CN109852066A - A kind of High thermal-conductive silicone grease and preparation method - Google Patents
A kind of High thermal-conductive silicone grease and preparation method Download PDFInfo
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- CN109852066A CN109852066A CN201910094991.7A CN201910094991A CN109852066A CN 109852066 A CN109852066 A CN 109852066A CN 201910094991 A CN201910094991 A CN 201910094991A CN 109852066 A CN109852066 A CN 109852066A
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Abstract
The present invention provides a kind of High thermal-conductive silicone grease, and constitutive material includes: liquid silicone grease, alumina particle, sheet zinc oxide, platelet boron nitride, aluminium powder, nanometer diamond powder, silane coupling agent;Wherein liquid silicone grease accounting is 7%-9%, and alumina particle accounting is 20%-30%, and sheet zinc oxide accounting is 20%-30%, platelet boron nitride accounting is 5%-10%, aluminium powder accounting is 30%-40%, and nanometer diamond powder accounting is 2%-5%, and silane coupling agent accounting is 0.5%-0.9%;The liquid silicone resin is long chain alkyl modified dimethyl siloxane, and viscosity is 500~600mpa;Silane coupling agent is the mixture of octyl trimethoxy siloxane and phenyl siloxane, and above scheme has the characteristics that higher heating conduction compared with the prior art and silicone grease will not be precipitated.
Description
Technical field
The invention belongs to Heat Conduction Material fields, in particular to the improvement to heat sink material silicone grease ingredient and preparation method.
Background technique
Quickly, part electronic component such as power tube, CPU etc. can release during the work time for electronic enterprises development
Big calorimetric, electronic component temperature sharply increase and cause localized hyperthermia, and high temperature can seriously affect the performance and drop of electronic component
Its low service life.This is very high to the cooling requirements of electronic component.Heat-conducting silicone grease is the common product of cooling electronic component,
It can be used for a long time and keep paste at 120 DEG C, with good insulating properties and non-toxic and tasteless chemical property is stablized to electronics device
The corrosion-free effect of part.Heat-conducting silicone grease sufficiently stirs mainly metal powder, metal oxide dispersion in liquid silicone resin at present
It mixes grinding and obtains heat-conducting silicone grease.
The metal powder, metal oxide are that inorganic matter liquid silicone grease is organic matter, the metal powder and metal oxygen
Compound with liquid-state silicon lipid phase capacitive is not high that powder granule is caused to be unevenly distributed in resin, be easy to cause fission after long-term storage
It is separated with resin and makes powder oil layer and the defect of condensate oil occur.
Adding powder is common metal powder or metal oxide, and such powder of low loading cannot increase substantially it
Thermal conductivity can energy.
Summary of the invention
First aspect present invention provides a kind of silicone grease formula scheme that can overcome silicone grease condensate oil defect, utilizes octyl three
Methoxy radical siloxane compounds the compatibility improved between inorganic fill powder and silicone grease as coupling agent system with phenyl siloxane
So that silicone grease is not easy to be precipitated.Second aspect of the present invention provides a kind of silicone grease formula of high thermal conductivity by improving metal heat-conducting
The proportion of powder and increase nanometer diamond heat filling.
The High thermal-conductive silicone grease, constitutive material include: liquid silicone grease, alumina particle, sheet zinc oxide, sheet nitridation
Boron, aluminium powder, nanometer diamond powder, silane coupling agent;
Wherein liquid silicone grease accounting is 7%-9%, and alumina particle accounting is 20%-30%, and sheet zinc oxide accounting is
20%-30%, platelet boron nitride accounting are 5%-10%, and aluminium powder accounting is 30%-40%, and nanometer diamond powder accounting is 2%-
5%, silane coupling agent accounting is 0.5%-0.9%;The liquid silicone resin is long chain alkyl modified dimethyl siloxane, viscosity
For 500~600mpa;Silane coupling agent is the mixture of octyl trimethoxy siloxane and phenyl siloxane.
As a preferred solution, the aluminium oxide is ball-type aluminium oxide, and partial size is 1~3um;The sheet zinc oxide
Partial size be 1~3um;The partial size of the platelet boron nitride is 1~3um;The aluminium powder is ball-type aluminium powder, and partial size is 5~10um;
The diamond dust that the diamond dust is 200~500 nanometers of partial size.
As a preferred solution, the compound proportion of silane coupling agent is 70% phenyl silicon of octyl trimethoxy siloxane
Oxygen alkane 30%.
As a preferred solution, the liquid silicone grease is 7.1 parts, and the alumina particle is 20 parts, the sheet
Zinc oxide is 25 parts, and platelet boron nitride is 10 parts, and the aluminium powder is 32 parts, and the nanometer diamond powder is 5 parts, and silane coupling agent is
0.9 part.
