CN114276790A - Preparation method of insulating high-thermal-conductivity silicone grease - Google Patents
Preparation method of insulating high-thermal-conductivity silicone grease Download PDFInfo
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 53
- 239000004519 grease Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 114
- 239000002131 composite material Substances 0.000 claims abstract description 81
- 229920002545 silicone oil Polymers 0.000 claims abstract description 34
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000012986 modification Methods 0.000 claims abstract description 17
- 230000004048 modification Effects 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 9
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 9
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 9
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 7
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 6
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 20
- 239000000839 emulsion Substances 0.000 claims description 18
- 238000005507 spraying Methods 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 11
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 11
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000012756 surface treatment agent Substances 0.000 claims description 10
- 239000003963 antioxidant agent Substances 0.000 claims description 9
- 230000003078 antioxidant effect Effects 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 238000005260 corrosion Methods 0.000 claims description 6
- 230000007797 corrosion Effects 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 4
- 125000005609 naphthenate group Chemical group 0.000 claims description 4
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 claims description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 238000005461 lubrication Methods 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011593 sulfur Substances 0.000 claims description 2
- 229910052717 sulfur Inorganic materials 0.000 claims description 2
- 239000000945 filler Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000002103 nanocoating Substances 0.000 abstract description 2
- GVPWHKZIJBODOX-UHFFFAOYSA-N dibenzyl disulfide Chemical compound C=1C=CC=CC=1CSSCC1=CC=CC=C1 GVPWHKZIJBODOX-UHFFFAOYSA-N 0.000 description 8
- 239000003921 oil Substances 0.000 description 6
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- 238000010586 diagram Methods 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000000314 lubricant Substances 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 230000009974 thixotropic effect Effects 0.000 description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229940120693 copper naphthenate Drugs 0.000 description 2
- SEVNKWFHTNVOLD-UHFFFAOYSA-L copper;3-(4-ethylcyclohexyl)propanoate;3-(3-ethylcyclopentyl)propanoate Chemical compound [Cu+2].CCC1CCC(CCC([O-])=O)C1.CCC1CCC(CCC([O-])=O)CC1 SEVNKWFHTNVOLD-UHFFFAOYSA-L 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 2
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- FYKBHPZYQWSXTG-UHFFFAOYSA-L iron(2+);octanoate Chemical compound [Fe+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O FYKBHPZYQWSXTG-UHFFFAOYSA-L 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of insulating high-thermal-conductivity silicone grease, and relates to a preparation method of high-thermal-conductivity silicone grease. The technical problems of poor fluidity and low insulativity of the conventional high-thermal-conductivity composite silicone grease are solved. The method comprises the following steps: taking alumina as a main filler, adding aluminum nitride, boron nitride, silicon nitride and silicon carbide to mix into composite heat-conducting powder; and then the composite heat-conducting powder is subjected to nano coating modification by adopting an organic treating agent, and then is stirred, mixed, dispersed and ground with the silicone oil functional auxiliary agent to obtain the insulating high heat-conducting silicone grease. The addition amount of the powder in the insulating high-thermal-conductivity silicone grease can reach more than 90%, the thermal conductivity coefficient is 4-6W/(m.K), and the insulating high-thermal-conductivity silicone grease has good insulating property and can be used in the field of electronic product manufacturing.
Description
Technical Field
The invention relates to a preparation method of high-thermal-conductivity silicone grease, belonging to the field of thermal interface materials.
Background
With the increasing density, miniaturization and high efficiency of electronic products, the durability of the electronic products is of great importance. However, the electronic products generally have a heat accumulation problem, that is, a large amount of heat energy is generated during the use process, thereby directly affecting the reliability and the service life of the electronic products. There is an increasing need to develop thermal management materials. The heat-conducting silicone grease is used as a paste-shaped thermal interface heat-conducting material, can be used for heat dissipation of heating or heat dissipation elements, has good heat-conducting property, and is often applied to the fields of electronic products and the like. The heat-conducting silicone grease is a grease-like substance filled with a large amount of heat-conducting fillers and containing silicone oil, and has better heat-conducting property. The electronic component is limited by the manufacturing process and the clamping method, a tiny gap is always formed between the heating element and the heat sink, and the heat resistance of air is high, so that the heat dissipation of the electronic component is negatively influenced. The heat-conducting silicone grease has good fluidity and can fill the gap, thereby ensuring the close contact between the electronic element and the radiating fin, increasing the contact area, improving the heat transfer efficiency, further quickly and uniformly transferring the heat generated by the heating element during the work to the radiating fin to the maximum extent, and ensuring the best radiating effect.
