CN104788968B - Organosilicon heat-conducting insulating sheet and preparation method thereof - Google Patents

Organosilicon heat-conducting insulating sheet and preparation method thereof Download PDF

Info

Publication number
CN104788968B
CN104788968B CN201510191264.4A CN201510191264A CN104788968B CN 104788968 B CN104788968 B CN 104788968B CN 201510191264 A CN201510191264 A CN 201510191264A CN 104788968 B CN104788968 B CN 104788968B
Authority
CN
China
Prior art keywords
heat conductive
organosilicon heat
organosilicon
hydrogen
isolation sheet
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510191264.4A
Other languages
Chinese (zh)
Other versions
CN104788968A (en
Inventor
李云
张耀湘
覃剑
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHENZHEN ANPIN SILICONE MATERIAL CO Ltd
Original Assignee
SHENZHEN ANPIN SILICONE MATERIAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHENZHEN ANPIN SILICONE MATERIAL CO Ltd filed Critical SHENZHEN ANPIN SILICONE MATERIAL CO Ltd
Priority to CN201510191264.4A priority Critical patent/CN104788968B/en
Publication of CN104788968A publication Critical patent/CN104788968A/en
Application granted granted Critical
Publication of CN104788968B publication Critical patent/CN104788968B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Compositions Of Macromolecular Compounds (AREA)
  • Laminated Bodies (AREA)

Abstract

The invention discloses an organosilicon heat-conducting insulating sheet and a preparation method thereof, wherein the organosilicon heat-conducting insulating sheet at least comprises a heat-conducting insulating layer, the heat-conducting insulating layer is prepared from an organosilicon heat-conducting insulating composition by a sheet forming process, the organosilicon heat-conducting insulating sheet can comprise a base material, and the organosilicon heat-conducting insulating composition is prepared from linear organopolysiloxane containing alkenyl, heat-conducting filler, a cross-linking agent, a platinum catalyst, a vulcanizing agent and the like. The organic silicon heat-conducting insulating sheet has high heat-conducting property, good insulating property, puncture resistance and tear resistance, the product performance can be flexibly adjusted, the preparation method is simple, and the adaptability is wide.

