CN115838535A - Bi-component heat-conducting gel and preparation method thereof - Google Patents
Bi-component heat-conducting gel and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title abstract description 23
- 238000001879 gelation Methods 0.000 title description 2
- 229920002545 silicone oil Polymers 0.000 claims abstract description 124
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 79
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 79
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 66
- 239000001257 hydrogen Substances 0.000 claims abstract description 66
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 61
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 44
- 239000003054 catalyst Substances 0.000 claims abstract description 35
- 239000000843 powder Substances 0.000 claims abstract description 26
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims description 40
- 238000002156 mixing Methods 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 230000009471 action Effects 0.000 claims description 4
- 238000006459 hydrosilylation reaction Methods 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 2
- VMAWODUEPLAHOE-UHFFFAOYSA-N 2,4,6,8-tetrakis(ethenyl)-2,4,6,8-tetramethyl-1,3,5,7,2,4,6,8-tetraoxatetrasilocane Chemical compound C=C[Si]1(C)O[Si](C)(C=C)O[Si](C)(C=C)O[Si](C)(C=C)O1 VMAWODUEPLAHOE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 11
- 230000032683 aging Effects 0.000 abstract description 14
- 238000011417 postcuring Methods 0.000 abstract description 9
- 230000008859 change Effects 0.000 abstract description 3
- 239000000499 gel Substances 0.000 description 47
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002994 raw material Substances 0.000 description 7
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 238000003878 thermal aging Methods 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 125000003944 tolyl group Chemical group 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- INASARODRJUTTN-UHFFFAOYSA-N 3-methyldodec-1-yn-3-ol Chemical compound CCCCCCCCCC(C)(O)C#C INASARODRJUTTN-UHFFFAOYSA-N 0.000 description 1
- DTGUZRPEDLHAAO-UHFFFAOYSA-N 3-methylhex-1-yn-3-ol Chemical compound CCCC(C)(O)C#C DTGUZRPEDLHAAO-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- -1 phenyl vinyl Chemical group 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Classifications
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- 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 discloses a bi-component heat-conducting gel and a preparation method thereof. The bi-component heat-conducting gel comprises a component A and a component B, wherein the component A comprises the following components in parts by weight and a platinum catalyst: 100 parts of branched vinyl silicone oil and 500-1500 parts of heat-conducting powder; the content of the platinum catalyst is 5ppm to 15ppm by mass of platinum; the component B comprises the following components in parts by weight: 100 parts of branched vinyl silicone oil, 20-80 parts of branched hydrogen-containing silicone oil, 500-2000 parts of heat-conducting powder and 0.01-0.3 part of inhibitor. The bi-component heat-conducting gel has excellent heat aging reliability, and has the advantages of small hardness change, low thermal resistance rise, no post-curing phenomenon and excellent heat aging resistance after 150 ℃/1000h heat aging test.
Description
Technical Field
The invention relates to the technical field of heat-conducting gel, in particular to bi-component heat-conducting gel and a preparation method thereof.
Background
Along with the continuous increase of the power of electronic devices, the heat dissipation problem becomes an increasingly critical problem in the electronic industry, and novel heat dissipation materials are continuously emerging. Due to the excellent aging resistance of the organic silicon, the organic silicon heat conduction material occupies an important position in the field of heat dissipation materials. Silicone thermal gels are attractive as a new thermal interface material due to the advantages of both thermally conductive gaskets and thermally conductive silicone greases. From the current application form, the silicone heat-conducting gel is mainly divided into a single-component heat-conducting gel and a two-component heat-conducting gel. The double-component heat-conducting gel is in a double-agent/double-pipe packaging form, the component A and the component B are vulcanized after being mixed and dispensed through the mixing pipe, and the double-component heat-conducting gel has a certain bonding and fixing effect because the compression stress is low and a soft rubber state is formed after vulcanization, and is very widely applied to the field of new energy automobiles.