At present, a heat-conducting filler of a heat-conducting silicone grease mainly comprises metal powder and metal oxide, but the heat-conducting silicone grease containing metal powder cannot achieve good insulation, so that research and development of a high-heat-conducting powder filler are also key points for preparing high-quality heat-conducting silicone grease, and a patent with the application number of CN10305742. X discloses a high-heat-conducting composite silicone grease and a preparation method thereof, which solve the problem of low heat conductivity of the existing heat-conducting silicone grease.
Disclosure of Invention
The invention provides a preparation method of insulating high-thermal-conductivity silicone grease, aiming at solving the technical problems of poor fluidity and low insulativity of the existing high-thermal-conductivity composite silicone grease. The insulating high-thermal-conductivity silicone grease mainly takes high-thermal-conductivity inorganic composite ceramic powder as a main filler, and is subjected to nano coating modification by adopting an organic treating agent, so that the insulating high-thermal-conductivity silicone grease has good dispersibility and high filling property in a silicone oil system, and is high in thermal conductivity, fine and smooth, good in thixotropic property, good in fluidity and excellent in blade coating effect.
The preparation method of the insulating high-thermal-conductivity silicone grease comprises the following steps:
weighing 85-95 parts of composite heat-conducting powder, 5-15 parts of silicone oil and 0-3 parts of functional auxiliary agent according to the mass part ratio; wherein the composite heat-conducting powder is formed by mixing 50-95% of alumina and 5-50% of auxiliary powder according to the mass percentage, and the auxiliary powder is one or a combination of more of aluminum nitride, boron nitride, silicon nitride and silicon carbide;
secondly, performing surface modification treatment on the composite heat-conducting powder by using a surface treatment agent, namely putting the composite powder into a high-speed mixer with a spraying device, spraying the surface treatment agent in a spraying mode, fully mixing the surface treatment agent with the composite powder, and drying the mixture to obtain modified composite heat-conducting powder with a coated surface; the compatibility of the composite heat-conducting powder and the silicone oil is improved through surface modification treatment, and the oil separation rate is reduced;
adding silicone oil into a planetary stirrer, heating to 40-60 ℃, sequentially adding the surface-coated modified composite heat-conducting powder and the functional auxiliary agent, fully stirring for 30min, starting vacuum to-0.01 MPa, and continuously stirring and dispersing for 2-3 h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Furthermore, the composite heat-conducting powder in the first step comprises a large-particle-size powder with the diameter of 15-30 microns, a medium-particle-size powder with the diameter of 1-10 microns and a small-particle-size powder with the diameter of 0.5-1 microns, wherein the ratio of the large-particle-size powder to the medium-particle-size powder to the small-particle-size powder is (1-3): (6-7): (1-2) performing composite gradation.
Further, the alumina in the first step is one or more of spherical alumina, rhombohedral alumina and flake alumina.
Further, the silicone oil in the first step is dimethyl silicone oil, methyl phenyl silicone oil, chlorohydrocarbon-based modified silicone oil or long-chain alkyl silicone oil.
Furthermore, the viscosity of the silicone oil in the first step is 350 CS-1000 CS.
Further, the functional assistant in the first step is one or more of an antioxidant, a corrosion inhibitor, an antiwear agent and a lubrication promoter.
Further, the antioxidant in the first step is iron octoate.
Further, the corrosion inhibitor in the first step is naphthenate.
Further, the antiwear agent in the first step is a sulfur-containing compound or a phosphorus-containing compound.
Further, the lubricant improver in the first step is mineral oil.
Further, the surface treatment agent in the second step is one or more of KH550, KH560, zinc stearate emulsion and sodium stearate emulsion.
Furthermore, the dosage of the surface treating agent in the step two is 1 to 5 percent of the mass of the composite heat-conducting powder.
The invention has the following advantages:
(1) the heat-conducting silicone grease takes the insulating powder such as alumina, aluminum nitride, boron nitride, silicon carbide and the like as the composite heat-conducting filler, has higher insulating property, and protects the safe use of electronic elements.
(2) The composite heat-conducting filler takes alumina as a main body, and has wide raw material source and lower cost.
(3) The insulating high-thermal-conductivity silicone grease product can be obtained by compounding powder types, grading particle sizes and the like, performing surface coating modification on the powder through a powder modification process, greatly improving the addition amount of the thermal-conductivity powder, enabling the composite thermal-conductivity powder to have good dispersibility and high filling property in a silicone oil system, performing stirring dispersion through a double-planet stirrer, and finally performing dispersion grinding through a three-roll grinder. The addition amount of the powder in the insulating high-thermal-conductivity silicone grease can reach more than 90 percent, the thermal conductivity coefficient is 4-6W/(m.K), and the volume resistivity is 1.07 multiplied by 1013～2.87×1013Omega cm, dielectric constant of 5.0-5.4, and good insulating property. The composite heat-conducting powder has good dispersibility in a silicone oil system and high filling property; the insulating high-heat-conductivity silicone grease has good fineness, good thixotropic property, good fluidity and excellent scraping effect. Can be used for manufacturing electronic productsThe field is as follows.
