CN104710792A - Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof - Google Patents
Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof Download PDFInfo
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- CN104710792A CN104710792A CN201510132588.0A CN201510132588A CN104710792A CN 104710792 A CN104710792 A CN 104710792A CN 201510132588 A CN201510132588 A CN 201510132588A CN 104710792 A CN104710792 A CN 104710792A
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Abstract
The invention discloses a spherical core-shell structured Al2O3/AlN thermal-conducting powder and a high-thermal-conductivity insulating silicone grease and preparation methods thereof. The method is implemented by taking spherical Al2O3 as a raw material through reacting the spherical Al2O3 with a carbon source for 8-12h in a N2 atmosphere and at a temperature of 1400-1650 DEG C so as to obtain the spherical core-shell structured Al2O3/AlN thermal-conducting powder, and after the powder is treated by using a coupling agent, mixing the obtained object with silicone oil. According to the invention, a thermal-conducting silicone grease is prepared by using the high filling and excellent thermal-conducting and insulating properties of the spherical core-shell structured Al2O3/AlN thermal-conducting powder, the coefficient of thermal conductivity is not less than 5.0 W/m.k, the volume resistivity is greater than 1.0*10<15>Omega. cm<-1>, and the viscosity is not greater than 100000 mPa. S (25 DEG C), so that the silicone grease can be kept in a paste state after being placed for a long time, and is oiltight, therefore, the silicone grease can meet the operating requirements of high-power electronic devices which need high heat dissipation and insulation properties; and the silicone grease is simple and efficient in operation and low in production cost.
Description
Technical field
the present invention relates to a kind of ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder and high heat conducting insulating silicon grease and preparation method thereof, be mainly used in the heat radiation of high-power electronic device.
Background technology
Along with microprocessor function and usefulness strengthen and the miniaturization of electronic product day by day, high efficiency, also more and more high to the requirement of dissipation from electronic devices on market, problems of excessive heat has become the bottleneck of restriction electronic technology development, and heat-conducting silicone grease is in Electron Heat management system, be used for shortening heat transfer path, reduce a kind of heat interfacial material of thermal resistance.Because it has low temperature not retrogradation, also can not be thinning under high temperature, and non-volatile, do not solidify, low oil is from degree, the feature such as fat state when can keep for a long time using at the temperature of-50 DEG C ~+230 DEG C, in other heat interfacial materials, over-all properties is best, and obtains increasing concern and attention, be applied to electronic product heat radiation in, extend its reliability and work-ing life.
In the market, existing multiple heat-conducting silicone grease, TC-5022 type heat-conducting silicone grease (3.89 W/m.k, 4.85 × 10 of Dow corning company (Dow Corning)
10..cm
-1), the G751 type heat-conducting silicone grease (4.5 W/m.k) of Japan XINYUE (ShinEtsu), good heat dispersion performance, but it adopts up-to-date nanotechnology mostly than the heat conduction product of higher-end, complex process, because nanometer size effect is easy to reunite, easy impact coating effect and heat dispersion, and it is expensive, insulating coefficient is not high.
In addition, the higher heat-conducting cream of current thermal conductivity, except filling nano material, also fills silver powder, Graphite Powder 99, carbon nanotube etc. mostly, expensive, and not easily reaches high and fill.
Summary of the invention
for the problems of the prior art, the present invention proposes a kind of ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder, utilize its height to fill and excellent heat conduction and insulating property, the heat conductivity of heat-conduction silicone grease that filling obtains is good, and insulating coefficient is high, and simple to operate, with low cost.
A kind of ball-type nucleocapsid structure Al of the present invention
2o
3/ AlN conduction powder, it is with Al
2o
3for core, AlN is shell, wherein shell AlN mass content 10 ~ 50%.
Ball-type nucleocapsid structure Al of the present invention
2o
3the preparation method of/AlN conduction powder, it is by ball-type Al
2o
3put into the baking oven 2 ~ 4h of 100 ~ 120 DEG C, take out, by carbon source and ball-type Al
2o
3the mol ratio of 1 ~ 3:1 takes powder, at N
2atmosphere, reacts 8 ~ 12h at 1400 ~ 1650 DEG C, obtains ball-type nucleocapsid structure Al
2o
3/ AlN.