The crosslinking density of the bi-component heat-conducting gel is far greater than that of the single-component heat-conducting gel, so that the problem of serious oil leakage/oil outflow does not exist after the bi-component heat-conducting gel is cured, but the high-temperature aging reliability of the bi-component heat-conducting gel is always a pain point in the industry, namely, the hardness is increased due to high-temperature baking, so that the contact thermal resistance of a heat dissipation interface is greatly improved, and the heat dissipation reliability is seriously influenced. CN115216154A discloses a heat-stable two-component heat-conducting gel and a preparation method thereof, wherein phenyl vinyl silicone oil is adopted, compared with common vinyl silicone oil, phenyl-containing vinyl silicone oil has higher high-temperature resistance, aging resistance and yellowing resistance, and the heat stability of the heat-conducting gel can be effectively improved. But the patent does not disclose high temperature durability data. CN113773649A discloses a high-reliability low-viscosity high-heat-conductivity heat-conducting gel, a preparation method and an application thereof, wherein a novel silane coupling agent with large molecular weight is added to prepare the heat-conducting gel, so that volatilization caused by working at high temperature can be effectively reduced, and a more stable high-reliability low-viscosity high-heat-conductivity heat-conducting gel is prepared. However, the patent only discloses a volatile content of 125 ℃/48h, and the hardness, thermal resistance and the like of the heat-conducting gel after long-term aging are not evaluated.
From the prior published documents, the thermal aging problem of the thermal conductive gel is generally improved by a novel powder modifier or an anti-aging agent, but the bi-component thermal conductive gel also has the post-curing problem (namely, the hardness is increased by further vulcanizing through high-temperature baking after vulcanization), and if the cross-linking system is not properly designed, the post-curing problem is serious, so that the thermal conductive gel is hardened and ceramized, and the thermal conductive gel loses flexibility, so that the thermal resistance is rapidly increased.
Disclosure of Invention
The invention aims to provide a bi-component heat-conducting and heat-conducting gel which has no problem of post-curing and has excellent heat-aging resistance.
In order to achieve the above object, the present invention includes the following technical solutions.
A two-component heat-conducting gel comprises a component A and a component B,
the component A comprises the following components in parts by weight and a platinum catalyst:
branched vinyl silicone oil 100 parts
500-1500 parts of heat-conducting powder;
the content of the platinum catalyst is 5ppm to 15ppm by mass of platinum;
the component B comprises the following components in parts by weight:
branched vinyl silicone oil 100 parts
20 to 80 portions of branched hydrogen-containing silicone oil
500-2000 parts of heat-conducting powder
0.01 to 0.3 portion of inhibitor;
the structure of the branched vinyl silicone oil is as follows:
the structure of the branched hydrogen-containing silicone oil is as follows:
in some of these embodiments, the mass ratio of the a component to the B component is 1:0.5 to 1.5.
In some of these embodiments, the mass ratio of the a component to the B component is 1:0.8 to 1.2.
In some embodiments, the branched vinyl silicone oil is a terminal vinyl silicone oil and a side hydrogen-containing silicone oil prepared by a hydrosilylation reaction under the action of a platinum catalyst, and the reaction formula is as follows:
in some embodiments, the mass ratio of the terminal vinyl silicone oil to the side hydrogen-containing silicone oil is 5 to 6:1.
in some of these embodiments, the vinyl-terminated silicone oil has a vinyl content of 0.5wt% to 1.5wt%; the viscosity of the lateral hydrogen-containing silicone oil is 50 cP-500 cP, and the hydrogen content is 0.05wt% -0.2 wt%.
In some of the embodiments, the vinyl-terminated silicone oil has a vinyl content of 0.8wt% to 1.2wt%; the viscosity of the lateral hydrogen-containing silicone oil is 80 cP-200 cP, and the hydrogen content is 0.08wt% -0.12 wt%.
In some of these embodiments, the vinyl-terminated silicone oil has a vinyl content of 1wt%; the viscosity of the lateral hydrogen-containing silicone oil is 90 cP-150 cP, and the hydrogen content is 0.1wt%.
