CN104788968A - Organosilicone heat conduction insulating piece and preparation method thereof - Google Patents
Organosilicone heat conduction insulating piece and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an organosilicone heat conduction insulating piece and a preparation method thereof. The organosilicone heat conduction insulating piece at least comprises a heat conduction insulating layer, wherein the heat conduction insulating layer is prepared from an organosilicone heat conduction insulating composition by using a sheet material forming process; the organosilicone heat conduction insulating piece comprises a substrate; the organosilicone heat conduction insulating composition is prepared from linear organopolysiloxane containing alkenyl, heat conduction packing, a cross-linking agent, a platinum catalyst, a vulcanizing agent and the like. The organosilicone heat conduction insulating piece disclosed by the invention is high in heat conductivity, good in insulating property, good in stabbing resistance and tearing resistance, flexible in adjusting product property, simple in preparation method and wide in adaptability.
Description
Technical field
The invention belongs to organosilicon material technical field, relate to a kind of organosilicon heat conductive isolation sheet and preparation method thereof.
Technical background
In the design of device miniaturization and ultrathin, the heat trnasfer between heating position and heat radiation position, sealing, insulation are one of key factors needing to consider, at present, heat conductive insulating packing material is the Main Means of this problem of solution.Heat conductive insulating packing material requires to have good heat conduction, insulating property, and has stronger stretching resistance under low thickness condition, can anti-puncture, anti tear, comprises heat-conducting silica gel sheet.
Heat-conducting silica gel sheet is using glass fibre etc. as base material, take silica gel as the organosilicon macromolecule polymer elastomer of material of main part, and by adding heat conduction in silica gel, fire-retardantly wait filler and there is heat conduction, flame retardant properties, usual in prior art is that material of main part prepares silica gel piece with low viscosity silicone rubber, under the prerequisite meeting manufacturing technique requirent, the heat conductivility of amount of filler and final sheet material can be improved, but the sheet material tear resistance of preparation is poor, poor reliability after application, or with polymer silicon raw rubber for material of main part, obtain the sheet material that tear resistance is good, but the media-filling rate of product is low, heat conductivility cannot be improved further.
Summary of the invention
For above-mentioned the deficiencies in the prior art, the invention provides a kind of organosilicon heat conductive isolation sheet and preparation method thereof, insulating trip prepared by the present invention can have high thermal conductivity coefficient, good insulating property and the mechanical property such as anti-puncture, anti tear simultaneously.
Object of the present invention is achieved through the following technical solutions:
The invention provides a kind of organosilicon heat conductive isolation sheet, it at least comprises thermally conductive insulating layer, and described thermally conductive insulating layer is prepared through sheet forming process by organosilicon heat conductive insulating composition, and described organosilicon heat conductive insulating composition comprises following component:
Base polymer: being the line style organopolysiloxane of the alkenyl containing two or more and silicon bonding, is 50 ~ 50000mpas at the viscositys of 25 DEG C;
Heat conductive filler;
Linking agent: being the organopolysiloxane containing more than three or three the hydrogen bases be connected with silicon, is 10-50000mpas at the viscositys of 25 DEG C;
Platinum catalyst and vulcanizing agent, described vulcanizing agent is organo-peroxide;
1 is greater than with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in described base polymer.
Described sheet forming process comprises calendering, mold pressing, curtain coating, injection molding, extrusion moulding etc.Preferably, described organosilicon heat conductive isolation sheet also comprises base material, and described thermally conductive insulating layer and described base material compound obtain organosilicon heat conductive isolation sheet, and now base material forms the substrate layer in heat conductive isolation sheet, obtains thermally conductive insulating layer by organosilicon heat conductive insulating composition.Comprising in the heat conductive isolation sheet of base material can containing multiple thermally conductive insulating layer of being arranged alternately and substrate layer.
Preferably, described base material is glasscloth, polyimide film, aluminium foil, poly-naphthalene ester film or carbon cloth.
Preferably, in described organosilicon heat conductive insulating composition, be greater than 1 with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in base polymer and be less than or equal to 3.5.
