CN117801776A - High-heat-conductivity addition type organic silicon electronic pouring sealant and preparation method thereof - Google Patents
High-heat-conductivity addition type organic silicon electronic pouring sealant and preparation method thereof Download PDFInfo
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- CN117801776A CN117801776A CN202311658200.1A CN202311658200A CN117801776A CN 117801776 A CN117801776 A CN 117801776A CN 202311658200 A CN202311658200 A CN 202311658200A CN 117801776 A CN117801776 A CN 117801776A
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- 239000000565 sealant Substances 0.000 title claims abstract description 69
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 44
- 239000010703 silicon Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 70
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 55
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 50
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 50
- 239000001257 hydrogen Substances 0.000 claims abstract description 48
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 45
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 41
- 229920002545 silicone oil Polymers 0.000 claims abstract description 39
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 36
- 239000003054 catalyst Substances 0.000 claims abstract description 31
- 238000004132 cross linking Methods 0.000 claims abstract description 31
- 239000003112 inhibitor Substances 0.000 claims abstract description 22
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 21
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 18
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 7
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 17
- 239000003431 cross linking reagent Substances 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 11
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 6
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 5
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 3
- 235000012431 wafers Nutrition 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 abstract description 9
- 239000011230 binding agent Substances 0.000 abstract 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 28
- 229920002379 silicone rubber Polymers 0.000 description 12
- 239000000084 colloidal system Substances 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 11
- 239000013354 porous framework Substances 0.000 description 10
- 239000004945 silicone rubber Substances 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 5
- 238000012545 processing Methods 0.000 description 5
- 238000007259 addition reaction Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005191 phase separation Methods 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 229920005601 base polymer Polymers 0.000 description 3
- 238000010292 electrical insulation Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000006459 hydrosilylation reaction Methods 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 2
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001845 chromium compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- IOCYQQQCJYMWDT-UHFFFAOYSA-N (3-ethyl-2-methoxyquinolin-6-yl)-(4-methoxycyclohexyl)methanone Chemical compound C=1C=C2N=C(OC)C(CC)=CC2=CC=1C(=O)C1CCC(OC)CC1 IOCYQQQCJYMWDT-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 description 1
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical compound C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-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
- 239000002033 PVDF binder Substances 0.000 description 1
- 241000403513 Schizostachyum chinense Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000008054 signal transmission Effects 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a high-heat-conductivity addition type organic silicon electronic pouring sealant which comprises an A component and a B component in equal parts by mass; the component A comprises the following components: base material, hydrogen-containing silicone oil, methyl silicone oil and crosslinking inhibitor; the component B comprises the following components: a binder, a platinum catalyst; the base material comprises the following components: vinyl polydimethylsiloxane and heat conducting powder; wherein, the vinyl polydimethylsiloxane is a linear chain or branched chain organopolysiloxane containing at least two alkenyl groups bonded with silicon in the molecule; the hydrogen-containing silicone oil is polysiloxane with more than two hydrogen groups bonded with silicon in the molecule; a preparation method of high-heat-conductivity addition type organic silicon electronic pouring sealant. The invention realizes that the heat conductivity coefficient of the pouring sealant is convenient to be 1.6-2.8W.m ‑1 .K ‑1 The linear thermal expansion coefficient is regulated and controlled between 25 and 113 mu m/(m DEG C), the hardness is convenient to regulate and control, and the application field of the organic silicon pouring sealant is widened.
Description
Technical Field
The invention relates to the field of pouring sealants, in particular to a high-heat-conductivity addition type organic silicon electronic pouring sealant and a preparation method thereof.
Background
Heat generated by the operation of the electronic device is typically dissipated by heat conduction, typically using heat sinks, micro-circulation tubes, cooling fans, etc. to cool the microprocessor assembly. However, the heat-generating body (such as an integrated circuit) and the radiator generate larger interface thermal resistance due to poor surface contact and unmatched roughness, and the heat flow conduction efficiency is greatly reduced.
