CN105754342A - Low-viscosity heat conducting silicone grease and preparation method thereof - Google Patents
Low-viscosity heat conducting silicone grease and preparation method thereof Download PDFInfo
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- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
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Abstract
The invention discloses low-viscosity heat conducting silicone grease. Composition of the low-viscosity heat conducting silicone grease comprises components of dimethyl silicone oil, heat conducting powder of class I, heat conducting powder of class II, a coupling agent and an auxiliary. A preparation method of the low-viscosity heat conducting silicone grease comprises steps as follows: step 1, the dimethyl silicone oil, the coupling agent and the auxiliary are added to a double-planet stirring machine to be mixed uniformly; step 2, the heat conducting powder of class II is added to a mixed liquid obtained in the step 1 and mixed uniformly; step 3, the heat conducting powder of the class I is added to a mixed liquid obtained in the step 2 and mixed uniformly; step 4, a mixed liquid obtained in the step 3 is sufficiently stirred and subjected to vacuum pumping and defoaming. The heat conducting silicone grease produced with the method has the characteristics of low viscosity, high heat conduction coefficient, low probability of sedimentation, low permeability, good long-term stability and the like.
Description
Technical field
The present invention relates to electronic devices and components thermal interfacial material, particularly to low viscous heat-conducting silicone grease and preparation method thereof.
Background technology
Heat-conducting silicone grease is also referred to as thermal grease, and it is the paste heat sink material containing silicone oil.Because by the limitation of manufacturing process and clamping method, being constantly present small spaces between components and parts and fin, being flooded with air, and air is the non-conductor of heat in space, the heat conductivity of air is very low, has a strong impact on the integral heat sink effect of electronic devices and components.Heat-conducting silicone grease is filled in the crack between components and parts and fin, can ensure that and be in close contact between components and parts and fin, increase contact area, improve heat transfer efficiency, the heat produced when being worked by components and parts propagates fin quickly and evenly, takes away finally by fan, thus optimizing heat dissipation, visible, the heat radiation work of components and parts is played an important role by the performance of heat-conducting silicone grease.
In recent years, along with the fast development of China's intellectuality, automatic industrial, the central processor CPU on such as computer is along with the lifting of arithmetic speed, and caloric value is consequently increased, and heat dissipation problem then increasingly highlights；LED chip technology only has the electric energy of 30% to be converted to light, and the electric energy of other 70% is converted to heat, if these heats can not be dissipated effectively, then causes burning of chip, reduces service life.It is to say, heat-conducting silicone grease is difficult to the requirement meeting electronics industry to heat radiation gradually, therefore, the heat conductivility improving heat-conducting silicone grease becomes more and more important.
At present, the Chinese patent that application publication number is CN104231634A discloses a kind of high efficiency insulation heat-conducting silicone grease and preparation method thereof, including dimethicone, end hydroxyl silicone oil, aluminium oxide and coupling agent.The heat-conducting silicone grease that this method obtains is the heat-conducting silicone grease goods with higher heat conductivity, insulation and low thermal contact resistance, add coupling agent and can reduce the viscosity of system, but the viscosity of the heat-conducting silicone grease obtained after mix homogeneously is close to 350,000 centipoises, viscosity is still very big, heat-conducting silicone grease surface wettability is poor, causing that interface resistance increases, overall heat-conducting effect is deteriorated, and is unfavorable for the heat radiation between electronic device.
Summary of the invention
For the deficiency that prior art exists, low viscous heat-conducting silicone grease that it is an object of the invention to provide heat conductivity and the long service life with excellence and preparation method thereof.
For achieving the above object, the technical scheme is that
A kind of low viscous heat-conducting silicone grease, it is characterised in that include the component of following weight portion:
Dimethicone: 5 ~ 20 mass parts；I class conduction powder: 50 ~ 80 mass parts；II class conduction powder: 5 ~ 15 mass parts；Coupling agent: 0.5 ~ 2 mass parts；Auxiliary agent: 0.1 ~ 1 mass parts.
By adopting technique scheme, dimethicone is the base oil of this heat-conducting silicone grease, II class conduction powder and I class conduction powder is added in base oil, the heat conductivity of this heat-conducting silicone grease and resistance to usability can be obviously enhanced, but can there is the situation that viscosity increases, adding auxiliary agent makes the viscosity of this heat-conducting silicone grease drop to below 100,000 centipoises from 300,000 centipoises, and viscosity substantially reduces, and improves the ease of use of this heat-conducting silicone grease.Simultaneously, moreover it is possible to improve the stability of this silicone grease, sedimentation and permeability it are not susceptible to during storage.