Ball-type nucleocapsid structure Al described above
2o
3in the preparation method of/AlN conduction powder, described spherical Al
2o
3particle diameter is 0.5 ~ 50 μm, and described carbon source is carbon black or Graphite Powder 99.
A kind of high heat conducting insulating silicon grease provided by the invention, it is with ball-type nucleocapsid structure Al described above
2o
3/ AlN conduction powder and silicone oil are mixed to get, described ball-type nucleocapsid structure Al
2o
3the mass ratio of/AlN conduction powder and silicone oil is 85% ~ 95%:5% ~ 15%.
Present invention also offers a kind of preparation method of high heat conducting insulating silicon grease described above, it is by ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder is placed in high-speed mixer high speed and stirs, when material temperature is raised to 100 ~ 120 DEG C, start to spray into coupling agent hydrolyzed solution, continue stirring 15 ~ 30min, stop stirring, put it into 120 DEG C of baking oven 2 ~ 4h, then the conduction powder after taking 85% ~ 95% oven dry by quality mixes with 5% ~ 15% silicone oil and obtains heat-conducting silicone grease.
In the preparation method of high heat conducting insulating silicon grease described above, described coupling agent hydrolyzed solution is by coupling agent: ethanol: the mass ratio of deionized water=20%:72%:8% takes, be uniformly mixed, be hydrolyzed 15 ~ 30min under room temperature and obtain, described coupling agent consumption is ball-type nucleocapsid structure Al
2o
31% ~ 2% of/AlN conduction powder quality.
In the preparation method of high heat conducting insulating silicon grease described above, described coupling agent is one or more mixing in silane coupling agent JHN313, silane coupling agent JHN318, Silane coupling agent KH550, silane coupling agent KH560, silane coupling agent KH570.
In the preparation method of high heat conducting insulating silicon grease described above, described silicone oil is one or more mixtures in dimethyl silicone oil, phenyl methyl silicone oil, methyl dodecyl siloxane, methyidecyl silicone, and viscosity is 10 ~ 500 mPa.S.
The present invention is with ball-type Al
2o
3for raw material, with carbon source at N
2atmosphere, reacts the ball-type nucleocapsid structure Al that 8 ~ 12h obtains at 1400 ~ 1650 DEG C
2o
3/ AlN conduction powder, after coupling agent treatment, mixes with silicone oil.The present invention utilizes ball-type nucleocapsid structure Al
2o
3the height of/AlN conduction powder is filled and excellent heat conducting and insulating property obtain heat-conducting silicone grease, and thermal conductivity is not less than 5.0W/m.k (ASTMD5470, Hot Disk method), and volume specific resistance is greater than 1.0 × 10
15..cm
-1, viscosity is not higher than 100000mPa.S(25 DEG C), long-time placement can keep lotion state, oil-tight; The present invention adopts ball-type nucleocapsid Al
2o
3/ AlN conduction powder, as the obtained heat-conducting silicone grease of filler, can possess higher insulating coefficient again while reaching high heat conduction, and can meet need the service requirements of high-power electronic device of higher heat radiation and insulating property, and efficiently simple to operate, low production cost.
Embodiment
Following embodiment further illustrates using as the explaination to the technology of the present invention content for content of the present invention; but flesh and blood of the present invention is not limited in described in following embodiment; those of ordinary skill in the art can and should know any simple change based on connotation of the present invention or replace all should belong to protection domain of the presently claimed invention, described in embodiment, number is mass parts.
Embodiment 1
By 204 parts of ball-type Al
2o
3powder, carbon black 72 parts put into the baking oven 2h of preheating 120 DEG C, take out, at N
2atmosphere, reacts 8h at 1600 DEG C.
