CN106810699A - A kind of organic siliconresin and its conjuncted series high-performance organosilicon thermal conductive insulation glue of the double cross being prepared from - Google Patents

A kind of organic siliconresin and its conjuncted series high-performance organosilicon thermal conductive insulation glue of the double cross being prepared from Download PDF

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CN106810699A
CN106810699A CN201710043733.7A CN201710043733A CN106810699A CN 106810699 A CN106810699 A CN 106810699A CN 201710043733 A CN201710043733 A CN 201710043733A CN 106810699 A CN106810699 A CN 106810699A
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organic siliconresin
thermal conductive
conjuncted
insulation glue
double cross
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庞浩
莫文蔚
廖兵
黄健恒
年福伟
王坤
赵阳阳
黄福仁
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Foshan Function High Polymer Materials & Fine Chemicals Professional Center
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Foshan Function High Polymer Materials & Fine Chemicals Professional Center
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/38Polysiloxanes modified by chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/12Polysiloxanes containing silicon bound to hydrogen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

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  • Organic Chemistry (AREA)
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  • Health & Medical Sciences (AREA)
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  • Organic Insulating Materials (AREA)
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Abstract

The invention belongs to technical field of semiconductor illumination, the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross for disclosing a kind of organic siliconresin and its being prepared from.The present invention is formed by mixing vacuum defoamation hot setting by organic siliconresin, catalyst, crosslinking agent and heat filling.Present invention vinylsiloxane to containing hydrogen silicone oil it is modified obtain it is a kind of with from thickening function, can be formed self-crosslinking solidification and with the double cross of vinyl silicone oil crosslinking curing connection organic siliconresin.By autonomous synthesis, the problems such as solving organosilicon material and need to add tackifier, need Cord blood, and the aging defect of the poor heat resistance of traditional epoxy-based material, easy xanthochromia is overcome.The method obtains a kind of preservation of energy normal temperature, the thermal conductive insulation glue that heat-resist, mechanical strength is high, caking property is good.

Description

A kind of organic siliconresin and its conjuncted series high-performance organosilicon of the double cross being prepared from are led Heat insulation glue
Technical field
The invention belongs to electronic device and technical field of semiconductor illumination, and in particular to a kind of organic siliconresin and its system The standby conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross.
Background technology
As long as having epoxies and organic silicon currently used for the binding material between chip and base material.Epoxies has good Caking property, chemical resistance and excellent mechanical property etc..But, in use find epoxy systems meeting by Gradually there is xanthochromia and melanism, greatly reduce light output efficiency so as to have impact on the reliability requirement of whole device.
In order to solve these problems, Dow corning, Japanese SHIN-ETSU HANTOTAI, Wan Neidengduo companies have studied and use organosilicon Instead of traditional epoxy material.Because organosilicon has good heat resistance and uvioresistant performance, disclosure satisfy that powerful It is required that.But the thermal conductive insulation glue of organic silicon has that mechanical property is not good enough, adhesive property is bad, such as Mentioned in two patent documents of CN201510418308 and CN200910251588, CN201510418308 needs to add tackifier To increase the adhesion strength between chip and support, the preservation condition of this organic silica gel synthesized in CN200910251588 will Seek low temperature.Tackifier are likely to occur therebetween the problem of phase separation with matrix resin, and this influences heat resistance and device indirectly Light output performance.And preservation condition requirement low temperature, this is also a big problem for the consumption of the energy.
The content of the invention
In order to overcome the deficiencies in the prior art and shortcoming, primary and foremost purpose of the invention is to provide a kind of organosilicon Resin.The present invention is directed to above present situation, on the basis of organosilicon characteristic is fully understood, will be with vinyl by designing synthesis Siloxanes synthesized with containing hydrogen silicone oil, this new organic siliconresin for obtaining has and base material (such as aluminium flake, copper sheet Deng) formed chemical bond unit structure, be not required to additional tackifier and improve cementation, and itself also can condensation cross-linking enter One step lifts the mechanical property of matrix resin;According to obtained after formula design mixing a kind of pair of cross-linking system with from increasing The organosilicon material of viscous, high temperature resistant, excellent in mechanical performance and energy normal temperature storage, solves what above-mentioned organosilicon material was present Shortcoming.