Traditionally, a layer of insulating medium, i.e., thermal interface material (thermal interface material, TIM), such as thermally conductive ceramic materials, polymers, thermally conductive pastes, thermally conductive esters, etc., is interposed between the interfaces. However, although the heat conductive ceramic material (such as silicon carbide, boron nitride, aluminum nitride, etc.) has high heat conductivity, it has extremely high melting point, high brittleness, difficult processing, no flexibility, and difficult filling into the micro gaps between interfaces. Polymers (such as silicone rubber, polyvinylidene fluoride, etc.) have better flexibility, good processability, excellent electrical insulation performance, etc., but have lower thermal conductivity, and are difficult to meet the thermal conductivity requirement of devices. Although the heat conducting paste and the heat conducting ester have certain effects, the heat conducting paste and the heat conducting ester have low weather resistance, strength, fluidity and the like, and have limited heat conducting effect. Meanwhile, besides the high thermal conductivity and the high resistivity, the electronic components need low dielectric constant for high-speed signal transmission, and low thermal expansion coefficient for thermal fatigue resistance.
In order to further improve the performance of the heat sink and ensure that heat generated by the heating element can be rapidly transferred to the heat sink, the contact gap needs a TIM with high thermal conductivity, electrical insulation, softness, easy processing, low thermal expansion coefficient and low dielectric constant to fill the package, and the potting adhesive material is generated.
The pouring sealant is a thermosetting polymer material formed by pouring a liquid adhesive into a device with electronic elements and circuits in a mechanical or manual mode and solidifying the liquid adhesive at normal temperature or under a heating condition. The organic silicon pouring sealant is a pouring sealant commonly used in the field of electronic pouring sealant. However, typical unfilled silicone rubbers have poor thermal conductivity, with a thermal conductivity of only 0.2W.m -1 .K -1 About, a common method for improving the heat conduction performance of the silicone rubber is to fill the silicone rubber with a heat conduction filler (such as alumina, aluminum nitride, etc.) with good insulation property, but to prepare a silicone rubber with high heat conduction (such as a heat conduction coefficient of more than 1.0W.m -1 .K -1 ) The filling amount of the filler is often large, which can lead to the increase of the viscosity of the liquid silicone rubber and is unfavorable for filling and sealing.
For example, chinese patent 200410055033.2 discloses an RTV heat-conducting silicone rubber composition which can be used for preparing a heat-conducting material with a heat conductivity of more than 2.0W.m when the heat-conducting material is filled with more than 900 parts -1 .K -1 But with a viscosity exceeding 60pa.s. U.S. patent 6,169,142 utilizes spherical alumina and common alumina to prepare heat conductive silicon rubber, and when 640 parts of spherical alumina with the particle size of 16 microns and 160 parts of common alumina with the particle size of 3 microns are filled, the heat conductive coefficient can reach 2.0W.m -1 .K -1 The above, however, has a room temperature viscosity as high as 1900Pa.s. Chinese patent 200810219101.2 discloses a heat-conducting flame-retardant liquid silicone rubber for electronics, which has higher heat conductivity coefficient (heat conductivity coefficient: 1.5-2.5 W.m) -1 .K -1 ) And flame retardant properties, but because the viscosity is above 20pa.s, the electronic pouring sealant lacks good flow properties and is difficult to use as the electronic pouring sealant.
Therefore, along with the development of modern technology, the application scene of the pouring sealant is increasingly complex and the requirement is higher, but the prior art is difficult to meet the requirements of pouring sealing performance, electric insulation, softness, easy processing and low thermal expansion coefficient performance while improving the heat conduction effect. Therefore, there is a need for a pouring sealant that can meet the requirements of heat conduction, electrical insulation, softness, easy processing and low thermal expansion coefficient.
Disclosure of Invention
The invention aims to provide a high-heat-conductivity addition type organic silicon electronic pouring sealant and a preparation method thereof, which are used for solving the technical problems that the pouring sealant in the prior art is difficult to meet the requirements of high heat-conductivity, electric insulation, softness, easiness in processing, low thermal expansion coefficient, low dielectric constant and the like.