As a preferred solution, the heat-conducting silicone grease K value is 5.5w/ (m.k), and thermal impedance is 0.05 DEG C of * cm2/w
Viscosity (25 DEG C): 2,800,000mpa.s, high temperature resistant: solidification temperature is greater than 160 DEG C.
11. the liquid silicone grease is 8.2 parts such as power 1, the alumina particle is 30 parts, and the sheet zinc oxide is 15
Part, platelet boron nitride is 15 parts, and the aluminium powder is 26 parts, and the nanometer diamond powder is 5 parts, and silane coupling agent is 0.8 part.
As a preferred solution, the liquid silicone grease K value is 5.2w/ (m.k), and thermal impedance is 0.05 DEG C of * cm2/
W, viscosity is 2,200,000mpa.s under 25 DEG C of temperature environments, and solidification temperature is greater than 160 DEG C.
Preferably to solve the above problems, the present invention further provides a kind of preparation method of High thermal-conductive silicone grease, step
It include: the liquid silicone grease that prepared accounting is 7%-9%, accounting is the alumina particle of 20%-30%, accounting 20%-30%
Sheet zinc oxide, accounting is the platelet boron nitride of 5%-10%, and accounting is the aluminium powder of 30%-40%, and accounting is 2%-5%
Nanometer diamond powder, accounting are the silane coupling agent of 0.5%-0.9%;
Liquid silicone resin and silane coupling agent are poured into planet dispersion machine and are heated to 70 DEG C;
Alumina particle is added, stirs 30 minutes;
Sheet zinc oxide is added, stirs 30 minutes;
Platelet boron nitride is added, stirs 30 minutes;
Aluminium powder is added, stirs 30 minutes;
Nanometer diamond powder is added, stirs 30 minutes;
Stirring 60 minutes;
Above-mentioned mixture is transferred into three-roller from planet dispersion machine and grinds twice of grinding;
Above-mentioned mixture is transferred into planet dispersion machine from three-roll grinder to stir 30 minutes.
In preferably technical solution, alumina particle, sheet zinc oxide, platelet boron nitride, nanometer diamond powder is being added
The revolving speed of planet dispersion machine described in described the step of stirring 30 minutes is 200-300r/min afterwards;In the last one step planet
Dispersing speed is 600-800r/min.
In preferably technical solution, the revolving speed of the planet dispersion machine described in described the step of stirring 60 minutes is 600-
800r/min。
First aspect present invention increases inorganic particle and organic liquor as coupling agent using the mixture of small molecule siloxanes
The compatibility of state silicone resin stores silicone grease for a long time and powder is not readily separated so as to avoid the skill of prior art heat-conducting silicone grease condensate oil
Art defect.Second aspect of the present invention, which improves powder (aluminium powder, zinc oxide, boron nitride, aluminium powder) adding proportion, makes powder total amount exist
92.5%-90.1% and introduce introduce nanoscale diamond powder the overall thermal conductivity of silicone grease is improved.
Specific embodiment
The proportion material of High thermal-conductive silicone grease of the invention includes: that its accounting of liquid silicone resin is 7-9%, its accounting of aluminium oxide
For 20-30%, its accounting of zinc oxide is 20-30%, its accounting of boron nitride is 5~10%, its accounting of aluminium powder is 30~40%, is received
Its accounting 2~5% of meter level diamond dust, its accounting of silane coupling agent are 0.5-0.9%.The silane coupling agent can be improved aluminium
The compatibility of powder, aluminium oxide, zinc oxide and liquid silicone grease is in always so that mixed silicone grease mixture is in powder always
Suspended state.The metal or metal-oxide powder filler material of the high mixture ratio can be improved its heating conduction, nanoscale diamond
Powder filled material then further the lower silicone grease mixture thermal impedance.
The liquid silicone resin is long chain alkyl modified dimethyl siloxane, and viscosity is 500~600mpa.s.Aluminium oxide is
Ball-type aluminium oxide, partial size are 1~3um;Zinc oxide is sheet zinc oxide, and partial size is 1~3um;Boron nitride is platelet boron nitride, grain
Diameter is 1~3um;Aluminium powder is ball-type aluminium powder, and partial size is 5~10um, the diamond dust that diamond dust is 200~500 nanometers of partial size;Silane
Coupling agent are as follows: the mixture of octyl trimethoxy siloxane and phenyl siloxane, compound proportion are octyl trimethoxy siloxane
70% phenyl siloxane 30%.