It is still another object of the present invention to provide a kind of preparation method of above-mentioned organic siliconresin.
A further object of the present invention is that to provide a kind of double cross-linking systems being prepared from by above-mentioned organic siliconresin high Performance organosilicon thermal conductive insulation glue.
It is still another object of the present invention to provide a kind of system of the above-mentioned conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross Preparation Method.
A further object of the present invention is to provide the application of the above-mentioned conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross.
The object of the invention is achieved through the following technical solutions:
A kind of organic siliconresin, the organic siliconresin has following structure:
Wherein R1It is-H or-CH3, R2For-CH3Or-CH2CH3, R3It is-H ,-CH3Or-Ph, n are the integer between 5~30, m It is the integer between 5~30, z is the integer between 5~20.
The preparation method of above-mentioned organic siliconresin, according to following operating procedure:By containing hydrogen silicone oil dissolving in organic solvent, And the mixed solution of Karstedt catalyst and vinylsiloxane is added dropwise to, revolving removes solvent after completion of the reaction, and depressurizes Remove unreacted small molecule, you can obtain organic siliconresin.
The vinylsiloxane is vinyltrimethoxy silane, vinyl-dimethyl methoxylsilane, vinyl two Methylethoxy base silane, 3- (isobutene acyl-oxygen) propyl trimethoxy silicanes and 3- (isobutene acyl-oxygen) propyl-triethoxysilicane One or more of.
Organic siliconresin of the present invention can form two kinds of cross-linking systems in solidification, and one kind is organic siliconresin itself Siloxanes hydrolytic condensation solidified, another is remaining si-h bond and additional vinyl silicone oil in organic siliconresin Si―H addition reaction is carried out so as to solidify.
A kind of conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross being prepared from by above-mentioned organic siliconresin, this has Machine silicon thermal conductive insulation glue is made up of the following component counted by weight:0~30 part of vinyl silicone oil, organic siliconresin 50~70 Part, 0.05~1 part of catalyst, 10~30 parts of heat filling, 0.05~5 part of other functions auxiliary agent.
The heat filling is one or more of carborundum, aluminium nitride, aluminum oxide and boron nitride.
The other functions auxiliary agent is one or more of polymerization inhibitor, antioxidant, reinforcing agent and heat filling.
The vinyl silicone oil includes more than two vinyl for line style in molecular structure, vinyl is distributed in point Son amount two ends or centre, the mass percentage content of vinyl between 0.2~5%, viscosity 500~10,000mPas it Between, vinyl silicone oil can be the mixture of one or more of which;The catalyst is the metallic compound of VIII, VII race Or complex compound, preferred platinum group catalyst:Speier catalyst or Karstedt catalyst, Pt contents 1000~5000ppm it Between.
The preparation method of the above-mentioned conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross, according to following operating procedure:Weigh The weight portion of vinyl silicone oil 0~30, the weight portion of organic siliconresin 50~70, the weight portion of catalyst 0.05~1, heat filling 10~ 30 weight portions and the weight portion of other functions auxiliary agent 0.05~5, after being uniformly mixed, bubble removing are vacuumized at 30~60 DEG C 20~60min, in 80~100 DEG C of precuring 1h, then is warming up to 130~150 DEG C of 1.5~2h of solidification, obtains double cross-linking systems high Performance organosilicon thermal conductive insulation glue.
The method for preparing above-mentioned organosilicon thermal conductive insulation glue, first using cyclosiloxane and vinylcyclosiloxanes or hydrogeneous Cyclosiloxane open loop under catalyst action prepares line style silicone oil, then containing hydrogen silicone oil is modified obtains organosilicon tree Fat, then mixes it with catalyst, polymerization inhibitor etc., and vacuum defoamation, pours into mould, and solidification at a certain temperature is Obtain organosilicon thermal conductive insulation glue.
The conjuncted series high-performance organosilicon thermal conductive insulation glue of above-mentioned double cross can be realized in micro-circuit board, surface-mounted integrated circuit And the application in great power LED.
