CN111849426B - Insulating heat-conducting grease and preparation method thereof - Google Patents
Insulating heat-conducting grease and preparation method thereof Download PDFInfo
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- CN111849426B CN111849426B CN201910332407.7A CN201910332407A CN111849426B CN 111849426 B CN111849426 B CN 111849426B CN 201910332407 A CN201910332407 A CN 201910332407A CN 111849426 B CN111849426 B CN 111849426B
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- 239000004519 grease Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002199 base oil Substances 0.000 claims abstract description 27
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 21
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 109
- 229920002545 silicone oil Polymers 0.000 claims description 33
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 23
- 239000011258 core-shell material Substances 0.000 claims description 22
- 238000001354 calcination Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 10
- 239000011231 conductive filler Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 238000007254 oxidation reaction Methods 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 238000010292 electrical insulation Methods 0.000 abstract description 15
- 238000009776 industrial production Methods 0.000 abstract description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 63
- 239000002245 particle Substances 0.000 description 22
- 230000017525 heat dissipation Effects 0.000 description 10
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 229940083037 simethicone Drugs 0.000 description 8
- 238000005303 weighing Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
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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
- C09K5/10—Liquid materials
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Lubricants (AREA)
Abstract
The invention discloses an insulating heat-conducting grease and a preparation method thereof. The preparation method of the insulating heat-conducting grease comprises the following steps: forming an aluminum oxide layer on the surface of aluminum powder to obtain a heat-conducting filler; and then mixing the heat conducting filler with carrier oil to obtain the insulating heat conducting grease. The insulating heat-conducting grease provided by the invention has high heat conductivity and electrical insulation property, and has a wide application range. The preparation method of the insulating heat-conducting grease provided by the invention is low in cost, simple and efficient, and can effectively reduce the industrial production cost.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to insulating heat conduction grease and a preparation method thereof.
Background
The electronic products are developed in the directions of miniaturization, integration and functionalization at a high speed, and the problem of heat dissipation of the electronic products is one of the barriers for further development of the electronic product industry. In order to solve the heat dissipation problem of electronic components, a heat dissipation device is usually mounted on the electronic components. However, due to the limitation of industrial technology production, the surfaces of the devices cannot be completely contacted, and when the electronic components are attached to the heat dissipation device, air exists at the contact interface, so that the overall heat dissipation effect is seriously affected. Therefore, the common practice is to fill heat-conducting grease between the electronic component and the heat dissipation device so as to fill the gap between the electronic component and the heat dissipation device, reduce interface contact thermal resistance and improve the overall heat dissipation performance of the device.
The existing heat-conducting grease can not achieve the effects of high heat-conducting performance and electrical insulation performance, and the application range of the heat-conducting grease is greatly limited.
Disclosure of Invention
In order to solve the problem that the heat conduction grease in the prior art cannot have high heat conduction and electrical insulation properties, so that the application range is limited, the invention provides the insulating heat conduction grease with low cost and high heat conduction performance, and provides the preparation method of the insulating heat conduction grease.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
an insulating heat-conducting grease comprises carrier oil and a heat-conducting filler which are mixed with each other, wherein the heat-conducting filler is core-shell structure powder taking aluminum powder as a core and an aluminum oxide layer as a shell.
Further, in the insulating heat-conducting grease, the content of the heat-conducting filler is 80-90% in percentage by mass.
Preferably, in the core-shell structure powder, the particle diameter of the aluminum powder is 3-20 μm, and the thickness of the aluminum oxide layer is 340-450 nm.
Further, the carrier oil is dimethyl silicone oil and phenyl silicone oil.
Preferably, the viscosity of the carrier oil is from 50 mPas to 200 mPas.
The invention also provides a preparation method of the insulating heat-conducting grease, which comprises the following steps:
s1, providing aluminum powder, carrying out oxidation treatment on the aluminum powder, forming an aluminum oxide layer on the surface of the aluminum powder, and preparing and obtaining a heat-conducting filler, wherein the heat-conducting filler is core-shell structure powder taking the aluminum powder as a core and the aluminum oxide layer as a shell;
and S2, providing carrier oil, and stirring and mixing the carrier oil and the heat conducting filler to obtain the insulating heat conducting grease.
Further, in the step S1, the method specifically includes: calcining the aluminum powder in air or oxygen atmosphere to obtain the heat-conducting filler.
Further, the calcination temperature is 300-600 ℃ and the calcination time is 12-24 hours.
Further, a mixer is used to mix the thermally conductive filler with the carrier oil.