In order to solve the technical problems, the invention specifically provides the following technical scheme:
the invention provides a high-heat-conductivity addition type organic silicon electronic pouring sealant and a preparation method thereof, wherein the pouring sealant comprises an A component and a B component in equal parts by mass;
the component A comprises the following components in parts by weight: 100 parts of base material, 1-50 parts of hydrogen-containing silicone oil, 0.1-50 parts of methyl silicone oil and 0.002-0.01 part of crosslinking inhibitor;
the component B comprises the following components in parts by weight: 100 parts of base material and 0.01-2.0 parts of catalyst;
the base material comprises the following components in parts by weight: 100 parts of vinyl polydimethylsiloxane and 900-1200 parts of heat conducting powder;
the vinyl polydimethylsiloxane is any one or more of linear vinyl polydimethylsiloxane or branched vinyl polydimethylsiloxane;
the hydrogen-containing silicone oil is polysiloxane with more than two silicon-bonded hydrogen groups in the molecule;
when equal parts by mass of the component A and the component B are mixed, the vinyl polydimethylsiloxane containing Si-Vi and the hydrogen-containing silicone oil containing Si-H undergo addition reaction under the catalysis of the platinum catalyst to form a three-dimensional cross-linked structure of an SiOC porous framework, and the three-dimensional cross-linked structure is separated from the methyl-terminated methyl silicone oil phase to form a polymer colloid system;
and as the methyl silicone oil component changes, the three-dimensional cross-linking structure of the SiOC porous framework of the polymer colloid system correspondingly changes, so that the regulation and control of the system performance are realized.
As a preferable mode of the present invention, the methyl silicone oil is a conventional methyl silicone oil 201, and the viscosity of the methyl silicone oil 201 at 25 ℃ satisfies 10 to 10000 Pa.s.
As a preferred embodiment of the present invention, the vinyl content of the vinyl polydimethylsiloxane is 0.3 to 3.0% and the viscosity at 25℃is 10 to 1100 Pa.s.
As a preferable mode of the invention, the form of the heat conducting powder is any one or more of particles, fibers, whiskers and wafers.
As a preferable scheme of the invention, the heat conducting powder is any one or more of aluminum oxide, boron nitride, silicon carbide and zirconium boride.
As a preferable scheme of the invention, the hydrogen content of the active hydrogen of the hydrogen-containing silicone oil is 0.3-0.8 percent (mass), and the hydrogen content is the mass percent of hydrogen atoms in the silicon-hydrogen bond of the polysiloxane;
the dynamic viscosity value of the hydrogen-containing silicone oil at 25 ℃ is 5-300 mPa.s;
the dynamic viscosity value of the hydrogen-containing silicone oil at 25 ℃ is 10-100 mPa.s.
As a preferred embodiment of the present invention, the crosslinking inhibitor is an alkynol compound, and the crosslinking inhibitor is any one or more of 2-methyl-3-butynyl-2-ol, 2-methyl-1-hexynyl-3-ol, 3, 5-dimethyl-1-hexynyl-3-ol, and 1-ethynyl-1-cyclohexanol.
As a preferred scheme of the invention, the catalyst is a platinum catalyst or dibutyl tin dilaurate;
the platinum catalyst is any one or more of chloroplatinic acid, platinum tetrachloride, an alcohol solution of chloroplatinic acid, a platinum-olefin complex, a platinum-alkenyl siloxane complex and a platinum-carbonyl complex.
As a preferred embodiment of the present invention, the platinum catalyst is chloroplatinic acid having a platinum content of 1000 to 5000ppm or a chromium compound of the chloroplatinic acid.
