressing of black media sheet is made；Finally eight layer of sheet material are cut, again It is folded that white media sheet and the alternatively distributed unvulcanized 16 layer of sheet material material of cold pressing of black media sheet are obtained by cold compaction；
(3) it will be cold-pressed unvulcanized multi-layer sheet material obtained by step (2) and carry out high temperature vulcanized, temperature when primary vulcanization is 170 DEG C, pressure 10MPa, vulcanization time 20min；It is put into 200 DEG C of high temperature ovens and vulcanizes 4 hours when post-cure；Vulcanization Later it respectively obtains with 2 layers of structure (embodiment 1), 4 layers of structure (embodiment 2), 8 layers of structure (embodiment 3), 16 (embodiments 4) silica gel of layer structure/boron nitride/graphene nanometer sheet insulation thermal interfacial material；Its thermal coefficient, volume resistivity and hits Wearing intensity, the results are shown in Table 1；Silica obtained in Examples 1 to 4/boron nitride/graphene nanometer sheet insulation thermal interfacial material Optical picture it is as shown in Figure 2.
In addition, the present invention is also prepared and tested pure silicone rubber (comparative example 1), boron nitride filling gel (comparative example 2) is non- The boron nitride of multilayered structure and the thermal coefficient of graphene nanometer sheet filling gel (comparative example 3), volume resistivity and breakdown are strong Degree, the results are shown in Table 1.
The preparation process of comparative example 2 are as follows: 100g silicon rubber and 2g cumyl peroxide amine, 5g fumed silica and 2g Dimethylsiloxane oligomer uniformly mixes to obtain rubber compound by two-roll mill at room temperature, then weighs 50g boron nitride and adds Enter into rubber compound, boron nitride filling gel is made by identical sulfuration process；Compare with embodiment 1, difference is: right Ratio 2 is only added to boron carbide and no multilayered structure.
The preparation process of comparative example 3 are as follows: 100g silicon rubber and 2g cumyl peroxide amine, 5g fumed silica and 2g Dimethylsiloxane oligomer uniformly mixes to obtain rubber compound by two-roll mill at room temperature, then weigh 25g boron nitride and 25g graphene nanometer sheet is added in rubber compound together, is made by identical sulfuration process；Compare with embodiment 1, distinguishes Be: boron nitride and graphene nanometer sheet in comparative example 3 are disorder distributions and do not have multilayered structure.
1 silica gel of table/boron nitride/graphene nanometer sheet thermal interfacial material thermal coefficient, volume resistivity and breakdown strength
Embodiment 5~10:
A kind of multilayer insulation silica gel/aluminium oxide/graphite thermal interfacial material, preparation carry out in accordance with the following steps:
(1) by 100g silicon rubber and bis- (tert-butyl peroxide) hexanes of 1g 2,5- dimethyl -2,5- and 5g dimethyl silica Alkane oligomer is uniformly mixed at room temperature by two-roll mill；It is 0.10% that wherein silicon rubber, which selects vinyl molar fraction, Soft methyl vinyl silicone rubber；Then 50g aluminium oxide is weighed respectively or 100g graphite is added in rubber compound and is made mixed The white material of refining glue and the black material of rubber compound；
(2) it takes appropriate rubber compound in being put into vulcanizing press on mold, is first cold-pressed 1 minute at room temperature 10MPa, exhaust three It is secondary, in case there is bubble in sample interior；Being made using the preparation process of multilayer insulation thermal interfacial material shown in Fig. 1 has different layers Several unvulcanized multi-layer sheets, the size of unvulcanized multi-layer sheet are 2mm × 60mm × 60mm；
(3) progress of unvulcanized multi-layer sheet is high temperature vulcanized, once temperature when vulcanization is 170 DEG C, pressure 10MPa, Vulcanization time is 20min；It is put into 190 DEG C of high temperature ovens and vulcanizes 2 hours when post-cure；Vulcanization is respectively obtained with 2 later Layer (embodiment 5), 4 layers (embodiment 6), 8 layers (embodiment 7), 16 layers (embodiment 8), 32 layers (embodiment 9), 64 layers of (embodiment 10) silica gel of structure/aluminium oxide/graphite insulation thermal interfacial material.The following table 2 gives 5~embodiment of embodiment, 10 gained silicon Glue/aluminium oxide/graphite thermal interfacial material thermal coefficient, volume resistivity and breakdown strength.
