CN108587576A - A kind of computer heat transmission heat-conducting silicone grease and preparation method thereof - Google Patents
A kind of computer heat transmission heat-conducting silicone grease and preparation method thereof Download PDFInfo
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- CN108587576A CN108587576A CN201810810804.6A CN201810810804A CN108587576A CN 108587576 A CN108587576 A CN 108587576A CN 201810810804 A CN201810810804 A CN 201810810804A CN 108587576 A CN108587576 A CN 108587576A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F1/00—Details not covered by groups G06F3/00 - G06F13/00 and G06F21/00
- G06F1/16—Constructional details or arrangements
- G06F1/20—Cooling means
Abstract
The invention belongs to heat-conducting silicone grease technical fields, and in particular to a kind of computer heat transmission heat-conducting silicone grease and preparation method thereof；The computer heat transmission heat-conducting silicone grease is made of organic silicone oil and nanometer Al-Si composites；The nanometer Al-Si composites be aluminum nitrate be silicon source, ethyl orthosilicate is silicon source prepares gained using sol-gal process.As heat filling, compared with single nano-aluminium oxide, the heat conductivity of heat conduction silicate prepared significantly improves the nanometer Al-Si composites prepared using the present invention, reaches as high as 5.8W/ (m K), can be used for mainframe computer cpu heat.
Description
Technical field
The invention belongs to heat-conducting silicone grease technical fields, and in particular to a kind of computer heat transmission heat-conducting silicone grease and its preparation side
Method.
Background technology
With being increasingly enhanced for microprocessor function and efficiency, the miniaturization of electronic product and high efficiency, currently to electronics
The cooling requirements of component are higher and higher, and own through becoming limitation electricity by bad the caused electronic component problems of excessive heat that radiates
The important bottleneck of sub- technology development.The heat conduction fat of consulting is to be used for shortening heat transfer path in Electron Heat management system, reduces the one of thermal resistance
Kind thermal interfacial material.Heat conduction osmanthus fat has low Warm not retrogradation, and high temperature is not thinning, non-volatile, does not cure, and low oil is held a little from degree etc..
Compared with other thermal interfacial materials, the comprehensive performance of heat conduction baby's fat is best, to get growing concern for, and extensive use
In being widely used between electronic component and heat sink or radiator, such as power amplifier, transistor, electron tube, CPU electronics
On prototype part.
With the rapid development of computer technology, the central processing unit (Central as computer system core
Processing Unit, CPU) arithmetic speed be getting faster, but calorific value also constantly increases therewith, if heat dispersal situations are not
Good, cpu temperature is excessively high, it is easy to lead to problems such as computer occur automatic thermal starting, crash in the process of running, therefore be
It is the essential condition for ensureing computer normal work that CPU, which provides good cooling system,.According to statistics, it is calculated caused by overheat
Machine CPU failures account for the 55% of CPU failure sums, moreover, operating temperature often increases 10%, reliability just reduces by 50%.In order to carry
Solid content in the thermal conductivity generally use raising heat conductive silicone grease composition of high thermal conductive silicon oil/fat composition, but existing heat-conducting silicone grease group
The solid content for closing object has reached 90%, so having improved the thermal conductivity of heat conductive silicone grease composition in terms of improving solid content merely
Through no room for promotion.
Al2O3In thermal conductive polymer composite material, such as dispersibility very well, is distributed inside heat-conducting silicon rubber, heat-conducting silicone grease
Uniformly, there is good heat-conducting effect, so more come the research for improving heat conduction baby's resin composite material thermal conductivity with Al2O3；But
Al2O3The heat conductivity of heat conduction silicate prepared when as heat filling is not high；HeFei University of Technology Feng Yan et al. (Chinese adhesive,
2016,8:451-454, the preparation of low-viscosity high heat conducting insulating silicon grease and performance study) even if middle report to Al2O3Using silane
Coupling agent is surface-treated, loading be 88.8% when, thermal conductivity is also only 1.34W/ (m.K), subsequently using ZnO with
Al2O3It is compounded under special ratios and thermal conductivity has only also been increased to 3.98W/ (m.K), loading has had reached 92% at this time.
Invention content
The purpose of the present invention is overcoming deficiency in the prior art, a kind of computer heat transmission heat-conducting silicone grease, this hair are provided
It is bright to form heat conductive silicone grease composition, the nano aluminum silicon composite wood as filler and organic silicone oil using nanometer Al-Si composites
Material be aluminum nitrate be silicon source, ethyl orthosilicate is silicon source prepares gained using sol-gel method.Heat-conducting silicone grease prepared by the present invention
Thermal conductivity is high, can be used for the heat dissipation of the positions such as mainframe computer CPU.