Description

Organosilicon heat conductive isolation sheet and preparation method thereof
Technical field
The invention belongs to organosilicon material technical field, it is related 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 between heating position and heat dissipation position is transmitted, sealing, insulate It is one of key factor needed to be considered, currently, heat conductive insulating packing material is to solve the problems, such as this main means.Heat conductive insulating Packing material has stronger stretching resistance under the conditions of requiring good heat conduction, insulation performance and low thickness, can resist thorn It wears, tear-proof, including heat-conducting silica gel sheet.
Heat-conducting silica gel sheet be using glass fibre etc. as base material, based on silica gel material organosilicon macromolecule polymer Elastomer, and there is heat conduction, flame retardant property by heat conduction, the fillers such as fire-retardant are added in silica gel, in the prior art usually with Amount of filler and most can be improved under the premise of meeting manufacturing technique requirent in material preparation silica gel piece based on low viscosity silicone rubber The heat conductivility of whole sheet material, but the sheet material tear resistance prepared is poor, using rear poor reliability, or with macromolecule silicon raw rubber Based on material, obtain the good sheet material of tear resistance, but the media-filling rate of product is low, can not further increase thermal conductivity Energy.
Invention content
In view of the above shortcomings of the prior art, a kind of organosilicon heat conductive isolation sheet of present invention offer and preparation method thereof, this Insulating trip prepared by invention can have the mechanical properties such as high thermal conductivity coefficient, good insulation performance and anti-puncture, tear-proof simultaneously.
The purpose of the present invention is achieved through the following technical solutions:
The present invention provides a kind of organosilicon heat conductive isolation sheet, includes at least thermally conductive insulating layer, the thermally conductive insulating layer by Organosilicon heat conductive insulating composition is prepared through sheet forming process, and the organosilicon heat conductive insulating composition includes with the following group Point:
Base polymer:For the line style organopolysiloxane containing two or more and the alkenyl of silicon bonding, 25 DEG C viscosity be 50~50000mpas;
Heat filling;
Crosslinking agent:Organopolysiloxane for the hydrogen-based being connect with silicon containing three or three or more is in 25 DEG C of viscositys 10-50000mpa·s;
Platinum catalyst and vulcanizing agent, the vulcanizing agent are organic peroxide;
It rubs with the hydrogen-based that is connect with silicon in the mole of the alkenyl of silicon bonding and crosslinking agent in the base polymer The ratio between your amount is more than 1.
The sheet forming process includes calendering, molding, curtain coating, injection moulding, extrusion molding etc..Preferably, described to have Machine silicon heat conductive isolation sheet further includes base material, the thermally conductive insulating layer and the compound obtained organosilicon heat conductive isolation sheet of the base material, this Shi Jicai forms the substrate layer in heat conductive isolation sheet, and thermally conductive insulating layer is made by organosilicon heat conductive insulating composition.Including base material Heat conductive isolation sheet in can contain multiple thermally conductive insulating layer being arranged alternately and substrate layer.
Preferably, the base material is glass fabric, polyimide film, aluminium foil, poly- naphthalene ester film or carbon cloth.
Preferably, in the organosilicon heat conductive insulating composition, in base polymer with mole of the alkenyl of silicon bonding It measures and is more than 1 less than or equal to 3.5 with the ratio between the mole of hydrogen-based being connect with silicon in crosslinking agent.
Preferably, in the organosilicon heat conductive insulating composition, organic peroxide is chosen in particular from 2,5- dimethyl -2,5- Bis(t-butylperoxy) hexane, peroxidating pair-(2,4 dichloro benzene formyl), peroxidating bis- (4- toluyls), peroxidating Dibenzoyl, peroxidized t-butyl perbenzoate, 1,1- bis(t-butylperoxy) -3,3,5- trimethyl-cyclohexanes, the bis- (uncles of 1,1- Butyl peroxy) one or several kinds in hexamethylene.
In organosilicon heat conductive insulating composition, base polymer is containing two or more and the alkenyl of silicon bonding Line style organopolysiloxane, with the position of the alkenyl of silicon bonding can be on molecule both ends or strand or molecule both ends with Contain the alkenyl being connect with silicon atom on strand simultaneously.Preferably, the base polymer is selected from α, and ω-divinyl is poly- Dimethyl siloxane, the dimethyl silicone polymer of methyl phenyl vinyl siloxy sealing end, dimethylvinyl siloxy sealing end Polymethylphenylsiloxane, dimethylvinyl siloxy sealing end methyl phenyl siloxane and dimethyl siloxane copolymerization Condensation polymer, the dimethylvinyl siloxy sealing end for the dimethyl silicone polymer that object, methyl methoxy base vinyl siloxy block Poly- methyl (3,3,3- trifluoro propyl) siloxanes, and the organopolysiloxane that is expressed from the next:(CH3)2(CH2=CH) SiO [(CH3)2SiO]n[(CH3)PhSiO]m[(CH3)(CH2=CH) SiO]pSi (CH=CH2)(CH3)2One or more of.
Preferably, heat filling be magnesia, aluminium oxide, iron oxide, calcium oxide, titanium oxide, silica, aluminium nitride, One or more of boron nitride and silicon nitride.
Crosslinking agent is the organopolysiloxane for the hydrogen-based being connect with silicon containing three or three or more, and the hydrogen-based being connect with silicon Position can be located in molecular end and side chain on side chain or simultaneously.Preferably, the hydrogen content of crosslinking agent is 0.01- 3% (quality).
Preferably, crosslinking agent is 10-1000mpas in 25 DEG C of viscosity.
