CN107739513A - A kind of heat-conducting silicone grease and its processing method and application - Google Patents
A kind of heat-conducting silicone grease and its processing method and application Download PDFInfo
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- CN107739513A CN107739513A CN201711149304.4A CN201711149304A CN107739513A CN 107739513 A CN107739513 A CN 107739513A CN 201711149304 A CN201711149304 A CN 201711149304A CN 107739513 A CN107739513 A CN 107739513A
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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
- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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- 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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- 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
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Abstract
The present invention relates to a kind of heat-conducting silicone grease and its processing method and application, including the material such as dimethicone, heat filling, coupling agent, auxiliary agent, methyl-silicone oil, gas phase silica gel；In the prior art, when using viscosity larger heat-conducting silicone grease, generally use surface cladding process, heat-conducting silicone grease is coated into thicker one layer on electronic component surface, fin is adhered to it again, this mode of operation causes heat-conducting silicone grease consumption more, and hole generation is tended to have between fin and heat-conducting silicone grease；And in the heat-conducting silicone grease in using this programme, heat-conducting silicone grease point can be dropped on electronic component, fin is firmly attached on heat-conducting silicone grease again, because heat-conducting silicone grease viscosity is relatively low, mobility is preferable, therefore fin firmly attach when, heat-conducting silicone grease caters to the shape of fin and electronic component opposing sides completely, so avoid between fin and electronic component because have retaining for hole and caused by radiating effect reduce.
Description
Technical field
The present invention relates to a kind of processing method of heat-conducting silicone grease, more particularly to a kind of heat-conducting silicone grease and its processing method are with answering
With.
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 manufacture craft and clamping side
The limitation of method, milling hole is constantly present between component and fin, is flooded with air in space, and air be heat not
Good conductor, the thermal conductivity factor of air is very low, has a strong impact on the integral heat sink effect of electronic component.Heat-conducting silicone grease is filled in member
In crack between device and fin, it is ensured that be in close contact between component and fin, increase contact area, improved
Heat transfer efficiency, heat caused by component operating room is rapidly and uniformly traveled into fin, taken away finally by fan, so as to
Optimize heat dissipation.
In recent years, with China's intellectuality, the fast development of automatic industrial, such as the central processing unit on computer
CPU is consequently increased with the lifting of arithmetic speed, caloric value, and heat dissipation problem then increasingly highlights, and LED core chip technology is only
The electric energy for having 30% is converted to light, and 70% electric energy is converted to heat in addition, if these heats can not effectively be dissipated, can cause
Chip burns, and reduces service life.
At present, application publication number for " CN104231634 " Chinese patent disclose a kind of high efficiency insulation heat-conducting silicone grease and
Its preparation method, including dimethicone, end hydroxyl silicone oil, aluminum oxide and coupling agent；The heat-conducting silicone grease that this method obtains is
With higher heat-conducting system.Insulation and the heat-conducting silicone grease of low thermal contact resistance, add coupling agent；The thermal conductive silicon that this method obtains
Fat is the heat-conducting silicone grease product with higher heat-conducting system, insulation and thermal contact resistance, and system can be reduced by adding coupling agent
Viscosity, but the viscosity of the heat-conducting silicone grease obtained after being well mixed, close to 350,000 centipoises, viscosity is still very big, heat-conducting silicone grease surface
Wetability is poor, causes section thermal resistance increase, and overall heat-conducting effect is deteriorated, the radiating being unfavorable between electronic device.
The content of the invention
It is an object of the invention to provide a kind of relatively low heat-conducting silicone grease of viscosity.
The present invention above-mentioned technical purpose technical scheme is that：A kind of heat-conducting silicone grease, with the following group
Part is by weight：
Dimethicone 5-20 parts
Heat filling 50-80 parts
Coupling agent 0.5-2 parts
Auxiliary agent 0.1-1 parts
Methyl-silicone oil 0.1-5 parts
Gas phase silica gel 0.1-3 parts.
Preferably, the heat filling is aluminum oxide, zinc oxide, gallium nitride, one kind in boron nitride or any several.