Further, the rotating speed of the mixer is 1500 rpm-2500 rpm, and the mixing time is 20 min-50 min.
According to the invention, the core-shell structure powder taking aluminum powder as a core and an aluminum oxide layer as a shell is used as the heat conducting filler, and the heat conducting filler is mixed with the carrier oil to obtain the heat conducting grease with high heat conducting property and electrical insulating property, so that the heat conducting grease can be widely applied to the field of heat dissipation of electronic components. Meanwhile, the preparation method of the insulating heat-conducting grease provided by the invention is low in cost, simple and efficient, and can be well applied to industrial production.
Drawings
The above and other aspects, features and advantages of embodiments of the present invention will become more apparent from the following description when taken in conjunction with the accompanying drawings in which:
FIG. 1 is a flow chart of a preparation method of insulating and heat conducting grease according to the invention;
FIG. 2 is a diagram of Al in example 1 2 O 3 SEM scan of @ Al powder;
FIG. 3 is Al in example 1 2 O 3 TEM scan of @ Al powder;
FIG. 4 is a diagram of Al in example 2 2 O 3 TEM image of @ Al powder;
FIG. 5 is a diagram of Al in example 3 2 O 3 TEM image of @ Al powder;
FIG. 6 is Al in example 4 2 O 3 SEM image of @ Al powder;
FIG. 7 is a diagram of Al in example 5 2 O 3 SEM image of @ Al powder.
Detailed Description
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the specific embodiments set forth herein. Rather, these embodiments are provided to explain the principles of the invention and its practical application so that others skilled in the art will be able to understand the invention for various embodiments and with various modifications as are suited to the particular use contemplated.
The inventor of the invention provides an insulating heat-conducting grease with simple preparation process and low cost and a preparation method thereof based on the problem that the existing heat-conducting grease cannot have both high heat-conducting performance and electric insulation performance.
The embodiment of the invention provides insulating heat-conducting grease which comprises carrier oil and heat-conducting filler which are mixed with each other. Wherein the heat conductive filler takes aluminum (Al) powder as a core and aluminum oxide (Al) 2 O 3 ) Core-shell structured powders with shell layers, i.e. Al 2 O 3 @ Al powder.
Preferably, in the insulating heat-conducting grease, al is calculated as mass percent 2 O 3 The content of the @ Al powder is 80-90%.
Preferably, in Al 2 O 3 In the @ Al powder, the particle size of the aluminum powder is 3-20 mu m, and the thickness of the aluminum oxide layer is 340-450 nm.
Further, the carrier oil is dimethyl silicone oil or phenyl silicone oil.
The viscosity of the carrier oil has no effect on the heat conducting properties of the final product. However, oil bleeding occurs when the viscosity of the carrier oil is less than 50 mPas; and when the viscosity of the carrier oil is higher than 200mpa·s, the filling amount of the heat conductive filler therein is limited. Therefore, the viscosity of the carrier oil is preferably 50 mPas to 200 mPas.
The invention provides a preparation method of insulating and heat-conducting grease, as shown in figure 1, which comprises the following steps:
step S1, providing aluminum powder, oxidizing the aluminum powder to form an aluminum oxide layer on the surface of the aluminum powder, and preparing and obtaining Al 2 O 3 @ Al powder.
Further, the particle diameter of the aluminum powder is preferably 3 μm to 20 μm, and of course, aluminum powder having other particle diameters may be used as a raw material.
The aluminum oxide layer is formed on the surface of the aluminum powder to ensure the electrical insulation performance of the subsequent heat conduction grease, and the aluminum powder can be oxidized by adopting a high-temperature calcination method, and other oxidation methods can be adopted.
Calcining the aluminum powder for 12-24 hours in air or oxygen atmosphere at 300-600 ℃ by adopting a high-temperature calcining method to prepare the Al 2 O 3 @ Al powder.
Step S2,Providing a carrier oil, mixing the carrier oil with Al 2 O 3 Stirring and mixing the @ Al powder to obtain the insulating heat-conducting grease.
Further, al 2 O 3 The mass ratio of the @ Al powder to the carrier oil is as follows: 80% -90%.
Further, the carrier oil is dimethyl silicone oil or phenyl silicone oil.
Preferably, the viscosity of the carrier oil is from 50 mPas to 200 mPas.
Further, a mixer is adopted to mix Al 2 O 3 Stirring and mixing the @ Al powder and carrier oil. Of course, other mixing methods can be used to mix Al 2 O 3 @ Al powder with a carrier oil.
