Graphene oxide modified compound type heat conducting silicone rubber and preparation method thereof

Abstract

The invention discloses graphene oxide modified compound type heat conducting silicone rubber and a preparation method thereof. According to the preparation method, the compound type silicon resin with high heat conduction property and low expansion factor is prepared by using 0.5-1 part of graphene oxide as heat conducting stuffing and an inorganic crosslinking agent, 10-50 parts of nanometer SiO2 as the heat conducting stuffing, 5-30 parts of compound of two MQ silicone resin containing hydroxyl and vinyl and different in viscosity as a special bonding modifying agent, 1-10 parts of organic hydrogen polysiloxane as an organic crosslinking agent, 0.1-2 parts of platinum complex as a catalyst, 0.01-0.001 part of alkynol substance as an inhibitor and 60-100 parts of polysiloxane resin as base rubber and adopting a nanometer compounding method, wherein the graphene oxide is partially modified by a silane coupling agent, and the nanometer SiO2 is prepared by a sol-gel method. The compound type silicon resin can be widely applied to encapsulation of various electronic components and plays a role in shock absorption and heat dissipation.

Description

technical field

[0001] The invention relates to the technical field of silicone rubber, in particular to a graphene oxide modified composite heat-conducting silicone rubber and a preparation method thereof. Background technique

[0002] With the development of microelectronics technology, electronic components are becoming thinner, lighter, smaller, and multifunctional, and the assembly density of components is getting higher and higher. The heat dissipation of heating elements has become a prominent problem. If the accumulated heat cannot be dissipated in time, it will lead to an increase in the operating temperature of the components, which will directly affect the life and reliability of various high-precision equipment. In the packaging process of electronic components, in order to better reduce the thermal resistance during device assembly and improve the overall heat transfer capability, it is necessary to use a thermal interface material (TIM) between the heat tra...

Examples

Embodiment 1

[0025] Add 230ml of concentrated sulfuric acid into a 1000ml three-neck flask, place it in an ice-water bath, add 10g of primary graphite powder and 5g of sodium nitrate under stirring, stir for 25 minutes, add 30g of oxidant potassium permanganate within 30 minutes, and react for 1 hour. Move the flask to a 35°C water bath and continue to stir for 30 minutes, then add 460ml of deionized water to dilute, and the temperature rises to 95°C. After stirring for 15 minutes, transfer the mixture into a beaker, dilute to 1L with deionized water, add 25ml of H2O2 solution with a mass concentration of 30%, until the color of the reaction solution is golden yellow; wash 3 times with deionized water, add 3 drops HCl solution with a mass concentration of 36.5%; the above reaction solution was repeatedly washed with deionized water until pH=6.5, and finally the washed graphite oxide suspension was vacuum filtered with a Buchner funnel to obtain dry graphene oxide;

[0026]Add 50g of tetrae...

Embodiment 2

[0031] Add 500ml of concentrated sulfuric acid to a 1000ml three-neck flask, place it in an ice-water bath, add 25g of primary graphite powder and 10g of sodium nitrate under stirring, stir for 25 minutes, add 60g of oxidant potassium permanganate within 30 minutes, and react for 1.5h. Move the flask to a 35°C water bath and continue to stir for 25 minutes, then add 500ml of deionized water for dilution, and the temperature rises to 90°C. After stirring for 15 minutes, the mixture was transferred into a beaker, diluted to 1.5 L with deionized water, and 50 ml of 30% H 2 o 2 solution until the color of the reaction solution is golden yellow; wash 5 times with deionized water, add 5 drops of HCl solution with a mass concentration of 35%; wash the above reaction solution repeatedly with deionized water until pH=7.5, and finally Washed graphite oxide suspension is vacuum-filtered with a Buchner funnel to obtain dry graphene oxide;

[0032] Add 50g of tetraethoxysilane, 100g of a...