Description of the drawings:
FIG. 1 is a particle size distribution diagram of the composite thermal conductive powder of example 5.
Detailed Description
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1: the preparation method of the insulating high-thermal-conductivity silicone grease of the embodiment is carried out according to the following steps:
weighing 92 parts of composite heat-conducting powder, 6 parts of dimethyl silicone oil, 1 part of antioxidant iron octoate and 1 part of antiwear agent sulfurized isobutylene according to the mass part ratio;
wherein the composite heat-conducting powder is formed by mixing 70% of spherical alumina, 15% of aluminum nitride, 10% of boron nitride and 5% of silicon carbide according to mass percentage; meanwhile, the composite heat-conducting powder comprises large-particle-size powder with the diameter of 15-30 mu m, medium-particle-size powder with the diameter of 1-10 mu m and small-particle-size powder with the diameter of 0.5-1 mu m according to the mass ratio of 2: 6: 2, carrying out compound grading;
secondly, performing surface modification treatment on the composite heat-conducting powder by using a surface treatment agent KH550, and specifically, putting the composite powder into a high-speed mixer with a spraying device, spraying the KH550 in a spraying mode, fully mixing the KH550 with the composite powder, drying and drying the mixture to obtain modified composite heat-conducting powder with a coated surface, and improving the compatibility of the composite heat-conducting powder and silicone oil through the surface modification treatment to reduce the oil separation rate;
adding 350CS dimethyl silicone oil into a planetary stirrer, heating to 50 ℃, sequentially adding the surface-coated modified composite heat-conducting powder, iron octoate and sulfurized isobutylene, fully stirring for 30min, starting vacuum pumping to-0.01 MPa, and continuously stirring and dispersing for 2h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Example 2: the preparation method of the insulating high-thermal-conductivity silicone grease of the embodiment is carried out according to the following steps:
weighing 91 parts of composite heat-conducting powder, 7 parts of dimethyl silicone oil, 1 part of antioxidant iron octoate, 0.5 part of antiwear agent triethyl phosphate and 0.5 part of lubricant mineral oil according to the mass part ratio;
wherein the composite heat-conducting powder is formed by mixing 50% of spherical alumina, 25% of rhombic alumina, 10% of aluminum nitride, 10% of boron nitride and 5% of silicon nitride according to mass percentage; meanwhile, the composite heat-conducting powder comprises large-particle-size powder with the diameter of 15-30 mu m, medium-particle-size powder with the diameter of 1-10 mu m and small-particle-size powder with the diameter of 0.5-1 mu m according to the mass ratio of 3: 13: 4, carrying out compound grading;
secondly, performing surface modification treatment on the composite heat-conducting powder by using QTT-1036 zinc stearate emulsion with the solid content of 36%, wherein the using amount of the zinc stearate emulsion is 2% of the mass of the composite heat-conducting powder; the specific method is that the composite powder is put into a high-speed mixer with a spraying device, QTT-1036 zinc stearate emulsion is sprayed in a spraying mode and is fully mixed with the composite powder, and the mixture is dried to obtain modified composite heat-conducting powder with a coated surface, and the compatibility of the composite heat-conducting powder and silicone oil is improved through surface modification treatment, so that the oil separation rate is reduced;
adding 350CS dimethyl silicone oil into a planetary stirrer, heating to 50 ℃, sequentially adding the surface-coated modified composite heat-conducting powder, antioxidant iron octoate, anti-wear agent triethyl phosphate and lubricant mineral oil, fully stirring for 30min, starting vacuum pumping to-0.01 MPa, and continuously stirring and dispersing for 2h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Example 3: the preparation method of the insulating high-thermal-conductivity silicone grease of the embodiment is carried out according to the following steps:
weighing 88 parts of composite heat-conducting powder, 9 parts of dimethyl silicone oil, 1 part of antioxidant iron octoate, 1 part of resist naphthenate and 1 part of antiwear agent triphenyl phosphate according to the mass part ratio;
the composite heat conducting powder is formed by mixing 62% of spherical alumina, 13% of aluminum nitride, 12% of boron nitride, 7% of silicon carbide and 6% of silicon nitride according to mass percentage; meanwhile, the composite heat-conducting powder comprises large-particle-size powder with the diameter of 15-30 mu m, medium-particle-size powder with the diameter of 1-10 mu m and small-particle-size powder with the diameter of 0.5-1 mu m according to the mass ratio of 3: 6: 1, carrying out compound grading;
secondly, performing surface modification treatment on the composite heat-conducting powder by using QTT-1036 zinc stearate emulsion with the solid content of 36%, wherein the using amount of the zinc stearate emulsion is 1% of the mass of the composite heat-conducting powder; the specific method is that the composite powder is put into a high-speed mixer with a spraying device, QTT-1036 zinc stearate emulsion is sprayed in a spraying mode and is fully mixed with the composite powder, and the mixture is dried to obtain modified composite heat-conducting powder with a coated surface, and the compatibility of the composite heat-conducting powder and silicone oil is improved through surface modification treatment, so that the oil separation rate is reduced;