The present invention has the advantages that following prominent and beneficial effect compared with prior art:
(1) present invention synthesizes a kind of organic siliconresin with alkoxy and si-h bond by autonomous Design, and by its with Curing agent, inhibitor and heat filling are mixed to get one kind to be had from viscosifying action, and hardness double cross high, heat-resist is conjuncted It is thermal conductive insulation glue, solves the problems, such as xanthochromia and melanism at present with epoxy resin as material of main part.
(2), without Cord blood, easy to use, condition of cure is gentle for the thermal conductive insulation glue obtained by the present invention, it is to avoid Some unnecessary wastes, reduce cost in use.
Brief description of the drawings
Fig. 1 is the IR Characterization data of the gained organic siliconresin of embodiment 1-4;
Fig. 2 is the nuclear-magnetism characterize data of the gained organic siliconresin of embodiment 1-4.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Embodiment 1
(1) by the D of 29.662g (100mmol)4The D of (octamethylcy-clotetrasiloxane) and 2.405g (10mmol)4 H(tetramethyl Base tetrahydrochysene basic ring tetrasiloxane) add there-necked flask in, 40 DEG C/- 0.09Mpa vacuumize 1h water removal after, be warming up to 60~70 DEG C Acidic anionic exchanger resin is added as catalyst and the MM of 0.489g (1mmol)H(the hydrogen-based disiloxane of tetramethyl two) As end-capping reagent, 4~6h is reacted.
(2) suction filtration removes catalyst, is continuously heating to 190~200 DEG C/- 0.09Mpa and removes unreacted small molecule reaction Thing, obtains the thick liquid containing hydrogen silicone oil PHMS-10 of water white transparency.
(3) the containing hydrogen silicone oil PHMS-10 (hydrogen content is 0.1%) that will be obtained takes 5g and is dissolved in 15ml toluene addition reactor In, the Karstedt catalyst of 3- (isobutene acyl-oxygen) trimethoxy silanes and 0.05g that separately weigh 1.242g is dissolved in 5ml toluene In, and reaction system is added dropwise to together, in 70 DEG C/N2Protection 4~6h of lower reaction, revolving is except solvent and that unreacted is removed under reduced pressure is small Molecule, obtains the organic siliconresin of water white transparency;The organic siliconresin has following structure:(n=5~7 in following formula, m=5 ~7, z=18~20).
The IR Characterization data of gained organic siliconresin are as shown in Figure 1:In 2156cm-1There is Si-H peaks in place, but modified There is obvious decrease afterwards, the Si -- H bond of declaratives occurs and vinylsiloxane there occurs hydrosilylation.And 3000cm-1Occur without peak above, illustrate that vinylsiloxane does not occur hydrolysis during the course of the reaction, there is no-OH to go out It is existing.In 1722cm-1Handle affairs the characteristic peak of C=O, illustrate that 3- (isobutene acyl-oxygen) trimethoxy silane has been successfully introduced into PMHS.
The nuclear-magnetism characterize data of gained organic siliconresin is as shown in Figure 2:Dan Qiangfeng at 3.5ppm is Si-O-CH3 first The characteristic peak of base, illustrates that methoxyl group is not hydrolyzed during the course of the reaction, and this is the same with the infrared conclusion for obtaining; It is silicon hydrogen into the characteristic peak on rear β positions at 2.45ppm;There are weaker Si-H peaks to occur at 4.55ppm in addition, illustrate only to carry out The hydrosilylation of part, the Si-H of still member-retaining portion can be used for the solidification in later stage.
(4) 1.0g organic siliconresins are carried out with the vinyl silicone oil (contents of ethylene=0.6%) of 2.0g in beaker After mixing, add the inhibitor and 0.8g aluminium nitride (2um) of 0.15g to continue to stir and evenly mix in beaker, add 0.06g's Karstedt catalyst, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in poly- Teflon mould, 90 DEG C precuring 1h, then it is warming up to the conjuncted series high-performance organosilicon heat conduction of double cross that 130 DEG C of 2~3h of solidification can obtain water white transparency Insulating cement.Gained organosilicon thermal conductive insulation glue, hardness 70A, shear tension intensity 2.3MPa, temperature when weightless 5% are 411 DEG C, thermal conductivity factor 0.368.Performance is held essentially constant afterwards for room temperature 5 months.