In some of these embodiments, the branched vinyl silicone oil has a viscosity of 200cP to 2000cP and a vinyl content of 0.1wt% to 1wt%.
In some of these embodiments, the branched vinyl silicone oil has a viscosity of 500cP to 1000cP and a vinyl content of 0.3wt% to 0.5wt%.
In some of these embodiments, the branched vinyl silicone oil has a viscosity of 800cP to 900cP and a vinyl content of 0.4wt%.
In some of the embodiments, the preparation method of the branched vinyl silicone oil comprises the following steps:
adding the side hydrogen-containing silicone oil, the platinum catalyst and the solvent into a reaction bottle, uniformly stirring, dripping the vinyl-terminated silicone oil, heating to 70-90 ℃ after dripping, and reacting for 0.8-2 h to obtain the catalyst.
In some of these embodiments, the solvent is toluene.
In some embodiments, the branched hydrogen-containing silicone oil is prepared by hydrosilylation reaction of terminal hydrogen-containing silicone oil and side vinyl silicone oil under the action of a platinum catalyst, and the reaction formula is as follows:
in some embodiments, the mass ratio of the terminal hydrogen-containing silicone oil to the side vinyl silicone oil is 1:2 to 3.
In some of these embodiments, the side vinyl silicone oil has a viscosity of 100cP to 500cP and a vinyl content of 0.3wt% to 1.0wt%; the hydrogen content of the hydrogen-terminated silicone oil is 0.1wt% -0.3 wt%.
In some of these embodiments, the side vinyl silicone oil has a viscosity of 150cP to 300cP and a vinyl content of 0.4wt% to 0.6wt%; the hydrogen content of the hydrogen-terminated silicone oil is 0.15wt% -0.25 wt%.
In some of these embodiments, the side vinyl silicone oil has a viscosity of 180cP to 250cP and a vinyl content of 0.5wt%; the hydrogen content of the terminal hydrogen-containing silicone oil is 0.2wt%.
In some embodiments, the branched hydrogen-containing silicone oil has a viscosity of 200cP to 1000cP and a hydrogen content of 0.03wt% to 0.15wt%.
In some embodiments, the branched hydrogen-containing silicone oil has a viscosity of 500cP to 700cP and a hydrogen content of 0.02wt% to 0.04wt%.
In some of these embodiments, the branched hydrogen-containing silicone oil has a viscosity of 550cP to 650cP and a hydrogen content of 0.03wt%.
In some of these embodiments, the method of preparing the branched hydrogen-containing silicone oil comprises the steps of:
and adding the side vinyl silicone oil, the platinum catalyst and the solvent into a reaction bottle, uniformly stirring, dripping the hydrogen-containing silicone oil into the reaction bottle, heating to 70-90 ℃ after dripping, and reacting for 0.8-2 hours to obtain the catalyst.
In some of these embodiments, the solvent is toluene.
In some embodiments, the heat conductive powder is one or a combination of aluminum oxide, zinc oxide, magnesium oxide, aluminum nitride and boron nitride.
In some of these embodiments, the platinum catalyst is one or a combination of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and a kast catalyst.
In some of these embodiments, the inhibitor is one or a combination of 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butyn-2-ol, 3-methyl-1-hexyn-3-ol, 3, 5-dimethyl-1-hexyn-3-ol, and 3-methyl-1-dodecyn-3-ol.
The invention also provides a preparation method of the bi-component heat-conducting gel, which comprises the following technical scheme.
The preparation method of the bi-component heat-conducting gel comprises the following steps:
(1) Putting the branched vinyl silicone oil and the platinum catalyst into a planetary stirrer, stirring for 5-10 min, uniformly mixing, then putting the heat-conducting powder in batches, and stirring for 20-30 min after putting until uniformly mixing to obtain a component A;
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 5-10 min, then putting the heat-conducting powder in batches, and stirring for 20-30 min after putting until the components are uniformly mixed to obtain the component B.