Preferably, crosslinking agent is selected from the polymethyl hydrogen siloxane of trimethylsiloxy group sealing end, trimethylsiloxy group blocks The methyl hydrogen siloxane and aminomethyl phenyl of the copolymer of methyl hydrogen siloxane and dimethyl siloxane, dimethyl hydrogen siloxy sealing end Copolymer, the trimethyl of the copolymer of siloxanes, the methyl hydrogen siloxane and dimethyl siloxane of dimethyl hydrogen siloxy sealing end The methyl hydrogen silica of the methyl hydrogen siloxane of siloxy sealing end and the copolymer of methyl phenyl siloxane, trimethylsiloxy group sealing end Copolymer, cyclic methyl hydrogen polysiloxane or four (the dimethyl hydrogen silane oxygen of alkane and methyl (3,3,3- trifluoro propyl) siloxanes One or more of base) silane.
Preferably, the organosilicon heat conductive insulating composition includes chain extender, contains the hydrogen-based being connect with silicon for both ends Line style organopolysiloxane, i.e. its molecule both ends and the end of silicon bonding position group include hydrogen-based, remaining position is free of and silicon original The hydrogen-based of son connection.
Preferably, the hydrogen content of the chain extender is 0.01%-0.5% (quality), and organosilicon heat conductive insulating combines at this time It rubs with the mole of the alkenyl of silicon bonding and the hydrogen-based that is connect with silicon in crosslinking agent and chain extender in the base polymer of object The ratio of the sum of your amount is more than 1.
Preferably, the chain extender is 100-50000mpas in 25 DEG C of viscosity.
Preferably, the chain extender is selected from α, and ω-two hydrogen-baseds dimethyl silicone polymer, aminomethyl phenyl hydrogen siloxy block The poly- first of dimethyl silicone polymer, the polymethylphenylsiloxane of dimethyl hydrogen siloxy sealing end and dimethyl hydrogen siloxy sealing end One or more of base (3,3,3- trifluoro propyl) siloxanes.
Preferably, contain silicones in organosilicon heat conductive insulating composition, selected from methyl phenyl silicone resin, methyl silicon tree One or more of fat, vinyl polysiloxane or hydrogeneous silicones.
Preferably, the platinum catalyst is platinum catalyst or chloroplatinic acid.
Preferably, the organosilicon heat conductive insulating composition includes following components by weight:
It is highly preferred that the organosilicon heat conductive insulating composition includes following components by weight:
The preparation method of above-mentioned organosilicon heat conductive isolation sheet, including following operating procedure:
A, the component for being included by organosilicon heat conductive insulating composition is uniformly mixed according to proportioning, obtains mixture;
B, type is made in mixture, is cured at 40~90 DEG C, obtain one-step solidification sheet material;
C, 110~250 DEG C are warming up to vulcanize one-step solidification sheet material, obtains organosilicon heat conductive isolation sheet.
Preferably, the cured time, which is cured for mixture to crosslink density, reaches maximum value required time.
It is described that type is made in mixture is that will be mixed using calendering, curtain coating, molding, injection moulding, the techniques such as extrusion molding Object is closed to be made with certain thickness sheet material.
Preferably, the temperature of the vulcanization is 50-180 DEG C higher than the cured temperature.
Preferably, the cured time is 5-30min.
Preferably, the time of the vulcanization is 3-120min.
The beneficial effects of the invention are as follows:The organosilicon heat conductive isolation sheet of the present invention is passed through by organosilicon heat conductive insulating composition The method of secondary curing is prepared, while having high thermal conductivity coefficient, good insulation performance and anti-puncture, tear resistance, And properties of product can flexible modulation, wide adaptability, and preparation method is simple, application prospect is good.
Specific implementation mode
The present invention provides a kind of organosilicon heat conductive isolation sheet, includes at least thermally conductive insulating layer, the thermally conductive insulating layer by Organosilicon heat conductive insulating composition is prepared through sheet forming process, and the organosilicon heat conductive insulating composition includes with the following group Point:
Base polymer:For the line style organopolysiloxane containing two or more and the alkenyl of silicon bonding, 25 DEG C viscosity be 50~50000mpas;
Heat filling;
Crosslinking agent:Organopolysiloxane for the hydrogen-based being connect with silicon containing three or three or more is in 25 DEG C of viscositys 10-50000mpa·s;
Platinum catalyst and vulcanizing agent, the vulcanizing agent are organic peroxide;
It rubs with the hydrogen-based that is connect with silicon in the mole of the alkenyl of silicon bonding and crosslinking agent in the base polymer The ratio between your amount is more than 1.
The sheet forming process includes calendering, molding, curtain coating, injection moulding, extrusion molding etc..Preferably, described to have Machine silicon heat conductive isolation sheet further includes base material, the organosilicon heat conductive insulating composition and the compound obtained organosilicon heat conduction of the base material Insulating trip, at this time base material formed heat conductive isolation sheet in substrate layer, by organosilicon heat conductive insulating composition be made thermally conductive insulating layer. Multiple thermally conductive insulating layer being arranged alternately and substrate layer can be contained in heat conductive isolation sheet including base material.
Preferably, the base material is glass fabric, polyimide film, aluminium foil, poly- naphthalene ester film or carbon cloth.
Preferably, in the organosilicon heat conductive insulating composition, in base polymer with mole of the alkenyl of silicon bonding It measures and is more than 1 less than or equal to 3.5 with the ratio between the mole of hydrogen-based being connect with silicon in crosslinking agent.
In organosilicon heat conductive insulating composition, the organic peroxide is chosen in particular from bis- (the tertiary fourths of 2,5- dimethyl -2,5- Base peroxy) hexane, peroxidating be double-(2,4 dichloro benzene formyl), peroxidating bis- (4- toluyls), diphenyl peroxide first Acyl, peroxidized t-butyl perbenzoate, 1,1- bis(t-butylperoxy) -3,3,5- trimethyl-cyclohexanes, bis- (the tertiary butyl mistakes of 1,1- Oxygroup) one or several kinds in hexamethylene.