The silicone grease mixture is prepared according to following step, is with accounting by the liquid silicone resin that accounting is 7%-9%
The silane coupling agent of 0.5%-0.9%, which pours into planet dispersion machine, is heated to 70 DEG C.Sequentially add the oxygen that accounting is 20%-30%
Change aluminium powder that boron nitride powder, accounting that zinc oxide, accounting that aluminium, accounting are 20%-30% are 5%-10% are 30%-40%,
Accounting is the diamond dust of 2%-5%, and the above process is every, which to be added a kind of powder, to stir 30min under the revolving speed of 200-300r/min
After add a kind of lower powder, after powder all adds revolving speed be 600-800r/min revolving speed under stir 1 hour.It will
Above-mentioned silicone grease mixture is transferred in three-roller from planet dispersion machine to be ground twice again, is finally mixed again from three-roller by the silicone grease
Conjunction object, which is transferred in planet dispersion machine, obtains final products with the revolving speed 30min of 600-800r/min.
According to the above scheme present invention provide the first silicone grease mixture material proportion with and preparation method thereof according to total amount
100 parts of 8.2 parts of proportion preparation liquid silicone resin, 30 parts of aluminium oxide, 15 parts of zinc oxide, 15 parts of boron nitride, aluminium powder 26 part, nanometer
Grade 5 parts of diamond dust, 0.8 part of silane coupling agent.
The liquid silicone resin and silane coupling agent are poured into planet dispersion machine and are heated to 70 DEG C;
Aluminium oxide is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Zinc oxide is added into the planet dispersion machine, is rotated 30 minutes with revolving speed for the transfer of 200-300r/min;
Boron nitride is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Aluminium powder is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Nanometer diamond powder is added into the planet dispersion machine, is divided with revolving speed for the rotational speed 60 of 600-800r/min
Clock;
The silicone grease mixture is transferred in three-roller from planet dispersion machine and is ground twice;
Finally by the silicone grease mixture from transferred in three-roller in planet dispersion machine with 600-800r/min turn
Speed stirring 30min obtains finished product.
There is the silicone grease its main performance feature of high thermal conductivity to be as follows:
Second of silicone grease mixture material proportion is provided according to the above scheme present invention and preparation method is 100 in an amount
7.1 parts of the liquid silicone resin prepared respectively of part, 20 parts of aluminium oxide, 25 parts of zinc oxide, 10 parts of boron nitride, 32 parts of aluminium powder, nanoscale
5 parts of diamond dust, 0.9 part of silane coupling agent.
The liquid silicone resin and silane coupling agent are poured into planet dispersion machine and are heated to 70 DEG C
Aluminium oxide is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Zinc oxide is added into the planet dispersion machine, is rotated 30 minutes with revolving speed for the transfer of 200-300r/min;
Boron nitride is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Aluminium powder is added into the planet dispersion machine, is rotational speed 30 minutes of 200-300r/min with revolving speed;
Nanometer diamond powder is added into the planet dispersion machine, is divided with revolving speed for the rotational speed 60 of 600-800r/min
Clock;
The silicone grease mixture is transferred in three-roller from planet dispersion machine and is ground twice;
Finally by the silicone grease mixture from transferred in three-roller in planet dispersion machine with 600-800r/min turn
Speed stirring 30min obtains finished product.
There is the silicone grease its main performance feature of high thermal conductivity to be as follows:
The application is compared with the prior art using a high proportion of powder filled to improve its whole heat dissipation performance, addition silane
Coupling agent makes the compatibility of the liquid silicone resin Yu metal powder and oxidied metal powder, and the metal powder begins in liquid silicone grease
It is not easy to be precipitated in silicone grease described in suspended state eventually.
Claims (10)
1. a kind of High thermal-conductive silicone grease, it is characterised in that constitutive material includes: liquid silicone grease, alumina particle, sheet zinc oxide, piece
Shape boron nitride, aluminium powder, nanometer diamond powder, silane coupling agent;
Wherein liquid silicone grease accounting is 7%-9%, and alumina particle accounting is 20%-30%, and sheet zinc oxide accounting is 20%-
30%, platelet boron nitride accounting is 5%-10%, and aluminium powder accounting is 30%-40%, and nanometer diamond powder accounting is 2%-5%, silicon
Alkane coupling agent accounting is 0.5%-0.9%;
The liquid silicone resin is long chain alkyl modified dimethyl siloxane, and viscosity is 500~600mpa;
Silane coupling agent is the mixture of octyl trimethoxy siloxane and phenyl siloxane.
2. a kind of High thermal-conductive silicone grease as described in claim 1, which is characterized in that the aluminium oxide is ball-type aluminium oxide, partial size
For 1~3um;The partial size of the sheet zinc oxide is 1~3um;The partial size of the platelet boron nitride is 1~3um;The aluminium powder is
Ball-type aluminium powder, partial size are 5~10um;The diamond dust that the diamond dust is 200~500 nanometers of partial size.
3. a kind of High thermal-conductive silicone grease as described in claim 1, which is characterized in that the compound proportion of silane coupling agent is octyl three
70% phenyl siloxane 30% of methoxy radical siloxane.