The invention has the following beneficial effects:
the invention synthesizes novel branched vinyl silicone oil and branched hydrogen-containing silicone oil, further adopts the branched vinyl silicone oil to replace the traditional terminal vinyl silicone oil as a vinyl component, adopts the branched hydrogen-containing silicone oil to replace the traditional side hydrogen-containing silicone oil as a cross-linking agent component, and prepares the bi-component heat-conducting gel which has no post-curing and excellent thermal aging reliability under the coordination of a certain dosage. The branched vinyl silicone oil is adopted to replace the traditional terminal vinyl silicone oil as the vinyl component, so that the reactivity of the vinyl component is improved, and the branched vinyl silicone oil can react with the hydrogen-containing vinyl silicone oil more quickly; the branched hydrogen-containing silicone oil is adopted to replace the traditional lateral hydrogen-containing silicone oil as a cross-linking agent component, so that the problems of concentration and reaction blockage of Si-H active groups of the lateral hydrogen-containing silicone oil can be avoided, and the Si-H groups can be fully reacted in a short time without generating the problem of high-temperature post-curing. The invention adopts a novel curing system, and under the synergistic cooperation of the branched vinyl silicone oil and the branched hydrogen-containing silicone oil, the obtained bi-component heat-conducting gel has excellent heat aging reliability, and the thermal aging test at 150 ℃/1000h shows that the bi-component heat-conducting gel has small hardness change, low rise of thermal resistance, no post-curing phenomenon and excellent heat aging resistance.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusions. For example, a process, method, apparatus, article, or device that comprises a list of steps is not limited to only those steps or modules listed, but may alternatively include other steps not listed or inherent to such process, method, article, or device.
The "plurality" referred to in the present invention means two or more. "and/or" describes the association relationship of the associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a exists alone, A and B exist simultaneously, and B exists alone. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
The viscosity in the invention refers to the viscosity under the test condition of 25 ℃.
In the following examples, the content of the Kanst catalyst is based on the mass of platinum.
Example 1 preparation of branched vinyl Silicone oils
Wherein Vi means vinyl.
a: 100 parts of lateral hydrogen-containing silicone oil having a viscosity of 100cP and a hydrogen content of 0.1wt%, 5ppm (in terms of Pt content) of a Kaster catalyst and 500 parts of toluene were charged in a three-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, and stirred uniformly;
b: slowly dripping 550 parts of vinyl-terminated silicone oil with the vinyl content of 1.0wt% into the mixed solution, and heating to 80 ℃ for reflux reaction for 1h after dripping;
c: after the reaction is finished, evaporating to remove toluene, and adsorbing by activated carbon to remove the catalyst to obtain branched vinyl silicone oil; the viscosity was determined to be 850cP with a vinyl content of 0.4wt%.
Example 2 preparation of branched Hydrogen-containing Silicone oils
Wherein Vi means vinyl.
a: 100 parts of side vinyl silicone oil having a viscosity of 200cP and a vinyl content of 0.5wt%, 5ppm (in terms of Pt content) of a Kaster catalyst and 200 parts of toluene were charged in a three-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, and stirred uniformly;
b: slowly dripping 40 parts of hydrogen-terminated silicone oil with the hydrogen content of 0.2wt% into the mixed solution, and heating to 80 ℃ for reflux reaction for 1h after dripping;
c: after the reaction is finished, evaporating to remove toluene, and adsorbing by activated carbon to remove the catalyst to obtain branched hydrogen-containing silicone oil; the viscosity was determined to be 600cP with a hydrogen content of 0.03wt%.
EXAMPLE 3 preparation of two-component thermally conductive gel
The two-component heat-conducting gel prepared in the embodiment comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the branched vinyl silicone oil and the Kanster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, putting the heat-conducting powder in batches, and stirring for 30min after putting until the mixture is uniformly mixed to obtain the component A.
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1.
