CN107304294A - A kind of organosilicon thermally conductive sheet and preparation method thereof - Google Patents

A kind of organosilicon thermally conductive sheet and preparation method thereof Download PDF

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Publication number
CN107304294A
CN107304294A CN201610242402.1A CN201610242402A CN107304294A CN 107304294 A CN107304294 A CN 107304294A CN 201610242402 A CN201610242402 A CN 201610242402A CN 107304294 A CN107304294 A CN 107304294A
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parts
thermally conductive
conductive sheet
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rpm
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冒小峰
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New Technology (changzhou) Co Ltd
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New Technology (changzhou) Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02Materials undergoing a change of physical state when used
    • C09K5/06Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
    • C09K5/066Cooling mixtures; De-icing compositions
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/003Additives being defined by their diameter
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • 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
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Physics & Mathematics (AREA)
  • Combustion & Propulsion (AREA)
  • Thermal Sciences (AREA)
  • Materials Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a kind of organosilicon thermally conductive sheet that can be applied to electronic component and electronic product, including substrate and include phase change microsphere in the substrate, the substrate includes following components:100 parts of vinyl silicone oils, 40~60 parts of MQ resins, 8~12 parts of containing hydrogen silicone oils, 140~160 parts of Zinc oxide powders, 840~960 parts of alumina powders and 20~40 parts of reinforced white carbon blacks, the substrate also include catalyst and inhibitor.The invention further relates to the preparation method of above-mentioned organosilicon thermally conductive sheet.A kind of organosilicon thermally conductive sheet of the present invention can reach the purpose for keeping electronic equipment surface temperature to be no more than phase transition temperature within a certain period of time by introducing phase change microsphere in heat-conducting pad.