Preferably, the auxiliary agent is polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem
One kind or any several in TMOS.
Preferably, also include nano-graphene, CNT, one kind in carbon nano-fiber or any several.
Preferably, also include 1-3 part calcium carbonate powders.
The present invention above-mentioned technical purpose technical scheme is that：One kind is used to process above-mentioned heat conduction
The processing method of silicone grease, comprises the following steps：
Step 1：Stirring is ground during calcium carbonate powder is added into gas phase silica gel, milling time was more than 2 hours；
Step 2：By one kind in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem oxosilane
Or any several additions, lasting stirring；
Step 3：Dimethicone, methyl-silicone oil are poured slowly into and continue to stir；
Step 4：Vacuumizing and defoaming processing, it is 35-40 DEG C to control this link temperature；
Step 5：Coupling agent, heat filling, auxiliary agent are added to wherein, persistently stirred；
Step 6：By one kind in nano-graphene, CNT, carbon nano-fiber or any several additions to wherein, stirring is extremely
Uniformly；
Step 7：Secondary vacuum pumping deaeration is handled.
Preferably, a length of 0.3-0.6 μm of the calcium carbonate powder footpath.
The present invention above-mentioned technical purpose technical scheme is that：A kind of heat-conducting silicone grease is used to be lifted
The thermal diffusivity of electronic chip.
In summary, the invention has the advantages that：
（1）Dimethicone is the base oil of the heat-conducting silicone grease, and the heat filling material added wherein can significantly increase this and lead
The thermal conductivity of hot silicone grease and resistance to usability, the material in material and methyl-silicone oil in auxiliary agent can play certain diluting effect,
Contribute to the viscosity of reduction heat-conducting silicone grease；But after the viscosity of heat-conducting silicone grease reduces, can have to the gumminess of heat-conducting silicone grease
Certain influence, adds a certain amount of gas phase silica gel thereto, and gas phase silica gel can increase the gumminess of heat-conducting silicone grease, but due to
Gas phase silica gel can increase the viscosity of heat-conducting silicone grease, thus should not add；Secondly gas phase silica gel can slow down heat-conducting silicone grease desiccation
Speed, in viscous glutinous electronic component, heat-conducting silicone grease point can be dropped on electronic component, then fin is firmly attached to
Heat-conducting silicone grease, the sandwich sandwich biscuits shape of fin-heat-conducting silicone grease-electronic component three is formed, due to heat-conducting silicone grease viscosity
Relatively low, mobility is preferable, therefore when fin firmly attaches, heat-conducting silicone grease caters to fin and electronic component phase completely
To the shape on two sides, so avoid between fin and electronic component because have retaining for hole and caused by radiating effect drop
It is low；In the prior art, when using viscosity larger heat-conducting silicone grease, generally use surface cladding process, i.e., by heat-conducting silicone grease in electricity
Sub- component surface coats thicker one layer, then fin is adhered to it, and this mode of operation causes heat-conducting silicone grease to consume
Measure it is more, and tended to have between fin and heat-conducting silicone grease hole generation；And in the heat-conducting silicone grease in using this programme, it is only necessary to
Heat-conducting silicone grease is uniformly put and dropped on electronic component, reduces the dosage of heat-conducting silicone grease；
（2）Nano-graphene, CNT, carbon nano-fiber, these three materials are that particle diameter is smaller and have thermal conductive resin
Material, be by the row of honeycomb-patterned ordered in layer in addition, there is more special structure such as this kind of material of nano-graphene
The planar carbon atom of row is stacked and formed, and has preferable thermal conductivity, and has preferable lubricity, and fin firmly is being pressed into pressure viscosity
Stick at electronic component surface, this kind of material enables heat-conducting silicone grease preferably to be pushed open to surrounding；
（3）The micro molecule form of gas phase silica gel is netted, and calcium carbonate powder is mixed with gas phase silica gel, and continues stirring with grinding
Mill, calcium carbonate powder cut off the middle moieties chain of netted silica gel in process of lapping so that molecule cross-link in gas phase silica gel
Degree declines, even if the viscosity of gas phase silica gel declines, reduces afterwards because of the addition of gas phase silica gel and to the shadow of heat-conducting silicone grease viscosity
Ring；
（4）It will be ground using calcium carbonate powder in gas phase silica gel after finishing, by polyvinyl alcohol, HMDO, silicic acid
The materials such as tetra-ethyl ester, sub- silester, tetrem oxosilane are added to wherein, and these materials again will after being sufficiently mixed with gas phase silica gel
The materials such as dimethicone, methyl-silicone oil are added to wherein, and gas phase silica gel is soaked after standing wherein, and uniform with other materials
Be mixed to form uniform mixing dispersion, carry out first time vacuumizing and defoaming processing afterwards, make mixing dispersion volumetric expansion
And bubble therein is removed, the materials such as coupling agent, heat filling, auxiliary agent are added to wherein again afterwards, stirred, then will be received
Rice graphene, CNT, carbon nano-fiber etc. are added to wherein uniformly mixing, to substantially uniformity, are vacuumized again
Deaeration is handled, so as to complete the preparation of heat-conducting silicone grease.