Embodiment 3

[0037] Add 300ml of concentrated hydrochloric acid into a 1000ml three-neck flask, place it in an ice-water bath, add 15g of primary graphite powder and 7g of sodium nitrate under stirring, stir for 25 minutes, add 45g of oxidant potassium chlorate within 30 minutes, and react for 1 hour. Move the flask to a 30°C water bath and continue stirring for 30 minutes, then add 480ml of deionized water to dilute, and the temperature rises to 95°C; after stirring for 15 minutes, transfer the mixture to a beaker, dilute to 1L with deionized water, and add 30ml of 30%H 2 o 2 solution, until the color of the reaction solution is golden yellow; wash 4 times with deionized water, and add 3 drops of HCl solution with a mass concentration of 36.5%. Repeatedly washing the above-mentioned reaction solution with deionized water until pH=7.0, and finally vacuum-filtering the washed graphite oxide suspension with a Buchner funnel to obtain dry graphene oxide;

[0038] Add 50g of tetramethoxysila...

technical field

[0001] The invention relates to the technical field of silicone rubber, in particular to a graphene oxide modified composite heat-conducting silicone rubber and a preparation method thereof. Background technique

[0002] With the development of microelectronics technology, electronic components are becoming thinner, lighter, smaller, and multifunctional, and the assembly density of components is getting higher and higher. The heat dissipation of heating elements has become a prominent problem. If the accumulated heat cannot be dissipated in time, it will lead to an increase in the operating temperature of the components, which will directly affect the life and reliability of various high-precision equipment. In the packaging process of electronic components, in order to better reduce the thermal resistance during device assembly and improve the overall heat transfer capability, it is necessary to use a thermal interface material (TIM) between the heat tra...

Examples

Embodiment 1

[0025] Add 230ml of concentrated sulfuric acid into a 1000ml three-neck flask, place it in an ice-water bath, add 10g of primary graphite powder and 5g of sodium nitrate under stirring, stir for 25 minutes, add 30g of oxidant potassium permanganate within 30 minutes, and react for 1 hour. Move the flask to a 35°C water bath and continue to stir for 30 minutes, then add 460ml of deionized water to dilute, and the temperature rises to 95°C. After stirring for 15 minutes, transfer the mixture into a beaker, dilute to 1L with deionized water, add 25ml of H2O2 solution with a mass concentration of 30%, until the color of the reaction solution is golden yellow; wash 3 times with deionized water, add 3 drops HCl solution with a mass concentration of 36.5%; the above reaction solution was repeatedly washed with deionized water until pH=6.5, and finally the washed graphite oxide suspension was vacuum filtered with a Buchner funnel to obtain dry graphene oxide;

[0026]Add 50g of tetrae...

Embodiment 2

[0031] Add 500ml of concentrated sulfuric acid to a 1000ml three-neck flask, place it in an ice-water bath, add 25g of primary graphite powder and 10g of sodium nitrate under stirring, stir for 25 minutes, add 60g of oxidant potassium permanganate within 30 minutes, and react for 1.5h. Move the flask to a 35°C water bath and continue to stir for 25 minutes, then add 500ml of deionized water for dilution, and the temperature rises to 90°C. After stirring for 15 minutes, the mixture was transferred into a beaker, diluted to 1.5 L with deionized water, and 50 ml of 30% H 2 o 2 solution until the color of the reaction solution is golden yellow; wash 5 times with deionized water, add 5 drops of HCl solution with a mass concentration of 35%; wash the above reaction solution repeatedly with deionized water until pH=7.5, and finally Washed graphite oxide suspension is vacuum-filtered with a Buchner funnel to obtain dry graphene oxide;

[0032] Add 50g of tetraethoxysilane, 100g of a...

Embodiment 3

[0037] Add 300ml of concentrated hydrochloric acid into a 1000ml three-neck flask, place it in an ice-water bath, add 15g of primary graphite powder and 7g of sodium nitrate under stirring, stir for 25 minutes, add 45g of oxidant potassium chlorate within 30 minutes, and react for 1 hour. Move the flask to a 30°C water bath and continue stirring for 30 minutes, then add 480ml of deionized water to dilute, and the temperature rises to 95°C; after stirring for 15 minutes, transfer the mixture to a beaker, dilute to 1L with deionized water, and add 30ml of 30%H 2 o 2 solution, until the color of the reaction solution is golden yellow; wash 4 times with deionized water, and add 3 drops of HCl solution with a mass concentration of 36.5%. Repeatedly washing the above-mentioned reaction solution with deionized water until pH=7.0, and finally vacuum-filtering the washed graphite oxide suspension with a Buchner funnel to obtain dry graphene oxide;

[0038] Add 50g of tetramethoxysila...