EXAMPLE 4 preparation of two-component thermally conductive gel
The two-component heat-conducting gel prepared in the embodiment comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the branched vinyl silicone oil and the Kanster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, putting the heat-conducting powder in batches, and stirring for 30min after putting until the mixture is uniformly mixed to obtain the component A.
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When the paint is used, the component A and the component B are mixed according to the mass ratio of 1.
EXAMPLE 5 preparation of two-component thermally conductive gel
The two-component heat-conducting gel prepared in the embodiment comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the branched vinyl silicone oil and the Kanster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, putting the heat-conducting powder in batches, and stirring for 30min after putting until the mixture is uniformly mixed to obtain the component A.
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1.
EXAMPLE 6 preparation of two-component thermally conductive gel
The two-component heat-conducting gel prepared in the embodiment comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the branched vinyl silicone oil and the Kanster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, putting the heat-conducting powder in batches, and stirring for 30min after putting until the mixture is uniformly mixed to obtain the component A.
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1.
EXAMPLE 7 preparation of two-component thermally conductive gel
The two-component heat-conducting gel prepared in the embodiment comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the branched vinyl silicone oil and the Kanster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, putting the heat-conducting powder in batches, and stirring for 30min after putting until the mixture is uniformly mixed to obtain the component A.
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1.
Comparative example 1
The two-component heat-conducting gel prepared by the comparative example comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the vinyl-terminated silicone oil and the Kaster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, then putting the heat-conducting powder in batches, and stirring for 30min after the putting till uniform mixing to obtain the component A.
(2) And putting the vinyl-terminated silicone oil, the lateral hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When the paint is used, the component A and the component B are mixed according to the mass ratio of 1.
Comparative example 2
The two-component heat-conducting gel prepared by the comparative example comprises the following raw materials:
the preparation method comprises the following steps:
(1) And (3) putting the vinyl-terminated silicone oil and the Kaster catalyst into a planetary stirrer, stirring for 10min, uniformly mixing, then putting the heat-conducting powder in batches, and stirring for 30min after the putting till uniform mixing to obtain the component A.
(2) And putting the vinyl-terminated silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 10min, then putting the heat-conducting powder in batches, and stirring for 30min after putting till mixing uniformly to obtain the component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1.
The thermally conductive gels prepared in the above examples and comparative examples were mixed at a mass ratio of component a to component B of 1, vulcanized at 120 ℃/30min, and tested for hardness, which was an initial hardness, followed by aging at 150 ℃/1000h, and the change in hardness during aging was measured with reference to astm d2240standard test method for rubber property-durometer hardness, using a shore 00 durometer and shore a durometer.
The detection results are as follows:
the results in the table show that the hardness of the thermal conductive gels prepared in examples 3-7 does not increase more than 10 Shore 00 after aging at 150 ℃/1000h, and no post-curing problem exists. The difference between the comparative example 1 and the example 5 is that the traditional crosslinking system is adopted, the terminal vinyl silicone oil and the side hydrogen-containing silicone oil are used, the final hardness of the obtained heat-conducting gel after aging is increased to 45 Shore A, and the post-curing is very serious; comparative example 2 is a thermal conductive gel in which the hardness of the thermal conductive gel after aging is also increased to some extent by using terminal vinyl silicone oil as a vinyl component and using branched hydrogen-containing silicone oil, but the increase is significantly reduced compared to comparative example 1.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The bi-component heat-conducting gel is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight:
branched vinyl silicone oil 100 parts
500-1500 parts of heat-conducting powder;
the content of the platinum catalyst is 5ppm to 15ppm by mass of platinum;
the component B comprises the following components in parts by weight:
the structure of the branched vinyl silicone oil is as follows:
the structure of the branched hydrogen-containing silicone oil is as follows:
2. the two-component thermally conductive gel of claim 1, wherein the mass ratio of the a component to the B component is 1:0.5 to 1.5.