The present invention is further arranged to: described II class conduction powder is one or more in nanometer carbon black, CNT or nano-graphite.
By adopting technique scheme, in the silicone oil of basis, add II class conduction powder, be remarkably improved the heat conductivity of this heat-conducting silicone grease so that it is heat dispersion is higher.II class conduction powder is specially one or more in nanometer carbon black, CNT or nano-graphite, these are all the thermosensitive fillers with excellent heat conducting performance, a small amount of interpolation is then greatly improved the heat conductivility of this heat-conducting silicone grease, nanometer carbon black low price, heat conductivity is not so good as CNT, CNT heat conductivity is best but expensive, and integrated cost considers, can mix the above-mentioned II class conduction powder of interpolation.
The present invention is further arranged to: the particle diameter of described II class conduction powder is 50 ~ 200nm.
By adopting technique scheme, select particle size range II class conduction powder between 50 ~ 200nm, nano level II class conduction powder has the heat conductivility of excellence, a small amount of interpolation can improve the heat conductivity of heat-conducting silicone grease, also can be filled between the gap of the dimethicone that micron-sized I class conduction powder is not filled by, make the viscosity of this heat-conducting silicone grease and hardness all strengthen.
The present invention is further arranged to: described I class conduction powder is at least one in aluminium oxide, zinc oxide, aluminium nitride or boron nitride.
By adopting technique scheme, I class conduction powder is added in above-mentioned mixture, I class conduction powder is specially one or more in aluminium oxide, zinc oxide, aluminium nitride, boron nitride, it is known that, aluminium oxide, zinc oxide are the good fillers of heat conductivity in metal-oxide, above-mentioned filler adds in dimethicone, adds the heat conductivility of this system.
The present invention is further arranged to: the particle diameter of described I class conduction powder is 0.1 ~ 30 μm.
By adopting technique scheme, for increasing the heat conductivility of dimethicone, need to add substantial amounts of I class conduction powder, consideration for addition Yu cost, select micron-sized I class conduction powder, its particle diameter is all between 0.1 ~ 30 μm, and the I class conduction powder within the scope of this can quickly make this heat-conducting silicone grease have certain viscosity, facilitates the preparation of this heat-conducting silicone grease.
The present invention is further arranged to: described coupling agent is at least one in dodecyltrimethoxysilane, vinyltrimethoxy silane, methacryloxypropyl trimethoxy silane.
By adopting technique scheme, matrix is dimethicone, filler is I class conduction powder and II class conduction powder, in order to improve the compatible interface between matrix resin and filler, need to add coupling agent, coupling agent is chosen in dodecyltrimethoxysilane, vinyltrimethoxy silane, methacryloxypropyl trimethoxy silane at least one, powder body class filler is added to by these coupling agents can play the boundary defect eliminating between matrix resin and filler preferably in dimethicone, improve its stability in the large.
The present invention is further arranged to: described auxiliary agent is one or more in tetraethyl orthosilicate, sub-silester, tetraethoxysilane.
By adopting technique scheme, interpolation along with II class conduction powder, I class conduction powder, the viscosity of this mixed system significantly increases, the excessive heat-conducting silicone grease of viscosity is unfavorable for using practically, auxiliary agent is one or more in tetraethyl orthosilicate, sub-silester, tetraethoxysilane, a small amount of interpolation then can obviously reduce the viscosity of heat-conducting silicone grease, improves the storage stability of silicone grease simultaneously, is not susceptible to the phenomenons such as powder body sedimentation and surface permeability.
As it is preferred that: described auxiliary agent is mass ratio is the tetraethyl orthosilicate of A:B:C, sub-silester, tetraethoxysilane.
The preparation method that present invention also offers a kind of low viscous heat-conducting silicone grease:
Step 1: according to dimethicone 5 ~ 20 mass parts；Coupling agent 0.5 ~ 2 mass parts；Auxiliary agent 0.1 ~ 1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: II class conduction powder 5 ~ 15 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: I class conduction powder 50 ~ 80 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
By adopting technique scheme, according to the preparation method of above-mentioned heat-conducting silicone grease, first adding in double planetary mixer by base oil dimethicone, coupling agent and auxiliary agent, liquid to be mixed is sufficiently mixed；Then, in mixed liquor, add I class conduction powder and II class conduction powder, increase high intensity and the high-termal conductivity of heat-conducting silicone grease respectively；The mixing liquid of mix homogeneously processes being higher than under-0.6Mpa condition vacuumizing and defoaming well-beaten while, and the heat-conducting silicone grease modest viscosity so prepared extends its service life so that it is more robust and have excellent heat conductivility.