adding methyl phenyl silicone oil with the viscosity of 500CS into a planetary stirrer, heating to 50 ℃, sequentially adding the modified composite heat-conducting powder coated on the surface, antioxidant iron octoate, resist naphthenate and antiwear agent triphenyl phosphate, fully stirring for 30min, starting vacuum pumping to-0.01 MPa, and continuously stirring and dispersing for 2h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Example 4: the preparation method of the insulating high-thermal-conductivity silicone grease of the embodiment is carried out according to the following steps:
weighing 92 parts of composite heat-conducting powder, 7 parts of dimethyl silicone oil, 0.5 part of corrosion inhibitor copper naphthenate and 0.5 part of antiwear agent dibenzyl disulfide according to the mass part ratio;
wherein the composite heat-conducting powder is formed by mixing 73% of spherical alumina, 11% of rhombic alumina, 6% of aluminum nitride, 5% of boron nitride and 5% of silicon nitride according to mass percentage; meanwhile, the composite heat-conducting powder comprises large-particle-size powder with the diameter of 15-30 microns, medium-particle-size powder with the diameter of 1-10 microns and small-particle-size powder with the diameter of 0.5-1 microns according to the mass ratio of 1: 7: 2, carrying out compound grading;
firstly, dissolving sodium stearate solid in deionized water at 80 ℃ to prepare sodium stearate emulsion with the solid content of 20%, and then taking the sodium stearate emulsion as a surface modifier to carry out surface modification treatment on the composite powder, wherein the using amount of the sodium stearate emulsion is 2% of the mass of the composite heat-conducting powder; the method comprises the steps of putting the composite powder into a high-speed mixer with a spraying device, spraying sodium stearate emulsion in a spraying mode, fully mixing the sodium stearate emulsion with the composite powder, drying and drying to obtain modified composite heat-conducting powder with a coated surface, improving the compatibility of the composite heat-conducting powder and silicone oil through surface modification treatment, and reducing the oil separation rate;
adding methyl phenyl silicone oil with the viscosity of 350CS into a planetary stirrer, heating to 60 ℃, sequentially adding composite heat-conducting powder, corrosion inhibitor copper naphthenate and antiwear agent dibenzyl disulfide, fully stirring for 30min, starting vacuum pumping to-0.01 MPa, and continuously stirring and dispersing for 2h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Example 5: the preparation method of the insulating high-thermal-conductivity silicone grease of the embodiment is carried out according to the following steps:
weighing 93 parts of composite heat-conducting powder, 6 parts of dimethyl silicone oil, 0.5 part of oxidant iron octoate and 0.5 part of antiwear agent dibenzyl disulfide according to the mass part ratio;
wherein the composite heat-conducting powder is formed by mixing 68% of spherical alumina, 10% of rhombic alumina, 5% of flaky alumina, 10% of aluminum nitride, 5% of boron nitride and 2% of silicon carbide according to mass percentage; meanwhile, the composite heat-conducting powder comprises large-particle-size powder with the diameter of 15-30 mu m, medium-particle-size powder with the diameter of 1-10 mu m and small-particle-size powder with the diameter of 0.5-1 mu m according to the mass ratio of 2: 13: 5 carrying out compound grading;
secondly, performing surface modification treatment on the composite heat-conducting powder by using QTT-1036 zinc stearate emulsion with the solid content of 36%, wherein the using amount of the zinc stearate emulsion is 2% of the mass of the composite heat-conducting powder; the specific method is that the composite powder is put into a high-speed mixer with a spraying device, QTT-1036 zinc stearate emulsion is sprayed in a spraying mode and is fully mixed with the composite powder, and the mixture is dried to obtain modified composite heat-conducting powder with a coated surface, and the compatibility of the composite heat-conducting powder and silicone oil is improved through surface modification treatment, so that the oil separation rate is reduced;
adding the dimethyl silicone oil with the viscosity of 350CS into a planetary stirrer, heating to 50 ℃, then sequentially adding the composite heat-conducting powder, the oxidant iron caprylate and the antiwear agent dibenzyl disulfide, fully stirring for 30min, starting vacuum pumping to-0.01 MPa, and continuously stirring and dispersing for 2h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
Fig. 1 is a particle size distribution diagram of the composite heat-conducting powder in the insulating high heat-conducting silicone grease prepared in example 5, and it can be seen from the diagram that the heat-conducting powder is mainly medium-small particle size powder with a particle size of less than 10 μm, and a compact powder stacking structure is more easily formed.