The invention also provides a preparation method of the high-heat-conductivity addition type organic silicon electronic pouring sealant, which comprises the following steps:
mixing vinyl polydimethylsiloxane into heat conducting powder, stirring and blending at 20-35 ℃ for 60-120 minutes, heating, dehydrating and stirring and blending at 100-150 ℃ for 120-180 minutes, and cooling to obtain a base material;
adding a hydrogen-containing silicone oil cross-linking agent, methyl silicone oil and a cross-linking inhibitor into the base material, and stirring for 30-60 minutes to prepare a component A;
adding a catalyst into the base material at normal temperature, and stirring for 30-60 minutes to prepare a component B;
and uniformly mixing the component A and the component B in equal weight, and defoaming for 5-30 minutes under the vacuum degree of 0.06-0.1MPa to obtain the addition type high-heat-conductivity organic silicon electronic pouring sealant.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention has the advantages that the Si-Vi vinyl polydimethylsiloxane and Si-H hydrogen-containing silicone oil are subjected to addition reaction under the catalysis of a platinum catalyst to form a three-dimensional crosslinking structure of an SiOC porous framework; according to the invention, the three-dimensional cross-linking structure of the SiOC porous skeleton is regulated by using the methyl silicone oil, and the pore diameter and the porosity of the SiOC porous skeleton formed by the Si-H, si-Vi reaction are different along with the different components of the methyl silicone oil in a reaction system, namely, the three-dimensional cross-linking structure of the SiOC porous skeleton of the polymer colloid system is correspondingly changed along with the change of the components of the methyl silicone oil, so that the regulation and control of the system performance are realized.
3. The invention realizes that the heat conductivity coefficient of the pouring sealant is 1.6-2.8W.m -1 .K -1 The linear thermal expansion coefficient is adjustable between 25 and 113 mu m/(m DEG C), the hardness is adjustable, and the application field of the organic silicon pouring sealant is widened.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It will be apparent to those of ordinary skill in the art that the drawings in the following description are exemplary only and that other implementations can be obtained from the extensions of the drawings provided without inventive effort.
FIG. 1 is a schematic flow chart of a method for preparing an addition type organic silicon electronic pouring sealant with high heat conductivity;
FIG. 2 is a diagram showing an example of regulation and control of heat conduction performance of methyl silicone oil 201 on pouring sealant;
FIG. 3 is a graph showing an example of the performance regulation of the linear thermal expansion coefficient of the silicone oil 201 to the pouring sealant;
fig. 4 is a graph showing an example of the hardness performance adjustment of the silicone oil 201 to the pouring sealant according to the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a high-heat-conductivity addition type organic silicon electronic pouring sealant which comprises an A component and a B component in equal parts by mass;
the component A comprises the following components in parts by weight: 100 parts of base material, 1-50 parts of hydrogen-containing silicone oil, 0.1-50 parts of methyl silicone oil and 0.002-0.01 part of crosslinking inhibitor;
the component B comprises the following components in parts by weight: 100 parts of base material and 0.01-2.0 parts of catalyst;
the base material comprises the following components: 100 parts of vinyl polydimethylsiloxane and 900-1200 parts of heat conducting powder.
The addition type organosilicon pouring sealant generally uses vinyl-containing polydimethylsiloxane (commonly called vinyl silicone oil) as a base polymer, hydrogen-containing silicone oil is used as a cross-linking agent, and the vinyl-containing polydimethylsiloxane (commonly called vinyl silicone oil) is cross-linked into an elastomer through hydrosilylation under the action of a platinum-series catalyst. The working mechanism is that the vinyl in the vinyl silicone oil and the hydrogen in the hydrogen-containing silicone oil are subjected to addition reaction at room temperature or under heating condition under the catalysis of platinum, so as to generate the silicon rubber with the three-dimensional cross-linked structure of the SiOC porous framework.
Research shows that in the silicone rubber, the three-dimensional crosslinking structure of the SiOC porous framework is an important index for influencing the performances such as the heat conductivity, the linear thermal expansion coefficient, the hardness and the like of the organosilicon pouring sealant. Because the three-dimensional cross-linking structure of the SiOC porous skeleton is influenced by various factors, the molecular structures and molecular masses of the reacted vinyl silicone oil and the hydrogen-containing silicone oil not only influence the structure and the performance of the vulcanized rubber, but also influence the corresponding vulcanization process, the positions, the contents and the molecular masses of the reactive groups in the reactive silicone oil are controlled, so that the reactive silicone oil has proper activity, and the required three-dimensional cross-linking structure of the SiOC porous skeleton is obtained. Therefore, when the organic silicon pouring sealant is prepared, the three-dimensional crosslinking structure of the SiOC porous framework needs to be regulated and controlled in detail according to actual needs.