Embodiment 2
(1)D4 HThe consumption of (tetramethyl tetrahydrochysene basic ring tetrasiloxane) be 4.81g (20mmol), other steps with embodiment 1, The containing hydrogen silicone oil PHMS-20 (hydrogen content is 0.2%) that will be obtained takes 5g and is dissolved in 15ml toluene addition reactor, separately weighs 3- (isobutene acyl-oxygen) trimethoxy silanes of 2.4835g and the Karstedt catalyst of 0.05g are dissolved in 5ml toluene, and one Rise and be added dropwise to reaction system, in 70 DEG C/N2Protection 4~6h of lower reaction, revolving is except solvent and unreacted small molecule is removed under reduced pressure, and obtains The organic siliconresin of water white transparency;The organic siliconresin has following structure:(n=8~10 in following formula, m=8~10, z =15~18).
Infrared and nuclear-magnetism characterization result is as shown in Figure 1 and Figure 2.
(2) 1.0g organic siliconresins are carried out with the vinyl silicone oil (contents of ethylene=0.6%) of 2.0g in beaker After mixing, add the inhibitor and 0.8g aluminium nitride (2um) of 0.15g to continue to stir and evenly mix in beaker, add 0.06g's Karstedt catalyst, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in Teflon mould, 90 DEG C Precuring 1h, then be warming up to 130 DEG C solidification 2~3h can obtain water white transparency the conjuncted series high-performance organosilicon heat conduction of double cross it is exhausted Edge glue.Gained organosilicon thermal conductive insulation glue, hardness 75A, shear tension intensity 2.6MPa, temperature when weightless 5% are 416 DEG C, Thermal conductivity factor 0.418.Performance is held essentially constant afterwards for room temperature 5 months.
Embodiment 3
(1)D4 HThe consumption of (tetramethyl tetrahydrochysene basic ring tetrasiloxane) is 7.215g (30mmol), the same embodiment of other steps 1, the containing hydrogen silicone oil PHMS-30 (hydrogen content is 0.31%) that will be obtained take 5g and are dissolved in 15ml toluene addition reactor, separately weigh 3- (isobutene acyl-oxygen) trimethoxy silanes of 3.808g and the Karstedt catalyst of 0.05g are dissolved in 5ml toluene, and together Reaction system is added dropwise to, in 70 DEG C/N2Protection 4~6h of lower reaction, revolving is except solvent and unreacted small molecule is removed under reduced pressure, and obtains nothing Color is transparent with machine silicones;The organic siliconresin has following structure:(n=10~12 in following formula, m=10~12, z =10~12).
Infrared and nuclear-magnetism characterization result is as shown in Figure 1 and Figure 2.
(2) 1.0g organic siliconresins are carried out with the vinyl silicone oil (contents of ethylene=0.6%) of 2.0g in beaker After mixing, add the inhibitor and 0.8g aluminium nitride (2um) of 0.15g to continue to stir and evenly mix in beaker, add 0.06g's Karstedt catalyst, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in Teflon mould, 90 DEG C Precuring 1h, then be warming up to 130 DEG C solidification 2~3h can obtain water white transparency the conjuncted series high-performance organosilicon heat conduction of double cross it is exhausted Edge glue.Gained organosilicon thermal conductive insulation glue, hardness 80A, shear tension intensity 3.0MPa, temperature when weightless 5% are 425 DEG C, Thermal conductivity factor 0.45.Performance is held essentially constant afterwards for room temperature 5 months.
Embodiment 4
(1)D4 HThe consumption of (tetramethyl tetrahydrochysene basic ring tetrasiloxane) is 14.43g (60mmol), the same embodiment of other steps 1, the containing hydrogen silicone oil PHMS-60 (hydrogen content is 0.5%) that will be obtained take 5g and are dissolved in 15ml toluene addition reactor, separately weigh 3- (isobutene acyl-oxygen) trimethoxy silanes of 5.073g and the Karstedt catalyst of 0.05g are dissolved in 5ml toluene, and together Reaction system is added dropwise to, in 70 DEG C/N2Protection 4~6h of lower reaction, revolving is except solvent and unreacted small molecule is removed under reduced pressure, and obtains nothing Color is transparent with machine silicones;The organic siliconresin has following structure:(n=18~20 in following formula, m=18~20, z =8~10).
