CN105400202A - Boron nitride/graphene composite heat-conducting silicone grease and preparation method thereof - Google Patents
Boron nitride/graphene composite heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- CN105400202A CN105400202A CN201510919619.7A CN201510919619A CN105400202A CN 105400202 A CN105400202 A CN 105400202A CN 201510919619 A CN201510919619 A CN 201510919619A CN 105400202 A CN105400202 A CN 105400202A
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Abstract
The invention discloses a boron nitride/graphene composite heat-conducting silicone grease and a preparation method thereof. The boron nitride/graphene composite heat-conducting silicone grease is prepared from methyl phenyl silicone oil, boron nitride, graphene, a coupling agent, a cross-linking agent, a structure improving aid and an anti-oxidant through mixing and uniform stirring via an internal mixer. The heat-conducting silicone grease can effectively reduce interfacial thermal contact resistance of a large-power electronic component heat-generating body and a heat radiation apparatus and accelerates heat transfer; and the preparation method is simple and has high cost performance and a wide application scope.
Description
Technical field
The present invention relates to a kind of boron nitride/Graphene composite heat-conducting silicone grease and preparation method thereof, be mainly applicable to the fields such as high-power electronic component package cooling.
Background technology
Heat-conducting silicone grease is a kind of high heat conduction organosilicon material, can keep paste for a long time at-50 ~ 300 DEG C of temperature, is widely used in, between high power electronic components and parts heating element and cooling base, significantly reducing interface contact heat resistance.Along with electronic devices and components are to high-power, intensivization development, excellent heat stability high to thermal conductivity, the high-performance heat-conducting silicone grease demand analysing oil value low are increasing.
Boron nitride has good electrical insulating property, thermal conductivity and chemical resistance, has now been widely used in heat conduction functional materials.Along with going deep into of research, the Application Areas of Graphene is constantly expanded, and excellent heat conductivility becomes a megatrend of preparation High-performance heat conduction material.By boron nitride, Graphene composite, be filled into and inside silicone oil, can obtain that thermal conductivity is high, the heat-conducting silicone grease of excellent insulation performance.
Summary of the invention
The object of the present invention is to provide a kind of a kind of boron nitride for high-power electronic component package cooling/Graphene composite heat-conducting silicone grease.
A kind of boron nitride provided by the invention/Graphene composite heat-conducting silicone grease, this heat-conducting silicone grease fills methyl phenyl silicone oil by the composite heat conductive filler of modification boron nitride/Graphene, is made by Banbury mixer banburying.Wherein each component and massfraction thereof are: methyl phenyl silicone oil 10 ~ 30 parts (preferably 20 parts), the composite heat conductive filler of modification boron nitride/Graphene 60 ~ 90 parts (preferably 75 parts), silane coupling agent is the 3% ~ 8%(preferably 5% of heat conductive filler), linking agent is the 0.1% ~ 1%(preferably 0.5% of methyl phenyl silicone oil), structure improves auxiliary agent 0.1 ~ 1 part (preferably 0.5 part), 0.1 ~ 1 part, oxidation inhibitor (preferably 0.5 part).
Described methyl phenyl silicone oil viscosity when temperature is 25 DEG C is the preferred 300cps of 100 ~ 500cps().
The D50 of described boron nitride is the preferred 10um of 5 ~ 20um().
Described Graphene is the function graphene oxide obtained by strong acid reduction-oxidation.
Described coupling agent is: γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560): γ-aminopropyl triethoxysilane (KH550)=1:1.
Described linking agent combines by dicumyl peroxide (DCP) and cyanacrylate (TAIC) mass parts 1:1 and obtains.
Described structure activator is aerosil.
Described oxidation inhibitor is diisooctyl aniline.
The preparation of described a kind of boron nitride/Graphene composite heat-conducting silicone grease comprises the following steps:
(1) accurately take the Graphene of the boron nitride of 55 ~ 75 parts (preferably 65 parts), 5 ~ 15 parts (preferably 10 parts), by the preferred 2400r/min of high-speed mixer 1800 ~ 3000r/min(), the preferred 10min of 5 ~ 15min() mix, stand-by;
(2) 3% ~ 8%(preferably 5% is got) silane coupling agent of heat conductive filler joins in the dehydrated alcohol of 300 parts, constant temperature water bath 60 ~ 100 DEG C (preferably 80 DEG C), heat conductive filler in (1) is joined in ethanolic soln, the preferred 3h of ultrasonic agitation 2 ~ 4h(), treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(3) 0.1% ~ 1%(of the modification heat conductive filler (2) obtained 60 ~ 90 parts, methyl phenyl silicone oil 10 ~ 30 parts, methyl phenyl silicone oil parts by volume preferably 0.5%) linking agent, the structure activator of 0.1 ~ 1 part (preferably 0.5 part), the oxidation inhibitor of 0.1 ~ 1 part (preferably 0.5 part) join in Banbury mixer, 80 DEG C, 10r/min, 95 DEG C, 20r/min, 115 DEG C, the preferred 50min of each banburying 40 ~ 60min(in 30r/min situation), obtain composite heat-conducting silicone grease.
The present invention takes full advantage of the characteristic of Graphene high thermal conductivity coefficient, and by composite with boron nitride, both effectively improves thermal conductivity, guarantees again its insulating property.Heat conductive filler through coupling agent modified, with oil compatibility is good, filler is not reunited, interracial contact is good.The heat-conducting silicone grease excellent heat stability of preparation, analyses oil value low, uses without dry and cracked, powder phenomenon-tion for a long time.Meanwhile, preparation technology is simple, the cycle is short, significant to lifting industry product quality.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
(1) accurately take the boron nitride of 55 parts, the Graphene of 15 parts, by high-speed mixer 2400r/min, stir 10min, mix, stand-by;
(2) silane coupling agent measuring 3.5 parts joins in the dehydrated alcohol of 300 parts, and constant temperature water bath selects 80 DEG C, joins in ethanolic soln, ultrasonic agitation 3h by the heat conductive filler in (1), treats that ethanol evaporation is complete, obtains the composite heat conductive filler of modification;
(3) the modification heat conductive filler (2) obtained, 25 parts of methyl phenyl silicone oils, the linking agent of 0.4 part, the aerosil of 0.5 part, diisooctyl aniline of 0.5 part, join in Banbury mixer, 80 DEG C, 10r/min, 95 DEG C, 20r/min, 115 DEG C, each banburying 50min in 30r/min situation, obtain composite heat-conducting silicone grease.
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 4.6W/ (mK), and through 230 DEG C, the continuous heat treatment of 5000h, result display heat-conducting silicone grease coating still keeps paste, after thermal treatment, thermal conductivity is 4.5W/ (mK), Heat stability is good.
Embodiment 2:
(1) accurately take the boron nitride of 65 parts, the Graphene of 10 parts, by high-speed mixer 2400r/min, stir 10min, mix, stand-by;
(2) silane coupling agent measuring 4 parts joins in the dehydrated alcohol of 300 parts, and constant temperature water bath selects 80 DEG C, joins in ethanolic soln, ultrasonic agitation 3h by the heat conductive filler in (1), treats that ethanol evaporation is complete, obtains the composite heat conductive filler of modification;
(3) the modification heat conductive filler (2) obtained, 19.6 parts of methyl phenyl silicone oils, the linking agent of 0.4 part, the aerosil of 0.5 part, diisooctyl aniline of 0.5 part, join in Banbury mixer, 80 DEG C, 10r/min, 95 DEG C, 20r/min, 115 DEG C, each banburying 50min in 30r/min situation, obtain composite heat-conducting silicone grease;
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 5.2W/ (mK), and through 230 DEG C, the continuous heat treatment of 5000h, result display heat-conducting silicone grease coating still keeps paste, after thermal treatment, thermal conductivity is 5.1W/ (mK), Heat stability is good.
Embodiment 3:
(1) accurately take the boron nitride of 75 parts, the Graphene of 5 parts, by high-speed mixer 2400r/min, stir 10min, mix, stand-by;
(2) silane coupling agent measuring 4 parts joins in the dehydrated alcohol of 300 parts, and constant temperature water bath selects 80 DEG C, joins in ethanolic soln, ultrasonic agitation 3h by the heat conductive filler in (1), treats that ethanol evaporation is complete, obtains the composite heat conductive filler of modification;
(3) the modification heat conductive filler (2) obtained, 14.6 parts of methyl phenyl silicone oils, the linking agent of 0.4 part, the aerosil of 0.5 part, diisooctyl aniline of 0.5 part, join in Banbury mixer, 80 DEG C, 10r/min, 95 DEG C, 20r/min, 115 DEG C, each banburying 50min in 30r/min situation, obtain composite heat-conducting silicone grease;
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 4.7W/ (mK), and through 230 DEG C, the continuous heat treatment of 5000h, result display heat-conducting silicone grease coating still keeps paste, after thermal treatment, thermal conductivity is 4.5W/ (mK), Heat stability is good.
Claims (8)
1. boron nitride/Graphene composite heat-conducting silicone grease, each component and mass fraction consist of: methyl phenyl silicone oil 10 ~ 30 parts, the composite heat conductive filler of modification boron nitride/Graphene 60 ~ 90 parts, silane coupling agent is 3% ~ 8% of heat conductive filler, linking agent is 0.1% ~ 1% of methyl phenyl silicone oil, structure improves auxiliary agent 0.1 ~ 1 part, 0.1 ~ 1 part, oxidation inhibitor.
2. the composite heat conductive filler of modification boron nitride/Graphene according to claim 1, is characterized in that comprising the following steps:
(1): take the boron nitride of 55 ~ 75 parts, the Graphene of 5 ~ 15 parts, mixed by high-speed mixer 1800 ~ 3000r/min, 5 ~ 15min, stand-by;
(2): the silane coupling agent measuring 3% ~ 8% heat conductive filler joins in the dehydrated alcohol of 300 parts, constant temperature water bath 60 ~ 100 DEG C, joins in ethanolic soln by the heat conductive filler in (1), ultrasonic agitation 2 ~ 4h, treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(3): the modification heat conductive filler that (2) are obtained 60 ~ 90 parts, methyl phenyl silicone oil 10 ~ 30 parts, methyl phenyl silicone oil parts by volume 0.1% ~ 1% linking agent, the structure activator of 0.1 ~ 1 part, the oxidation inhibitor of 0.1 ~ 1 part join in Banbury mixer, at 80 DEG C, 10r/min, 95 DEG C, 20r/min, 115 DEG C, each banburying 40 ~ 60min in 30r/min situation, obtain composite heat-conducting silicone grease.
3. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: described Graphene is the function graphene oxide obtained by strong acid reduction-oxidation.
4. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: the D50 of described boron nitride is 5 ~ 20um.
5. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: described coupling agent is: γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560): γ-aminopropyl triethoxysilane (KH550)=1:1.
6. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: described linking agent combines with cyanacrylate (TAIC) mass parts 1:1 by dicumyl peroxide (DCP).
7. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: described structure activator is aerosil.
8. a kind of boron nitride according to claim 1/Graphene composite heat-conducting silicone grease, is characterized in that: described oxidation inhibitor is diisooctyl aniline.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733265A (en) * | 2016-03-25 | 2016-07-06 | 江南石墨烯研究院 | Preparation method of heat-conducting silicone grease |
| CN105838077A (en) * | 2016-04-06 | 2016-08-10 | 深圳市欧普特工业材料有限公司 | Surface treatment method of graphene used for producing heat conducting silicon sheets |
| CN107033602A (en) * | 2017-05-17 | 2017-08-11 | 醴陵市时代鑫湘科技有限公司 | Used in composite insulator high-strength silicone rubber insulating materials |
| CN107216850A (en) * | 2017-06-20 | 2017-09-29 | 东莞市联洲知识产权运营管理有限公司 | A kind of highly conductive organic silicon adhesive of high heat conduction and preparation method thereof |
| CN107345071A (en) * | 2017-07-05 | 2017-11-14 | 安徽中威光电材料有限公司 | A kind of high heat conductive insulating type silicone grease of modified graphene microplate filling and preparation method thereof |
| CN108148558A (en) * | 2016-12-06 | 2018-06-12 | 中国科学院金属研究所 | A kind of thermally conductive gel of graphene-containing and its preparation method and application |
| CN108219757A (en) * | 2017-12-27 | 2018-06-29 | 复旦大学 | The preparation method of heat conductive insulating composite membrane in a kind of high face |
| CN108624226A (en) * | 2018-05-25 | 2018-10-09 | 国网江苏省电力有限公司电力科学研究院 | A kind of graphene electric force compounded grease and preparation method thereof |
| CN110862670A (en) * | 2019-12-12 | 2020-03-06 | 罗更荣 | Heat-conducting boron nitride-modified polyurea insulating composite material and preparation method thereof |
| CN111393856A (en) * | 2020-04-20 | 2020-07-10 | 苏州锦富技术股份有限公司 | Graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste and preparation method thereof |
| CN113429878A (en) * | 2021-06-30 | 2021-09-24 | 成都新柯力化工科技有限公司 | Low-cost high-temperature-resistant graphene composite heat dissipation coating and preparation method thereof |
| CN114181532A (en) * | 2021-12-22 | 2022-03-15 | 仲恺农业工程学院 | Phase-change heat-conducting silicone grease containing macromolecular modifier and preparation method thereof |
| CN114907698A (en) * | 2022-07-01 | 2022-08-16 | 深圳清华大学研究院 | Modified graphene oxide heat-conducting silicone grease and preparation method thereof |
| CN114940828A (en) * | 2022-06-30 | 2022-08-26 | 深圳市傲川科技有限公司 | Insulating high-thermal-conductivity film and preparation method thereof |
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| CN105733265A (en) * | 2016-03-25 | 2016-07-06 | 江南石墨烯研究院 | Preparation method of heat-conducting silicone grease |
| CN105838077A (en) * | 2016-04-06 | 2016-08-10 | 深圳市欧普特工业材料有限公司 | Surface treatment method of graphene used for producing heat conducting silicon sheets |
| CN108148558A (en) * | 2016-12-06 | 2018-06-12 | 中国科学院金属研究所 | A kind of thermally conductive gel of graphene-containing and its preparation method and application |
| CN107033602A (en) * | 2017-05-17 | 2017-08-11 | 醴陵市时代鑫湘科技有限公司 | Used in composite insulator high-strength silicone rubber insulating materials |
| CN107216850A (en) * | 2017-06-20 | 2017-09-29 | 东莞市联洲知识产权运营管理有限公司 | A kind of highly conductive organic silicon adhesive of high heat conduction and preparation method thereof |
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| CN108624226A (en) * | 2018-05-25 | 2018-10-09 | 国网江苏省电力有限公司电力科学研究院 | A kind of graphene electric force compounded grease and preparation method thereof |
| CN110862670A (en) * | 2019-12-12 | 2020-03-06 | 罗更荣 | Heat-conducting boron nitride-modified polyurea insulating composite material and preparation method thereof |
| CN111393856A (en) * | 2020-04-20 | 2020-07-10 | 苏州锦富技术股份有限公司 | Graphene-based high-thermal-conductivity low-thermal-resistance thermal conductive paste and preparation method thereof |
| CN113429878A (en) * | 2021-06-30 | 2021-09-24 | 成都新柯力化工科技有限公司 | Low-cost high-temperature-resistant graphene composite heat dissipation coating and preparation method thereof |
| CN114181532A (en) * | 2021-12-22 | 2022-03-15 | 仲恺农业工程学院 | Phase-change heat-conducting silicone grease containing macromolecular modifier and preparation method thereof |
| CN114181532B (en) * | 2021-12-22 | 2023-01-03 | 仲恺农业工程学院 | Phase-change heat-conducting silicone grease containing macromolecular modifier and preparation method thereof |
| CN114940828A (en) * | 2022-06-30 | 2022-08-26 | 深圳市傲川科技有限公司 | Insulating high-thermal-conductivity film and preparation method thereof |
| CN114907698A (en) * | 2022-07-01 | 2022-08-16 | 深圳清华大学研究院 | Modified graphene oxide heat-conducting silicone grease and preparation method thereof |
| CN114907698B (en) * | 2022-07-01 | 2023-08-15 | 深圳清华大学研究院 | Modified graphene oxide heat-conducting silicone grease and preparation method thereof |
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