Preferably, in described organosilicon heat conductive insulating composition, organo-peroxide is specifically selected from 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, peroxidation two-(2,4-dichloro-benzoyl), peroxidation two (4-toluyl), dibenzoyl peroxide, peroxidized t-butyl perbenzoate, 1,1-bis(t-butylperoxy)-3,3, one or several in 5-trimethyl-cyclohexane, 1,1-bis(t-butylperoxy) cyclohexane.
In organosilicon heat conductive insulating composition, base polymer is the line style organopolysiloxane of the alkenyl containing two or more and silicon bonding, can be on molecule two ends or molecular chain with the position of the alkenyl of silicon bonding, or molecule two ends with on molecular chain simultaneously containing the alkenyl be connected with Siliciumatom.Preferably, described base polymer is selected from α, ω-divinyl polydimethylsiloxane, the polydimethylsiloxane of methyl phenyl vinyl siloxy end-blocking, the PSI of dimethyl ethenyl siloxy end-blocking, the methylphenyl siloxane of dimethyl ethenyl siloxy end-blocking and the multipolymer of dimethyl siloxane, the polycondensate of the polydimethylsiloxane of methyl methoxy base vinyl siloxy end-blocking, the poly-methyl (3 of dimethyl ethenyl siloxy end-blocking, 3, 3-trifluoro propyl) siloxanes, and the organopolysiloxane be expressed from the next: (CH
3)
2(CH
2=CH) SiO [(CH
3)
2siO]
n[(CH
3) PhSiO]
m[(CH
3) (CH
2=CH) SiO]
psi (CH=CH
2) (CH
3)
2in one or more.
Preferably, heat conductive filler is one or more in magnesium oxide, aluminum oxide, ferric oxide, calcium oxide, titanium oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon nitride.
Linking agent is the organopolysiloxane containing more than three or three the hydrogen bases be connected with silicon, and the position of the hydrogen base be connected with silicon can be on side chain or be positioned on molecular end and side chain simultaneously.Preferably, the hydrogen content of linking agent is 0.01-3% (quality).
Preferably, linking agent is 10-1000mpas at the viscosity of 25 DEG C.
Preferably, linking agent is selected from the polymethyl hydrogen siloxane of trimethylsiloxy group end-blocking, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and the multipolymer of dimethyl siloxane, the methyl hydrogen siloxane of dimethyl hydrogen siloxy end-blocking and the multipolymer of methylphenyl siloxane, the methyl hydrogen siloxane of dimethyl hydrogen siloxy end-blocking and the multipolymer of dimethyl siloxane, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and the multipolymer of methylphenyl siloxane, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and methyl (3, 3, 3-trifluoro propyl) multipolymer of siloxanes, one or more in Cyclic methyl hydrogen polysiloxanes or four (dimethyl hydrogen silicon alkoxyl group) silane.
Preferably, described organosilicon heat conductive insulating composition comprises chainextender, and for the line style organopolysiloxane of the hydrogen base be connected with silicon is contained at two ends, namely the end position group of its molecule two ends and silicon bonding all comprises hydrogen base, and all the other positions are not containing the hydrogen base be connected with Siliciumatom.
Preferably, the hydrogen content of described chainextender is 0.01%-0.5% (quality), is greater than 1 in the base polymer of now organosilicon heat conductive insulating composition with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight sum of the hydrogen base be connected with silicon in linking agent and chainextender.
Preferably, described chainextender is 100-50000mpas at the viscosity of 25 DEG C.
Preferably, described chainextender is selected from α, the poly-methyl (3 of ω-dihydro base polydimethylsiloxane, the polydimethylsiloxane of aminomethyl phenyl hydrogen siloxy end-blocking, the PSI of dimethyl hydrogen siloxy end-blocking and dimethyl hydrogen siloxy end-blocking, 3,3-trifluoro propyl) one or more in siloxanes.
Preferably, containing silicone resin in organosilicon heat conductive insulating composition, one or more in methyl phenyl silicone resin, methyl silicon resin, vinyl polysiloxane or Silicon Containing Hydrogen resin are selected from.