Infrared and nuclear-magnetism characterization result is as shown in Figure 1 and Figure 2.
(2) 1.0g organic siliconresins are carried out with the vinyl silicone oil (contents of ethylene=0.6%) of 2.0g in beaker After mixing, add the inhibitor and 0.8g aluminium nitride (2um) of 0.15g to continue to stir and evenly mix in beaker, add 0.06g's Karstedt catalyst, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in Teflon mould, 90 DEG C Precuring 1h, then be warming up to 130 DEG C solidification 2~3h can obtain water white transparency the conjuncted series high-performance organosilicon heat conduction of double cross it is exhausted Edge glue.Gained organosilicon thermal conductive insulation glue, hardness 72A, shear tension intensity 2.7MPa, temperature when weightless 5% are 421 DEG C, Thermal conductivity factor 0.412.Performance is held essentially constant afterwards for room temperature 5 months.
Comparative example 1
Weigh respectively in embodiment 1 organic siliconresin product 1.5g, vinyl silicone oil 2.0g (contents of ethylene= 0.6%), the Karstedt catalyst of 0.06g, 0.15g inhibitor, 0.8g aluminium nitride (2um) is well mixed in beaker, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in poly- four volts of ethene moulds, 90 DEG C of precuring 1h, then be warming up to 130 DEG C solidification 2~3h.The organosilicon die bond material of White-opalescent is obtained, hardness 75A, shear tension intensity 2.5MPa lose Temperature when weighing 5% is 419 DEG C, thermal conductivity factor 0.388.Performance is held essentially constant afterwards for room temperature 5 months.
Comparative example 3
Weigh respectively in embodiment 3 organic siliconresin product 1.5g, vinyl silicone oil 2.0g (contents of ethylene= 0.6%), the Karstedt catalyst of 0.06g, 0.15g inhibitor, 0.8g aluminium nitride (5um) is well mixed in beaker, is placed in 20~60min of normal temperature deaeration in vacuum drying chamber, pours in poly- four volts of ethene moulds, 90 DEG C of precuring 1h, then be warming up to 130 DEG C solidification 2~3h.The organosilicon die bond material of White-opalescent is obtained, hardness 85A, shear tension intensity 3.5MPa lose Temperature when weighing 5% is 425 DEG C, thermal conductivity factor 0.432.Performance is held essentially constant afterwards for room temperature 5 months.
By above example 1~4 as can be seen that with the increase of the silicone-modified ratio of organic siliconresin medium vinyl, obtaining To organosilicon thermal conductive insulation glue mechanical property and heat conductivility all gradually increase.Be can be seen that by comparison example 1 and 3 The increase of the addition of same organic siliconresin, the mechanical property of organosilicon thermal conductive insulation glue, heat resistance and thermal conductivity by It is cumulative to add.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (10)

1. a kind of organic siliconresin, it is characterised in that:The organic siliconresin has following structure:
Wherein R1It is-H or-CH3, R2For-CH3Or-CH2CH3, R3It is-H ,-CH3Or-Ph, n are the integer between 5~30, m is 5 Integer between~30, z is the integer between 5~20.
2. the preparation method of a kind of organic siliconresin according to claim 1, it is characterised in that according to following operating procedure: By containing hydrogen silicone oil dissolving in organic solvent, and after Karstedt catalyst and vinylsiloxane are mixed it is added dropwise to reactant In system, revolving removes solvent after completion of the reaction, and unreacted small molecule is removed under reduced pressure, you can obtain organic siliconresin.
3. the preparation method of above-mentioned a kind of organic siliconresin according to claim 2, it is characterised in that:The vinyl Siloxanes is vinyltrimethoxy silane, vinyl-dimethyl methoxylsilane, vinyl dimethylethoxysilane, 3- One or more of (isobutene acyl-oxygen) propyl trimethoxy silicane and 3- (isobutene acyl-oxygen) propyl-triethoxysilicane.
4. the conjuncted series high-performance organosilicon heat conductive insulating of double cross that a kind of organic siliconresin by described in claim 1 is prepared from Glue, it is characterised in that:The organosilicon thermal conductive insulation glue is made up of the following component counted by weight:Vinyl silicone oil 0~30 Part, 50~70 parts of organic siliconresin, 0.05~1 part of catalyst, 0.05~1 part of inhibitor, 10~30 parts of heat filling, other work( Can 0.05~5 part of auxiliary agent.