The present invention is achieved through the following technical solutions above-mentioned purpose, and a kind of computer heat transmission heat-conducting silicone grease is described
Computer heat transmission heat-conducting silicone grease is made of organic silicone oil and nanometer Al-Si composites；The nanometer Al-Si composites are nitre
Sour aluminium is silicon source, ethyl orthosilicate is that silicon source prepares gained using sol-gel method；
Preferably, the specific preparation method of nanometer Al-Si composites is：
Aluminum nitrate is dissolved in deionized water, ethyl orthosilicate is then added, ammonium hydroxide, which is added dropwise, after being mixed at 30-50 DEG C is adjusted
System pH to 7-8；Insulated and stirred 1-4h carries out aging, is then cooled to filtering, washing after room temperature, is dried extremely at 100-120 DEG C
Constant weight is finally warming up to 300-400 DEG C of roasting 4-6h and obtains a nanometer Al-Si composites；It is calculated according to molar ratio, ethyl orthosilicate：
Aluminum nitrate=1:5-8；Preferably, insulated and stirred 2h carries out aging in preparation process, is calculated according to molar ratio, ethyl orthosilicate：
Aluminum nitrate=1:7；
During the present invention prepares nanometer Al-Si composites by sol-gel method, ethyl orthosilicate constantly hydrolyzes
At SiO2, and combined with Al species, it is aluminium oxide, dopant material SiO to form material of main part by later stage aging, roasting2Receive
Rice Al-Si composites, aluminium oxide and SiO in the composite material2Form the structure mutually included；By controlling ethyl orthosilicate
A nanometer Al-Si composites structure is adjusted with the proportioning of aluminum nitrate and its ageing time, to influence its property.
Preferably, the organic silicone oil be dimethicone, epoxy modified polysiloxane, vinyl silicone oil, polymethylphenyl siloxane fluid or
Hydroxy silicon oil, further preferably epoxy modified polysiloxane；The present invention has surprisingly found that epoxy-modified silicon when screening organic silicone oil
The heat conductivity of heat conduction silicate that oil is prepared is high, it may be possible to since the introducing of epoxy group can improve the compatibility with filler, to
So that the thermal conducting path of heat-conducting silicone grease improves.
Preferably, the weight of the nanometer Al-Si composites is the 40-75% of heat-conducting silicone grease weight, further preferably
68%；
According to another aspect of the present invention, the present invention provides a kind of preparation sides of computer heat transmission heat-conducting silicone grease
Method, addition nanometer Al-Si composites after mixing with colloid mill are dried in 150 DEG C of baking oven in organic silicone oil
30min makes its thickening, and then ultrasound obtains the heat-conducting silicone grease of the Al-Si composites containing nanometer in 1-2 days at 60-70 DEG C.
The present invention uses sol-gel method to prepare with Al for the first time2O3Based on material, SiO2For the mutual of dopant material
The nanometer Al-Si composites of inclusion are used as the Heat Conduction Material of heat-conducting silicone grease, and compared with prior art, the present invention has following excellent
Point：
1) first passage sol-gel method of the present invention prepares nanometer Al-Si composites and substitutes tradition Al2O3It is filled out as heat conduction
Material, improves the thermal conductivity of heat-conducting silicone grease；
2) compared with traditional silane coupling agent surface coating modification, the present invention use sol-gel method to prepare with
Al2O3Based on material, SiO2For the nanometer Al-Si composites of dopant material mutually included；
3) heat-conducting silicone grease that the present invention is prepared using self-control nanometer Al-Si composites with epoxy modified polysiloxane, thermal conductivity
Rate is up to 5.8W/ (mK).
Specific implementation mode
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Raw material sources：Dimethicone is from the silicone oil that the DOW CORNING trade name PMX-200 trades mark are 50CS；It is epoxy-modified
Silicone oil comes from Shandong Dayi Chemical Industry Co., Ltd, model DY-E701 epoxy modified polysiloxanes, epoxide number 0.08mol/
100g, viscosity are 1100cp (25 DEG C)；Vinyl silicone oil comes from pure prosperous chemical industry organosilicon material company of Shenzhen, and viscosity is
2060mPa.S, contents of ethylene 1.1%wt；Polymethylphenyl siloxane fluid comes from pure prosperous chemical industry organosilicon material company of Shenzhen
BSO-30150 polymethylphenyl siloxane fluids；Hydroxy silicon oil comes from pure prosperous chemical industry organosilicon material company of Shenzhen, and hydroxy radical content is
7.2%wt；Remaining reagent is commercially available conventional reagent in embodiment.