In sum, the invention have the benefit that 1, low viscosity: a small amount of increase silester analog assistant, make the viscosity of this heat-conducting silicone grease significantly reduce, improve the practicality of this heat-conducting silicone grease, meanwhile, auxiliary agent also can eliminate the boundary defect between powder body and silicone oil, improves the stability of blend；2, high-termal conductivity: except the effect that interpolation I class conduction powder can play heat conduction, being also added with II class conduction powder class filler, a small amount of interpolation then can be played the heat conductivity of excellence and be uniformly dispersed in mixed system, and stability is strong.Thus, prepare and there is heat-conducting silicone grease that is low viscous and that have excellent heat conducting performance.
Complete necessary scheme and the principle of the present invention:
In recipe ingredient, micron-sized I class conduction powder adds the viscosity of system, plays the effect improving heat-conducting silicone grease intensity；Nano level II class conduction powder can be filled up in the space that I class conduction powder is not filled by, and makes the intensity of system improve further, improves resistance to serviceability, substantially increases the heat conductivility of this heat-conducting silicone grease simultaneously；After substantial increase powder stuffing, the viscosity of mixed system is uprushed, it is unfavorable for using, add silester analog assistant, utilize auxiliary agent and water that hydrolysis condensation reaction slowly occurs, generate the cross-linking products with low polymerization degree, make the overall viscosity of system significantly reduce, and different auxiliary agent is the most notable with the use of decrease in viscosity；Meanwhile, adding coupling agent and can improve the interface between powder body and silicone oil, eliminate boundary defect, the heat-conducting silicone grease structural integrity making preparation is higher, easy for people to use.
Present invention have the advantage that
The invention provides a kind of low viscous heat-conducting silicone grease and preparation method thereof, the formula that usual this patent provides can be substantially reduced the viscosity of heat-conducting silicone grease, viscosity controls within 100,000 centipoises, and this heat-conducting silicone grease has heat conductivility and the storage stability of excellence, it is not susceptible to sedimentation and permeability, is resistant to the long-time use of user.
Detailed description of the invention
Below in conjunction with embodiment, specific embodiment of the invention process is described in further detail.
Testing index:
(1) heat conductivity: stable when, by the time rate of change of the hot-fluid of the unit are of certain heterogeneous material divided by the unit temperature gradient being perpendicular to area direction；(2) thermal resistance: the obstruction to hot-fluid that material list reveals；
Sample prepares: determine the size of the thickness range of sample and sample and the equivalently-sized of contact surface according to different materials；
Adopt Taiwan auspicious neck LW-9389 type thermal conductivity test machine, test according to the standard method of test of the heat-conduction electric insulation material heat conveyance performance of ASTMD5470；
(3) viscosity: adopt RVDT2T type viscosity apparatus that sample is carried out viscosity test.
The experiment concrete scheme done is as follows:
Step 1: according to dimethicone 5 mass parts；Coupling agent 0.1 mass parts；Auxiliary agent 0.1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: II class conduction powder 5 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: I class conduction powder 50 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
The experimental result obtained is as shown in the table
As seen from table, in I class conduction powder, under same experimental conditions, the thermal resistance of aluminium oxide and zinc oxide reduces, and heat conductivility improves, compared to aluminium nitride and boron nitride, good heat dispersion performance；Adding in the experiment that coupling agent is more with auxiliary agent, the viscosity obtained has reduction.
Another group experiment concrete scheme is as follows:
Step 1: according to dimethicone 10 mass parts；Coupling agent 1 mass parts；Auxiliary agent 0.1 ~ 1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: II class conduction powder 5 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: aluminium oxide 60 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
It is as shown in the table for the experimental result obtained:
As seen from table, a small amount of interpolation I class conduction powder, heat conductivity is up to, between 4 ~ 5 scopes, significantly improving the heat conductivity of this heat-conducting silicone grease.
Another group of experiment concrete scheme is as follows:
Step 1: according to dimethicone 20 mass parts；Coupling agent 1 ~ 2 mass parts；Auxiliary agent 0.5 ~ 1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: CNT 5 ~ 10 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: aluminium oxide 60 ~ 80 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
It is as shown in the table for the experimental result obtained:
As seen from table, along with increasing of aluminium oxide, CNT, coupling agent and auxiliary agent, the thermal resistance of this heat-conducting silicone grease reduces, and heat conductivity increases, and meanwhile, reduces the viscosity of heat-conducting silicone grease.