When the mixer is used for mixing, as long as the heat-conducting filler can be uniformly mixed, the final result is not affected by the parameter setting of the mixer, so that the rotating speed of the mixer can be selected to be 1500 rpm-2500 rpm; the mixing time is 20 min-50 min.
The invention provides the method adopting Al 2 O 3 Insulating heat-conducting grease with high heat-conducting property and 4.8 W.m heat conductivity by using @ Al powder as heat-conducting filler -1 ·K -1 ～8.0W·m -1 ·K -1 The method comprises the steps of carrying out a first treatment on the surface of the Meanwhile, due to the existence of the alumina layer, the insulating heat-conducting grease also has good electrical insulation property, and the resistivity of the insulating heat-conducting grease is not lower than 10 13 Ω·cm。
The above-described insulating and heat-conducting grease and the method of preparing the same of the present invention will be described below with reference to specific examples, which are understood by those skilled in the art to be merely specific examples of the above-described insulating and heat-conducting grease and the method of preparing the same of the present invention, and are not intended to limit the scope of the present invention.
Example 1
Calcining Al powder with average particle diameter of about 20 μm in air at 300deg.C for 12 hr to obtain Al 2 O 3 @ Al powder.
For the Al obtained 2 O 3 The @ Al powder was scanned by a Scanning Electron Microscope (SEM), and the scanning results are shown in FIG. 2. As can be seen from FIG. 2, al 2 O 3 Flat of @ Al powderThe average particle diameter was 20. Mu.m.
For Al 2 O 3 The result of performing Transmission Electron Microscope (TEM) scanning on a part of @ Al powder is shown in fig. 3. As can be seen from FIG. 3, al is prepared in this example 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 Core-shell structure with shell layer, al 2 O 3 The thickness of the layer was about 340nm.
Weighing 90g of Al 2 O 3 The @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 8.0 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 2
Calcining Al powder with average particle diameter of 20 μm in air at 450deg.C for 18 hr to obtain Al 2 O 3 @ Al powder.
For Al 2 O 3 TEM scan of a part of the @ Al powder was performed, and the obtained results are shown in FIG. 4. As can be seen from FIG. 4, al is prepared in this example 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 Core-shell structure with shell layer, al 2 O 3 The thickness of the layer was about 414nm.
Weighing 90g of Al 2 O 3 The @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 7.6W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 414nm.
Example 3
Calcining Al powder with average particle diameter of 20 μm in air at 600deg.C for 24 hr to obtain Al 2 O 3 @ Al powder.
For Al 2 O 3 TEM scan of a part of the @ Al powder was performed, and the obtained results are shown in FIG. 5. As can be seen from FIG. 5, al is prepared in this example 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 Core-shell structure with shell layer, al 2 O 3 The thickness of the layer was about 450nm.
Weighing 90g of Al 2 O 3 The @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
At room temperature, the insulating heat conducting oil is prepared by adopting the Hot-DiskCharacterization of thermal conductivity of the fat gave a thermal conductivity of 7.3 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 450nm.
Example 4
Calcining Al powder with average particle diameter of 8 μm in air at 300deg.C for 12 hr to obtain Al 2 O 3 @ Al powder.
For the Al obtained 2 O 3 Scanning Electron Microscope (SEM) scanning was performed on Al powder, and the scanning results are shown in fig. 6. As can be seen from FIG. 6, al 2 O 3 The average particle diameter of the @ Al powder was 8. Mu.m.
Weighing 90g of Al 2 O 3 The @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 7.1 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has a composition of AlThe powder is core, al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 8. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 5
Calcining Al powder with average particle diameter of 3 μm in air at 300deg.C for 12 hr to obtain Al 2 O 3 @ Al powder.
For the Al obtained 2 O 3 SEM scan of @ Al powder was performed and the scan results are shown in FIG. 7. As can be seen from FIG. 7, al 2 O 3 The average particle diameter of the @ Al powder was 3. Mu.m.