The insulating high thermal conductive silicone greases obtained in examples 1 to 5 were subjected to performance tests, and the test results are listed in table 1.
Table 1 insulating high thermal conductive silicone grease performance test results
As can be seen from Table 1, the insulating high thermal conductivity silicone grease prepared in the embodiments 1 to 5 has the highest thermal conductivity coefficient of 6.05W/(m.K), low volatility and volume resistivity of 1.07 x 1013～2.87×1013Omega cm, dielectric constant of 5.0-5.4, and good insulating property.
In the insulating high-thermal-conductivity silicone grease prepared in the embodiments 1 to 5, the composite thermal-conductivity powder has good dispersibility in a silicone oil system, the addition amount of the powder can reach more than 90%, and the filling property is high; the insulating high-heat-conductivity silicone grease has good fineness, good thixotropic property, good fluidity and excellent scraping effect.
Claims (10)
1. The preparation method of the insulating high-thermal-conductivity silicone grease is characterized by comprising the following steps of:
weighing 85-95 parts of composite heat-conducting powder, 5-15 parts of silicone oil and 0-3 parts of functional auxiliary agent according to the mass part ratio; wherein the composite heat-conducting powder is formed by mixing 50-95% of alumina and 5-50% of auxiliary powder according to the mass percentage, and the auxiliary powder is one or a combination of more of aluminum nitride, boron nitride, silicon nitride and silicon carbide;
secondly, performing surface modification treatment on the composite heat-conducting powder by using a surface treatment agent, namely putting the composite powder into a high-speed mixer with a spraying device, spraying the surface treatment agent in a spraying mode, fully mixing the surface treatment agent with the composite powder, and drying the mixture to obtain modified composite heat-conducting powder with a coated surface;
adding silicone oil into a planetary stirrer, heating to 40-60 ℃, sequentially adding the surface-coated modified composite heat-conducting powder and the functional auxiliary agent, fully stirring for 30min, starting vacuum to-0.01 MPa, and continuously stirring and dispersing for 2-3 h to obtain a mixture;
and fourthly, dispersing and grinding the mixture for 3 times by using a three-roll grinder to obtain the insulating high-thermal-conductivity silicone grease.
2. The method for preparing the insulating high thermal conductive silicone grease as claimed in claim 1, wherein the alumina is one or more of spherical alumina, rhombic alumina and flake alumina.
3. The preparation method of the insulating high thermal conductive silicone grease according to claim 1 or 2, characterized in that the silicone oil in the step one is dimethyl silicone oil, methylphenyl silicone oil, chlorohydrocarbon-based modified silicone oil or long-chain alkyl silicone oil.
4. The preparation method of the insulating high thermal conductive silicone grease as claimed in claim 1 or 2, characterized in that the viscosity of the silicone oil in the first step is 350 CS-1000 CS.
5. The method for preparing the insulating high thermal conductive silicone grease as claimed in claim 1 or 2, wherein the functional assistant in step one is one or more of an antioxidant, a corrosion inhibitor, an antiwear agent and a lubrication improver.
6. The method as claimed in claim 5, wherein the antioxidant in step one is iron octoate.
7. The method for preparing insulating high thermal conductivity silicone grease according to claim 5, characterized in that the corrosion inhibitor in step one is naphthenate.
8. The method for preparing the insulating high thermal conductivity silicone grease as claimed in claim 5, characterized in that in step one, the antiwear agent is a sulfur-containing compound or a phosphorus-containing compound.
9. The method for preparing the insulating high thermal conductive silicone grease as claimed in claim 1 or 2, wherein the surface treatment agent in step two is one or more of KH550, KH560, zinc stearate emulsion, and sodium stearate emulsion.
10. The preparation method of the insulating high thermal conductive silicone grease according to claim 1 or 2, characterized in that the amount of the surface treatment agent in the second step is 1-5% of the mass of the composite thermal conductive powder.
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