CN103333494B - A kind of Thermal-conductive insulation silicone rubber thermal interface material and preparation method thereof - Google Patents
A kind of Thermal-conductive insulation silicone rubber thermal interface material and preparation method thereof Download PDFInfo
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- CN103333494B CN103333494B CN201310205354.5A CN201310205354A CN103333494B CN 103333494 B CN103333494 B CN 103333494B CN 201310205354 A CN201310205354 A CN 201310205354A CN 103333494 B CN103333494 B CN 103333494B
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Abstract
The invention discloses a kind of Thermal-conductive insulation silicone rubber thermal interface material and preparation method thereof, it comprises the following steps: the 1) surface treatment of heat conductive filler; 2) heat conductive filler of different-grain diameter is blended with silicone rubber matrix successively by size; 3) hot press moulding or calendering sulfuration; 4) post cure, obtains that thickness 0.2 ~ 5mm is controlled, Shore A hardness 10 ~ 60 degree is controlled, thermal conductivity 0.8 ~ 2.5W/ (mK) is controlled, and tear strength is greater than 3kN/mm sheet heat conductive insulating silica gel heat interfacial material; 5) release film is pasted.This sheet Thermal-conductive insulation silicone rubber thermal interface material has that thermal conductivity is high, good insulation preformance, tear strength are large, stable performance, the feature such as easy to use, be applicable to the radiating gasket of the electron devices such as great power LED, panel computer, mobile phone, power supply.
Description
Technical field
The invention belongs to heat interfacial material field, relate to that a kind of thermal conductivity is high, good insulation preformance, tear strength are large, the Thermal-conductive insulation silicone rubber thermal interface material of good stability and preparation method thereof.
Background technology
In recent years, along with the fast development of semiconducter device integrated technique, microminiaturized, lightness and high efficiency future development make to dispel the heat becomes a more and more important problem, and it is also more and more higher to the requirement of heat radiation.Due to the contact interface of scatterer and semiconductor integrated device and unfairness, generally contact with each other only less than 20% area, this to carry out the effect of heat trnasfer to scatterer from have impact on semiconducter device greatly, thus between the contact interface of scatterer and semiconducter device, increase one deck heat interfacial material just seem very necessary to the thermal conduction increased between interface.
The object of heat interfacial material reduces the thermal resistance between device and scatterer.After adding heat interfacial material, thermal resistance generally can be divided into two portions, and a part is the thermal resistance of heat interfacial material itself, and this part thermal resistance is proportional to the thickness of heat interfacial material, the thermal conductivity of inverse ratio and heat interfacial material, thus need that the thermal conductivity of heat interfacial material is high, thickness is thin.Another part thermal resistance is heat interfacial material and heater members and the thermal contact resistance between heat interfacial material and scatterer.Affect the many factors of this part thermal resistance, comprising the thermal conductivity etc. of heat interfacial material to the filling ratio of heater members and scatterer uneven surface, contact pressure and heat interfacial material, thus require that the kindliness of heat interfacial material is good, joint filling is good, hardness low thermal conductivity is high.In addition, consider from the use angle of heat interfacial material, generally need the performances such as heat interfacial material will have good cold cycling stability, ageing resistance, construction is simple, detachable, cost is low.
Silicon rubber has the advantages such as good insulation preformance, rebound resilience is high, kindliness is good, but unfilled silicon rubber heat conductivility is very poor, thermal conductivity generally only has 0.2W/ (mK) left and right, general needs improve its heat conductivility by filling heat conductive filler, thus reach the requirement of heat interfacial material.The heat conduction of heat conductive filler filled silicon rubber matrix material depends primarily on the thermal conduction between filler.Between single common micro-scaled filler filled silicon rubber filler, interface is few, phon scattering is little, thus thermal contact resistance is little between filler, but common micro-scaled filler particle diameter is large, the space formed between filler also compared with large, the indirect contact of filler is few, cannot be formed and pile up more closely, thus limit the raising of thermal conductivity.Single nano-sized filler filled silicon rubber, the interaction force between filler and silicone rubber matrix is large, and thermal contact resistance is little, and Nano filling is easier well fills coarse device surface, thus obtains low thermal resistance.But the problem of nano-sized filler is that between filler, interface ratio is large, and phon scattering is serious, thus can limit the raising of thermal conductivity of composite materials.In addition, the thermal conductivity of filling family macromolecule matrix material depends on the loading level of heat conductive filler to a great extent, and loading level is larger, and the heat conduction network formed between heat conductive filler is more intensive, and thermal conductivity is higher.But ordinary tablet shape filler, along with the increase of loading level, the viscosity of matrix material sharply increases, the very difficult processing that matrix material becomes after filler is filled into certain volume mark, thus cannot obtain high filling, also just have impact on the raising of thermal conductivity.