Brief description of the drawings
Fig. 1 is overall flow schematic diagram in embodiment 1- embodiments 3.
Embodiment
The present invention is described in further detail below in conjunction with accompanying drawing.
This specific embodiment is only explanation of the invention, and it is not limitation of the present invention, people in the art
Member can make the modification of no creative contribution to the present embodiment as needed after this specification is read, but as long as at this
All protected in the right of invention by Patent Law.
Embodiment 1：
A kind of processing method of heat-conducting silicone grease, as shown in figure 1, comprising the following steps：
Step 1：Stirring is ground during calcium carbonate powder is added into gas phase silica gel, milling time was more than 2 hours, wherein Paris white
Between last particle diameter is 0.3-0.6 μm, less calcium carbonate powder use in the present embodiment, controls particle diameter as between 0.3-0.4 μm.
Step 2：By in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem oxosilane
A kind of or any several additions, lasting stirring.
Step 3：Dimethicone, methyl-silicone oil are poured slowly into and continue to stir.
Step 4：Vacuumizing and defoaming processing, it is 35-40 DEG C to control this link temperature, and it is 35 that temperature is controlled in the present embodiment
℃。
Step 5：Coupling agent, heat filling, auxiliary agent are added to wherein, persistently stirred；
Step 6：By one kind in nano-graphene, CNT, carbon nano-fiber or any several additions to wherein, stirring is extremely
Uniformly.
Step 7：Secondary vacuum pumping deaeration is handled.
Embodiment 2：
A kind of processing method of heat-conducting silicone grease, as shown in figure 1, comprising the following steps：
Step 1：Stirring is ground during calcium carbonate powder is added into gas phase silica gel, milling time was more than 2 hours, wherein Paris white
Between last particle diameter is 0.3-0.6 μm, less calcium carbonate powder use in the present embodiment, controls particle diameter as between 0.5-0.6 μm.
Step 2：By in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem oxosilane
A kind of or any several additions, lasting stirring.
Step 3：Dimethicone, methyl-silicone oil are poured slowly into and continue to stir.
Step 4：Vacuumizing and defoaming processing, it is 35-40 DEG C to control this link temperature, and it is 40 that temperature is controlled in the present embodiment
℃。
Step 5：Coupling agent, heat filling, auxiliary agent are added to wherein, persistently stirred；
Step 6：By one kind in nano-graphene, CNT, carbon nano-fiber or any several additions to wherein, stirring is extremely
Uniformly.
Step 7：Secondary vacuum pumping deaeration is handled.
Embodiment 3：
A kind of processing method of heat-conducting silicone grease, as shown in figure 1, comprising the following steps：
Step 1：Stirring is ground during calcium carbonate powder is added into gas phase silica gel, milling time was more than 2 hours, wherein Paris white
Between last particle diameter is 0.3-0.6 μm, less calcium carbonate powder use in the present embodiment, controls particle diameter as between 0.4-0.5 μm.
Step 2：By in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem oxosilane
A kind of or any several additions, lasting stirring.
Step 3：Dimethicone, methyl-silicone oil are poured slowly into and continue to stir.