In organosilicon heat conductive insulating composition, base polymer is containing two or more and the alkenyl of silicon bonding Line style organopolysiloxane, with the position of the alkenyl of silicon bonding can be on molecule both ends or strand or molecule both ends with Contain the alkenyl being connect with silicon atom on strand simultaneously, preferably molecule both ends are contained has with the line style of the alkenyl of silicon bonding Machine polysiloxanes.Wherein, alkenyl includes vinyl, allyl, cyclobutenyl or pentenyl, preferably vinyl or allyl. In base polymer besides alkenyl groups with the group of silicon bonding, it may also include alkyl, naphthenic base, aryl, aralkyl, alkoxy Or halogenated alkyl, alkyl can enumerate methyl, ethyl, propyl or butyl etc., naphthenic base can enumerate cyclohexyl, cyclopenta etc., aryl Phenyl, tolyl, xylyl etc. can be enumerated, aralkyl can enumerate benzyl, phenethyl etc., and halogenated alkyl can enumerate 3,3,3- tri- Fluoropropyl, alkoxy can enumerate methoxyl group, ethyoxyl, propoxyl group etc..Preferably methyl and phenyl.Base polymer can be two kinds Or the mixture of a variety of linear organosilicon polysiloxanes described above.
Base polymer is preferably 50~5000mpas in 25 DEG C of viscosity, ensures the anti-of polymer in base polymer Operability when answering activity and being mixed with heat filling.
Base polymer can enumerate α, ω-divinyl polydimethylsiloxane, methyl phenyl vinyl siloxy sealing end Dimethyl silicone polymer, dimethylvinyl siloxy sealing end polymethylphenylsiloxane, dimethylvinyl siloxy The poly- diformazan of the methyl phenyl siloxane of sealing end and the copolymer of dimethyl siloxane, methyl methoxy base vinyl siloxy sealing end The condensation polymer of radical siloxane, poly- methyl (3,3,3- trifluoro propyl) siloxanes of dimethylvinyl siloxy sealing end, Yi Jiyou The organopolysiloxane that following formula indicates:(CH3)2(CH2=CH) SiO [(CH3)2SiO]n[(CH3)PhSiO]m[(CH3)(CH2= CH)SiO]pSi (CH=CH2)(CH3)2
Heat filling can enumerate the metal oxides such as aluminium oxide, zinc oxide, titanium oxide, beryllium oxide;Aluminium hydroxide, hydroxide The metal hydroxides such as magnesium;The nitride such as aluminium nitride, silicon nitride, boron nitride;The carbide such as silicon carbide, boron carbide;And it is above-mentioned The mixture of substance, preferably silicon carbide, magnesia, aluminium oxide, iron oxide, calcium oxide, titanium oxide, silica, aluminium nitride, One or more of boron nitride and silicon nitride.
Preferably, it is 1-10 μm of 0.1-1 that heat filling, which is heat filling and average grain diameter that average grain diameter is 20-100 μm, μm, the mixture of one or more of 0.1 μm of heat filling below.
Preferably, heat filling is the heat conduction that the heat filling that average grain diameter is 20-100 μm is 1-10 μm with average grain diameter Filler is according to mass ratio (2-4):(3-1) is mixed to get.
It is preferred that surface modification treatment, the method for surface modification treatment and inorganic agent are carried out without specifically limited to heat filling, Uniformly spray silane coupling agent on heat filling surface for example, by using spray-on process, silane coupling agent include KH-550, KH-560, One or more of KH-570, KH-792, A-1160, A-171, processing method is unlimited, and the conductive powder after surface treatment also may be used Directly buy.It is preferred that heat filling is dried before, drying condition is preferably in 90-150 DEG C of dry 1-8h.
In practice, heat filling can be partly or totally replaced with fire-retardant filler, color stuffing etc., so that material is met corresponding Performance requirement.
Crosslinking agent is the organopolysiloxane for the hydrogen-based being connect with silicon containing three or three or more, and the hydrogen-based being connect with silicon Position can be located in molecular end and side chain on side chain or simultaneously.In the molecular structure of crosslinking agent in addition to silicon bonding Hydrogen-based, may also include alkyl, naphthenic base, aryl, aralkyl or halogenated alkyl, alkyl can enumerate methyl, ethyl, propyl or fourth Base etc., naphthenic base can enumerate cyclohexyl, cyclopenta etc., and aryl can enumerate phenyl, tolyl, xylyl etc., and aralkyl can arrange Benzyl, phenethyl etc. are lifted, halogenated alkyl can enumerate 3,3,3- trifluoro propyls.Optimizing alkyl and aryl, more preferable methyl and phenyl.
The molecular structure of crosslinking agent is not particularly limited, and can be the straight chain for having branch, straight chain, part branched, ring-type Or the molecular structure of branch shape, can be single polymers or mixture with these structures, preferably its hydrogen content is 0.01- 3% (quality), hydrogen content is the mass percent of hydrogen-based being connect with silicon in crosslinking agent in the present invention.Crosslinking agent is glutinous at 25 DEG C Degree is preferably 10-1000mpas, more preferably 10-500mpas.
Crosslinking agent can enumerate the methyl hydrogen of the polymethyl hydrogen siloxane of trimethylsiloxy group sealing end, trimethylsiloxy group sealing end The methyl hydrogen siloxane and methyl phenyl siloxane of the copolymer of siloxanes and dimethyl siloxane, dimethyl hydrogen siloxy sealing end Copolymer, dimethyl hydrogen siloxy sealing end methyl hydrogen siloxane and dimethyl siloxane copolymer, trimethylsiloxy group The methyl hydrogen siloxane and first of the methyl hydrogen siloxane of sealing end and the copolymer of methyl phenyl siloxane, trimethylsiloxy group sealing end Copolymer, cyclic methyl hydrogen polysiloxane or four (two methyl hydrogen silicone alkoxy) silicon of base (3,3,3- trifluoro propyl) siloxanes Alkane.
Preferably, the organosilicon heat conductive insulating composition includes chain extender, contains the hydrogen-based being connect with silicon for both ends Line style organopolysiloxane, i.e. its molecule both ends and the end of silicon bonding position group include hydrogen-based, remaining position is free of and silicon original The hydrogen-based of son connection.Alkenyl occurs during the reaction for composition after addition chain extender and the chain growth after si-h bond addition is anti- It answers, the mechanical properties such as the tensile strength of final piece is adjusted.