4. a kind of High thermal-conductive silicone grease as described in claim 1, which is characterized in that the liquid silicone grease is 7.1 parts, the oxidation
Alumina particles are 20 parts, and the sheet zinc oxide is 25 parts, and platelet boron nitride is 10 parts, and the aluminium powder is 32 parts, and the nanometer is bored
Mountain flour is 5 parts, and silane coupling agent is 0.9 part.
5. a kind of High thermal-conductive silicone grease as claimed in claim 4, which is characterized in that the heat-conducting silicone grease K value is 5.5w/ (m.k),
Thermal impedance is 0.05 DEG C of * cm2/w viscosity (25 DEG C): 2,800,000mpa.s, high temperature resistant: solidification temperature is greater than 160 DEG C.
6. a kind of High thermal-conductive silicone grease as described in claim 1, which is characterized in that the liquid silicone grease is 8.2 parts, the oxidation
Alumina particles are 30 parts, and the sheet zinc oxide is 15 parts, and platelet boron nitride is 15 parts, and the aluminium powder is 26 parts, and the nanometer is bored
Mountain flour is 5 parts, and silane coupling agent is 0.8 part.
7. a kind of High thermal-conductive silicone grease as claimed in claim 6, which is characterized in that the liquid silicone grease K value is 5.2w/ (m.k),
Thermal impedance is 0.05 DEG C of * cm2/w, and viscosity is 2,200,000mpa.s under 25 DEG C of temperature environments, and solidification temperature is greater than 160 DEG C.
8. a kind of preparation method of High thermal-conductive silicone grease, which is characterized in that comprising steps of the liquid-state silicon that preparation accounting is 7%-9%
Rouge, accounting are the alumina particle of 20%-30%, and accounting is the sheet zinc oxide of 20%-30%, and accounting is the piece of 5%-10%
Shape boron nitride, accounting are the aluminium powder of 30%-40%, and accounting is the nanometer diamond powder of 2%-5%, and accounting is 0.5%-0.9%'s
Silane coupling agent;
Liquid silicone resin and silane coupling agent are poured into planet dispersion machine and are heated to 70 DEG C;
Alumina particle is added, stirs 30 minutes;
Sheet zinc oxide is added, stirs 30 minutes;
Platelet boron nitride is added, stirs 30 minutes;
Aluminium powder is added, stirs 30 minutes;
Nanometer diamond powder is added, stirs 30 minutes;
Stirring 60 minutes;
Above-mentioned mixture is transferred into three-roller from planet dispersion machine and grinds twice of grinding;
Above-mentioned mixture is transferred into planet dispersion machine from three-roll grinder to stir 30 minutes.
9. a kind of preparation method of High thermal-conductive silicone grease as claimed in claim 8, which is characterized in that be added alumina particle,
The revolving speed of planet dispersion machine described in described the step of stirring 30 minutes after sheet zinc oxide, platelet boron nitride, nanometer diamond powder
For 200-300r/min;It is 600-800r/min in the last one step planet dispersing speed.
10. a kind of preparation method of High thermal-conductive silicone grease as claimed in claim 8, which is characterized in that in the stirring 60 minutes
The step of described in planet dispersion machine revolving speed be 600-800r/min.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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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 |
CN112625659A (en) * | 2020-12-22 | 2021-04-09 | 广东鼎泰新材料科技有限公司 | High-thermal-conductivity heat-conducting silicone grease and preparation process thereof |
CN113604048A (en) * | 2021-07-14 | 2021-11-05 | 昆山纳诺新材料科技有限公司 | Heat-conducting silicone grease |
CN114773859A (en) * | 2022-04-24 | 2022-07-22 | 深圳市汉华热管理科技有限公司 | Heat-conducting silica gel composite material and preparation method thereof |
-
2019
- 2019-01-26 CN CN201910094991.7A patent/CN109852066A/en active Pending
Non-Patent Citations (1)
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周文英 等著: "《聚合物基导热复合材料》", 30 June 2017, 国防工业出版社 * |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN111534358B (en) * | 2020-05-09 | 2022-03-29 | 中山市特好德润滑科技有限公司 | Heat-conducting lubricating grease and preparation method and application thereof |
CN112625659A (en) * | 2020-12-22 | 2021-04-09 | 广东鼎泰新材料科技有限公司 | High-thermal-conductivity heat-conducting silicone grease and preparation process thereof |
CN113604048A (en) * | 2021-07-14 | 2021-11-05 | 昆山纳诺新材料科技有限公司 | Heat-conducting silicone grease |
CN114773859A (en) * | 2022-04-24 | 2022-07-22 | 深圳市汉华热管理科技有限公司 | Heat-conducting silica gel composite material and preparation method thereof |
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