Description

A kind of organosilicon thermally conductive sheet and preparation method thereof
Technical field
The present invention relates to organosilicon Heat Conduction Material technology, and in particular to a kind of organosilicon thermally conductive sheet and preparation method thereof, should Organic thermally conductive sheet can be applied to the radiating of electronic component and electronic product.
Background technology
In heat dissipation design, thermal contact resistance is produced due to insufficient contact between hot interface, cause hot-fluid conduction by Serious obstruction.To solve this problem, one layer of thermal interfacial material of pad between heater and radiator.Organosilicon thermally conductive sheet is Based on addition-type silicon rubber, a kind of soft heat conduction circle that addition heat filling, auxiliary agent etc. pass through addition reaction curing molding Facesheet, can blind, complete the heat transfer of heating position and radiating part interdigit, at the same insulation can also be played, it is damping, close The effect such as envelope, meets electronic component and miniaturization of electronic products and the design requirement of ultrathin.Organosilicon thermally conductive sheet has matter Gently, the features such as resistant to chemical etching, easy processing shaping, excellent electrical insulation capability, mechanics and excellent anti-fatigue performance, add higher Heat conductivility, thus with extensively using field.But there is following technical problem in prior art:Existing heat treatment technics is main Using heat conduction technology, while heater element radiates, the also rapid rise therewith of equipment surface temperature is easily sent out when in use Scald, be unfavorable for the stability of nonrefractory material, for handheld devices such as mobile phones, have a strong impact on its sense of touch.
The content of the invention
For defect present in prior art, the technical problems to be solved by the invention are to provide a kind of with certain storage Hot merit energy, can make the temperature of electronic equipment maintain organosilicon thermally conductive sheet within specified temp within a certain period of time.
In order to solve the above technical problems, the organosilicon thermally conductive sheet of the present invention includes substrate, phase is also included in the substrate Change microsphere.
It is preferred that, the phase change microsphere is core-shell structure.
It is preferred that, the phase transition temperature of the phase change microsphere is 35 DEG C~70 DEG C.
It is preferred that, the particle diameter distribution of the phase change microsphere is 10 μm~50 μm.
It is preferred that, the substrate is according to the mass fraction, composed of the following components:
100 parts of vinyl silicone oil,
40~60 parts of MQ resins,
8~12 parts of containing hydrogen silicone oil,
140~160 parts of Zinc oxide powder,
840~960 parts of alumina powder,
20~40 parts of reinforced white carbon black,
The substrate also includes catalyst and inhibitor.
It is preferred that, the catalyst is liquid platinum organic chelate.
It is preferred that, the platinum content of the catalyst is 1000 ppm.
It is preferred that, the mass fraction of the catalyst is 2 parts.
It is preferred that, the inhibitor is acetylene cyclohexanol.
It is preferred that, the mass fraction of the inhibitor is 0.2~0.5 part.
It is preferred that, the viscosity of the vinyl silicone oil is the mPas of 3000 mPas~5000.
It is preferred that, the contents of ethylene of the vinyl silicone oil is 0.1%~0.3%.
It is preferred that, the molecular weight of the MQ resins is 2000~3000.
It is preferred that, the ratio between the single functionality siloxane unit of the MQ resins and the amount of tetra functional siloxane polycondensation chain link For 7:3~8:2.
It is preferred that, the hydrogen content of the containing hydrogen silicone oil is 0.15%~0.75%.
It is preferred that, the Zinc oxide powder is indirect process zinc oxide.
It is preferred that, the average grain diameter of the Zinc oxide powder is 5 μm~40 μm.
It is preferred that, the alumina powder is ball-aluminium oxide.
It is preferred that, the alumina powder includes alumina powder I and alumina powder II, wherein alumina powder I's Average grain diameter is 40 μm~50 μm, and alumina powder II average grain diameter is 3 μm~8 μm.
It is preferred that, the mass fraction of the alumina powder I is 500~580 parts.
It is preferred that, the mass fraction of the alumina powder II is 340~380 parts.
It is preferred that, the reinforced white carbon black is Hydrophobic White carbon black.
Present invention also offers a kind of method for preparing above-mentioned organosilicon thermally conductive sheet, by vinyl silicone oil, MQ resins, oxidation Zinc powder body, alumina powder and reinforced white carbon black are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 1 h is stirred, 80 DEG C are cooled to, phase change microsphere is added, 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, room temperature is cooled to, adds Catalyst, inhibitor and containing hydrogen silicone oil, 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, and vacuumizing and defoaming obtains creme;By institute Stating creme, to be rolled into the mm of 0.2 mm~5 thick, solidifies 0.5 h under the conditions of 120 DEG C~130 DEG C, you can obtain organosilicon heat conduction Piece.
A kind of organosilicon thermally conductive sheet of the present invention can be reached in a timing by introducing phase change microsphere in heat-conducting pad The interior purpose for keeping electronic equipment surface temperature to be no more than phase transition temperature.
Embodiment
With reference to embodiment, embodiments of the invention are made and further elaborated, following examples Described in number be mass fraction.
Embodiment 1