It, can also be including alkyl, naphthenic base, aryl, virtue other than hydrogen-based with silicon bonding in the molecular structure of chain extender Alkyl or halogenated alkyl, alkyl can enumerate methyl, ethyl, propyl or butyl etc., and naphthenic base can enumerate cyclohexyl, cyclopenta etc., Aryl can enumerate phenyl, tolyl, xylyl etc., and aralkyl can enumerate benzyl, phenethyl etc., and halogenated alkyl can enumerate 3,3, 3- trifluoro propyls.Optimizing alkyl and aryl, more preferable methyl and phenyl.Chain extender can be two or more straight-chains described above The mixture of organosilicon polysiloxane.
The hydrogen content of chain extender is 0.01%-0.5% (quality), at this time the base polymer of organosilicon heat conductive insulating composition In object with the ratio of the mole of the alkenyl of silicon bonding and the sum of the mole of hydrogen-based that is connect with silicon in crosslinking agent and chain extender Value is more than 1.Chain extender 25 DEG C viscosity be 100-50000mpas, preferably 100-10000mpas, most preferably 100-5000mpa·s。
Chain extender can enumerate α, the poly dimethyl that ω-two hydrogen-baseds dimethyl silicone polymer, aminomethyl phenyl hydrogen siloxy block Siloxanes, dimethyl hydrogen siloxy sealing end polymethylphenylsiloxane and dimethyl hydrogen siloxy sealing end poly- methyl (3,3, 3- trifluoro propyls) siloxanes etc..
Preferably, contain silicones in organosilicon heat conductive insulating composition, be the poly-organosilicon with cross-linked structure Hardness and tear resistance after composition solidification can be improved, selected from methyl phenyl silicone resin, methyl silicon resin, ethylene in oxygen alkane Base silicones, hydrogeneous silicones etc., concrete structure and its dosage are not particularly limited.
Platinum catalyst is not particularly limited, and can enumerate the platinum complexing of platinum micro mist, platinum black, chloroplatinic acid, platinum tetrachloride, alkene Object, the platinum complex of carbonyl or the thermoplasticity organic resin powder containing the above platinum group catalyst, preferably platinum catalyst or Chloroplatinic acid.
Above-mentioned organosilicon heat conductive insulating composition, preferably includes following components by weight:
The organosilicon heat conductive insulating composition more preferably includes following components by weight:
The preparation method of above-mentioned organosilicon heat conductive isolation sheet, including following operating procedure:
A, the component for being included by organosilicon heat conductive insulating composition is uniformly mixed according to proportioning, obtains mixture;
B, type is made in mixture, is cured at 40~90 DEG C, obtain one-step solidification sheet material;
C, 110~250 DEG C are warming up to vulcanize one-step solidification sheet material, obtains organosilicon heat conductive isolation sheet.
It is described that type is made in mixture is that will be mixed using calendering, curtain coating, molding, injection moulding, the techniques such as extrusion molding Object is closed to be made with certain thickness sheet material.
Preferably, it is in stepb, mixture system is molding same when the organosilicon heat conductive isolation sheet further includes base material When it is compound with base material, then cured.
Preferably, the cured time, which is cured for mixture to crosslink density, reaches maximum value required time.Institute Stating the cured time can be obtained by being tested on vulcameter after being sampled to mixture, vulcameter model high ferro M-3000A, Sampling amount is 6g ± 0.5g, at any time by torque (corresponding crosslink density) in measurement mixture at a certain temperature sulfidation Variation, the time required to obtaining when torque reaches maximum value, as hardening time.
Preferably, the cured time is 5-30min.
Preferably, the time of the vulcanization is 3-120min.
In the preparation method of organosilicon heat conductive isolation sheet, it is preferable that the temperature of the vulcanization is than the cured temperature It is 50-180 DEG C high.
In the preparation method of organosilicon heat conductive isolation sheet, the mixed time, preferably 3-20min was pinched without specifically limited It is carried out at normal temperatures in conjunction machine.
In the preparation method of organosilicon heat conductive isolation sheet, mixing preferably carries out under vacuum, and vacuum condition is preferred It is -0.09Mpa~-0.1Mpa for relative degree of vacuum.
It may be noted that 25 DEG C of viscosity of the present invention is dynamic viscosity value of the substance at 25 DEG C.
The specific embodiment of organosilicon heat conductive insulating composition and organosilicon heat conductive isolation sheet of the present invention is given below.
The organosilicon heat conductive insulating composition proportioning that organosilicon heat conductive isolation sheet is used to prepare in Examples 1 to 3 is shown in Table 1, Unit is mass fraction.
Table 1
Embodiment 1
In organosilicon heat conductive insulating composition, base polymer is the α that 25 DEG C of viscositys are 100mpas, ω-divinyl Dimethyl silicone polymer (mass percentage of vinyl is 2.5%);Heat filling is the aluminium oxide that average grain diameter is 30 μm; Crosslinking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 100mpas, and hydrogen content is 0.2% (quality);Chain extender is 25 DEG C of viscositys For the α of 100mpas, ω-two hydrogen-baseds dimethyl silicone polymer (hydrogen content is 0.18% (quality)).Ethylene in base polymer Base (- CH=CH2) mole and crosslinking agent and chain extender in the ratio of the sum of mole of hydrogen-based be 2.87.
In organosilicon heat conductive insulating composition, silicones DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile platinum Catalyst is platinum catalyst, and vulcanizing agent is that peroxidating is bis- (2,4- dichloro-benzoyl).
The preparation method of organosilicon heat conductive isolation sheet, including following operating procedure:
Test hardening time:Heat filling is placed in 100 DEG C of dry 3h, then according to the number take base polymer, Heat filling, crosslinking agent, chain extender, silicones, vulcanizing agent and platinum catalyst, in room temperature and -0.09MPa relative degree of vacuum conditions Lower mixing 3min, obtains mixture, take 6g mixtures high ferro M-3000A sulphur become instrument on tested, set reaction temperature as 80 DEG C, record torque changes with time, and it is hardening time to take torque to reach the maximum value corresponding time, and measuring hardening time is 5min。