Another group experiment concrete scheme is as follows:
Step 1: according to dimethicone 20 mass parts；Coupling agent 1.5 mass parts；Auxiliary agent 0.8 ~ 1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: CNT 8 ~ 10 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: aluminium oxide 60 ~ 80 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
Experimental result is as shown in the table:
As seen from table, when auxiliary agent loading is 1 mass parts left and right, the viscosity degradation of heat-conducting silicone grease is 100,000 below mpa s, and viscosity significantly reduces, and, three kinds of auxiliary agents with mass ratio for 1:1:1 with the use of time viscosity degradation the most obvious, be low to moderate 66000 centipoises；Along with aluminium oxide, CNT, coupling agent increase, the thermal resistance of this heat-conducting silicone grease reduces, and heat conductivity increases, and heat dispersion strengthens.
This specific embodiment is only explanation of the invention; it is not limitation of the present invention; the present embodiment can be made the amendment not having creative contribution as required by those skilled in the art after reading this specification, but as long as being affected by the protection of Patent Law in scope of the presently claimed invention.
Claims (9)
1. a low viscous heat-conducting silicone grease, it is characterised in that include the component of following weight portion:
Dimethicone: 5 ~ 20 mass parts；
I class conduction powder: 50 ~ 80 mass parts；
II class conduction powder: 5 ~ 15 mass parts；
Coupling agent: 0.5 ~ 2 mass parts；
Auxiliary agent: 0.1 ~ 1 mass parts.
2. low viscous heat-conducting silicone grease according to claim 1, it is characterised in that: described II class conduction powder is at least one in nanometer carbon black, CNT or nano-graphite.
3. low viscous heat-conducting silicone grease according to claim 2, it is characterised in that: the particle diameter of described II class conduction powder is 50 ~ 200nm.
4. low viscous heat-conducting silicone grease according to claim 1, it is characterised in that: described I class conduction powder is at least one in aluminium oxide, zinc oxide, aluminium nitride or boron nitride.
5. low viscous heat-conducting silicone grease according to claim 4, it is characterised in that: the particle diameter of described I class conduction powder is 0.1 ~ 30 μm.
6. low viscous heat-conducting silicone grease according to claim 1, it is characterised in that: described coupling agent is at least one in dodecyltrimethoxysilane, vinyltrimethoxy silane, methacryloxypropyl trimethoxy silane.
7. low viscous heat-conducting silicone grease according to claim 1, it is characterised in that: described auxiliary agent is at least one in tetraethyl orthosilicate, sub-silester, tetraethoxysilane.
8. low viscous heat-conducting silicone grease according to claim 1, it is characterised in that: described auxiliary agent is mass ratio is the tetraethyl orthosilicate of A:B:C, sub-silester, tetraethoxysilane.
9. the preparation method of the low viscous heat-conducting silicone grease according to claim 1 ~ 8, it is characterised in that comprise the following steps:
Step 1: according to dimethicone 5 ~ 20 mass parts；Coupling agent 0.5 ~ 2 mass parts；Auxiliary agent 0.1 ~ 1 mass parts joins mix homogeneously in double planetary mixer；
Step 2: II class conduction powder 5 ~ 15 mass parts is joined in the mixing liquid of step 2, to be mixed uniformly；
Step 3: I class conduction powder 50 ~ 80 mass parts is joined in the mixing liquid of step 1, to be mixed uniformly；
Step 4: mixing liquid step 3 obtained is sufficiently stirred for and evacuation deaeration process under being higher than-0.6Mpa condition.
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| CN106566481A (en) * | 2016-10-25 | 2017-04-19 | 东莞市联洲知识产权运营管理有限公司 | Carbon nano-tube/heat conduction silicone grease composite material and preparation method thereof |
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| CN108384245A (en) * | 2018-04-04 | 2018-08-10 | 宁波伟铄电子科技有限公司 | A kind of polynary silicone grease heat conducting nanometer material of electronic component |
| CN109233623A (en) * | 2018-09-19 | 2019-01-18 | 南京禾鑫坊电子科技有限公司 | A kind of electronic component magnetic screen heat dissipating silicone grease coating |
| CN110591365A (en) * | 2019-09-29 | 2019-12-20 | 太仓陶氏电气有限公司 | High-thermal-conductivity nano silicone grease for heat dissipation of semiconductor chip |
| CN111534358A (en) * | 2020-05-09 | 2020-08-14 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
| CN112724677A (en) * | 2020-12-29 | 2021-04-30 | 中山大学 | Dopamine modified boron nitride heat-conducting silicone grease and preparation method thereof |
| CN113881406A (en) * | 2021-10-22 | 2022-01-04 | 梅剑雄 | High-thermal-conductivity heat-conducting silicone grease and preparation method thereof |
| CN116622286A (en) * | 2023-05-26 | 2023-08-22 | 广东电网有限责任公司 | Conductor protective grease and preparation method and application thereof |
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