Step 4：Vacuumizing and defoaming processing, it is 35-40 DEG C to control this link temperature, and it is 38 that temperature is controlled in the present embodiment
℃。
Step 5：Coupling agent, heat filling, auxiliary agent are added to wherein, persistently stirred；
Step 6：By one kind in nano-graphene, CNT, carbon nano-fiber or any several additions to wherein, stirring is extremely
Uniformly.
Step 7：Secondary vacuum pumping deaeration is handled.
Embodiment 4-10：
Wherein, each component content in heat-conducting silicone grease is as follows：
Dimethicone 5-20 parts
Heat filling 50-80 parts
Coupling agent 0.5-2 parts
Auxiliary agent 0.1-1 parts
Methyl-silicone oil 0.1-5 parts
Gas phase silica gel 0.1-3 parts.
Heat filling is aluminum oxide, zinc oxide, gallium nitride, one kind in boron nitride or any several.
Auxiliary agent is in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetraethoxysilane
It is a kind of or any several.
Coupling agent is dodecyltrimethoxysilane, vinyltrimethoxy silane, methacryloxypropyl three
One kind or any several in methoxy silane.
The content of each component is as shown in table 1 in embodiment 4- embodiments 10；
Table 1：
Batch ingredients in embodiment 4- embodiments 10 are processed according to according to the processing method disclosed in embodiment 3
To silicone grease carry out thermal conductivity factor, viscosity and thermal resistance are measured and recorded in table 2：
| Thermal resistance（θ） | Viscosity（mpa·s） | Thermal conductivity factor（λ） | |
| Embodiment 4 | 0.023 | 150000 | 1.912 |
| Embodiment 5 | 0.018 | 160000 | 2.347 |
| Embodiment 6 | 0.021 | 140000 | 2.123 |
| Embodiment 7 | 0.022 | 150000 | 3.126 |
| Embodiment 8 | 0.019 | 160000 | 3.264 |
| Embodiment 9 | 0.02 | 130000 | 3.109 |
| Embodiment 10 | 0.022 | 110000 | 2.331 |
Thermal conductivity factor：Under conditions of stabilization, by the time rate of change of the hot-fluid of the unit area of certain heterogeneous material divided by
Unit temperature gradient perpendicular to area direction, it is exhausted according to ASTM D5470 heat conduction electricity using LW-9389 type thermal conductivity test machines
The standard method of test of edge material Heat transmission is tested.
Thermal resistance：Material shows the obstruction to hot-fluid.
Viscosity：Viscosity test is carried out to sample using RVDT2T types viscosity apparatus.
Conclusion can be obtained according to table 2：The heat-conducting silicone grease that scheme according to recording to obtain in the application text is prepared, with the back of the body
For heat-conducting silicone grease in scape technology compared to having lower coefficient of viscosity, thermal resistance and thermal conductivity factor are essentially identical.
Claims (8)
1. a kind of heat-conducting silicone grease, it is characterised in that following component is by weight：
Dimethicone 5-20 parts
Heat filling 50-80 parts
Coupling agent 0.5-2 parts
Auxiliary agent 0.1-1 parts
Methyl-silicone oil 0.1-5 parts
Gas phase silica gel 0.1-3 parts.
A kind of 2. heat-conducting silicone grease according to claim 1, it is characterised in that：The heat filling be aluminum oxide, zinc oxide,
One kind or any several in gallium nitride, boron nitride.
A kind of 3. heat-conducting silicone grease according to claim 1, it is characterised in that：The auxiliary agent is polyvinyl alcohol, hexamethyl two
Siloxanes, tetraethyl orthosilicate, sub- silester, one kind in tetraethoxysilane or any several.
A kind of 4. heat-conducting silicone grease according to claim 1, it is characterised in that：Also include nano-graphene, CNT, receive
One kind or any several in rice carbon fiber.
A kind of 5. heat-conducting silicone grease according to claim 1, it is characterised in that：Also include 1-3 part calcium carbonate powders.