Weighing 90g of Al 2 O 3 The @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 6.5 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 3. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 6
90g of Al from example 1 above was weighed out 2 O 3 @ Al powder, 10g of twoAnd (3) in the methyl silicone oil, the viscosity of the dimethyl silicone oil is 50 mPas, and the methyl silicone oil is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 8.0 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 7
90g of Al from example 1 were weighed out 2 O 3 And @ Al powder is mixed into 10g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 20min at the rotating speed of 1500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 8.0 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 @ Al powderThe mass fraction of the body was 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 8
80g of Al from example 1 were weighed out 2 O 3 The @ Al powder is mixed into 20g of dimethyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the mixture is placed in a mixer and mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 4.8 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder and simethicone. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 80%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 9
85g of Al from example 1 above was weighed out 2 O 3 The @ Al powder is mixed into 15g of phenyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the phenyl silicone oil and the dimethyl silicone oil are placed in a mixer to be mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 6.7W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder with phenyl silicone oil. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 85%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
Example 10
90g of Al from example 1 above was weighed out 2 O 3 The @ Al powder is mixed into 10g of phenyl silicone oil, the viscosity of the dimethyl silicone oil is 150 mPa.s, and the phenyl silicone oil and the dimethyl silicone oil are placed in a mixer to be mixed for 50min at the rotating speed of 2500rpm, so that the insulating heat-conducting grease is obtained.
Under the condition of room temperature, the heat conduction performance of the insulating and heat conduction grease is characterized by adopting the Hot-Disk, and the obtained heat conduction coefficient result is 7.8 W.m -1 ·K -1 。
The electrical insulation property of the insulating and heat conducting grease is characterized under the room temperature condition, and the obtained resistivity is about 10 13 Ω·cm。
The insulating and heat-conducting grease prepared in the embodiment comprises mutually mixed Al 2 O 3 @ Al powder with phenyl silicone oil. Al (Al) 2 O 3 The @ Al powder has an Al powder as a core and Al 2 O 3 The layer is a core-shell structure of the shell.
Wherein Al is 2 O 3 The mass fraction of the @ Al powder is 90%.
Al 2 O 3 The average particle diameter of the @ Al powder was 20. Mu.m, wherein Al 2 O 3 The thickness of the layer was 340nm.
While the invention has been shown and described with reference to certain embodiments, those skilled in the art will appreciate that: various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims and their equivalents.
Claims (8)
1. The insulating heat-conducting grease is characterized by comprising carrier oil and a heat-conducting filler which are mixed with each other, wherein the heat-conducting filler is core-shell structure powder taking aluminum powder as a core and an aluminum oxide layer as a shell; in the core-shell structure powder, the average grain diameter of the core-shell structure powder is 20 mu m, and the thickness of the aluminum oxide layer is 340nm; in the insulating heat-conducting grease, the content of the heat-conducting filler is 90% in percentage by mass.
2. The insulating and heat conducting grease according to claim 1, wherein the carrier oil is dimethyl silicone oil or phenyl silicone oil.
3. The insulating and heat-conducting grease according to claim 2, wherein the viscosity of the carrier oil is 50 mPa-s to 200 mPa-s.
4. A method for preparing the insulating and heat-conducting grease according to any one of claims 1 to 3, comprising:
s1, providing aluminum powder, carrying out oxidation treatment on the aluminum powder, forming an aluminum oxide layer on the surface of the aluminum powder, and preparing and obtaining a heat-conducting filler, wherein the heat-conducting filler is core-shell structure powder taking the aluminum powder as a core and the aluminum oxide layer as a shell;
and S2, providing carrier oil, and stirring and mixing the carrier oil and the heat conducting filler to obtain the insulating heat conducting grease.
5. The method according to claim 4, wherein in the step S1, specifically comprising: calcining the aluminum powder in air or oxygen atmosphere to obtain the heat-conducting filler.
6. The method according to claim 5, wherein the calcination temperature is 300 to 600 ℃ and the calcination time is 12 to 24 hours.
7. The method of claim 4, wherein the thermally conductive filler is mixed with the carrier oil using a blender.
8. The preparation method according to claim 7, wherein the rotational speed of the mixer is 1500rpm to 2500rpm and the mixing time is 20min to 50min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003725A (en) * | 2006-01-21 | 2007-07-25 | 富准精密工业(深圳)有限公司 | Heat interface material, and preparation method |
| CN104710792A (en) * | 2015-03-25 | 2015-06-17 | 合肥工业大学 | Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof |
| CN107141719A (en) * | 2017-05-27 | 2017-09-08 | 中国科学院深圳先进技术研究院 | Filled-type thermally conductive composite and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003725A (en) * | 2006-01-21 | 2007-07-25 | 富准精密工业(深圳)有限公司 | Heat interface material, and preparation method |
| CN104710792A (en) * | 2015-03-25 | 2015-06-17 | 合肥工业大学 | Spherical core-shell structured Al2O3/AlN thermal-conducting powder and high-thermal-conductivity insulating silicone grease and preparation methods thereof |
| CN107141719A (en) * | 2017-05-27 | 2017-09-08 | 中国科学院深圳先进技术研究院 | Filled-type thermally conductive composite and preparation method thereof |
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