By 100 parts of vinyl silicone oils, 40 parts of MQ resins, 140 parts of Zinc oxide powders, 500 parts of alumina powder I, 340 parts of aluminum oxide Powder II and 40 parts of reinforced white carbon blacks are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 stirrings 1 H, is cooled to 80 DEG C, adds 80 parts of phase change microspheres, stirs 0.5 h with the rpm of the rpm of rotating speed 30~40, is cooled to room temperature, adds 2 Part catalyst, 0.2 part of inhibitor and 8 parts of containing hydrogen silicone oils, stir 0.5 h, vacuumizing and defoaming is obtained with the rpm of the rpm of rotating speed 30~40 To creme;The creme is rolled into 3 mm thickness, solidifies 0.5 h under the conditions of 120 DEG C~130 DEG C, you can obtain organosilicon and lead Backing 1.
Embodiment 2
By 100 parts of vinyl silicone oils, 50 parts of MQ resins, 150 parts of Zinc oxide powders, 540 parts of alumina powder I, 360 parts of aluminum oxide Powder II and 30 parts of reinforced white carbon blacks are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 stirrings 1 H, is cooled to 80 DEG C, adds 90 parts of phase change microspheres, stirs 0.5 h with the rpm of the rpm of rotating speed 30~40, is cooled to room temperature, adds 2 Part catalyst, 0.4 part of inhibitor and 10 parts of containing hydrogen silicone oils, stir 0.5 h, vacuumizing and defoaming is obtained with the rpm of the rpm of rotating speed 30~40 To creme;The creme is rolled into 3 mm thickness, solidifies 0.5 h under the conditions of 120 DEG C~130 DEG C, you can obtain organosilicon and lead Backing 2.
Embodiment 3
By 100 parts of vinyl silicone oils, 60 parts of MQ resins, 160 parts of Zinc oxide powders, 580 parts of alumina powder I, 380 parts of aluminum oxide Powder II and 20 parts of reinforced white carbon blacks are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 stirrings 1 H, is cooled to 80 DEG C, adds 100 parts of phase change microspheres, stirs 0.5 h with the rpm of the rpm of rotating speed 30~40, is cooled to room temperature, adds 2 Part catalyst, 0.5 part of inhibitor and 12 parts of containing hydrogen silicone oils, stir 0.5 h, vacuumizing and defoaming is obtained with the rpm of the rpm of rotating speed 30~40 To creme;The creme is rolled into 3 mm thickness, solidifies 0.5 h under the conditions of 120 DEG C~130 DEG C, you can obtain organosilicon and lead Backing 3.
Comparative example 1
By 100 parts of vinyl silicone oils, 40 parts of MQ resins, 140 parts of Zinc oxide powders, 500 parts of alumina powder I, 340 parts of aluminum oxide Powder II and 40 parts of reinforced white carbon blacks are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 stirrings 1 H, is cooled to 80 DEG C, and 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, is cooled to room temperature, adds 2 parts of catalyst, 0.2 part of suppression Agent and 8 parts of containing hydrogen silicone oils, 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, and vacuumizing and defoaming obtains creme;By the creme pressure Prolong into 3 mm thick, 0.5 h is solidified under the conditions of 120 DEG C~130 DEG C, you can obtain contrast organosilicon thermally conductive sheet 2.
Comparative example 2
By 100 parts of vinyl silicone oils, 60 parts of MQ resins, 160 parts of Zinc oxide powders, 580 parts of alumina powder I, 380 parts of aluminum oxide Powder II and 20 parts of reinforced white carbon blacks are added in kneader with 120 DEG C of whipping temp, the rpm of the rpm of rotating speed 30~40 stirrings 1 H, is cooled to 80 DEG C, and 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, is cooled to room temperature, adds 2 parts of catalyst, 0.5 part of suppression Agent and 12 parts of containing hydrogen silicone oils, 0.5 h is stirred with the rpm of the rpm of rotating speed 30~40, and vacuumizing and defoaming obtains creme;By the creme It is rolled into 3 mm thick, 0.5 h is solidified under the conditions of 120 DEG C~130 DEG C, you can obtains contrast organosilicon thermally conductive sheet 2.
In above-mentioned implementation 1~3 and comparative example 1~2, the viscosity of vinyl silicone oil is 3000 mPas~5000 MPas, contents of ethylene is 0.1%~0.3%;The molecular weight of MQ resins be 2000~3000, single functionality siloxane unit with The ratio between amount of tetra functional siloxane polycondensation chain link is 7:3~8:2;Zinc oxide powder is indirect process zinc oxide, and average grain diameter is 5 μm~40 μm;Alumina powder I is ball-aluminium oxide, and average grain diameter is 40 μm~50 μm;Alumina powder II is spherical oxygen Change aluminium, average grain diameter is 3 μm~8 μm;Reinforced white carbon black is Hydrophobic White carbon black, and watt gram H2000 is selected in the present embodiment;Phase Change microsphere is core-shell structure, and phase transition temperature is 35 DEG C~37 DEG C, and particle diameter distribution is 10 μm~50 μm;Catalyst is liquid platinum Organic chelate, the platinum content of catalyst is 1000 ppm;Inhibitor is acetylene cyclohexanol.Above-mentioned each material is without specified otherwise , it can be bought from commercial channel.
With reference to ASTM-D5470 standards, the organosilicon thermally conductive sheet 1~3 that is obtained in above-described embodiment 1~3 is determined and above-mentioned right The thermal conductivity of the contrast organosilicon thermally conductive sheet 1~2 obtained in ratio 1~2;The organosilicon obtained in above-described embodiment 1~3 is led The contrast organosilicon thermally conductive sheet 1~2 obtained in backing 1~3 and above-mentioned comparative example 1~2 intercepts the mm samples of 200 mm × 100 respectively In product, the heating plate for being fitted tightly over 70 DEG C, test sample surface temperature after certain time(5 min / 10 min / 20 min / 30 min), test result is as shown in the table.
The organosilicon thermally conductive sheet of the present invention can have while thermal conductivity is ensured it can be seen from above-mentioned test result Effect ground reduces the programming rate of itself, and is maintained in certain time within the scope of certain temperature.