5. the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 4, it is characterised in that:The heat conduction Filler is one or more of carborundum, aluminium nitride, aluminum oxide and boron nitride.
6. the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 4, it is characterised in that:It is described other Function additive is one or more of polymerization inhibitor, antioxidant, reinforcing agent and heat filling.
7. the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 4, it is characterised in that:The ethene Base silicone oil is line style, and more than two vinyl are included in molecular structure, and vinyl is distributed in the two ends or centre of molecular weight, Between 0.2~5%, viscosity is between 500~10,000mPas for the mass percentage content of vinyl;The catalyst is The metallic compound or complex compound of VIII, VII race.
8. the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 7, it is characterised in that:The catalysis Agent is Speier catalyst or Karstedt catalyst, and Pt contents are between 1000~5000ppm.
9. the preparation method of the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 4, its feature exists According to following operating procedure:Weigh the weight portion of vinyl silicone oil 0~30, the weight portion of organic siliconresin 50~70, catalyst 0.05~1 weight portion, the weight portion of inhibitor 0.05~1, the weight portion of heat filling 10~30 and the weight of other functions auxiliary agent 0.05~5 Amount part, after being uniformly mixed, vacuumizes 20~60min of bubble removing at 30~60 DEG C, in 80~100 DEG C of precuring 1h, 130~150 DEG C of 1.5~2h of solidification are warming up to again, obtain the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross.
10. the conjuncted series high-performance organosilicon thermal conductive insulation glue of double cross according to claim 4 is in micro-circuit board, integrated electricity Application in road plate and great power LED.
CN201710043733.7A 2017-01-19 2017-01-19 A kind of organic siliconresin and its conjuncted series high-performance organosilicon thermal conductive insulation glue of the double cross being prepared from Pending CN106810699A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111041845A (en) * 2019-12-26 2020-04-21 深圳德邦界面材料有限公司 Organic silicon heat-conducting insulating sheet and preparation method thereof
CN112322251A (en) * 2020-10-27 2021-02-05 复旦大学 Thermosetting yellowing-resistant full-lamination special material and preparation method and application thereof
CN114350311A (en) * 2022-01-10 2022-04-15 东莞市佳迪新材料有限公司 Organic silicon heat-conducting pouring sealant composition for photovoltaic inverter and preparation method thereof
US20220135805A1 (en) * 2019-11-12 2022-05-05 Showa Denko K. K. Method for producing silicon-containing oxide-coated aluminum nitride particles and method for producing exoergic resin composition
CN116804086A (en) * 2023-08-25 2023-09-26 成都思立可科技有限公司 Long-chain alkyl-polar group co-modified polysiloxane and preparation method thereof

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CN105482120A (en) * 2015-12-18 2016-04-13 杭州福斯特光伏材料股份有限公司 Preparation method of tackifier for addition type liquid silicone rubber

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220135805A1 (en) * 2019-11-12 2022-05-05 Showa Denko K. K. Method for producing silicon-containing oxide-coated aluminum nitride particles and method for producing exoergic resin composition
CN111041845A (en) * 2019-12-26 2020-04-21 深圳德邦界面材料有限公司 Organic silicon heat-conducting insulating sheet 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
CN112322251A (en) * 2020-10-27 2021-02-05 复旦大学 Thermosetting yellowing-resistant full-lamination special material and preparation method and application thereof
CN112322251B (en) * 2020-10-27 2021-12-07 复旦大学 Thermosetting yellowing-resistant full-lamination special material and preparation method and application thereof
CN114350311A (en) * 2022-01-10 2022-04-15 东莞市佳迪新材料有限公司 Organic silicon heat-conducting pouring sealant composition for photovoltaic inverter and preparation method thereof
CN116804086A (en) * 2023-08-25 2023-09-26 成都思立可科技有限公司 Long-chain alkyl-polar group co-modified polysiloxane and preparation method thereof
CN116804086B (en) * 2023-08-25 2023-11-07 成都思立可科技有限公司 Long-chain alkyl-polar group co-modified polysiloxane and preparation method thereof

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Application publication date: 20170609