CN114276789B - High-thixotropic silicon-based heat-conducting gel and preparation method thereof - Google Patents
High-thixotropic silicon-based heat-conducting gel and preparation method thereof Download PDFInfo
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 23
- 239000010703 silicon Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000001879 gelation Methods 0.000 title description 2
- 239000000843 powder Substances 0.000 claims abstract description 123
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 55
- 238000000034 method Methods 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 17
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 229920002545 silicone oil Polymers 0.000 claims description 11
- -1 vinyl methyl Chemical group 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000001257 hydrogen Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 7
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003112 inhibitor Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 3
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- 239000012467 final product Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 3
- 239000002345 surface coating layer Substances 0.000 claims description 3
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 3
- 239000011787 zinc oxide Substances 0.000 claims description 3
- 230000009974 thixotropic effect Effects 0.000 abstract description 34
- 238000000576 coating method Methods 0.000 abstract description 9
- 230000001105 regulatory effect Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 7
- 230000001276 controlling effect Effects 0.000 abstract description 7
- 239000011247 coating layer Substances 0.000 abstract description 3
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract 1
- 239000004020 conductor Substances 0.000 abstract 1
- 239000000499 gel Substances 0.000 description 79
- 239000000463 material Substances 0.000 description 28
- 230000000052 comparative effect Effects 0.000 description 15
- 238000004381 surface treatment Methods 0.000 description 8
- 238000004073 vulcanization Methods 0.000 description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000013008 thixotropic agent Substances 0.000 description 6
- BAAAEEDPKUHLID-UHFFFAOYSA-N decyl(triethoxy)silane Chemical compound CCCCCCCCCC[Si](OCC)(OCC)OCC BAAAEEDPKUHLID-UHFFFAOYSA-N 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910021485 fumed silica Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000009472 formulation Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 229910003471 inorganic composite material Inorganic materials 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000009462 micro packaging Methods 0.000 description 1
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- 230000035484 reaction time Effects 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention provides a high-thixotropic silicon-based heat-conducting gel, which belongs to the technical field of heat-conducting materials and comprises heat-conducting powder, wherein the heat-conducting powder contains a linear or branched alkane-based surface coating structure with 3 carbon atoms or more, and the surface grafting rate of the heat-conducting powder ranges from 0.02% to 2.5%. The high thixotropic silicon-based heat-conducting gel provided by the invention directly regulates and controls the thixotropy of the high thixotropic heat-conducting gel by regulating and controlling the coating layer structure and grafting rate of the surface of the heat-conducting powder; has excellent anti-slip performance and can meet the increasingly severe application scene. The invention also provides a preparation method of the high-thixotropic silicon-based heat-conducting gel.
Description
Technical Field
The invention belongs to the technical field of heat conduction materials, and particularly relates to a high-thixotropic silicon-based heat conduction gel and a preparation method thereof.
Background
In recent years, with the rapid development of integration technology and micro-packaging technology, electronic components and electronic devices are being developed toward miniaturization and microminiaturization, and the processing speed of electronic components is continuously increased, so that more heat is generated in a limited volume. This heat can reduce the operating speed of the electronic components and even lead to failure of the electronic equipment. To eliminate such adverse effects caused by heat, the industry typically uses thermal interface materials with high thermal conductivity to transfer the generated heat to the outside of the electronic component. The heat-conducting gel is a flexible thermal interface filling material, has the advantages of high heat conductivity, low interface thermal resistance, low stress, large gap filling tolerance, automatic dispensing and suitability for various different regular shapes, and is widely applied to the fields of LED chips, communication equipment, consumer electronics, memory modules, IGBT, other power modules and power semiconductors.
Despite the above significant advantages of thermally conductive gels, there are still disadvantages: the heat conducting gel is a flexible organic-inorganic composite material, and the conditions of vertical placement, high-low temperature circulation alternate impact and vibration are unavoidable in the use process, so that the conventional heat conducting gel material can slide between the electronic components and the radiator to different degrees, the heat transfer efficiency of a heat conducting interface is obviously reduced, the temperature of the electronic components is further increased, and the stable operation of electronic equipment is influenced.