Preferably, described platinum catalyst is platinum catalyst or Platinic chloride.
Preferably, described organosilicon heat conductive insulating composition comprises following component according to the mass fraction:
More preferably, described organosilicon heat conductive insulating composition comprises following component according to the mass fraction:
The preparation method of above-mentioned organosilicon heat conductive isolation sheet, comprises following operation steps:
A, the component that organosilicon heat conductive insulating composition comprises to be mixed according to proportioning, obtain mixture;
B, mixture is made type, be cured at 40 ~ 90 DEG C, obtain one-step solidification sheet material;
C, be warming up to 110 ~ 250 DEG C sulfuration is carried out to one-step solidification sheet material, obtain organosilicon heat conductive isolation sheet.
Preferably, the time of described solidification is that mixture is cured to cross-linking density and reaches maximum value required time.
Namely described type of being made by mixture is adopt the techniques such as calendering, curtain coating, mold pressing, injection molding, extrusion moulding to be made by mixture to have certain thickness sheet material.
Preferably, the temperature of described sulfuration is than the temperature height 50-180 DEG C of described solidification.
Preferably, the time of described solidification is 5-30min.
Preferably, the time of described sulfuration is 3-120min.
The invention has the beneficial effects as follows: organosilicon heat conductive isolation sheet of the present invention is prepared by the method for regelate by organosilicon heat conductive insulating composition, there is high thermal conductivity coefficient, good insulating property and anti-puncture, tear resistance simultaneously, and product performance can flexible, wide adaptability, and preparation method is simple, application prospect is good.
Embodiment
The invention provides a kind of organosilicon heat conductive isolation sheet, it at least comprises thermally conductive insulating layer, and described thermally conductive insulating layer is prepared through sheet forming process by organosilicon heat conductive insulating composition, and described organosilicon heat conductive insulating composition comprises following component:
Base polymer: being the line style organopolysiloxane of the alkenyl containing two or more and silicon bonding, is 50 ~ 50000mpas at the viscositys of 25 DEG C;
Heat conductive filler;
Linking agent: being the organopolysiloxane containing more than three or three the hydrogen bases be connected with silicon, is 10-50000mpas at the viscositys of 25 DEG C;
Platinum catalyst and vulcanizing agent, described vulcanizing agent is organo-peroxide;
1 is greater than with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in described base polymer.
Described sheet forming process comprises calendering, mold pressing, curtain coating, injection molding, extrusion moulding etc.Preferably, described organosilicon heat conductive isolation sheet also comprises base material, described organosilicon heat conductive insulating composition and described base material compound obtain organosilicon heat conductive isolation sheet, and now base material forms the substrate layer in heat conductive isolation sheet, obtains thermally conductive insulating layer by organosilicon heat conductive insulating composition.Comprising in the heat conductive isolation sheet of base material can containing multiple thermally conductive insulating layer of being arranged alternately and substrate layer.
Preferably, described base material is glasscloth, polyimide film, aluminium foil, poly-naphthalene ester film or carbon cloth.
Preferably, in described organosilicon heat conductive insulating composition, be greater than 1 with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in base polymer and be less than or equal to 3.5.
In organosilicon heat conductive insulating composition, described organo-peroxide is specifically selected from 2,5-dimethyl-2,5-bis(t-butylperoxy) hexane, peroxidation two-(2,4-dichloro-benzoyl), peroxidation two (4-toluyl), dibenzoyl peroxide, peroxidized t-butyl perbenzoate, 1,1-bis(t-butylperoxy)-3,3, one or several in 5-trimethyl-cyclohexane, 1,1-bis(t-butylperoxy) cyclohexane.