Summary of the invention
For above-mentioned deficiency, the object of the invention is, provide that a kind of thermal conductivity is high, good insulation preformance, good stability, Thermal-conductive insulation silicone rubber thermal interface material easy to use and preparation method thereof.It is Thermal-conductive insulation silicone rubber thermal interface material and the preparation method of multiple dimensioned composite filling.Be applicable to the interface heat transfer between Heating element and heat dissipation element, the heat for being produced by Heating element distributes or similar applications.
For achieving the above object, technical scheme provided by the present invention is:
A kind of Thermal-conductive insulation silicone rubber thermal interface material, is characterized in that: it is made up of following mass percent component:
Described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm.
Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.
Described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69.
Described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
A kind of method preparing Thermal-conductive insulation silicone rubber thermal interface material described in right, it is characterized in that: in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler; Hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance.
Its concrete preparation process comprises the following steps:
1) surface treatment of multiple dimensioned composite heat conductive filler: surface treatment agent is made into corresponding solution, then respectively surface treatment is carried out to the heat conductive filler of various different scale, process rear filtration, drying, pulverizing, obtain the heat conductive filler that various surface treatment is good; The heat conductive filler of described various different scale comprises micrometer alumina, nano aluminium oxide, boron nitride and ZnOw; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) heat conductive filler that surface treatment step 1) obtained is good joins in silicone rubber matrix according to order from big to small successively according to particle diameter, and add softening agent, vacuum kneading is carried out mixing in vacuum kneader, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting silicon rubber rubber unvulcanizate;
3) by step 2) the rubber unvulcanizate thin-pass on a mill until that obtains, add vulcanizing agent in thin-pass process, carry out hot press moulding sulfuration or calendering sulfidization molding after thin-pass, obtain the sheet silicon glue material of forming;
4) the sheet silicon glue material high temperature secondary sulfuration of forming step 3) obtained, obtains the heat conductive insulating silica gel heat interfacial material of the sheet removing small molecules volatile matter; Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
It is further comprising the steps of:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Described micrometer alumina shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm; Described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.
Described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69; Described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
Relative to prior art, the present invention obtains following beneficial effect: by the composite filled silicon rubber of the heat conductive filler of different shapes, particle diameter and thermal conductivity, improve the loading level of heat conductive filler, volume loading level is made to reach more than 60%, thermal conductivity reaches 2.3W/ (mK), and there is good kindliness, tensile strength, tear strength and electrical insulation capability simultaneously, solve the problem that thermal conductivity in prior art, hardness, tear strength and electrical insulating property cannot be taken into account.The Thermal-conductive insulation silicone rubber thermal interface material of sheet of the present invention employs high temperature vulcanizable silicone, and low molecular weight polyorganosiloxane consumption is little, after the vulcanization of rubber, there is good rebound resilience, shock resistance is excellent, good, the convenient installation of ageing-resistant performance, dismounting, reusable.
Embodiment
Embodiment 1:
Thermal-conductive insulation silicone rubber thermal interface material provided by the invention, it is made up of following mass percent component:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.Described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69.Described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
The method of the aforementioned Thermal-conductive insulation silicone rubber thermal interface material of preparation provided by the invention, in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, the hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance.