Researches show that the conventional heat-conducting gel material with low thixotropy has obvious slip tendency in practical application, so that the heat transfer efficiency of a heat-conducting interface is affected, and the technical problem can be effectively avoided by the high-thixotropy heat-conducting gel. In order to improve the anti-slip performance of the heat-conducting gel, some patent and literature data at home and abroad are usually improved by adding a proper amount of thixotropic agent such as fumed silica, hydrogenated castor oil or organic bentonite into the system. However, the thixotropic agent is added to adjust the thixotropic property of the heat-conducting gel, and meanwhile, the viscosity of the heat-conducting gel is increased more obviously as the thixotropic property is stronger, and the viscosity increase directly influences the dispensing process performance of the heat-conducting gel.
Therefore, the development of a thermally conductive gel with high thixotropic properties is still of great importance.
Disclosure of Invention
The invention aims to provide a high-thixotropic silicon-based heat-conducting gel and a preparation method thereof, and aims to solve the technical problems in the prior art that the gel cannot have excellent anti-slip performance and good dispensing technology at the same time.
The invention provides a high thixotropic silicon-based heat conduction gel, which comprises the following components: the heat conducting powder comprises a surface coating layer structure, and the surface grafting rate of the heat conducting powder ranges from 0.02% to 2.5%.
Preferably, the heat conducting powder is composed of a first spherical powder, a second spherical powder and a third spherical powder; the particle size of the first spherical powder is 60-90 mu m; the particle size of the second spherical powder is 10-20 mu m; the particle size of the third spherical powder is 0.5-5 mu m.
Preferably, the volume ratio of the first spherical powder to the second spherical powder to the third spherical powder is 3:2:1.
Preferably, the heat conducting powder is one or more of aluminum oxide, zinc oxide, magnesium oxide, titanium oxide, aluminum nitride, boron nitride, silicon carbide, aluminum powder, copper powder and silver powder.
Preferably, the composition comprises the following components in percentage by mass:
2 to 6 percent of vinyl methyl silicone oil, 1 to 3 percent of methyl hydrogen silicone oil, 90 to 96 percent of heat conducting powder, 0.001 to 0.01 percent of ethynyl cyclohexanol and 0.005 to 0.02 percent of platinum catalyst coordinated by methyl vinyl siloxane.
A preparation method of a high-thixotropic silicon-based heat-conducting gel comprises the following steps:
firstly, modifying heat-conducting powder by using a treating agent to ensure that the surface grafting rate of the heat-conducting powder ranges from 0.02% to 2.5%;
weighing vinyl silicone oil, hydrogen-containing silicone oil, the heat-conducting powder prepared in the first step, an inhibitor and a catalyst according to a preset proportion;
step three, uniformly mixing the raw materials weighed in the step two, wherein the stirring speed is 20-50 rpm, and the stirring time is 30-90 min; and then vulcanizing for 20-40 min at 80-120 ℃ to obtain the final product.
Preferably, the treating agent used in the first step comprises a straight-chain or branched alkyl group having 3 or more carbon atoms.
Preferably, the first step includes the steps of:
preparing the treating agent into an alcohol solution;
dispersing the treating agent on the surface of the powder through a dry method or a wet method, and reacting and grafting the treating agent on the surface of the powder according to a characteristic structure through stepwise addition and multistage temperature control and heating; wherein the temperature of the first step is controlled for 2 to 4 hours at 60 ℃ after the treatment agent is added; the second step of adding the treating agent and then controlling the temperature at 85 ℃ for 3-5 hours; finally, the temperature is controlled for 1 to 2 hours at 120 ℃.
Preferably, the heat conducting powder is composed of a first spherical powder, a second spherical powder and a third spherical powder; the dosage of the treating agent for treating the first spherical powder is 0.1-0.8%, and the surface grafting rate is 0.02-0.05%; the dosage of the treating agent for treating the second spherical powder is 0.15-1.2%, and the surface grafting rate is 0.03-0.12%; the dosage of the treating agent for treating the third spherical powder is 0.2-5%, and the surface grafting rate is 0.10-2.50%.