Base polymer, heat filling, crosslinking agent, chain extender, silicones, vulcanizing agent and platinum catalysis are taken according to the number Agent mixing is added in kneader, mediates 10min under the conditions of room temperature and -0.09MPa relative degree of vacuum, obtains mixture, will mix Close object and with glass fabric roll compound, be carried out at the same time two sides coated with PET film, after molding at 80 DEG C progress curing reaction 5min removes PET film, obtains the one-step solidification sheet material that thickness is 0.3mm, and one-step solidification sheet material is vulcanized then at 120 DEG C 40min obtains organosilicon heat conductive isolation sheet.
Embodiment 2
In organosilicon heat conductive insulating composition, base polymer is the α that 25 DEG C of viscositys are 4000mpas, ω-divinyl Base dimethyl silicone polymer (mass percentage of vinyl is 0.50%);Heat filling is the nitridation that average grain diameter is 20 μm Aluminium;Crosslinking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 1000mpas, and hydrogen content is 0.08% (quality);Chain extender is 25 DEG C viscosity is the α of 1000mpas, ω-two hydrogen-baseds dimethyl silicone polymer (hydrogen content is 0.05% (quality)).Base polymer Object medium vinyl (- CH=CH2) mole and crosslinking agent and chain extender in the ratio of the sum of mole of hydrogen-based be 1.27.
In organosilicon heat conductive insulating composition, silicones DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile platinum Catalyst is platinum catalyst, and vulcanizing agent is that peroxidating is bis- (2,4- dichloro-benzoyl).
The preparation method of organosilicon heat conductive isolation sheet, including following operating procedure:
Test hardening time:Heat filling is placed in 100 DEG C of dry 3h, then according to the number take base polymer, Heat filling, crosslinking agent, chain extender, silicones, vulcanizing agent and platinum catalyst, in room temperature and -0.09MPa relative degree of vacuum conditions Lower mixing 3min, obtains mixture, take 6g mixtures high ferro M-3000A sulphur become instrument on tested, set reaction temperature as 70 DEG C, record torque changes with time, and it is hardening time to take torque to reach the maximum value corresponding time, and measuring hardening time is 12min。
Base polymer, heat filling, crosslinking agent, chain extender, silicones, vulcanizing agent and platinum catalysis are taken according to the number Agent mixing is added in kneader, mediates 10min under the conditions of room temperature and -0.09MPa relative degree of vacuum, obtains mixture, will mix Close object and with glass fabric roll compound, be carried out at the same time two sides coated with PET film, after molding at 70 DEG C progress curing reaction 12min removes PET film, obtains the one-step solidification sheet material that thickness is 0.3mm, and one-step solidification sheet material is vulcanized then at 120 DEG C 30min obtains organosilicon heat conductive isolation sheet.
Embodiment 3
In organosilicon heat conductive insulating composition, base polymer is the α that 25 DEG C of viscositys are 40000mpas, ω-divinyl Base dimethyl silicone polymer (mass percentage of vinyl is 0.20%), heat filling is the oxidation that average grain diameter is 3 μm The aluminium oxide in mass ratio 2 that aluminium and average grain diameter are 50 μm:3 are mixed to get;Crosslinking agent is Methyl Hydrogen Polysiloxane Fluid, and 25 DEG C of viscositys are 10000mpas, hydrogen content are 0.03% (quality).Base polymer medium vinyl (- CH=CH2) mole and crosslinking agent The ratio between mole of middle hydrogen-based is 1.54.
In organosilicon heat conductive insulating composition, silicones DY-MQ102, Shandong Dayi Chemical Industry Co., Ltd.Meanwhile platinum Catalyst is platinum catalyst, vulcanizing agent 2, bis- (tert-butyl peroxide) hexanes of 5- dimethyl -2,5-.
The preparation method of organosilicon heat conductive isolation sheet, including following operating procedure:
Test hardening time:Heat filling is placed in 100 DEG C of dry 3h, then according to the number take base polymer, Heat filling, crosslinking agent, silicones, vulcanizing agent and platinum catalyst mix under the conditions of room temperature and -0.09MPa relative degree of vacuum 10min obtains mixture, takes 6g mixtures to become on instrument in high ferro M-3000A sulphur and is tested, sets reaction temperature as 50 DEG C, Record torque changes with time, and it is hardening time to take torque to reach the maximum value corresponding time, and measuring hardening time is 25min。
Base polymer, heat filling, crosslinking agent, silicones, vulcanizing agent and platinum catalyst mixing are taken according to the number It is added in kneader, mediates 10min under the conditions of room temperature and -0.09MPa relative degree of vacuum, obtain mixture, mixture is noted The die cavity for entering 0.3mm thickness cures 25min at 50 DEG C after compression molding, the one-step solidification sheet material that thickness is 0.3mm is obtained, by one Secondary cured sheet obtains organosilicon heat conductive isolation sheet then at 170 DEG C of vulcanization 30min.
Testing example
The organosilicon heat conductive isolation sheet prepared to Examples 1 to 3 is tested for the property, including thermal coefficient, hardness, stretching Intensity, tearing strength, volume resistivity and breakdown voltage, test and performance data are shown in Table 2.
2 organosilicon heat conductive isolation sheet performance data of table
From the data in table 2, it can be seen that the present invention is to contain vinyl polysiloxane, heat filling, crosslinking agent, platinum catalyst and vulcanization Agent is that raw material prepares organosilicon heat conductive isolation sheet, and by the special process of secondary curing, final insulating trip is made to be provided simultaneously with High heat conduction, high rigidity and good tear resistance meet in practical application to the thermal conductivity and usability of the heat dissipation interface that generates heat Requirement, comprehensive performance protrudes, and preparation method is simple, and application prospect is wide.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than is protected to the present invention The limitation of range.It will be understood by those of skill in the art that several deductions can be carried out to technical scheme of the present invention or waited With replacing, without departing from the spirit and scope of technical solution of the present invention.