2 silica gel of table/aluminium oxide/graphite thermal interfacial material thermal coefficient, volume resistivity and breakdown strength
Sample Embodiment 5 Embodiment 6 Embodiment 7 Embodiment 8 Embodiment 9 Embodiment 10
Thermal coefficient (W/mK) 7.1 8.2 9.1 9.3 9.7 10.2
Volume resistivity (Ω cm) 1013 1013 1013 1012 1012 1011
Breakdown strength (KV/mm) 7.5 7.2 6.5 6.0 5.3 4.1
Although describing the present invention above in conjunction with embodiment, it would be clear to those skilled in the art that not departing from power In the case where the spirit and scope that benefit requires, above-described embodiment can be carry out various modifications.

Claims (10)

1. a kind of insulation thermal interfacial material, which is characterized in that the insulation thermal interfacial material is led by thermal insulation layer and conduction Thermosphere is by being alternately distributed the boundary material with multi-layer structure to be formed, wherein thermal insulation layer is by ceramic base heat filling Filled silicon rubber is prepared, and thermally conductive layer is prepared by carbon-based heat filling filled silicon rubber；In the multilayered structure Multilayer be 2nLayer, n >=1.
2. insulation thermal interfacial material according to claim 1, which is characterized in that the silicon rubber is referred to by adding sulphur Agent carries out the polysiloxane of high temperature vulcanized linear high polymerization degree；Further, the silicon rubber is selected from: methyl ethylene Silicon rubber, dimethyl silicone rubber, methyl phenyl vinyl silicone rubber or fluorine silicone rubber.
3. insulation thermal interfacial material according to claim 1 or 2, which is characterized in that the ceramic base heat filling is selected from: At least one of aluminium oxide, silicon carbide, boron nitride nanosheet or boron nitride；The carbon-based heat filling is selected from: graphene is micro- At least one of piece, graphene, carbon fiber and carbon nanotube.
4. described in any item insulation thermal interfacial materials according to claim 1~3, which is characterized in that ceramic in thermal insulation layer The ratio of based filler and silicon rubber are as follows: 100 parts by weight of silicon rubber, 20~300 parts by weight of ceramic base heat filling；Thermal insulation layer In carbon-based heat filling and silicon rubber ratio are as follows: 100 parts by weight of silicon rubber, carbon-based 20~300 parts by weight of heat filling.
5. insulation thermal interfacial material according to any one of claims 1 to 4, which is characterized in that the hot interface material of insulation The number of plies of material be 2~128, each layer with a thickness of 0.001~2mm.
6. the preparation method of the described in any item insulation thermal interfacial materials of Claims 1 to 5, which is characterized in that the preparation side Method are as follows: be separately added into ceramics-based filler in silicon rubber and carbon-based filler is blended and the white material of Blend rubber and the black material of Blend rubber is made；Again will The white material of Blend rubber and the black material of Blend rubber are pressed into sheet material；Then a piece of white media sheet and a piece of black media sheet are pressed into two The sheet material of layer structure, the sheet material with double-layer structure cut, overlap and suppress to obtain the sheet material with four-layer structure, have four The sheet material cutting of layer structure overlaps and suppresses to obtain the sheet material with eight layers of structure；And so on, utilize identical preparation side Method, which is made, has 2nThe sheet material of layer structure；To finally have 2nThe sheet material of layer structure is made 2 by vulcanizationnThe hot interface material of layer insulation Material；Wherein, n >=1.