A kind of 6. processing method for processing heat-conducting silicone grease described in any one in claim 1-5, it is characterised in that including
Following steps：
Step 1：Stirring is ground during calcium carbonate powder is added into gas phase silica gel, milling time was more than 2 hours；
Step 2：By one kind in polyvinyl alcohol, HMDO, tetraethyl orthosilicate, sub- silester, tetrem oxosilane
Or any several additions, lasting stirring；
Step 3：Dimethicone, methyl-silicone oil are poured slowly into and continue to stir；
Step 4：Vacuumizing and defoaming processing, it is 35-40 DEG C to control this link temperature；
Step 5：Coupling agent, heat filling, auxiliary agent are added to wherein, persistently stirred；
Step 6：By one kind in nano-graphene, CNT, carbon nano-fiber or any several additions to wherein, stirring is extremely
Uniformly；
Step 7：Secondary vacuum pumping deaeration is handled.
A kind of 7. processing method according to claim 4, it is characterised in that：A length of 0.3-0.6 μm of the calcium carbonate powder footpath.
8. a kind of heat-conducting silicone grease is used to lift heat dissipation of electronic chip.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711149304.4A CN107739513A (en) | 2017-11-18 | 2017-11-18 | A kind of heat-conducting silicone grease and its processing method and application |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711149304.4A CN107739513A (en) | 2017-11-18 | 2017-11-18 | A kind of heat-conducting silicone grease and its processing method and application |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456601A (en) * | 2018-11-30 | 2019-03-12 | 南昌科悦企业管理咨询有限公司 | A kind of computer heat-conducting silicone grease of anti-chap and preparation method thereof |
| CN110684511A (en) * | 2019-09-05 | 2020-01-14 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
| CN111718653A (en) * | 2020-06-12 | 2020-09-29 | 珠海凌达压缩机有限公司 | Solid silicone grease composition, use method thereof, compressor shell using composition and preparation method |
| CN112266618A (en) * | 2020-10-13 | 2021-01-26 | 无锡吉仓纳米材料科技有限公司 | Intelligent heat-conducting silica gel of composite heat-conducting network and preparation method thereof |
| CN113913018A (en) * | 2021-11-30 | 2022-01-11 | 四川大学 | High-fluidity insulating and heat-conducting silicone grease and preparation method thereof |
| CN114507446A (en) * | 2022-02-23 | 2022-05-17 | 南京欧瑞光电科技有限公司 | High-efficiency heat-conducting silicone grease and preparation method thereof |
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| CN105754342A (en) * | 2016-03-21 | 2016-07-13 | 苏州柯仕达电子材料有限公司 | Low-viscosity heat conducting silicone grease and preparation method thereof |
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| US20070131913A1 (en) * | 2005-12-09 | 2007-06-14 | Foxconn Technology Co., Ltd. | Thermal interface material and semiconductor device incorporating the same |
| CN102558867A (en) * | 2011-12-13 | 2012-07-11 | 北京海斯迪克新材料有限公司 | Low-trailing heat conductive silicone grease composition and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456601A (en) * | 2018-11-30 | 2019-03-12 | 南昌科悦企业管理咨询有限公司 | A kind of computer heat-conducting silicone grease of anti-chap and preparation method thereof |
| CN110684511A (en) * | 2019-09-05 | 2020-01-14 | 上海阿莱德实业股份有限公司 | Preparation method of heat-conducting interface material |
| CN111718653A (en) * | 2020-06-12 | 2020-09-29 | 珠海凌达压缩机有限公司 | Solid silicone grease composition, use method thereof, compressor shell using composition and preparation method |
| CN112266618A (en) * | 2020-10-13 | 2021-01-26 | 无锡吉仓纳米材料科技有限公司 | Intelligent heat-conducting silica gel of composite heat-conducting network and preparation method thereof |
| CN113913018A (en) * | 2021-11-30 | 2022-01-11 | 四川大学 | High-fluidity insulating and heat-conducting silicone grease and preparation method thereof |
| CN114507446A (en) * | 2022-02-23 | 2022-05-17 | 南京欧瑞光电科技有限公司 | High-efficiency heat-conducting silicone grease and preparation method thereof |
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Application publication date: 20180227 |