Claims (7)

1. a kind of organosilicon heat conductive isolation sheet, includes at least thermally conductive insulating layer, the thermally conductive insulating layer is exhausted by organosilicon heat conduction Edge composition is made through sheet forming process, and the organosilicon heat conductive insulating composition includes following components:
Base polymer:For the line style organopolysiloxane containing two or more and the alkenyl of silicon bonding, at 25 DEG C Viscosity is 50~50000mP as;The base polymer contains organic with the line style of the alkenyl of silicon bonding for molecule both ends Polysiloxanes;
Heat filling;
Crosslinking agent:Organopolysiloxane for the hydrogen-based being connect with silicon containing three or three or more is 10- in 25 DEG C of viscositys 50000mP a·s;
Platinum catalyst and vulcanizing agent, the vulcanizing agent are organic peroxide;
In the base polymer with the mole for the hydrogen-based being connect with silicon in the mole of the alkenyl of silicon bonding and crosslinking agent The ratio between be more than 1;
The preparation method of the organosilicon heat conductive isolation sheet includes following operating procedure:
A, the component for being included by organosilicon heat conductive insulating composition is uniformly mixed according to proportioning, obtains mixture;
B, type is made in mixture, is cured at 40~90 DEG C, obtain one-step solidification sheet material;
C, 110~250 DEG C are warming up to vulcanize one-step solidification sheet material, obtains organosilicon heat conductive isolation sheet;
The temperature of the vulcanization is 50-180 DEG C higher than the cured temperature.
2. organosilicon heat conductive isolation sheet as described in claim 1, which is characterized in that the organosilicon heat conductive isolation sheet further includes Base material, the thermally conductive insulating layer and the compound obtained organosilicon heat conductive isolation sheet of the base material.
3. organosilicon heat conductive isolation sheet as claimed in claim 2, which is characterized in that the base material is glass fabric, polyamides Imines film, aluminium foil, poly- naphthalene ester film or carbon cloth.
4. organosilicon heat conductive isolation sheet as claimed in claim 1,2 or 3, which is characterized in that the organosilicon heat conductive insulating group Close object in, in base polymer with the mole for the hydrogen-based being connect with silicon in the mole of the alkenyl of silicon bonding and crosslinking agent it It is less than or equal to 3.5 than being more than 1.
5. organosilicon heat conductive isolation sheet as claimed in claim 1,2 or 3, which is characterized in that the organosilicon heat conductive insulating group It includes chain extender to close object, and chain extender is the line style organopolysiloxane that the hydrogen-based being connect with silicon is contained at both ends.
6. organosilicon heat conductive isolation sheet as claimed in claim 1,2 or 3, which is characterized in that the organosilicon heat conductive insulating group It includes following components by weight to close object:
7. organosilicon heat conductive isolation sheet as claimed in claim 5, which is characterized in that the organosilicon heat conductive insulating composition packet Include following components by weight:
CN201510191264.4A 2015-04-21 2015-04-21 Organosilicon heat-conducting insulating sheet and preparation method thereof Active CN104788968B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510191264.4A CN104788968B (en) 2015-04-21 2015-04-21 Organosilicon heat-conducting insulating sheet and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510191264.4A CN104788968B (en) 2015-04-21 2015-04-21 Organosilicon heat-conducting insulating sheet and preparation method thereof