In organosilicon heat conductive insulating composition, base polymer is the line style organopolysiloxane of the alkenyl containing two or more and silicon bonding, can be on molecule two ends or molecular chain with the position of the alkenyl of silicon bonding, or molecule two ends with on molecular chain simultaneously containing the alkenyl that is connected with Siliciumatom, the line style organopolysiloxane with the alkenyl of silicon bonding is contained at preferred molecule two ends.Wherein, alkenyl comprises vinyl, allyl group, butenyl or pentenyl, is preferably vinyl or allyl group.In base polymer with the group of silicon bonding besides alkenyl groups, also can comprise alkyl, cycloalkyl, aryl, aralkyl, alkoxyl group or haloalkyl, alkyl can enumerate methyl, ethyl, propyl group or butyl etc., cycloalkyl can enumerate cyclohexyl, cyclopentyl etc., and aryl can enumerate phenyl, tolyl, xylyl etc., and aralkyl can enumerate benzyl, styroyl etc., haloalkyl can enumerate 3,3,3-trifluoro propyl, alkoxyl group can enumerate methoxyl group, oxyethyl group, propoxy-etc.Be preferably methyl and phenyl.Base polymer can be the mixture of two or more the above linear organosilicon polysiloxane.
Base polymer is preferably 50 ~ 5000mpas at the viscosity of 25 DEG C, operability when ensureing the reactive behavior of polymkeric substance in base polymer and mix with heat conductive filler.
Base polymer can enumerate α, the methylphenyl siloxane of the polydimethylsiloxane of ω-divinyl polydimethylsiloxane, methyl phenyl vinyl siloxy end-blocking, the PSI of dimethyl ethenyl siloxy end-blocking, dimethyl ethenyl siloxy end-blocking and the multipolymer of dimethyl siloxane, the polycondensate of polydimethylsiloxane of methyl methoxy base vinyl siloxy end-blocking, the poly-methyl (3 of dimethyl ethenyl siloxy end-blocking, 3,3-trifluoro propyl) siloxanes, and the organopolysiloxane be expressed from the next: (CH
3)
2(CH
2=CH) SiO [(CH
3)
2siO]
n[(CH
3) PhSiO]
m[(CH
3) (CH
2=CH) SiO]
psi (CH=CH
2) (CH
3)
2.
Heat conductive filler can enumerate the metal oxides such as aluminum oxide, zinc oxide, titanium oxide, beryllium oxide; The metal hydroxides such as aluminium hydroxide, magnesium hydroxide; The nitride such as aluminium nitride, silicon nitride, boron nitride; The carbide such as silicon carbide, norbide; And the mixture of above-mentioned substance, be preferably one or more in silicon carbide, magnesium oxide, aluminum oxide, ferric oxide, calcium oxide, titanium oxide, silicon-dioxide, aluminium nitride, boron nitride and silicon nitride.
Preferably, heat conductive filler to be median size the be heat conductive filler of 20-100 μm and median size are the mixture of one or more in the heat conductive filler of 1-10 μm 0.1-1 μm, less than 0.1 μm.
Preferably, heat conductive filler to be median size the be heat conductive filler of 20-100 μm and median size be the heat conductive filler of 1-10 μm according to mass ratio (2-4): (3-1) is mixed to get.
Preferably surface modification treatment is carried out to heat conductive filler, the method of surface modification treatment and treatment agent are without particular restriction, spray method is such as adopted to spray silane coupling agent at heat conductive filler surface uniform, silane coupling agent comprises one or more in KH-550, KH-560, KH-570, KH-792, A-1160, A-171, treatment process is not limit, and the conductive powder after surface treatment also can directly be bought.Preferably carry out drying to heat conductive filler before use, drying conditions is preferably at 90-150 DEG C of dry 1-8h.
In reality, heat conductive filler partly or entirely can replace with fire-retardant filler, color stuffing etc., makes material meet corresponding performance requriements.
Linking agent is the organopolysiloxane containing more than three or three the hydrogen bases be connected with silicon, and the position of the hydrogen base be connected with silicon can be on side chain or be positioned on molecular end and side chain simultaneously.Except the hydrogen base with silicon bonding in the molecular structure of linking agent, also can comprise alkyl, cycloalkyl, aryl, aralkyl or haloalkyl, alkyl can enumerate methyl, ethyl, propyl group or butyl etc., cycloalkyl can enumerate cyclohexyl, cyclopentyl etc., aryl can enumerate phenyl, tolyl, xylyl etc., and aralkyl can enumerate benzyl, styroyl etc., and haloalkyl can enumerate 3,3,3-trifluoro propyl.Preferred alkyl and aryl, more preferably methyl and phenyl.