The high-thixotropic silicon-based heat conduction gel and the preparation method thereof provided by the invention have the beneficial effects that: compared with the prior art, the thixotropy of the high-thixotropy heat-conducting gel is directly regulated and controlled by regulating and controlling the coating layer structure and the grafting rate of the surface of the heat-conducting powder; the thixotropic adjustment of the heat-conducting gel has little influence on the viscosity of the system, so that the heat-conducting gel has high thixotropic property, and meanwhile, the viscosity of the system is not increased, and the dispensing manufacturability of the gel is not influenced. The high-thixotropy heat-conducting gel has excellent anti-slip performance, and can meet increasingly severe application scenes.
In order to make the above objects, features and advantages of the present invention more comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a schematic flow chart of a method for preparing a high thixotropic silicon-based thermally conductive gel used in the prior art.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Referring to fig. 1, a description will now be given of a high thixotropic silicon-based thermally conductive gel provided by the present invention. The high thixotropic silicon-based heat conduction gel comprises the following components: the heat conducting powder contains a surface coating layer structure, and the surface grafting rate of the heat conducting powder ranges from 0.02% to 2.5%.
In this embodiment, the heat conductive powder is composed of a first spherical powder, a second spherical powder, and a third spherical powder; the particle size of the first spherical powder is 60-90 mu m; the particle size of the second spherical powder is 10-20 mu m; the particle size of the third spherical powder is 0.5-5 mu m.
In this embodiment, the volume ratio of the first spherical powder, the second spherical powder, and the third spherical powder is 3:2:1.
In this embodiment, the heat conductive powder is one or more of aluminum oxide, zinc oxide, magnesium oxide, titanium oxide, aluminum nitride, boron nitride, silicon carbide, aluminum powder, copper powder, and silver powder.
In this embodiment, the high thixotropic silicon-based thermally conductive gel comprises the following components in percentage by mass:
2 to 6 percent of vinyl methyl silicone oil, 1 to 3 percent of methyl hydrogen silicone oil, 90 to 96 percent of heat conducting powder, 0.001 to 0.01 percent of ethynyl cyclohexanol and 0.005 to 0.02 percent of platinum catalyst coordinated by methyl vinyl siloxane.
The invention also provides a preparation method of the high thixotropic silicon-based heat conduction gel, referring to fig. 1, comprising the following steps:
s1, modifying heat-conducting powder by using a treating agent to ensure that the surface grafting rate of the heat-conducting powder ranges from 0.02% to 2.5%;
in this step, the treating agent used contains a linear or branched alkyl group having 3 or more carbon atoms.
Step S1 may be implemented by:
preparing the treating agent into an alcohol solution;
treating the treating agent to the surface of the powder by a dry method or a wet method, and reacting and grafting the treating agent to the surface of the powder according to a characteristic structure by step addition and multistage temperature control and heating; wherein the temperature of the first step is controlled for 2 to 4 hours at 60 ℃ after the treatment agent is added; the second step of adding the treating agent and then controlling the temperature at 85 ℃ for 3-5 hours; finally, the temperature is controlled for 1 to 2 hours at 120 ℃.
The heat conducting powder consists of first spherical powder, second spherical powder and third spherical powder; the dosage of the treating agent for treating the first spherical powder is 0.1 to 0.8 percent, and the surface grafting rate is 0.02 to 0.05 percent; the dosage of the treating agent for treating the second spherical powder is 0.15-1.2%, and the surface grafting rate is 0.03-0.12%; the dosage of the treating agent for treating the third spherical powder is 0.2-5%, and the surface grafting rate is 0.10-2.50%.