In the invention, when equal parts by mass of the component A and the component B are mixed, si-Vi-containing vinyl polydimethylsiloxane and Si-H-containing hydrogen-containing silicone oil undergo hydrosilylation reaction under the catalysis of a platinum catalyst to form a three-dimensional cross-linked structure of an SiOC porous framework. The methyl-terminated polydimethylsiloxane does not contain a reactive functional group, does not react, and still maintains the linear state, so that the compatibility of the methyl-terminated polydimethylsiloxane and the methyl-terminated polydimethylsiloxane is changed. As the addition reaction proceeds, the degree of crosslinking of the reactive polysiloxane increases, the compatibility with the methyl-terminated polydimethylsiloxane gradually becomes worse, the polymer system begins to undergo phase separation, and eventually systemization, and the phase size is fixed, resulting in a polymer colloid system in which the methyl-terminated polydimethylsiloxane fills with the crosslinked polysiloxane as a hard skeletal network.
The polymer colloid is prepared from a mixture of reactive polysiloxane and nonreactive methyl-terminated polydimethylsiloxane. In colloids, the reactive polysiloxane is a hard skeletal network, with liquid methyl-terminated polydimethylsiloxane filled therein. The degree of phase separation of the polymer colloid can be adjusted, i.e. the mass fraction of the methyl-terminated polydimethylsiloxane in the mixed system of reactive polysiloxane and methyl-terminated polydimethylsiloxane affects the degree of phase separation. With the increase of the mass fraction of the methyl-terminated polydimethylsiloxane, the phase separation degree is increased, the three-dimensional crosslinking structure of the SiOC porous framework is regulated and the system performance is regulated and controlled.
According to the invention, a three-dimensional cross-linked structure of the SiOC porous skeleton is formed by utilizing hydrosilylation reaction to obtain vinyl silicone oil and hydrogen-containing silicone oil, and the three-dimensional cross-linked structure of the SiOC porous skeleton is further regulated and controlled by utilizing methyl silicone oil, so that the pore diameter and the porosity of the SiOC porous skeleton formed by Si-H, si-Vi reaction are different (the pores of the SiOC porous skeleton are occupied by methyl silicone oil) along with different components of the methyl silicone oil in a reaction system, so that the three-dimensional cross-linked structure of the SiOC porous skeleton is also different, and the performance of the pouring sealant is regulated and controlled. According to the invention, through reasonably constructing the three-dimensional cross-linked structure of the SiOC porous framework of the pouring sealant, the heat conduction performance of the pouring sealant is adjustable, the linear expansion coefficient is adjustable, the hardness is adjustable, and the stability is higher.
Namely, the invention adjusts the three-dimensional cross-linking structure of the colloid system by using methyl silicone oil, and the three-dimensional cross-linking structure is separated from methyl end-capped methyl silicone oil to form polymer colloid; the three-dimensional cross-linking structure of the SiOC porous framework of the polymer colloid correspondingly changes along with the change of methyl silicone oil component, so as to realize the regulation and control of the system performance.
Specific examples of base polymers are provided below:
vinyl polydimethylsiloxanes refer to a base polymer which generally contains in the molecule at least two organopolysiloxane groups of silicon-bonded alkenyl groups which may be located at the terminal and/or pendant positions of the organopolysiloxane molecule, preferably the silicon-bonded groups at both ends of the organopolysiloxane molecule comprise alkenyl groups with or without silicon-bonded alkenyl groups at the pendant positions. Alkenyl groups include vinyl, allyl, butenyl, or pentenyl, preferably vinyl or allyl, and further vinyl polydimethylsiloxane.
The vinyl polydimethylsiloxane is one or more than two of linear vinyl polydimethylsiloxane or branched vinyl polydimethylsiloxane, and the content of vinyl is 0.1wt% to 3wt%, such as 0.1wt%, 0.2wt%, 0.3wt%, 0.5wt%, 0.8wt%, 1wt%, 1.3wt%, 1.6wt%, 1.8wt%, 2.2wt%, 2.5wt%, 2.8wt%, etc. Preferably 0.5wt% to 2.5wt%.
The vinyl content of the vinyl polysiloxane is 0.3-3.0%, and the viscosity at 25 ℃ is 10-1100 Pa.s.