The molecular structure of linking agent is not particularly limited, it can be the molecular structure with side chain, straight chain, the straight chain of part branching, ring-type or a shape, can for having single polymers or the mixture of these structures, preferably its hydrogen content is 0.01-3% (quality), and in the present invention, hydrogen content is the mass percent of the hydrogen base be connected with silicon in linking agent.Linking agent is preferably 10-1000mpas at the viscosity of 25 DEG C, is more preferably 10-500mpas.
Linking agent can enumerate the polymethyl hydrogen siloxane of trimethylsiloxy group end-blocking, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and the multipolymer of dimethyl siloxane, the methyl hydrogen siloxane of dimethyl hydrogen siloxy end-blocking and the multipolymer of methylphenyl siloxane, the methyl hydrogen siloxane of dimethyl hydrogen siloxy end-blocking and the multipolymer of dimethyl siloxane, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and the multipolymer of methylphenyl siloxane, the methyl hydrogen siloxane of trimethylsiloxy group end-blocking and methyl (3, 3, 3-trifluoro propyl) multipolymer of siloxanes, Cyclic methyl hydrogen polysiloxanes or four (dimethyl hydrogen silicon alkoxyl group) silane.
Preferably, described organosilicon heat conductive insulating composition comprises chainextender, and for the line style organopolysiloxane of the hydrogen base be connected with silicon is contained at two ends, namely the end position group of its molecule two ends and silicon bonding all comprises hydrogen base, and all the other positions are not containing the hydrogen base be connected with Siliciumatom.After adding chainextender there is the transfer reaction after alkenyl and si-h bond addition in composition in reaction process, the mechanical properties such as the tensile strength of adjustable final piece.
In the molecular structure of chainextender, with silicon bonding can also comprise alkyl, cycloalkyl, aryl, aralkyl or haloalkyl except hydrogen base, alkyl can enumerate methyl, ethyl, propyl group or butyl etc., cycloalkyl can enumerate cyclohexyl, cyclopentyl etc., aryl can enumerate phenyl, tolyl, xylyl etc., and aralkyl can enumerate benzyl, styroyl etc., and haloalkyl can enumerate 3,3,3-trifluoro propyl.Preferred alkyl and aryl, more preferably methyl and phenyl.Chainextender can be the mixture of two or more the above straight-chain organosilicon polysiloxanes.
The hydrogen content of chainextender is 0.01%-0.5% (quality), is greater than 1 in the base polymer of now organosilicon heat conductive insulating composition with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight sum of the hydrogen base be connected with silicon in linking agent and chainextender.Chainextender is 100-50000mpas at the viscosity of 25 DEG C, is preferably 100-10000mpas, most preferably is 100-5000mpas.
Chainextender can enumerate α, the poly-methyl (3 of ω-dihydro base polydimethylsiloxane, the polydimethylsiloxane of aminomethyl phenyl hydrogen siloxy end-blocking, the PSI of dimethyl hydrogen siloxy end-blocking and dimethyl hydrogen siloxy end-blocking, 3,3-trifluoro propyl) siloxanes etc.
Preferably, containing silicone resin in organosilicon heat conductive insulating composition, it is the organopolysiloxane with cross-linked structure, the hardness after composition solidification and tear resistance can be improved, be selected from methyl phenyl silicone resin, methyl silicon resin, vinyl polysiloxane, Silicon Containing Hydrogen resin etc., concrete structure and consumption thereof are not particularly limited.
Platinum catalyst is not particularly limited, and can enumerate platinum micro mist, platinum black, Platinic chloride, Tetrachloroplatinum, the platinum complex of alkene, the platinum complex of carbonyl or the thermoplasticity organic resin powder containing above platinum group catalyst, be preferably platinum catalyst or Platinic chloride.