S2, weighing vinyl silicone oil, hydrogen-containing silicone oil, the heat-conducting powder prepared in the step S1, an inhibitor and a catalyst according to a preset proportion;
s3, uniformly mixing the raw materials weighed in the step S2, wherein the stirring speed is 20-50 rpm, and the stirring time is 30-90 min; and then vulcanizing for 20-40 min at 80-120 ℃ to obtain the final product.
Powder coating: refers to a method for coating a certain functional group or compound by physically or chemically treating the surface of the powder.
Compared with the prior art, the high thixotropic silicon-based heat conduction gel and the preparation method thereof provided by the invention have the advantages that the thixotropic property of the high thixotropic heat conduction gel is directly regulated and controlled by regulating and controlling the coating layer structure and the grafting rate of the surface of the heat conduction powder; the thixotropic adjustment of the heat-conducting gel has little influence on the viscosity of the system, so that the heat-conducting gel has high thixotropic property, and meanwhile, the viscosity of the system is not increased, and the dispensing manufacturability of the gel is not influenced. The thixotropic property of the heat-conducting gel can be adjusted by the type and the amount of the powder surface coating treating agent and the chemical coating process parameters, and the adjustable space is large. The high-thixotropy heat-conducting gel has excellent anti-slip performance and good dispensing technology, and can meet the increasingly severe application scene.
The thixotropic property of the heat-conducting gel is controlled by selecting the type of the treating agent coated on the surface of the heat-conducting powder. The chain segment length of the surface molecules of the heat conducting powder can be regulated and controlled by selecting different kinds of treating agents, and the thixotropic property of the heat conducting gel is regulated and controlled by utilizing the entanglement effect among molecular chains.
The thixotropic property of the heat conducting gel is regulated and controlled by controlling the dosage of the heat conducting powder surface coating treating agent and controlling the coating amount of the heat conducting powder surface treating agent.
The reaction temperature, stirring speed and reaction time are adjusted to control the reaction degree of the treating agent through a specific surface coating process of the heat conducting powder, so that the thixotropic property of the heat conducting gel is adjusted.
The collocation of the heat conducting powder with different particle sizes after the surface coating is adjusted, so that physical or chemical interaction is formed between the powder in the heat conducting gel (large particle size and large particle size powder, small particle size and small particle size powder, large particle size and small particle size powder) so as to generate thixotropic property.
Through a specific formula, vinyl silicone oil, hydrogen-containing silicone oil, heat conducting powder treated by a treating agent and having different particle diameters, an inhibitor and a catalyst are uniformly stirred by planetary dispersion equipment, and high-thixotropic silicon-based heat conducting gel is prepared after vulcanization.
Example 1
Example 1 provides a high thixotropic silicon-based heat conducting gel, the preparation raw materials and parts by weight of which are shown in the formula table 1.
The heat conducting powder is spherical aluminum oxide with median diameters of 1 mu m, 10 mu m and 70 mu m respectively, and the weight ratio of the spherical aluminum oxide to the heat conducting powder is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
and weighing a proper amount of decyl triethoxysilane to prepare a solution, uniformly dividing the solution into two parts, and dispersing the solution to the surface of 100.0g of heat conducting powder step by step.
The amounts of the treating agents for the spherical alumina with the median diameters of 1 μm, 10 μm and 70 μm are 1.2%, 1.0% and 0.5%, respectively;
the heat conducting powder needs to react for 4 hours at 60 ℃ after the first treating agent is added, and needs to react for 4 hours at 85 ℃ after the second treating agent is added, and then is baked for 2 hours at 120 ℃ for standby.
Example 2
Example 2 of the present invention provides a highly thixotropic silicon-based thermally conductive gel, the preparation materials and parts by weight of which are shown in formula table 2.
The heat conducting powder is spherical alumina with median diameters of 0.5 mu m, 10 mu m and 60 mu m respectively, and the weight ratio is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
weighing a proper amount of decyl triethoxysilane to prepare a solution, uniformly dividing the solution into two parts, and dispersing the two parts to the surface of 100.0g of heat conducting powder step by step, wherein the use amounts of the treating agents of the spherical alumina with the median diameters of 0.5 mu m, 10 mu m and 60 mu m are respectively 1.5%, 1.0% and 0.6%;
the heat conducting powder needs to react for 4 hours at 60 ℃ after the first treating agent is added, and needs to react for 4 hours at 85 ℃ after the second treating agent is added, and then is baked for 2 hours at 120 ℃ for standby.