Take 100 parts of ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder stirs in high-speed mixer high speed, claim silane coupling agent KH570 1 part, dehydrated alcohol 3.6 parts, deionized water 0.4 part is uniformly mixed, and is hydrolyzed 30min under room temperature, when material temperature is raised to 100 DEG C, start to spray into coupling agent hydrolyzed solution, continue to stir 30min and stop stirring, slightly cold discharging, put into 120 DEG C of preheated in advance oven drying 2h, the conduction powder 85 parts after claiming the powder mix handled well namely to dry mixes to obtain this heat-conducting silicone grease with 15 parts of silicone oil.
Gained heat-conducting silicone grease viscosity 65000mPa.S, thermal conductivity 5.0W/m.k, volume specific resistance is 1.16 × 10
15..cm
-1.
Embodiment 2
By 204 parts of ball-type Al
2o
3powder, carbon black 72 parts put into the baking oven 2h of preheating 120 DEG C, take out, at N
2atmosphere, reacts 10h at 1600 DEG C.
Take 100 parts of ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder stirs in high-speed mixer high speed, claim Silane coupling agent KH550 1 part, dehydrated alcohol 3.6 parts, deionized water 0.4 part is uniformly mixed, and is hydrolyzed 30min under room temperature, when material temperature is raised to 100 DEG C, start to spray into coupling agent hydrolyzed solution, continue to stir 30min and stop stirring, slightly cold discharging, put into 120 DEG C of preheated in advance oven drying 2h, claim the powder mix 90 parts handled well to mix to obtain this heat-conducting silicone grease with 10 parts of silicone oil.
Gained heat-conducting silicone grease viscosity 87000mPa.S, thermal conductivity 5.26W/m.k, volume specific resistance is 5.82 × 10
15..cm
-1.
Embodiment 3
By 204 parts of ball-type Al
2o
3powder, Graphite Powder 99 72 parts put into the baking oven 2h of preheating 120 DEG C, take out, at N
2atmosphere, reacts 12h at 1600 DEG C.
Take 100 parts of ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder stirs in high-speed mixer high speed, claim silane coupling agent JHN318 1 part, dehydrated alcohol 3.6 parts, deionized water 0.4 part is uniformly mixed, and is hydrolyzed 30min under room temperature, when material temperature is raised to 100 DEG C, start to spray into coupling agent hydrolyzed solution, continue to stir 30min and stop stirring, slightly cold discharging, put into 120 DEG C of preheated in advance oven drying 2h, claim the powder mix 94 parts handled well to mix to obtain this heat-conducting silicone grease with 6 parts of silicone oil.
Gained heat-conducting silicone grease viscosity 100000mPa.S, thermal conductivity 5.5W/m.k, volume specific resistance is 8.64 × 10
15..cm
-1.
Claims (8)
1. a ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder, it is with Al
2o
3for core, AlN is shell, wherein shell AlN mass content 10 ~ 50%.
2. ball-type nucleocapsid structure Al described in claim 1
2o
3the preparation method of/AlN conduction powder, it is by ball-type Al
2o
3put into the baking oven 2 ~ 4h of 100 ~ 120 DEG C, take out, by carbon source and ball-type Al
2o
3the mol ratio of 1 ~ 3:1 takes powder, at N
2atmosphere, reacts 8 ~ 12h at 1400 ~ 1650 DEG C, obtains ball-type nucleocapsid structure Al
2o
3/ AlN.
3. ball-type nucleocapsid structure Al as claimed in claim 2
2o
3the preparation method of/AlN conduction powder, is characterized in that, described spherical Al
2o
3particle diameter is 0.5 ~ 50 μm, and described carbon source is carbon black or Graphite Powder 99.
4. a high heat conducting insulating silicon grease, is characterized in that, obtain with method described according to claim 1 or claim 2 or claim 3 described in the obtained ball-type nucleocapsid structure Al of method
2o
3/ AlN conduction powder and silicone oil are mixed to get.