Above-mentioned organosilicon heat conductive insulating composition, preferably includes following component according to the mass fraction:
This organosilicon heat conductive insulating composition more preferably comprises following component according to the mass fraction:
The preparation method of above-mentioned organosilicon heat conductive isolation sheet, comprises following operation steps:
A, the component that organosilicon heat conductive insulating composition comprises to be mixed according to proportioning, obtain mixture;
B, mixture is made type, be cured at 40 ~ 90 DEG C, obtain one-step solidification sheet material;
C, be warming up to 110 ~ 250 DEG C sulfuration is carried out to one-step solidification sheet material, obtain organosilicon heat conductive isolation sheet.
Namely described type of being made by mixture is adopt the techniques such as calendering, curtain coating, mold pressing, injection molding, extrusion moulding to be made by mixture to have certain thickness sheet material.
Preferably, when described organosilicon heat conductive isolation sheet also comprises base material, in stepb, with base material compound while mixture is made type, be then cured.
Preferably, the time of described solidification is that mixture is cured to cross-linking density and reaches maximum value required time.The time of described solidification can by obtaining testing on vulkameter after mixture sampling, vulkameter model is high ferro M-3000A, sampling amount is 6g ± 0.5g, by moment of torsion (corresponding cross-linking density) in mensuration mixture at a certain temperature sulfidation over time, obtain required time when moment of torsion reaches maximum value, be set time.
Preferably, the time of described solidification is 5-30min.
Preferably, the time of described sulfuration is 3-120min.
In the preparation method of organosilicon heat conductive isolation sheet, preferably, the temperature of described sulfuration is than the temperature height 50-180 DEG C of described solidification.
In the preparation method of organosilicon heat conductive isolation sheet, the time of mixing, preferred 3-20min, carried out at normal temperatures in kneader without particular restriction.
In the preparation method of organosilicon heat conductive isolation sheet, mixing is preferably carried out under vacuum, and it is-0.09Mpa ~-0.1Mpa that vacuum condition is preferably relative vacuum degree.
It may be noted that the viscosity of 25 DEG C of the present invention is the kinetic viscosity value of material at 25 DEG C.
Provide the specific embodiment of organosilicon heat conductive insulating composition of the present invention and organosilicon heat conductive isolation sheet below.
In embodiment 1 ~ 3 for the preparation of the organosilicon heat conductive insulating composition proportioning of organosilicon heat conductive isolation sheet in table 1, unit is mass fraction.
Table 1
Embodiment 1
In organosilicon heat conductive insulating composition, base polymer is 25 DEG C of viscositys is the α of 100mpas, ω-divinyl polydimethylsiloxane (mass percentage of vinyl is 2.5%); Heat conductive filler to be median size the be aluminum oxide of 30 μm; Linking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 100mpas, and hydrogen content is 0.2% (quality); Chainextender is 25 DEG C of viscositys is the α of 100mpas, ω-dihydro base polydimethylsiloxane (hydrogen content is 0.18% (quality)).Base polymer medium vinyl (-CH=CH
2) molar weight and linking agent and chainextender in the ratio of molar weight sum of hydrogen base be 2.87.
In organosilicon heat conductive insulating composition, silicone resin is DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile, platinum catalyst is platinum catalyst, and vulcanizing agent is bis(2，4-dichlorobenzoyl)peroxide.
The preparation method of organosilicon heat conductive isolation sheet, comprises following operation steps:
Test set time: heat conductive filler is placed in 100 DEG C of dry 3h, then base polymer, heat conductive filler, linking agent, chainextender, silicone resin, vulcanizing agent and platinum catalyst is got according to described number, 3min is mixed under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, get 6g mixture to test on high ferro M-3000A sulphur change instrument, setting temperature of reaction is 80 DEG C, record moment of torsion over time, getting moment of torsion, to reach time corresponding to maximum value be set time, and recording set time is 5min.