3. The two-component heat-conducting gel of claim 1, wherein the branched vinyl silicone oil is a terminal vinyl silicone oil and a side hydrogen-containing silicone oil, which are prepared by a hydrosilylation reaction under the action of a platinum catalyst, and the reaction formula is as follows:
4. the two-component heat-conducting gel according to claim 3, wherein the mass ratio of the terminal vinyl silicone oil to the side hydrogen-containing silicone oil is 5-6: 1; and/or the presence of a gas in the gas,
the vinyl content of the vinyl-terminated silicone oil is 0.5 to 1.5 weight percent; the viscosity of the lateral hydrogen-containing silicone oil is 50 cP-500 cP, and the hydrogen content is 0.05wt% -0.2 wt%; and/or the presence of a gas in the gas,
the viscosity of the branched vinyl silicone oil is 200 cP-2000 cP, and the vinyl content is 0.1wt% -1 wt%.
5. The two-component thermally conductive gel of claim 3, wherein the branched vinyl silicone oil is prepared by a method comprising the steps of:
adding the side hydrogen-containing silicone oil, the platinum catalyst and the solvent into a reaction bottle, uniformly stirring, dripping the vinyl-terminated silicone oil, heating to 70-90 ℃ after dripping, and reacting for 0.8-2 h to obtain the catalyst.
6. The two-component heat-conducting gel of claim 1, wherein the branched hydrogen-containing silicone oil is prepared by hydrosilylation reaction of terminal hydrogen-containing silicone oil and side vinyl silicone oil under the action of a platinum catalyst, and the reaction formula is as follows:
7. the two-component thermal conductive gel of claim 6, wherein the mass ratio of the terminal hydrogen-containing silicone oil to the side vinyl silicone oil is 1:2 to 3; and/or the presence of a gas in the gas,
the viscosity of the side vinyl silicone oil is 100 cP-500 cP, and the vinyl content is 0.3wt% -1.0 wt%; the hydrogen content of the hydrogen-terminated silicone oil is 0.1-0.3 wt%; and/or the presence of a gas in the atmosphere,
the viscosity of the branched hydrogen-containing silicone oil is 200 cP-1000 cP, and the hydrogen content is 0.03wt% -0.15 wt%.
8. The two-component thermally conductive gel of claim 6, wherein the branched hydrogen-containing silicone oil is prepared by a method comprising the steps of:
and adding the side vinyl silicone oil, the platinum catalyst and the solvent into a reaction bottle, uniformly stirring, dripping the hydrogen-containing silicone oil into the reaction bottle, heating to 70-90 ℃ after dripping, and reacting for 0.8-2 hours to obtain the catalyst.
9. The two-component thermal conductive gel according to any one of claims 1 to 8, wherein the thermal conductive powder is one or a combination of aluminum oxide, zinc oxide, magnesium oxide, aluminum nitride and boron nitride; and/or the presence of a gas in the gas,
the platinum catalyst is one or the combination of chloroplatinic acid, chloroplatinic acid-isopropanol complex and a Kaster catalyst; and/or the presence of a gas in the gas,
the inhibitor is one or the combination of 1-ethynyl-1-cyclohexanol, tetramethyl tetravinylcyclotetrasiloxane, 2-methyl-3-butynyl-2-ol, 3-methyl-1-hexynyl-3-ol, 3, 5-dimethyl-1-hexynyl-3-ol and 3-methyl-1-dodecynyl-3-ol.
10. A method of preparing the two-component thermally conductive gel of any of claims 1-9, comprising the steps of:
(1) Putting the branched vinyl silicone oil and the platinum catalyst into a planetary stirrer, stirring for 5-10 min, uniformly mixing, then putting heat-conducting powder in batches, and stirring for 20-30 min after putting till uniform mixing to obtain a component A;
(2) And putting the branched vinyl silicone oil, the branched hydrogen-containing silicone oil and the inhibitor into a planetary stirrer, stirring and mixing for 5-10 min, then putting the heat-conducting powder in batches, and stirring for 20-30 min after putting until the components are uniformly mixed to obtain the component B.
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