The preparation method comprises the following steps: the materials in the formula table 2 are sequentially added into a planetary dispersing machine, the stirring speed is set to be 30rpm, the materials are mixed for 60min, the materials are continuously stirred for 20min under vacuum, and then the materials are placed into a 120 ℃ oven for vulcanization for 30min, so that the heat-conducting gel product is obtained.
Example 3
Example 3 provides a highly thixotropic silicon-based thermally conductive gel, the preparation raw materials and parts by weight of which are shown in formula table 3.
The heat conducting powder is spherical aluminum oxide with median diameters of 5 mu m, 20 mu m and 90 mu m respectively, and the weight ratio of the spherical aluminum oxide to the heat conducting powder is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
weighing a proper amount of decyl triethoxysilane to prepare a solution, dispersing the solution on the surface of 100.0g of heat conducting powder, wherein the dosage of the treating agents of spherical aluminum oxide with the median diameters of 5 mu m, 20 mu m and 90 mu m is 1.5%, 0.8% and 0.3% respectively;
the heat conducting powder needs to react for 4 hours at 60 ℃ after the first treating agent is added, and needs to react for 4 hours at 85 ℃ after the second treating agent is added, and then is baked for 2 hours at 120 ℃ for standby.
The preparation method comprises the following steps: the materials in the formula table 3 are sequentially added into a planetary dispersing machine, the stirring speed is set to be 30rpm, the materials are mixed for 60min, the materials are continuously stirred for 20min under vacuum, and then the materials are placed into a 120 ℃ oven for vulcanization for 30min, so that the heat-conducting gel product is obtained.
Comparative example 1
Comparative example 1 provides a thermally conductive gel whose raw materials and parts by weight are shown in formulation table 4.
The heat conducting powder is spherical aluminum oxide with median diameters of 1 mu m, 10 mu m and 70 mu m respectively, and the weight ratio of the spherical aluminum oxide to the heat conducting powder is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
weighing a proper amount of vinyl trimethoxy silane to prepare a solution, uniformly dividing the solution into two parts, and dispersing the two parts to the surface of 100.0g of heat conduction powder step by step, wherein the use amounts of the treating agents of the spherical aluminum oxide with the median diameters of 1 mu m, 10 mu m and 70 mu m are respectively 1.2%, 1.0% and 0.5%;
the heat conducting powder needs to react for 4 hours at 60 ℃ after the first treating agent is added, and needs to react for 4 hours at 85 ℃ after the second treating agent is added, and then is baked for 2 hours at 120 ℃ for standby.
The preparation method comprises the following steps: the materials in the formula table 4 are sequentially added into a planetary dispersing machine, the stirring speed is set to be 30rpm, the materials are mixed for 60min, the materials are continuously stirred for 20min under vacuum, and then the materials are placed into a 120 ℃ oven for vulcanization for 30min, so that the heat-conducting gel product is obtained.
Comparative example 2 provides a thermally conductive gel whose preparation materials and parts by weight are shown in formulation table 5.
The heat conducting powder is spherical aluminum oxide with median diameters of 1 mu m, 10 mu m and 70 mu m respectively, and the weight ratio of the spherical aluminum oxide to the heat conducting powder is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
weighing a proper amount of decyl triethoxysilane to prepare an alcohol solution, uniformly dispersing the alcohol solution on the surface of 100.0g of heat conducting powder, wherein the dosage of the treating agents of spherical alumina with the median diameters of 1 mu m, 10 mu m and 70 mu m is 1.2%, 1.0% and 0.5% respectively;
and (3) placing the heat conducting powder in an environment of 85 ℃ for reaction for 4 hours, and drying for standby.