Its concrete preparation process comprises the following steps:
1) surface treatment of multiple dimensioned composite heat conductive filler: surface treatment agent is made into corresponding solution, then respectively surface treatment is carried out to the heat conductive filler of various different scale, process rear filtration, drying, pulverizing, obtain the heat conductive filler that various surface treatment is good; The heat conductive filler of described various different scale comprises micrometer alumina, nano aluminium oxide, boron nitride and ZnOw; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) heat conductive filler that surface treatment step 1) obtained is good joins in silicone rubber matrix according to order from big to small successively according to particle diameter, and add softening agent, vacuum kneading is carried out mixing in vacuum kneader, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting silicon rubber rubber unvulcanizate;
3) by step 2) the rubber unvulcanizate thin-pass on a mill until that obtains, add vulcanizing agent in thin-pass process, carry out hot press moulding sulfuration or calendering sulfidization molding after thin-pass, obtain the sheet silicon glue material of forming;
4) the sheet silicon glue material high temperature secondary sulfuration of forming step 3) obtained, obtains the heat conductive insulating silica gel heat interfacial material of the sheet removing small molecules volatile matter; Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
It is further comprising the steps of: the heat conductive insulating silica gel heat interfacial material upper and lower surface of the sheet 5) step 4) obtained pastes one deck release film, to store and to use.
Described micrometer alumina shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm; Described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.Described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69; Described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
Embodiment 2:
Thermal-conductive insulation silicone rubber thermal interface material that the present embodiment provides and preparation method thereof, substantially the same with embodiment 1, its difference is, composition and the weight percent of this Thermal-conductive insulation silicone rubber thermal interface material are as follows:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 40 μm of ball-aluminium oxides 42% and 2 μm of ball-aluminium oxides 18% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm; Described ZnOw length-to-diameter ratio 10:1.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
The preparation method of this Thermal-conductive insulation silicone rubber thermal interface material, in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, the hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance.
Specific implementation process is as follows:
1) surface treatment of multiple dimensioned composite heat conductive filler: the dehydrated alcohol of 95 parts and 5 parts of deionized waters are made into alcohol solution, and regulate pH value to 4 with acetic acid; Add coupling agent KH570 according to the above ratio, induction stirring, after 10 minutes, obtains the KH570 surface treatment liquid prepared; The ZnOw of 40 μm of ball-aluminium oxides, 2 μm of ball-aluminium oxides, 40nm aluminum oxide, 35 μm of boron nitride and length-to-diameter ratio 10:1 is used the process of KH570 surface treatment liquid respectively, treatment condition are 60 ° of C, induction stirring 2 hours, dry after filtering, pulverizing, obtains the various heat conductive fillers that surface treatment is good; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) ZnOw of 40 μm of ball-aluminium oxides that surface treatment step 1) obtained is good, 35 μm of boron nitride, 2 μm of ball-aluminium oxides, 40nm aluminum oxide and length-to-diameter ratio 10:1, join successively in silicone rubber matrix according to order from big to small according to particle diameter, and add hydroxy silicon oil softening agent, vacuum kneading 30 minutes, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting insulating silicon rubber rubber unvulcanizate;
3) by step 2) rubber unvulcanizate that obtains thin-pass 4 ~ 6 times on twin shaft mixing roll, two-2 of silicone rubber matrix weight percentage 1.5% are added in thin-pass process, 5 vulcanizing agents, to carry out under 170 ° of C hot press moulding sulfuration 15 minutes, obtain the sheet silicon glue material of forming after thin-pass slice;
4) by the post cure 4 hours under 200 ° of C of the sheet silicon glue material of forming, the Thermal-conductive insulation silicone rubber thermal interface material of the sheet of the thickness 2mm removing small molecules volatile matter is obtained; Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 40 μm of ball-aluminium oxides 42% and 2 μm of ball-aluminium oxides 18% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm; Described ZnOw length-to-diameter ratio 10:1.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
Test its correlated performance as follows:
In the present embodiment, described micrometer alumina is particle diameter is that two kinds of particle diameters are composite, and it changes three kinds or more into, and composite particle size range, at 2 μm ~ 100 μm, is also suitable for.Described surface treatment agent changes one or more in KH550, KH560, KH570, A151, Si-69 into, is also suitable for.Described softening agent changes hydroxy silicon oil, magnesiumcarbonate into, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000, is also suitable for.