7. the preparation method of insulation thermal interfacial material according to claim 6, which is characterized in that described to state the hot interface of insulation Material the preparation method comprises the following steps:
Work as n=1, when the number of plies for the thermal interfacial material that insulate is 2 layers, the preparation method is that: first by silicon rubber and ceramics-based filler The white material of Blend rubber is blended to obtain, the black material of Blend rubber is blended to obtain in silicon rubber with carbon-based filler；Again by the white material of Blend rubber and the black material of Blend rubber It is pressed into white media sheet and black media sheet respectively；Then a piece of white media sheet and a piece of black media sheet are obtained into white material by cold compaction Sheet material and the alternatively distributed unvulcanized two sheets of cold pressing of black media sheet；Two layers of insulation finally is made by vulcanization in two sheets Thermal interfacial material；
Work as n > 1, the number of plies for the thermal interfacial material that insulate is 2nWhen layer, the preparation method is that: by the unvulcanized two sheets of cold pressing It is cut into the identical two panels of size, is then overlapped and is cold-pressed white media sheet and the alternatively distributed four layer of sheet material material of black media sheet is made Material；Four layer of sheet material materials are cut into the identical two panels of size again, is then overlapped and is cold-pressed white media sheet and black media sheet is made Alternatively distributed eight layer of sheet material material；And so on, 2 are made using identical methodnLayer of sheet material material；2nLayer of sheet material material is most 2 are made by vulcanization afterwardsnLayer insulation thermal interfacial material.
8. the preparation method of insulation thermal interfacial material according to claim 6 or 7, which is characterized in that in the method, silicon Rubber be blended with ceramics-based filler the white material of Blend rubber method are as follows: first by silicon rubber, vulcanizing agent, fumed silica and diformazan Radical siloxane oligomer is uniformly mixed to obtain Blend rubber in two-roll mill, and ceramics-based filler is then added and is uniformly mixed；Silicon rubber Be blended with carbon-based filler the black material of Blend rubber method are as follows: first by silicon rubber, vulcanizing agent, fumed silica and dimethyl silica Alkane oligomer is uniformly mixed to obtain Blend rubber in two-roll mill, and carbon-based filler is then added and is uniformly mixed；Further, silicon rubber, The ratio of vulcanizing agent, fumed silica and dimethylsiloxane oligomer are as follows: 100 parts by weight of silicon rubber, vulcanizing agent 0.2~5 Parts by weight, 0~20 parts by weight of fumed silica, dimethylsiloxane oligomer: 0~15 parts by weight.
9. the preparation method of insulation thermal interfacial material according to claim 7 or 8, which is characterized in that the preparation method In, in the cold-press process, cold pressing pressure is 2~10MPa, and the cold pressing time is 0.5~5 minute.
10. according to the preparation method of the described in any item insulation thermal interfacial materials of claim 6~9, which is characterized in that the system In Preparation Method, the sulfuration process is divided into primary vulcanization and post-cure, the temperature once vulcanized, time and pressure are respectively 120~180 DEG C, 5~30 minutes and 5~20MPa；The temperature and time of post-cure is respectively that 160~220 DEG C and 2~8 are small When.
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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218449A (en) * 2019-05-20 2019-09-10 陈朝明 A kind of preparation method of heat conductive insulating composite material
CN112195016A (en) * 2020-09-21 2021-01-08 深圳市鸿富诚屏蔽材料有限公司 Heat-conducting insulating carbon fiber silica gel gasket and preparation method thereof
CN113957702A (en) * 2021-10-27 2022-01-21 大连理工大学 Preparation method and application of thermal interface material based on high-graphitization asphalt-based carbon fiber
CN115181549A (en) * 2022-08-25 2022-10-14 青岛科技大学 Phase-change energy-storage heat-conducting membrane material based on crystalline trans-rubber and preparation method thereof
CN115505266A (en) * 2021-06-23 2022-12-23 嘉兴超维新材料科技有限公司 Silicone rubber gasket and preparation method and application thereof