The preparation method of the heat-conducting gel comprises the following steps: the materials in the formula table 5 are sequentially added into a planetary dispersing machine, the stirring speed is set to be 30rpm, the materials are mixed for 60min, the materials are continuously stirred for 20min under vacuum, and then the materials are placed into a 120 ℃ oven for vulcanization for 30min, so that the heat-conducting gel product is obtained.
Comparative example 3
Comparative example 3 provides a thermally conductive gel whose preparation raw materials and parts by weight are shown in formula table 6.
The heat conducting powder is spherical alumina with median diameters of 0.5 mu m, 10 mu m and 60 mu m respectively, and the weight ratio is 1:2:3.
The surface treatment process of the heat conducting powder comprises the following steps:
weighing a proper amount of decyl triethoxysilane to prepare a solution, uniformly dividing the solution into two parts, and dispersing the two parts to the surface of 100.0g of heat conducting powder step by step, wherein the use amounts of the treating agents of the spherical alumina with the median diameters of 0.5 mu m, 10 mu m and 60 mu m are respectively 0.5%, 0.3% and 0.1%;
the heat conducting powder needs to react for 4 hours at 60 ℃ after the first treating agent is added, and needs to react for 4 hours at 85 ℃ after the second treating agent is added, and then is baked for 2 hours at 120 ℃ for standby.
The preparation method comprises the following steps: sequentially adding the materials in the formula table 6 into a planetary dispersing machine, mixing for 60min at a stirring speed of 30rpm, continuously stirring for 20min under vacuum, and then putting into a 120 ℃ oven for vulcanization for 30min to obtain the heat-conducting gel.
Comparative example 4 (addition of thixotropic agent)
Comparative example 4 provides a thermally conductive gel whose raw materials and parts by weight are shown in formulation table 7.
The heat conducting powder is spherical aluminum oxide with median diameters of 1 mu m, 10 mu m and 70 mu m respectively, and the weight ratio of the spherical aluminum oxide to the heat conducting powder is 1:2:3.
The surface of the heat conducting powder is not treated.
The thixotropic agent is fumed silica.
The preparation method comprises the following steps: the materials in the formula table 7 are sequentially added into a planetary dispersing machine, the stirring speed is set to be 30rpm, the materials are mixed for 60min, the materials are continuously stirred for 20min under vacuum, and then the materials are placed into a 120 ℃ oven for vulcanization for 30min, so that the heat-conducting gel is obtained.
Comparative example 5
Comparative example 5 is substantially the same as comparative example 4 except that no thixotropic fumed silica is added to comparative example 5.
The heat conductive gel samples obtained in examples 1 to 3 and comparative examples 1 to 5 were subjected to thixotropic index test, slip resistance test and dispensing process performance test, and the evaluation methods were as follows:
thixotropic index test: the heat conductive gels obtained in examples 1 to 3 and comparative examples 1 to 5 were respectively tested by a rheometer to have gel shear rates of 1s -1 And 10s -1 The greater the thixotropic index, the greater the thixotropic properties of the sample, and the easier the reaction sample will remain in its original structural state under the influence of shear stress.