Embodiment 3: Thermal-conductive insulation silicone rubber thermal interface material that the present embodiment provides and preparation method thereof, with embodiment 1,2 substantially the same, its difference is, composition and the weight percent of this Thermal-conductive insulation silicone rubber thermal interface material are as follows:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 70 μm of ball-aluminium oxides 50% and 5 μm of ball-aluminium oxides 15% are composite.Described nano aluminium oxide, boron nitride are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
The preparation method of this Thermal-conductive insulation silicone rubber thermal interface material, in silicone rubber matrix, in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, the hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; Improve thermal conductivity further by the nano aluminium oxide of composite surface treatment agent process, boron nitride, reduce thermal resistance.
Specific implementation process is as follows:
1) surface treatment of multiple dimensioned composite heat conductive filler: the dehydrated alcohol of 95 parts and 5 parts of deionized waters are made into alcohol solution, and regulate pH value to 4 with acetic acid.Add coupling agent KH570 according to the above ratio, induction stirring, after 10 minutes, obtains the KH570 surface treatment liquid prepared; 70 μm of ball-aluminium oxides, 5 μm of ball-aluminium oxides, 40nm aluminum oxide and 35 μm of boron nitride are used the process of KH570 surface treatment liquid respectively, treatment condition are 60 ° of C, induction stirring 2 hours, dry after filtering, pulverizing, obtains the various heat conductive fillers that surface treatment is good; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride are auxiliary heat conduction filler;
2) 70 μm of ball-aluminium oxides that surface treatment step 1) obtained is good, 35 μm of boron nitride, 5 μm of ball-aluminium oxides and 40nm aluminum oxide, join successively in silicone rubber matrix according to order from big to small according to particle diameter, and add hydroxy silicon oil softening agent, vacuum kneading 30 minutes, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting insulating silicon rubber rubber unvulcanizate;
3) by step 2) rubber unvulcanizate that obtains thin-pass 4 ~ 6 times on twin shaft mixing roll, two-2 of silicone rubber matrix weight percentage 1.5% are added in thin-pass process, 5 vulcanizing agents, to carry out under 170 ° of C hot press moulding sulfuration 15 minutes, obtain the sheet silicon glue material of forming after thin-pass slice;
4) by the post cure 4 hours under 200 ° of C of the sheet silicon glue material of forming, the Thermal-conductive insulation silicone rubber thermal interface material of the sheet of the thickness 2mm removing small molecules volatile matter is obtained; Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 70 μm of ball-aluminium oxides 50% and 5 μm of ball-aluminium oxides 15% are composite.Described nano aluminium oxide, boron nitride are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
Test its correlated performance as follows:
In the present embodiment, described micrometer alumina is particle diameter is that two kinds of particle diameters are composite, and it changes three kinds or more into, and composite particle size range, at 2 μm ~ 100 μm, is also suitable for.Described surface treatment agent changes one or more in KH550, KH560, KH570, A151, Si-69 into, is also suitable for.Described softening agent changes hydroxy silicon oil, magnesiumcarbonate into, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000, is also suitable for.
Embodiment 4:
Thermal-conductive insulation silicone rubber thermal interface material that the present embodiment provides and preparation method thereof, all substantially the same with embodiment 1,2,3, its difference is, composition and the weight percent of this Thermal-conductive insulation silicone rubber thermal interface material are as follows:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 100 μm of ball-aluminium oxides 35% and 2 μm of ball-aluminium oxides 15% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 10nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 40 μm; Described ZnOw length-to-diameter ratio 20:1.Described surface treatment agent is KH550.Described softening agent is magnesiumcarbonate softening agent.
The preparation method of this Thermal-conductive insulation silicone rubber thermal interface material, in silicone rubber matrix, in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, the hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance.