5. the preparation method of high heat conducting insulating silicon grease described in claim 4, is characterized in that, by ball-type nucleocapsid structure Al
2o
3/ AlN conduction powder is placed in high-speed mixer high speed and stirs, when material temperature is raised to 100 ~ 120 DEG C, start to spray into coupling agent hydrolyzed solution, continue stirring 15 ~ 30min, stop stirring, put it into 120 DEG C of baking oven 2 ~ 4h, then the conduction powder after taking 85% ~ 95% oven dry by quality mixes with 5% ~ 15% silicone oil and obtains heat-conducting silicone grease.
6. the preparation method of a kind of high heat conducting insulating silicon grease as claimed in claim 5, it is characterized in that, described coupling agent hydrolyzed solution is by coupling agent: ethanol: the mass ratio of deionized water=20%:72%:8% takes, be uniformly mixed, be hydrolyzed 15 ~ 30min under room temperature to obtain, described coupling agent consumption is ball-type nucleocapsid structure Al
2o
31% ~ 2% of/AlN conduction powder quality.
7. the preparation method of a kind of high heat conducting insulating silicon grease as claimed in claim 6, it is characterized in that, described coupling agent is one or more mixing in silane coupling agent JHN313, silane coupling agent JHN318, Silane coupling agent KH550, silane coupling agent KH560, silane coupling agent KH570.
8. the preparation method of a kind of high heat conducting insulating silicon grease as claimed in claim 5, it is characterized in that, described silicone oil is one or more mixtures in dimethyl silicone oil, phenyl methyl silicone oil, methyl dodecyl siloxane, methyidecyl silicone, and viscosity is 10 ~ 500 mPa.S.
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| CN201510132588.0A CN104710792A (en) | 2015-03-25 | 2015-03-25 | Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof |
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|---|---|---|---|
| CN201510132588.0A CN104710792A (en) | 2015-03-25 | 2015-03-25 | Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof |
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| CN105347779A (en) * | 2015-10-26 | 2016-02-24 | 西宁科进工业设计有限公司 | Method for producing alumina and aluminium nitride composite powder |
| CN105733423A (en) * | 2016-03-14 | 2016-07-06 | 江苏中涂涂料检测中心有限公司 | Silane coupling agent hydrolysate and application thereof in polyaniline attapulgite nano composite coating |
| CN106002653A (en) * | 2016-05-25 | 2016-10-12 | 安徽砥钻砂轮有限公司 | Anti-wear and high-hardness modified resin grinding wheel and preparation method thereof |
| CN107629463A (en) * | 2017-11-15 | 2018-01-26 | 郴州国盛新材科技有限公司 | A kind of ball-aluminium oxide/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
| CN108949114A (en) * | 2018-07-23 | 2018-12-07 | 湖南宁乡吉唯信金属粉体有限公司 | A kind of powder stuffing preparation method for heat conductive insulating interface |
| CN109868118A (en) * | 2019-03-01 | 2019-06-11 | 安徽壹石通材料科技股份有限公司 | A kind of preparation method of the aluminum nitride-alumina core-shell structure with high heat conductance |
| CN111849426A (en) * | 2019-04-24 | 2020-10-30 | 中国科学院深圳先进技术研究院 | Insulating heat-conducting grease and preparation method thereof |
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| CN106002653A (en) * | 2016-05-25 | 2016-10-12 | 安徽砥钻砂轮有限公司 | Anti-wear and high-hardness modified resin grinding wheel and preparation method thereof |
| CN107629463A (en) * | 2017-11-15 | 2018-01-26 | 郴州国盛新材科技有限公司 | A kind of ball-aluminium oxide/micro- swollen graphite composite heat-conducting silicone grease and preparation method thereof |
| CN108949114A (en) * | 2018-07-23 | 2018-12-07 | 湖南宁乡吉唯信金属粉体有限公司 | A kind of powder stuffing preparation method for heat conductive insulating interface |
| CN109868118A (en) * | 2019-03-01 | 2019-06-11 | 安徽壹石通材料科技股份有限公司 | A kind of preparation method of the aluminum nitride-alumina core-shell structure with high heat conductance |
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| CN111849426B (en) * | 2019-04-24 | 2023-12-01 | 中国科学院深圳先进技术研究院 | Insulating heat-conducting grease and preparation method thereof |
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Application publication date: 20150617 |
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