Claims (10)

1. a kind of organosilicon thermally conductive sheet, including substrate, it is characterized in that, include phase change microsphere in the substrate.
2. organosilicon thermally conductive sheet according to claim 1, it is characterized in that, the phase change microsphere is core-shell structure;
It is preferred that, the phase transition temperature of the phase change microsphere is 35 DEG C~70 DEG C;
It is preferred that, the particle diameter distribution of the phase change microsphere is 10 μm~50 μm.
3. the organosilicon thermally conductive sheet according to any one in claim 1~2, it is characterized in that, the substrate presses mass parts Number meter, including following components:
100 parts of vinyl silicone oil,
40~60 parts of MQ resins,
8~12 parts of containing hydrogen silicone oil,
140~160 parts of Zinc oxide powder,
840~960 parts of alumina powder,
20~40 parts of reinforced white carbon black,
The substrate also includes catalyst and inhibitor;
It is preferred that, the reinforced white carbon black is Hydrophobic White carbon black;
It is preferred that, the hydrogen content of the containing hydrogen silicone oil is 0.15%~0.75%.
4. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the catalyst is that liquid platinum is organic chelated Thing;
It is preferred that, the platinum content of the catalyst is 1000 ppm;
It is preferred that, the mass fraction of the catalyst is 2 parts.
5. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the inhibitor is acetylene cyclohexanol;
It is preferred that, the mass fraction of the inhibitor is 0.2~0.5 part.
6. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the viscosity of the vinyl silicone oil is 3000 The mPas of mPas~5000;
It is preferred that, the contents of ethylene of the vinyl silicone oil is 0.1%~0.3%.
7. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the molecular weight of the MQ resins for 2000~ 3000;
It is preferred that, the ratio between the single functionality siloxane unit of the MQ resins and the amount of tetra functional siloxane polycondensation chain link are 7: 3~8:2.
8. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the Zinc oxide powder is indirect process zinc oxide;
It is preferred that, the average grain diameter of the Zinc oxide powder is 5 μm~40 μm.
9. organosilicon thermally conductive sheet according to claim 3, it is characterized in that, the alumina powder is ball-aluminium oxide;
It is preferred that, the alumina powder includes alumina powder I and alumina powder II, wherein alumina powder I particle diameter For 40 μm~50 μm, alumina powder II particle diameter is 3 μm~8 μm;
It is preferred that, the mass fraction of the alumina powder I is 500~580 parts;
It is preferred that, the mass fraction of the alumina powder II is 340~380 parts.
10. a kind of method for preparing organosilicon thermally conductive sheet, by vinyl silicone oil, MQ resins, Zinc oxide powder, alumina powder and Reinforced white carbon black is added in kneader, with 120 DEG C of temperature, the rpm of the rpm of rotating speed 30~40 stirring 1h, is cooled to 80 DEG C, addition Phase change microsphere, with the rpm of the rpm of rotating speed 30~40 stirring 0.5h, is cooled to room temperature, adds catalyst, inhibitor and containing hydrogen silicone oil, With the rpm of the rpm of rotating speed 30~40 stirring 0.5h, vacuumizing and defoaming obtains creme;By the creme calendering formation, 120 DEG C~ Solidify under the conditions of 130 DEG C, you can obtain organosilicon thermally conductive sheet.
CN201610242402.1A 2016-04-19 2016-04-19 A kind of organosilicon thermally conductive sheet and preparation method thereof Pending CN107304294A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109401732A (en) * 2018-10-31 2019-03-01 深圳联腾达科技有限公司 Hypotonic oil heat conductive silica gel gasket and preparation method thereof
CN114621591A (en) * 2022-02-17 2022-06-14 苏州佰旻电子材料科技有限公司 High-bending heat-conducting gasket

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103342896A (en) * 2013-06-26 2013-10-09 苏州天脉导热科技有限公司 High temperature resistant heat-conducting silica gel sheet and preparation method thereof
US20140030458A1 (en) * 2012-07-25 2014-01-30 Hutchinson Rubber Composition Based on a Silicone Elastomer and on a PCM, Process for the Preparation Thereof, Flexible Element and Thermal Control/Regulating System Incorporating Same
CN103773322A (en) * 2014-02-08 2014-05-07 中国电子科技集团公司第三十三研究所 Phase change microcapsule heat conduction material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20140030458A1 (en) * 2012-07-25 2014-01-30 Hutchinson Rubber Composition Based on a Silicone Elastomer and on a PCM, Process for the Preparation Thereof, Flexible Element and Thermal Control/Regulating System Incorporating Same
CN103342896A (en) * 2013-06-26 2013-10-09 苏州天脉导热科技有限公司 High temperature resistant heat-conducting silica gel sheet and preparation method thereof
CN103773322A (en) * 2014-02-08 2014-05-07 中国电子科技集团公司第三十三研究所 Phase change microcapsule heat conduction material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109401732A (en) * 2018-10-31 2019-03-01 深圳联腾达科技有限公司 Hypotonic oil heat conductive silica gel gasket and preparation method thereof
CN114621591A (en) * 2022-02-17 2022-06-14 苏州佰旻电子材料科技有限公司 High-bending heat-conducting gasket

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