Getting the mixing of base polymer, heat conductive filler, linking agent, chainextender, silicone resin, vulcanizing agent and platinum catalyst according to described number adds in kneader, 10min is mediated under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, mixture and glasscloth are carried out calendering compound, carry out two sides coated with PET film simultaneously, reaction 5min is cured at 80 DEG C after shaping, removing PET film, obtain the one-step solidification sheet material that thickness is 0.3mm, by one-step solidification sheet material again in 120 DEG C of sulfuration 40min, obtain organosilicon heat conductive isolation sheet.
Embodiment 2
In organosilicon heat conductive insulating composition, base polymer is 25 DEG C of viscositys is the α of 4000mpas, ω-divinyl polydimethylsiloxane (mass percentage of vinyl is 0.50%); Heat conductive filler to be median size the be aluminium nitride of 20 μm; Linking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 1000mpas, and hydrogen content is 0.08% (quality); Chainextender is 25 DEG C of viscositys is the α of 1000mpas, ω-dihydro base polydimethylsiloxane (hydrogen content is 0.05% (quality)).Base polymer medium vinyl (-CH=CH
2) molar weight and linking agent and chainextender in the ratio of molar weight sum of hydrogen base be 1.27.
In organosilicon heat conductive insulating composition, silicone resin is DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile, platinum catalyst is platinum catalyst, and vulcanizing agent is bis(2，4-dichlorobenzoyl)peroxide.
The preparation method of organosilicon heat conductive isolation sheet, comprises following operation steps:
Test set time: heat conductive filler is placed in 100 DEG C of dry 3h, then base polymer, heat conductive filler, linking agent, chainextender, silicone resin, vulcanizing agent and platinum catalyst is got according to described number, 3min is mixed under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, get 6g mixture to test on high ferro M-3000A sulphur change instrument, setting temperature of reaction is 70 DEG C, record moment of torsion over time, getting moment of torsion, to reach time corresponding to maximum value be set time, and recording set time is 12min.
Getting the mixing of base polymer, heat conductive filler, linking agent, chainextender, silicone resin, vulcanizing agent and platinum catalyst according to described number adds in kneader, 10min is mediated under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, mixture and glasscloth are carried out calendering compound, carry out two sides coated with PET film simultaneously, reaction 12min is cured at 70 DEG C after shaping, removing PET film, obtain the one-step solidification sheet material that thickness is 0.3mm, by one-step solidification sheet material again in 120 DEG C of sulfuration 30min, obtain organosilicon heat conductive isolation sheet.
Embodiment 3
In organosilicon heat conductive insulating composition, base polymer is 25 DEG C of viscositys is the α of 40000mpas, ω-divinyl polydimethylsiloxane (mass percentage of vinyl is 0.20%), heat conductive filler to be median size the be aluminum oxide of 3 μm and median size be 50 μm aluminum oxide in mass ratio 2:3 be mixed to get; Linking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 10000mpas, and hydrogen content is 0.03% (quality).Base polymer medium vinyl (-CH=CH
2) molar weight be 1.54 with the ratio of the molar weight of hydrogen base in linking agent.
In organosilicon heat conductive insulating composition, silicone resin is DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile, platinum catalyst is platinum catalyst, and vulcanizing agent is two (tert-butyl peroxide) hexane of 2,5-dimethyl-2,5-.
The preparation method of organosilicon heat conductive isolation sheet, comprises following operation steps:
Test set time: heat conductive filler is placed in 100 DEG C of dry 3h, then base polymer, heat conductive filler, linking agent, silicone resin, vulcanizing agent and platinum catalyst is got according to described number, 10min is mixed under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, get 6g mixture to test on high ferro M-3000A sulphur change instrument, setting temperature of reaction is 50 DEG C, record moment of torsion over time, getting moment of torsion, to reach time corresponding to maximum value be set time, and recording set time is 25min.
Getting the mixing of base polymer, heat conductive filler, linking agent, silicone resin, vulcanizing agent and platinum catalyst according to described number adds in kneader, 10min is mediated under normal temperature and-0.09MPa relative vacuum degree condition, obtain mixture, mixture is injected the die cavity that 0.3mm is thick, at 50 DEG C of solidification 25min after compression molding, obtain the one-step solidification sheet material that thickness is 0.3mm, by one-step solidification sheet material again in 170 DEG C of sulfuration 30min, obtain organosilicon heat conductive isolation sheet.