Thermal conductivity is tested：The present invention is tested not using heat flow method using the heat conduction coefficient tester of model DRL-III-P
The thermal conductivity of heat-conducting silicone grease, testing standard MIL-I-49456A are prepared with embodiment.
Viscosity test：According to GB/T2794-1995《The measurement of adhesive viscosity》Requirement, with NDJ-7 rotational viscometers
It measures；At 25 ± 0.1 DEG C, the heat-conducting silicone grease just prepared is poured into rotational viscometer, with the rotating speed continuous rotation of 7.5rpm
2min, the number of degrees after stablizing, average measurement three times, take averaging of income value three times；
Embodiment 1
Be added in dimethicone nanometer Al-Si composites (loading of nanometer Al-Si composites is 60%wt,
Dimethicone loading is 40%wt), after mixing with stainless steel colloid mill, drying 30min makes in 150 DEG C of baking oven
It is thickened, and then ultrasound obtains the heat-conducting silicone grease of the Al-Si composites containing nanometer in 1-2 days at 60-70 DEG C.
Prepare nanometer Al-Si composites：Aluminum nitrate is dissolved in deionized water, 20mmol ethyl orthosilicates are then added,
Ammonia water conditioning system pH to 7-8 is added dropwise after being mixed at 30-50 DEG C；Then insulated and stirred aging is cooled to filtering, water after room temperature
It washes, is dried to constant weight at 100-120 DEG C, be finally warming up to 300-400 DEG C of roasting 4-6h and obtain a nanometer Al-Si composites.
The present invention has investigated the ethyl orthosilicate and aluminum nitrate and its different insulated and stirred ageing time of different mol ratios
Influence of the nanometer Al-Si composites prepared to heat conductivity of heat-conduction silicone grease, is shown in Table 1：
The thermal conductivity of 1 heat-conducting silicone grease of table
Note：Si/Al molar ratios refer in nanometer Al-Si composites preparation process ethyl orthosilicate and aluminum nitrate mole with
The ratio between amount.
The above result shows that (the sequence 7, Si/Al=1 when adding a small amount of ethyl orthosilicate:10) thermal conductive silicon, prepared
The thermal conductivity of fat continues the mole dosage for increasing ethyl orthosilicate almost without raising, and the thermal conductivity of heat-conducting silicone grease significantly improves,
Work as Si/Al=1:When 7, thermal conductivity reaches 2.96W/ (mK), but continues to increase the mole dosage of ethyl orthosilicate, and thermal conductivity is anti-
And decline, work as Si/Al=1:When 1, thermal conductivity falls to 0.96, instead than being not added with ethyl orthosilicate when it is also low, so Si/
Al molar ratios are controlled in ethyl orthosilicate：Aluminum nitrate=1:It is advisable between 5-8；When preparing nanometer Al-Si composites, when aging
Between also have an impact to the heat conductivity of heat conduction silicate prepared, ageing time is advisable with 3h.
Embodiment 2
In the optimal preparation process of selected nanometer Al-Si composites, i.e.,：By 140mmol aluminum nitrates be dissolved in 500ml go from
In sub- water, 20mmol ethyl orthosilicates are then added, ammonia water conditioning system pH to 7-8 is added dropwise after being mixed at 30-50 DEG C；Heat preservation is stirred
Aging 3h is mixed, filtering, washing after room temperature is then cooled to, is dried to constant weight at 100-120 DEG C, be finally warming up to 300-400 DEG C
Roasting 4-6h obtains a nanometer Al-Si composites.
The present invention has screened influence of the different organic silicone oils to heat conductivity of heat conduction silicate, and method is as follows：
Be added in organic silicone oil nanometer Al-Si composites (loading of nanometer Al-Si composites is 60%wt, two
Methyl-silicone oil loading is 40%wt), after mixing with stainless steel colloid mill, drying 30min makes it in 150 DEG C of baking oven
Thickening, then ultrasound obtains the heat-conducting silicone grease containing nanometer copper particle in 1-2 days at 60-70 DEG C, and different organic silicone oils are prepared
The thermal conductivity of heat-conducting silicone grease be shown in Table 2：
Influence of the 2 organic silicone oil type of table to heat conductivity of heat conduction silicate
Test result shows that the heat conductivity of heat conduction silicate that different organic silicone oils are prepared is different, wherein with epoxy-modified silicon
The heat conductivity of heat conduction silicate effect that oil is prepared is best.