Slip resistance test: the heat conductive gels obtained in examples 1 to 3 and comparative examples 1 to 5 were sandwiched between an aluminum tool having a surface roughness of 3.20 μm.+ -. 0.20 μm and a glass plate, respectively, and the thickness and diameter of the sample were controlled to be 1.00mm and 20.00mm, respectively, and were placed vertically in a temperature cycle box at-40 to 85 ℃ for 1000 hours (wherein the temperature rise and fall stages and the high and low temperature holding stages were each set to 15 minutes and one cycle was 60 minutes), and the anti-slip properties of the gels were observed. And if the gel slides, measuring the sliding distance of the gel, and evaluating the anti-sliding performance of the gel according to the sliding distance of the gel. ( Anti-slip properties: the gel is used for guiding the anti-gravity capability of the thermal gel in the high-low temperature cycle alternate impact or the anti-slip capability of the gel in the impact, and the gel which is generally less prone to slip indicates that the better the performance is, the higher the heat conduction efficiency is )
And (3) testing the performance of the dispensing process: the heat conductive gels obtained in examples 1 to 3 and comparative examples 1 to 5 were respectively packed in standard 30 CC EDF tubes having a gel outlet diameter of 2.45mm, and the gel outlet weight of the gel under a pressure of 90PSI for 60 seconds was measured to measure the manufacturability of the gel by the gel outlet amount. ( Dispensing manufacturability: the method is used for guiding the dispensing capability of the thermal gel on dispensing equipment in actual application, and is often evaluated by the dispensing speed, the dispensing quantity, the dispensing shape and the like )
From the test results shown in Table 8, it can be seen that: the type of the treating agent, the dosage of the treating agent and the surface treatment process of the heat conducting powder have obvious influence on the thixotropic property, the anti-slip property and the dispensing manufacturability of the heat conducting gel. The thixotropic agent fumed silica can improve the thixotropic property of the heat-conducting gel to a certain extent, but the process performance of dispensing is sacrificed. The heat conducting gel which is not subjected to surface treatment and is not added with thixotropic agent has poor anti-slip performance and poor dispensing manufacturability. The heat-conducting gel prepared by the invention has the characteristics of high thixotropy, good anti-slip property and good dispensing manufacturability.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art can easily think about variations or alternatives within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. A preparation method of silicon-based heat conduction gel is characterized in that: the heat conducting powder comprises a surface coating layer structure, wherein the surface grafting rate of the heat conducting powder ranges from 0.02% to 2.5%;
the heat conducting powder consists of first spherical powder with the surface grafting rate of 0.02-0.05% of the treating agent, second spherical powder with the surface grafting rate of 0.03-0.12% of the treating agent and third spherical powder with the surface grafting rate of 0.10-2.50% of the treating agent; the particle size of the first spherical powder is 60-90 mu m; the particle size of the second spherical powder is 10-20 mu m; the particle size of the third spherical powder is 0.5-5 mu m; the heat conducting powder is one or more of aluminum oxide, zinc oxide, magnesium oxide, titanium oxide, aluminum nitride, boron nitride, silicon carbide, aluminum powder, copper powder and silver powder;
firstly, modifying heat-conducting powder by using a treating agent to ensure that the surface grafting rate of the heat-conducting powder ranges from 0.02% to 2.5%; the treating agent used in the first step comprises a linear or branched alkyl group having 3 or more carbon atoms; step one comprises the following steps:
preparing the treating agent into an alcohol solution;
dispersing the treating agent on the surface of the powder through a dry method or a wet method, and reacting and grafting the treating agent on the surface of the powder according to a characteristic structure through stepwise addition and multistage temperature control and heating; wherein the temperature of the first step is controlled for 2 to 4 hours at 60 ℃ after the treatment agent is added; the second step of adding the treating agent and then controlling the temperature at 85 ℃ for 3-5 hours; finally controlling the temperature at 120 ℃ for 1-2 h;
weighing vinyl silicone oil, hydrogen-containing silicone oil, the heat-conducting powder prepared in the first step, an inhibitor and a catalyst according to a preset proportion;
step three, uniformly mixing the raw materials weighed in the step two, wherein the stirring speed is 20-50 rpm, and the stirring time is 30-90 min; and then vulcanizing for 20-40 min at 80-120 ℃ to obtain the final product.
2. The method for preparing the silicon-based heat-conducting gel as claimed in claim 1, wherein: the volume ratio of the first spherical powder to the second spherical powder to the third spherical powder is 3:2:1.
3. The preparation method of the silicon-based heat-conducting gel as claimed in claim 1, which is characterized by comprising the following components in percentage by mass:
2 to 6 percent of vinyl methyl silicone oil, 1 to 3 percent of methyl hydrogen silicone oil, 90 to 96 percent of heat conducting powder, 0.001 to 0.01 percent of ethynyl cyclohexanol and 0.005 to 0.02 percent of platinum catalyst coordinated by methyl vinyl siloxane.
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