Specific implementation process is as follows:
1) surface treatment of multiple dimensioned composite heat conductive filler: the dehydrated alcohol of 95 parts and 5 parts of deionized waters are made into alcohol solution, and regulate pH value to 4 with acetic acid; Add coupling agent KH550 according to the above ratio, induction stirring, after 10 minutes, obtains the KH550 surface treatment liquid prepared; The ZnOw of 100 μm of ball-aluminium oxides, 2 μm of ball-aluminium oxides, 10nm aluminum oxide, 40 μm of boron nitride and length-to-diameter ratio 20:1 is used the process of KH550 surface treatment liquid respectively, treatment condition are 60 ° of C, induction stirring 2 hours, dry after filtering, pulverizing, obtains the various heat conductive fillers that surface treatment is good; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) ZnOw of 100 μm of ball-aluminium oxides that surface treatment step 1) obtained is good, 40 μm of boron nitride, 2 μm of ball-aluminium oxides, 10nm aluminum oxide and length-to-diameter ratio 20:1, join successively in silicone rubber matrix according to order from big to small according to particle diameter, and add magnesiumcarbonate softening agent, vacuum kneading 30 minutes, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting insulating silicon rubber rubber unvulcanizate;
3) by step 2) rubber unvulcanizate that obtains thin-pass 4 ~ 6 times on twin shaft mixing roll, two-2 of silicone rubber matrix weight percentage 1.5% are added in thin-pass process, 5 vulcanizing agents, to carry out under 170 ° of C hot press moulding sulfuration 15 minutes, obtain the sheet silicon glue material of forming after thin-pass slice;
4) by the post cure 4 hours under 200 ° of C of the sheet silicon glue material of forming, the Thermal-conductive insulation silicone rubber thermal interface material of the sheet of the thickness 2mm removing small molecules volatile matter is obtained;
Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 100 μm of ball-aluminium oxides 35% and 2 μm of ball-aluminium oxides 15% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 10nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 40 μm; Described ZnOw length-to-diameter ratio 20:1.Described surface treatment agent is KH550.Described softening agent is magnesiumcarbonate softening agent.
Test its correlated performance as follows:
In the present embodiment, described micrometer alumina is particle diameter is that two kinds of particle diameters are composite, and it changes three kinds or more into, and composite particle size range, at 2 μm ~ 100 μm, is also suitable for.Described surface treatment agent changes one or more in KH550, KH560, KH570, A151, Si-69 into, is also suitable for.Described softening agent changes hydroxy silicon oil, magnesiumcarbonate into, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000, is also suitable for.
Embodiment 5: Thermal-conductive insulation silicone rubber thermal interface material that the present embodiment provides and preparation method thereof, all substantially the same with embodiment 1,2,3,4, its difference is, composition and the weight percent of this Thermal-conductive insulation silicone rubber thermal interface material are as follows:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 60 μm of ball-aluminium oxides 50% and 8 μm of ball-aluminium oxides 20% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 100nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 10 μm; Described ZnOw length-to-diameter ratio 15:1.Described surface treatment agent is KH550.Described softening agent is the methyl polysiloxane softening agent containing hydrolization group.
The preparation method of this Thermal-conductive insulation silicone rubber thermal interface material, in silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, the hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance.
Specific implementation process is as follows:
1) surface treatment of multiple dimensioned composite heat conductive filler: the dehydrated alcohol of 95 parts and 5 parts of deionized waters are made into alcohol solution, and regulate pH value to 4 with acetic acid; Add coupling agent KH550 according to the above ratio, induction stirring, after 10 minutes, obtains the KH550 surface treatment liquid prepared; The ZnOw of 60 μm of ball-aluminium oxides, 8 μm of ball-aluminium oxides, 100nm aluminum oxide, 10 μm of boron nitride and length-to-diameter ratio 1:15 is used the process of KH550 surface treatment liquid respectively, treatment condition are 60 ° of C, induction stirring 2 hours, dry after filtering, pulverizing, obtains the various heat conductive fillers that surface treatment is good; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) ZnOw of 60 μm of ball-aluminium oxides that surface treatment step 1) obtained is good, 10 μm of boron nitride, 8 μm of ball-aluminium oxides, 100nm aluminum oxide and length-to-diameter ratio 1:15, join successively in silicone rubber matrix according to order from big to small according to particle diameter, and the methyl polysiloxane softening agent added containing hydrolization group, vacuum kneading 30 minutes, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting insulating silicon rubber rubber unvulcanizate;
3) by step 2) rubber unvulcanizate that obtains thin-pass 4 ~ 6 times on twin shaft mixing roll, two-2 of silicone rubber matrix weight percentage 1.5% are added in thin-pass process, 5 vulcanizing agents, to carry out under 170 ° of C hot press moulding sulfuration 15 minutes, obtain the sheet silicon glue material of forming after thin-pass slice;
4) by the post cure 4 hours under 200 ° of C of the sheet silicon glue material of forming, the Thermal-conductive insulation silicone rubber thermal interface material of the sheet of the thickness 2mm removing small molecules volatile matter is obtained;
Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 60 μm of ball-aluminium oxides 50% and 8 μm of ball-aluminium oxides 20% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 100nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 10 μm; Described ZnOw length-to-diameter ratio 15:1.Described surface treatment agent is KH550.Described softening agent is the methyl polysiloxane softening agent containing hydrolization group.