Embodiment 3
Make as the optimal preparation process of nanometer Al-Si composites, epoxy modified polysiloxane in the parameter of selected 1 sequence 5 of table
For organic silicone oil when, the present invention is studied the loading of nanometer Al-Si composites, and method is as follows：
The weight proportion for adjusting epoxy modified polysiloxane and nanometer Al-Si composites, is added nanometer in epoxy modified polysiloxane
After mixing with stainless steel colloid mill, drying 30min makes its thickening to Al-Si composites in 150 DEG C of baking oven, then exists
Ultrasound obtains the heat-conducting silicone grease containing nanometer copper particle for 1-2 days at 60-70 DEG C, prepared by different nanometer Al-Si composites loadings
The thermal conductivity of the heat-conducting silicone grease gone out is shown in Table 3：
Influence of the 3 nanometers of Al-Si composites loadings of table to the thermal conductivity of heat-conducting silicone grease
| Loading/wt% | Thermal conductivity/W/ (mK) | Viscosity/mPa.S |
| 40 | 2.79 | 6080 |
| 50 | 3.68 | 13600 |
| 60 | 4.28 | 28120 |
| 70 | 5.69 | 43640 |
| 80 | 5.60 | 62400 |
| 90 | 5.61 | 71600 |
| 63 | 5.72 | 29840 |
| 68 | 5.80 | 33680 |
Note：Loading refers to the weight percent that nanometer Al-Si composites account for heat-conducting silicone grease.
In general, with the increase of heat filling loading, thermal conductivity increases, generally for raising heat-conducting silicone grease
Thermal conductivity increases the loading of heat filling as far as possible；But after nanometer Al-Si composites loading is more than 70%wt in the present invention
It presents and slightly declines instead, viscosity is stepped up with the increase of nanometer Al-Si composites loading, so considering viscous
Degree and thermal conductivity, Selective filling amount of the present invention are 68% the most excellent.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, can embodiments of the present invention be made with various changes, replacement and change.
Claims (8)
1. a kind of computer heat transmission heat-conducting silicone grease, it is characterised in that：The computer heat transmission heat-conducting silicone grease is by organic silicone oil
It is formed with nanometer Al-Si composites；The nanometer Al-Si composites be aluminum nitrate be silicon source, ethyl orthosilicate is that silicon source is adopted
Gained is prepared with sol-gel method.
2. computer heat transmission heat-conducting silicone grease according to claim 1, it is characterised in that：The nanometer Al-Si composites
Specific preparation method be：Aluminum nitrate is dissolved in deionized water, ethyl orthosilicate is then added, is dripped after being mixed at 30-50 DEG C
Add ammonia water conditioning system pH to 7-8；Insulated and stirred 1-4h carries out aging, is then cooled to filtering, washing after room temperature, 100-120
It is dried to constant weight at DEG C, is finally warming up to 300-400 DEG C of roasting 4-6h and obtains a nanometer Al-Si composites；It is calculated according to molar ratio,
Ethyl orthosilicate：Aluminum nitrate=1:5-8.
3. computer heat transmission heat-conducting silicone grease according to claim 2, it is characterised in that：Insulated and stirred 2h carries out aging,
It is calculated according to molar ratio, ethyl orthosilicate：Aluminum nitrate=1:7.
4. according to claim 1-3 any one of them computer heat transmission heat-conducting silicone greases, it is characterised in that：The organic silicone oil
For dimethicone, epoxy modified polysiloxane, vinyl silicone oil, polymethylphenyl siloxane fluid or hydroxy silicon oil.
5. computer heat transmission heat-conducting silicone grease according to claim 4, it is characterised in that：The organic silicone oil changes for epoxy
Property silicone oil.
6. computer heat transmission heat-conducting silicone grease according to claim 5, it is characterised in that：The nanometer Al-Si composites
Weight be heat-conducting silicone grease weight 40-75%.
7. computer heat transmission heat-conducting silicone grease according to claim 6, it is characterised in that：The nanometer Al-Si composites
Weight be heat-conducting silicone grease weight 68%.
8. a kind of preparation method of computer heat transmission heat-conducting silicone grease described in claim 1, it is characterised in that：In organic silicone oil
Middle addition nanometer Al-Si composites, after mixing with colloid mill, drying 30min makes its thickening in 150 DEG C of baking oven, so
Ultrasound obtains the heat-conducting silicone grease of the Al-Si composites containing nanometer in 1-2 days at 60-70 DEG C afterwards.
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Address after: 255314 Unicom Road, Zibo New District, Shandong, Zibo Patentee after: ZIBO VOCATIONAL INSTITUTE Address before: 255000 No. 30 Century Road, Zhangdian District, Shandong, Zibo Patentee before: ZIBO VOCATIONAL INSTITUTE |