CN115505265A (en) * 2021-06-23 2022-12-23 嘉兴超维新材料科技有限公司 High-thermal-conductivity silicone rubber gasket and preparation method and application thereof
CN116874826A (en) * 2023-07-25 2023-10-13 常州宏巨电子科技有限公司 Heat-conducting silicone rubber composite material with directional arrangement of fillers and preparation method thereof

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6096414A (en) * 1997-11-25 2000-08-01 Parker-Hannifin Corporation High dielectric strength thermal interface material
US20040067372A1 (en) * 2002-10-04 2004-04-08 Shin-Etsu Chemical Co., Ltd. Heat conductive silicone rubber composite sheet
CN102576836A (en) * 2009-10-19 2012-07-11 日东电工株式会社 Thermally conductive member, and battery device using same
CN103333494A (en) * 2013-05-28 2013-10-02 东莞上海大学纳米技术研究院 Thermal-conductive insulation silicone rubber thermal interface material and preparation method thereof
CN105538647A (en) * 2015-07-13 2016-05-04 四川大学 Low-cost multifunctional high-efficiency polymer-based insulation and heat conduction composite material and preparation method thereof
CN106413367A (en) * 2016-09-05 2017-02-15 四川大学 Novel multifunctional macromolecule based multilayer electromagnetic shielding material and preparation method thereof
CN106833367A (en) * 2017-02-08 2017-06-13 昆山市中迪新材料技术有限公司 A kind of insulated type interface chill bar material and preparation method thereof
CN106854367A (en) * 2015-12-08 2017-06-16 信越化学工业株式会社 Rubber composition and its product of solidification
CN107851623A (en) * 2015-06-25 2018-03-27 保力马科技(日本)株式会社 Thermally conductive sheet

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6096414A (en) * 1997-11-25 2000-08-01 Parker-Hannifin Corporation High dielectric strength thermal interface material
US20040067372A1 (en) * 2002-10-04 2004-04-08 Shin-Etsu Chemical Co., Ltd. Heat conductive silicone rubber composite sheet
CN102576836A (en) * 2009-10-19 2012-07-11 日东电工株式会社 Thermally conductive member, and battery device using same
CN103333494A (en) * 2013-05-28 2013-10-02 东莞上海大学纳米技术研究院 Thermal-conductive insulation silicone rubber thermal interface material and preparation method thereof
CN107851623A (en) * 2015-06-25 2018-03-27 保力马科技(日本)株式会社 Thermally conductive sheet
CN105538647A (en) * 2015-07-13 2016-05-04 四川大学 Low-cost multifunctional high-efficiency polymer-based insulation and heat conduction composite material and preparation method thereof
CN106854367A (en) * 2015-12-08 2017-06-16 信越化学工业株式会社 Rubber composition and its product of solidification
CN106413367A (en) * 2016-09-05 2017-02-15 四川大学 Novel multifunctional macromolecule based multilayer electromagnetic shielding material and preparation method thereof
CN106833367A (en) * 2017-02-08 2017-06-13 昆山市中迪新材料技术有限公司 A kind of insulated type interface chill bar material and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110218449A (en) * 2019-05-20 2019-09-10 陈朝明 A kind of preparation method of heat conductive insulating composite material
CN112195016A (en) * 2020-09-21 2021-01-08 深圳市鸿富诚屏蔽材料有限公司 Heat-conducting insulating carbon fiber silica gel gasket and preparation method thereof
CN112195016B (en) * 2020-09-21 2021-12-24 深圳市鸿富诚屏蔽材料有限公司 Heat-conducting insulating carbon fiber silica gel gasket and preparation method thereof
CN115505266A (en) * 2021-06-23 2022-12-23 嘉兴超维新材料科技有限公司 Silicone rubber gasket and preparation method and application thereof
CN115505265A (en) * 2021-06-23 2022-12-23 嘉兴超维新材料科技有限公司 High-thermal-conductivity silicone rubber gasket and preparation method and application thereof
CN113957702A (en) * 2021-10-27 2022-01-21 大连理工大学 Preparation method and application of thermal interface material based on high-graphitization asphalt-based carbon fiber
CN115181549A (en) * 2022-08-25 2022-10-14 青岛科技大学 Phase-change energy-storage heat-conducting membrane material based on crystalline trans-rubber and preparation method thereof
CN115181549B (en) * 2022-08-25 2024-03-08 青岛科技大学 Phase-change energy-storage heat-conducting film material based on crystalline trans-rubber and preparation method thereof
CN116874826A (en) * 2023-07-25 2023-10-13 常州宏巨电子科技有限公司 Heat-conducting silicone rubber composite material with directional arrangement of fillers and preparation method thereof
CN116874826B (en) * 2023-07-25 2023-12-22 常州宏巨电子科技有限公司 Heat-conducting silicone rubber composite material with directional arrangement of fillers and preparation method thereof

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