Testing example
Carry out performance test to organosilicon heat conductive isolation sheet prepared by embodiment 1 ~ 3, comprise thermal conductivity, hardness, tensile strength, tear strength, volume specific resistance and voltage breakdown, test and performance data are in table 2.
Table 2 organosilicon heat conductive isolation sheet performance data
From table 2 data, the present invention is to prepare organosilicon heat conductive isolation sheet containing vinyl polysiloxane, heat conductive filler, linking agent, platinum catalyst and vulcanizing agent for raw material, and by the special process of regelate, make final insulating trip possess high heat conduction, high rigidity and good tear resistance simultaneously, meet in practical application the heating thermal conductivity of heat dissipation interface and the requirement of usability, over-all properties is given prominence to, and preparation method is simple, and application prospect is wide.
Finally it should be noted that above embodiment only in order to technical scheme of the present invention to be described but not limiting the scope of the invention.It will be understood by those of skill in the art that and can carry out some deductions or equivalent replacement to technical scheme of the present invention, and do not depart from essence and the scope of technical solution of the present invention.
Claims (9)
1. an organosilicon heat conductive isolation sheet, it at least comprises thermally conductive insulating layer, and described thermally conductive insulating layer is obtained through sheet forming process by organosilicon heat conductive insulating composition, and described organosilicon heat conductive insulating composition comprises following component:
Base polymer: being the line style organopolysiloxane of the alkenyl containing two or more and silicon bonding, is 50 ~ 50000mpas at the viscositys of 25 DEG C;
Heat conductive filler;
Linking agent: be containing the organopolysiloxane of more than three or three the hydrogen bases be connected with silicon, the viscositys of 25 DEG C be 10 ?50000mpas;
Platinum catalyst and vulcanizing agent, described vulcanizing agent is organo-peroxide;
1 is greater than with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in described base polymer.
2. organosilicon heat conductive isolation sheet as claimed in claim 1, it is characterized in that, described organosilicon heat conductive isolation sheet also comprises base material, and described thermally conductive insulating layer and described base material compound obtain organosilicon heat conductive isolation sheet.
3. organosilicon heat conductive isolation sheet as claimed in claim 2, is characterized in that, described base material is glasscloth, polyimide film, aluminium foil, poly-naphthalene ester film or carbon cloth.
4. the organosilicon heat conductive isolation sheet as described in claim 1,2 or 3, it is characterized in that, in described organosilicon heat conductive insulating composition, be greater than 1 with the molar weight of the alkenyl of silicon bonding with the ratio of the molar weight of the hydrogen base be connected with silicon in linking agent in base polymer and be less than or equal to 3.5.
5. the organosilicon heat conductive isolation sheet as described in claim 1,2 or 3, is characterized in that, described organosilicon heat conductive insulating composition comprises chainextender, and chainextender is the line style organopolysiloxane that the hydrogen base be connected with silicon is contained at two ends.
6. the organosilicon heat conductive isolation sheet as described in claim 1,2 or 3, is characterized in that, described organosilicon heat conductive insulating composition comprises following component according to the mass fraction:
7. organosilicon heat conductive isolation sheet as claimed in claim 5, it is characterized in that, described organosilicon heat conductive insulating composition comprises following component according to the mass fraction:
8. the preparation method of organosilicon heat conductive isolation sheet as claimed in claim 1 or 2, is characterized in that comprising following operation steps:
A, the component that organosilicon heat conductive insulating composition comprises to be mixed according to proportioning, obtain mixture;
B, mixture is made type, be cured at 40 ~ 90 DEG C, obtain one-step solidification sheet material;
C, be warming up to 110 ~ 250 DEG C sulfuration is carried out to one-step solidification sheet material, obtain organosilicon heat conductive isolation sheet.
9. the preparation method of organosilicon heat conductive isolation sheet as claimed in claim 7, the temperature higher than the temperature of described solidification 50 of described sulfuration ?180 DEG C.
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