Test its correlated performance as follows:
In the present embodiment, described micrometer alumina is particle diameter is that two kinds of particle diameters are composite, and it changes three kinds or more into, and composite particle size range, at 2 μm ~ 100 μm, is also suitable for.Described surface treatment agent changes one or more in KH550, KH560, KH570, A151, Si-69 into, is also suitable for.Described softening agent changes hydroxy silicon oil, magnesiumcarbonate into, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000, is also suitable for.
Embodiment 6: Thermal-conductive insulation silicone rubber thermal interface material that the present embodiment provides and preparation method thereof, all substantially the same with embodiment 1 ~ 5, its difference is, composition and the weight percent of this Thermal-conductive insulation silicone rubber thermal interface material are as follows:
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 40 μm of ball-aluminium oxides 25% and 2 μm of ball-aluminium oxides 5% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm; Described ZnOw length-to-diameter ratio 10:1.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
The preparation method of this Thermal-conductive insulation silicone rubber thermal interface material, in silicone rubber matrix, pass through softening agent, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler, and by the nano aluminium oxide of composite surface treatment agent process, boron nitride, ZnOw as auxiliary heat conduction filler, further raising thermal conductivity, reduces thermal resistance.
Specific implementation process is as follows:
1) surface treatment of multiple dimensioned composite heat conductive filler: the dehydrated alcohol of 95 parts and 5 parts of deionized waters are made into alcohol solution, and regulate pH value to 4 with acetic acid; Add coupling agent KH570 according to the above ratio, induction stirring, after 10 minutes, obtains the KH570 surface treatment liquid prepared; The ZnOw of 40 μm of ball-aluminium oxides, 2 μm of ball-aluminium oxides, 40nm aluminum oxide, 35 μm of boron nitride and length-to-diameter ratio 10:1 is used the process of KH570 surface treatment liquid respectively, treatment condition are 60 ° of C, induction stirring 2 hours, dry after filtering, pulverizing, obtains the various heat conductive fillers that surface treatment is good; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) ZnOw of 40 μm of ball-aluminium oxides that surface treatment step 1) obtained is good, 35 μm of boron nitride, 2 μm of ball-aluminium oxides, 40nm aluminum oxide and length-to-diameter ratio 10:1, join successively in silicone rubber matrix according to order from big to small according to particle diameter, and add hydroxy silicon oil softening agent, vacuum kneading 30 minutes, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting insulating silicon rubber rubber unvulcanizate;
3) by step 2) rubber unvulcanizate that obtains thin-pass 4 ~ 6 times on twin shaft mixing roll, two-2 of silicone rubber matrix weight percentage 1.5% are added in thin-pass process, 5 vulcanizing agents, to carry out under 170 ° of C hot press moulding sulfuration 15 minutes, obtain the sheet silicon glue material of forming after thin-pass slice;
4) by the post cure 4 hours under 200 ° of C of the sheet silicon glue material of forming, the Thermal-conductive insulation silicone rubber thermal interface material of the sheet of the thickness 2mm removing small molecules volatile matter is obtained; Each constituent mass per-cent of described heat conductive insulating silica gel heat interfacial material is as follows:
5) the heat conductive insulating silica gel heat interfacial material upper and lower surface of sheet step 4) obtained pastes one deck release film, to store and to use.
Wherein, described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and it is that 40 μm of ball-aluminium oxides 25% and 2 μm of ball-aluminium oxides 5% are composite.Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle diameter is 40nm; Described boron nitride is hexagonal boron nitride, and particle diameter is 35 μm; Described ZnOw length-to-diameter ratio 10:1.Described surface treatment agent is KH570.Described softening agent is hydroxy silicon oil softening agent.