Publications (2)

Publication Number Publication Date
CN104788968A CN104788968A (en) 2015-07-22
CN104788968B true CN104788968B (en) 2018-08-03

Family

ID=53554177

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510191264.4A Active CN104788968B (en) 2015-04-21 2015-04-21 Organosilicon heat-conducting insulating sheet and preparation method thereof

Country Status (1)

Country Link
CN (1) CN104788968B (en)

Families Citing this family (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105086464B (en) * 2015-07-28 2017-11-28 惠州市安品新材料有限公司 A kind of organosilicon heat-conducting composite sheet
CN105349113A (en) * 2015-10-14 2016-02-24 文雪烽 Heat-conductive interface material
CN106009688A (en) * 2016-05-19 2016-10-12 强新正品(苏州)环保材料科技有限公司 Heat-conducting silicon sheet formula
CN106272694A (en) * 2016-08-25 2017-01-04 强新正品(苏州)环保材料科技有限公司 A kind of dicing method of heat conductive silica gel material
CN106833545A (en) * 2016-12-01 2017-06-13 昆山裕凌电子科技有限公司 A kind of high heat conduction Composition spacer material and preparation method
CN106590548A (en) * 2016-12-01 2017-04-26 昆山裕凌电子科技有限公司 Low-density and high-strength heat-conducting silica gel gasket
CN110364648B (en) * 2018-04-11 2022-04-01 苏州矽美科导热科技有限公司 New energy lithium battery radiating gasket and preparation method thereof
CN109648940A (en) * 2018-12-06 2019-04-19 安徽旭川新材料科技有限公司 A kind of frosted PET hot pressing silica gel material and preparation method thereof
CN110257022B (en) * 2019-07-18 2022-05-10 深圳前海量子翼纳米碳科技有限公司 Insulated electromagnetic shielding heat-conducting silica gel pad and preparation method thereof
CN111041845B (en) * 2019-12-26 2022-06-17 深圳德邦界面材料有限公司 Organic silicon heat-conducting insulating sheet and preparation method thereof
CN112724685B (en) * 2020-12-28 2023-01-17 深圳市安品有机硅材料有限公司 Organic silicon heat-conducting sheet and preparation method thereof
CN112778932A (en) * 2021-01-12 2021-05-11 深圳德邦界面材料有限公司 Self-adhesive organic silicon heat-conducting insulating sheet and preparation method thereof
CN113122181A (en) * 2021-04-17 2021-07-16 深圳市益达兴科技股份有限公司 Production process of high-thermal-conductivity insulating material and insulating sheet
CN116285736A (en) * 2022-09-09 2023-06-23 惠科股份有限公司 Heat conduction fixing piece and display device

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103507353A (en) * 2012-06-18 2014-01-15 信越化学工业株式会社 Thermal conduction sheet and electronic device
CN104015433A (en) * 2013-02-28 2014-09-03 信越化学工业株式会社 Thermal conductivity composite silicone rubber sheet
CN104497574A (en) * 2014-12-10 2015-04-08 深圳市博恩实业有限公司 Multifunctional organic silicon thermal interface material

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5835100B2 (en) * 2012-05-22 2015-12-24 信越化学工業株式会社 Antistatic silicone rubber composition and method for inhibiting yellowing of cured antistatic silicone rubber

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103507353A (en) * 2012-06-18 2014-01-15 信越化学工业株式会社 Thermal conduction sheet and electronic device
CN104015433A (en) * 2013-02-28 2014-09-03 信越化学工业株式会社 Thermal conductivity composite silicone rubber sheet
CN104497574A (en) * 2014-12-10 2015-04-08 深圳市博恩实业有限公司 Multifunctional organic silicon thermal interface material

Also Published As

Publication number Publication date
CN104788968A (en) 2015-07-22

Similar Documents

Publication Publication Date Title
CN104788968B (en) Organosilicon heat-conducting insulating sheet and preparation method thereof
CN104788969B (en) Organosilicon heat-conducting and insulating composition and heat-conducting and insulating material
CN103881389B (en) Addition curable self-adhesive silicone rubber composition
CN104341778B (en) Conductive liquid silicone rubber compound and high-voltage cable room temperature contraction rubber component
CN105017542B (en) The preparation method of the organosilicon thermally conductive sheet of enhancing
CN104341777B (en) Electroconductive rubber composition and high-voltage cable room temperature contraction rubber component
GB2045790A (en) Organopolysiloxane composition
CN113913024B (en) Addition type liquid silicone rubber, vulcanized rubber and preparation method thereof
CN103421323B (en) The method of the xanthochromia of Antistatic silicone rubber composition and suppression antistatic behaviour silicon rubber solidfied material
JPH0514742B2 (en)
CN103087528A (en) Silicone resin composition, silicone resin sheet, optical semiconductor element device, and producing method of silicone resin sheet
CN105452385B (en) Silicone rubber compound
JP4676671B2 (en) Thermally conductive silicone elastomer composition
KR102556116B1 (en) Handling Additives for Silicone Elastomer Bases
CN112724685B (en) Organic silicon heat-conducting sheet and preparation method thereof
CN109863207A (en) Heat resistance mixed milling type silicon rubber composition
CN105199620B (en) The preparation method of gum silica gel piece
JP3904853B2 (en) Thermally conductive silicone rubber composition and heater roll using the same
JPS58219034A (en) Manufacture of electrical insulating heat dissipation rubber sheet
CN105273680B (en) A kind of two-component heat conductive silica gel sheet material and preparation method thereof and equipment
CN105086464B (en) A kind of organosilicon heat-conducting composite sheet
WO2020068528A1 (en) Silicone rubber composition
CN109564906A (en) Heat conductive sheet
JP3640301B2 (en) Sealing material for polymer electrolyte fuel cell separator
CN102532910A (en) Double-component room-temperature vulcanized silicon rubber having adhesiveness and acidosis resistance and preparation method

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
EXSB Decision made by sipo to initiate substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant