CN105348807A - Silicon dioxide/graphene/graphite compound heat-conducting silicone grease and preparation method thereof - Google Patents
Silicon dioxide/graphene/graphite compound heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- CN105348807A CN105348807A CN201510919527.9A CN201510919527A CN105348807A CN 105348807 A CN105348807 A CN 105348807A CN 201510919527 A CN201510919527 A CN 201510919527A CN 105348807 A CN105348807 A CN 105348807A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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
- C08L83/04—Polysiloxanes
- C08L83/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses silicon dioxide/graphene/graphite compound heat-conducting silicone grease and a preparation method thereof. The silicon dioxide/graphene/graphite compound heat-conducting silicone grease is a product obtained by mixing silicone oil, silicon dioxide, graphene, graphite, a coupling agent, a cross-linking agent, a surface modifier and an antioxygen, and then stirring evenly by an internal mixer. The heat-conducting silicone grease can effectively lower interface contact heat resistance between a high-power electrical appliance node and a cooling device, accelerates heat transfer, and meanwhile is simple in preparation process, high in cost performance and wide in application.
Description
Technical field
The present invention relates to a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease and preparation method thereof, be mainly applicable to the fields such as high-power electric appliance 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.
The performance of Graphene excellence, causes the attention of numerous investigators, the heat conductivility of its excellence, for the thermally conductive material of processability excellence provides direction.The present invention by the Surface coating of surface-modifying agent to Graphene, graphite, then under the prerequisite making full use of its heat conductivility, improves insulating property.Silicon-dioxide thermal conductivity is high, thermal expansivity is little, dielectric properties are good, and wide material sources.By composite with Graphene, graphite, can prepare that thermal conductivity is high, high, the widely used heat-conducting silicone grease of excellent insulation performance, cost performance.
Summary of the invention
The object of the present invention is to provide a kind of for high-power electric appliance package cooling, a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease.
A kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease provided by the invention, this heat-conducting silicone grease, by the composite heat conductive filler filling silicon oil of improved silica/Graphene/graphite, is made by Banbury mixer banburying.Wherein each component and mass fraction thereof are: silicone oil 20 ~ 40 parts (preferably 20 parts), the composite heat conductive filler of improved silica/Graphene/graphite 60 ~ 80 parts (preferably 70 parts), silane coupling agent is the 3% ~ 8%(preferably 5% of heat conductive filler volume), linking agent is the 0.1% ~ 1%(preferably 0.5% of dimethyl silicone oil number), surface-modifying agent 0.1 ~ 1 part (preferably 0.5 part), oxidation inhibitor are 0.1 ~ 1 part (preferably 0.5 part).
Described silicone oil is: dimethyl silicone oil: methyl phenyl silicone oil: MethylethoxylsiliconFluid Fluid=1:1:1, wherein dimethyl silicone oil viscosity when temperature is 25 DEG C is the preferred 500cps of 100 ~ 1000cps(), methyl phenyl silicone oil viscosity when temperature is 25 DEG C is the preferred 200cps of 50 ~ 500cps(), MethylethoxylsiliconFluid Fluid viscosity when temperature is 25 DEG C is the preferred 300cps of 100 ~ 500cps().
The D50 of described silicon-dioxide is the preferred 10um of 5 ~ 20um().
Described Graphene is the Graphene obtained by strong acid reduction-oxidation.
The particle diameter of described graphite is the preferred 15um of 10 ~ 20um().
Described coupling agent is γ-methacryloxypropyl trimethoxy silane (KH570): γ-glycidyl ether oxygen propyl trimethoxy silicane (K560)=1:1.
Described linking agent combines by dicumyl peroxide (DCP) and cyanacrylate (TAIC) mass parts 1:1 and obtains.
The solution that described surface-modifying agent obtains in dimethyl sulfoxide (DMSO) for polyvinyl alcohol dissolution.
Described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010).
The preparation of described a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease comprises the following steps:
(1) accurately take the graphite of the Graphene of 5 ~ 15 parts (preferably 10 parts), 5 ~ 15 parts (preferably 10 parts), by the preferred 2400r/min of high-speed mixer 1800 ~ 3000r/min(), the preferred 15min of 10 ~ 20min() mix, stand-by;
(2) dehydrated alcohol getting 200 parts in reactor in, the surface-modifying agent getting 0.1 ~ 1 part (preferably 0.5 parts by volume) joins in dehydrated alcohol, constant temperature 60 ~ 100 DEG C (preferably 80 DEG C), the preferred 200r/min of 100 ~ 300r/min() stir the preferred 15min of 10 ~ 20min() obtain ethanolic soln, heat conductive filler in (1) is joined in ethanolic soln, the preferred 1.5h of ultrasonic agitation 1 ~ 2h();
(3) again by filler 3% ~ 8%(preferably 5%) coupling agent join in reactor, constant temperature 60 ~ 100 DEG C (preferably 80 DEG C), the preferred 200r/min of 100 ~ 300r/min() stir the preferred 15min of 10 ~ 20min(), add the silicon-dioxide of 40 ~ 60 parts (preferably 50 parts), the preferred 1.5h of ultrasonic agitation 1 ~ 2h(), treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(4) 0.1% ~ 1% linking agent of the modification heat conductive filler 60 ~ 80 parts (3) obtained, 20 ~ 40 parts of silicone oil, silicone oil number, surface-modifying agent 0.1 ~ 1 part, oxidation inhibitor are 0.1 ~ 1 part, join in Banbury mixer, 80 DEG C, 15r/min, 100 DEG C, 25r/min, 120 DEG C, the preferred 50min of each banburying 40 ~ 60min(in 35r/min situation), obtain composite heat-conducting silicone grease.
The present invention takes full advantage of the characteristic of Graphene, graphite high thermal conductivity coefficient, and by composite with silicon-dioxide, both effectively improves thermal conductivity, guarantees again its insulating property.Heat conductive filler through surface-modifying agent, coupling agent modified, good with oil compatibility, do not reunite, 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 Graphene of 5 parts, the graphite of 5 parts, by high-speed mixer 2400r/min, stir 15min, mix, stand-by;
(2) dehydrated alcohol getting 200 parts in reactor in, the surface-modifying agent measuring 0.5 part joins in dehydrated alcohol, constant temperature 80 DEG C, and 200r/min stirs 15min and obtains ethanolic soln, heat conductive filler in (1) is joined in ethanolic soln, ultrasonic agitation 1.5h;
(3) again the coupling agent of 3 parts is joined in reactor, constant temperature 80 DEG C, 200r/min, stir 15min, add the silicon-dioxide of 60 parts, ultrasonic agitation 1.5h, treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(4) the modification heat conductive filler (3) obtained, 26 parts of silicone oil, the linking agent of 0.2 part, surface-modifying agent 0.5 part, 0.5 part, oxidation inhibitor, join in Banbury mixer, 80 DEG C, 15r/min, 100 DEG C, 25r/min, 120 DEG C, each banburying 50min in 35r/min situation, obtain composite heat-conducting silicone grease.
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 5.3W/ (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 5.0W/ (mK), Heat stability is good.
Embodiment 2:
(1) accurately take the Graphene of 10 parts, the graphite of 10 parts, by high-speed mixer 2400r/min, stir 15min, mix, stand-by;
(2) dehydrated alcohol getting 200 parts in reactor in, the surface-modifying agent measuring 0.5 part joins in dehydrated alcohol, constant temperature 80 DEG C, and 200r/min stirs 15min and obtains ethanolic soln, heat conductive filler in (1) is joined in ethanolic soln, ultrasonic agitation 1.5h;
(3) again the coupling agent of 3 parts is joined in reactor, constant temperature 80 DEG C, 200r/min, stir 15min, add the silicon-dioxide of 50 parts, ultrasonic agitation 1.5h, treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(4) the modification heat conductive filler (3) obtained, 26 parts of silicone oil, the linking agent of 0.2 part, surface-modifying agent 0.5 part, 0.5 part, oxidation inhibitor, join in Banbury mixer, 80 DEG C, 15r/min, 100 DEG C, 25r/min, 120 DEG C, each banburying 50min in 35r/min situation, obtain composite heat-conducting silicone grease.
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 5.6W/ (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 5.3W/ (mK), Heat stability is good.
Embodiment 3:
(1) accurately take the Graphene of 15 parts, the graphite of 15 parts, by high-speed mixer 2400r/min, stir 15min, mix, stand-by;
(2) dehydrated alcohol getting 200 parts in reactor in, the surface-modifying agent measuring 0.5 part joins in dehydrated alcohol, constant temperature 80 DEG C, and 200r/min stirs 15min and obtains ethanolic soln, heat conductive filler in (1) is joined in ethanolic soln, ultrasonic agitation 1.5h;
(3) again the coupling agent of 3 parts is joined in reactor, constant temperature 80 DEG C, 200r/min, stir 15min, add the silicon-dioxide of 40 parts, ultrasonic agitation 1.5h, treat that ethanol evaporation is complete, obtain the composite heat conductive filler of modification;
(4) the modification heat conductive filler (3) obtained, 26 parts of silicone oil, the linking agent of 0.2 part, surface-modifying agent 0.5 part, 0.5 part, oxidation inhibitor, join in Banbury mixer, 80 DEG C, 15r/min, 100 DEG C, 25r/min, 120 DEG C, each banburying 50min in 35r/min situation, obtain composite heat-conducting silicone grease.
After testing, the thermal conductivity of prepared heat-conducting silicone grease is 5.1W/ (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 5.0W/ (mK), Heat stability is good.
Claims (10)
1. silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease, each component and mass fraction thereof are: silicone oil 20 ~ 40 parts, the composite heat conductive filler of improved silica/Graphene/graphite 60 ~ 80 parts, coupling agent is 3% ~ 8% of heat conductive filler, linking agent is 0.1% ~ 1% of dimethyl silicone oil, and surface-modifying agent 0.1 ~ 1 part, oxidation inhibitor are 0.1 ~ 1 part.
2. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, it is characterized in that: described silicone oil is: dimethyl silicone oil: methyl phenyl silicone oil: MethylethoxylsiliconFluid Fluid=1:1:1, wherein dimethyl silicone oil viscosity when temperature is 25 DEG C is 100 ~ 1000cps, methyl phenyl silicone oil viscosity when temperature is 25 DEG C is 50 ~ 500cps, and MethylethoxylsiliconFluid Fluid viscosity when temperature is 25 DEG C is 100 ~ 500cps.
3. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, it is characterized in that: described improved silica/composite heat conductive filler of Graphene/graphite, its preparation comprises the following steps:
(1): accurately take the Graphene of 5 ~ 15 parts, the graphite of 5 ~ 15 parts, mixed by high-speed mixer 1800 ~ 3000r/min, 10 ~ 20min, stand-by; (2): the dehydrated alcohol getting 200 parts in reactor in, the surface-modifying agent getting 0.1 ~ 1 part joins in dehydrated alcohol, constant temperature 60 ~ 100 DEG C, and 100 ~ 300r/min stirs 10 ~ 20min and obtains ethanolic soln, heat conductive filler in (1) is joined in ethanolic soln, ultrasonic agitation 1 ~ 2h; (3): join in reactor by the coupling agent of filler 3% ~ 8% again, constant temperature 60 ~ 100 DEG C, 100 ~ 300r/min stirs 10 ~ 20min, adds the silicon-dioxide of 40 ~ 60 parts, ultrasonic agitation 1 ~ 2h, treats that ethanol evaporation is complete, obtains the composite heat conductive filler of modification.
4. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, it is characterized in that: its preparation comprises the following steps: the linking agent of modification heat conductive filler 60 ~ 80 parts, 20 ~ 40 parts of silicone oil, silicone oil quality 0.1% ~ 1%, surface-modifying agent 0.1 ~ 1 part, oxidation inhibitor are 0.1 ~ 1 part, join in Banbury mixer, 80 DEG C, 15r/min, 100 DEG C, 25r/min, 120 DEG C, each banburying 40 ~ 60min in 35r/min situation, obtain composite heat-conducting silicone grease.
5. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: the D50 of described silicon-dioxide is the preferred 10um of 5 ~ 20um().
6. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: described Graphene is the Graphene prepared by vapour deposition process (CVD).
7. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: the particle diameter of described graphite is the preferred 15um of 10 ~ 20um().
8. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: described coupling agent is γ-methacryloxypropyl trimethoxy silane (KH570): γ-glycidyl ether oxygen propyl trimethoxy silicane (KH560)=1:1.
9. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: described linking agent is dicumyl peroxide (DCP).
10. a kind of silicon-dioxide/Graphene/graphite composite heat-conducting silicone grease according to claim 1, is characterized in that: the solution that described surface-modifying agent obtains in dimethyl sulfoxide (DMSO) for polyvinyl alcohol dissolution.
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| CN201510919527.9A CN105348807A (en) | 2015-12-14 | 2015-12-14 | Silicon dioxide/graphene/graphite compound heat-conducting silicone grease and preparation method thereof |
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Cited By (7)
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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 |
| CN107722630A (en) * | 2017-11-15 | 2018-02-23 | 郴州国盛新材科技有限公司 | A kind of CNT/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
| CN107722631A (en) * | 2017-11-15 | 2018-02-23 | 郴州国盛新材科技有限公司 | A kind of CNT/zinc oxide/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
| CN107746576A (en) * | 2017-11-15 | 2018-03-02 | 郴州国盛新材科技有限公司 | A kind of silica/micro- swollen graphite/graphite composite heat-conducting silicone grease and preparation method thereof |
| CN109912980A (en) * | 2019-01-31 | 2019-06-21 | 无锡海特信成高分子科技有限公司 | A kind of High thermal-conductive silicone grease and preparation method thereof |
| CN113801476A (en) * | 2020-06-11 | 2021-12-17 | 山东海科创新研究院有限公司 | Nano-silica composite graphene heat-conducting silicone grease for GPU and preparation method thereof |
| CN116731690A (en) * | 2023-06-12 | 2023-09-12 | 长江大学 | Well cementation heat conduction material and preparation method thereof |
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Cited By (8)
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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 |
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| CN107722630A (en) * | 2017-11-15 | 2018-02-23 | 郴州国盛新材科技有限公司 | A kind of CNT/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
| CN107722631A (en) * | 2017-11-15 | 2018-02-23 | 郴州国盛新材科技有限公司 | A kind of CNT/zinc oxide/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
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| CN109912980A (en) * | 2019-01-31 | 2019-06-21 | 无锡海特信成高分子科技有限公司 | A kind of High thermal-conductive silicone grease and preparation method thereof |
| CN113801476A (en) * | 2020-06-11 | 2021-12-17 | 山东海科创新研究院有限公司 | Nano-silica composite graphene heat-conducting silicone grease for GPU and preparation method thereof |
| CN116731690A (en) * | 2023-06-12 | 2023-09-12 | 长江大学 | Well cementation heat conduction material and preparation method thereof |
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Application publication date: 20160224 |