Test its correlated performance as follows:
In the present embodiment, described micrometer alumina is particle diameter is that two kinds of particle diameters are composite, and it changes three kinds or more into, and composite particle size range, at 2 μm ~ 100 μm, is also suitable for.Described surface treatment agent changes one or more in KH550, KH560, KH570, A151, Si-69 into, is also suitable for.Described softening agent changes hydroxy silicon oil, magnesiumcarbonate into, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000, is also suitable for.
Be only better possible embodiments of the present invention described in upper, and be not used to limit to the scope of the claims of the present invention, therefore the equivalence change that all utilizations description of the present invention is done, be all included in protection scope of the present invention.
Claims (6)
1. a Thermal-conductive insulation silicone rubber thermal interface material, is characterized in that: it is made up of following mass percent component:
Described micrometer alumina is main heat conductive filler, and shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm; Described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler; Wherein, described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.
2. Thermal-conductive insulation silicone rubber thermal interface material as claimed in claim 1, is characterized in that: described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69.
3. Thermal-conductive insulation silicone rubber thermal interface material as claimed in claim 1, is characterized in that: described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
4. prepare a method for the described Thermal-conductive insulation silicone rubber thermal interface material of one of claims 1 to 3, it is characterized in that: its concrete preparation process comprises the following steps:
1) surface treatment of multiple dimensioned composite heat conductive filler: surface treatment agent is made into corresponding solution, then respectively surface treatment is carried out to the heat conductive filler of various different scale, process rear filtration, drying, pulverizing, obtain the heat conductive filler that various surface treatment is good; The heat conductive filler of described various different scale comprises micrometer alumina, nano aluminium oxide, boron nitride and ZnOw; Wherein, described micrometer alumina is main heat conductive filler, and described nano aluminium oxide, boron nitride, ZnOw are auxiliary heat conduction filler;
2) by step 1) heat conductive filler that the surface treatment that obtains is good joins in silicone rubber matrix according to order from big to small successively according to particle diameter, and add softening agent, vacuum kneading is carried out mixing in vacuum kneader, after taking out, normal temperature places 24 hours, obtains multiple dimensioned composite filling heat-conducting silicon rubber rubber unvulcanizate;
3) by step 2) the rubber unvulcanizate thin-pass on a mill until that obtains, add vulcanizing agent in thin-pass process, carry out hot press moulding sulfuration or calendering sulfidization molding after thin-pass, obtain the sheet silicon glue material of forming;
4) by step 3) the sheet silicon glue material high temperature secondary sulfuration of forming that obtains, obtain the Thermal-conductive insulation silicone rubber thermal interface material of the sheet removing small molecules volatile matter; Each constituent mass per-cent of described Thermal-conductive insulation silicone rubber thermal interface material is as follows:
In silicone rubber matrix, adopt the micrometer alumina of surface treatment agent process as main heat conductive filler, to reduce the viscosity of infill system, improve the loading level of heat conductive filler; Hardness after shaping by softening agent reduction heat-conducting insulating silicon rubber; By nano aluminium oxide, boron nitride, the ZnOw of composite surface treatment agent process, improve thermal conductivity further, reduce thermal resistance; Described micrometer alumina shape is spherical, and particle diameter is that multiple particle diameter is composite, and composite particle size range is at 2 μm ~ 100 μm; Described nano aluminium oxide particle size range is at 10 ~ 100nm; Described boron nitride is hexagonal boron nitride, and particle size range is at 1 ~ 40 μm; Described ZnOw length-to-diameter ratio is greater than 5:1.
5. prepare the method for Thermal-conductive insulation silicone rubber thermal interface material as claimed in claim 4, it is characterized in that: it is further comprising the steps of:
5) by step 4) the Thermal-conductive insulation silicone rubber thermal interface material upper and lower surface of sheet that obtains pastes one deck release film, to store and to use.
6. prepare the method for Thermal-conductive insulation silicone rubber thermal interface material as claimed in claim 4, it is characterized in that: described surface treatment agent is one or more in KH550, KH560, KH570, A151, Si-69; Described softening agent be hydroxy silicon oil, magnesiumcarbonate, containing one or more in the low polymerization degree polysiloxane of the methyl polysiloxane of hydrolization group, the polymerization degree 200 ~ 2000.
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