Specific examples of the heat conductive powder are provided below:
the heat conducting powder is one or more of aluminum oxide, boron nitride, silicon carbide and zirconium boride.
The aluminum oxide, boron nitride, silicon carbide and zirconium boride are one or more of particles, fibers, whiskers and wafers.
Specific examples of hydrogen containing silicone oils (i.e., cross-linking agents) are provided below:
the hydrogen-containing silicone oil crosslinking agent is polysiloxane with more than two silicon-bonded hydrogen groups in the molecule. The hydrogen content of the crosslinking agent is 0.3 to 0.8 mass percent, and in the invention, the hydrogen content is the mass percent of hydrogen atoms in the silicon-hydrogen bond of the polysiloxane, and the dynamic viscosity value of the crosslinking agent at 25 ℃ is 5 to 300 mPa.s, more preferably 10 to 100mPa.s.
Specific examples of catalysts are provided below:
the catalyst may be a platinum catalyst or dibutyltin dilaurate; the platinum catalyst may be chloroplatinic acid, karstedt's catalyst (1, 3-divinyl-1, 3-tetramethyldisiloxane platinum (0), CAS: 68478-92-2) or Speier's catalyst (isopropyl alcohol solution of chloroplatinic acid).
In the two-component addition type organic silicon heat conduction pouring sealant, the catalyst is preferably a platinum-based catalyst, and is selected from one or more of chloroplatinic acid, platinum tetrachloride, an alcohol solution of chloroplatinic acid, a platinum-olefin complex, a platinum-alkenyl siloxane complex and a platinum-carbonyl complex, and the dosage is not particularly limited.
In the two-component addition type organic silicon heat conduction pouring sealant, the component A can also contain an inhibitor, wherein the inhibitor is selected from one or more of 2-methyl-3-butyn-2-ol, 3, 5-dimethyl-1-hexyn-3-ol, 2-phenyl-3-butyn-2-ol, ethynyl cyclohexanol and tetramethyl tetravinyl cyclotetrasiloxane, or other curing inhibitors, and the dosage of the inhibitor is not particularly limited.
Specific examples of the methyl silicone oil are provided below:
the methyl silicone oil is conventional methyl silicone oil 201, and has a viscosity of 10-10000 Pa.s at 25deg.C.
Specific examples of crosslinking inhibitors are provided below:
the crosslinking inhibitor is an alkynol compound commonly used for addition type silicone rubber, such as 2-methyl-3-butynyl-2-ol, 2-methyl-1-hexynyl-3-ol, 3, 5-dimethyl-1-hexynyl-3-ol, 1-ethynyl-1-cyclohexanol or a mixture of more than two of the above.
As shown in fig. 1, the invention provides a preparation method of a high-heat-conductivity addition type organic silicon electronic pouring sealant, which comprises the following steps:
(1) Preparation of base material: mixing vinyl polydimethylsiloxane and heat conducting powder, stirring and blending at 20-35 ℃ for 60-120 minutes, heating, dehydrating and stirring and blending at 100-150 ℃ for 120-180 minutes, and cooling to obtain the base material.
(2) And (3) preparation of the component A: and (3) adding a hydrogen-containing silicone oil crosslinking agent and a crosslinking inhibitor with the hydrogen content of 0.05-2.0wt% into the base material prepared in the step (1) at normal temperature, and fully stirring for 30-60 minutes to prepare the component A.
(3) And (3) preparation of a component B: and (3) at normal temperature, adding chloroplatinic acid or chromium compound thereof with platinum content of 1000-5000ppm into the base material prepared in the step (1) as a platinum catalyst, and fully stirring for 30-60 minutes to prepare the component B.
(4) Preparation of high-heat-conductivity addition type organic silicon electronic pouring sealant: and (3) uniformly mixing the component A prepared in the step (2) and the component B prepared in the step (3) with equal weight at normal temperature, and defoaming for 5-30 minutes under the vacuum degree of 0.06-0.1MPa to obtain the high-heat-conductivity addition type organic silicon electronic pouring sealant.
The high heat conduction addition type organic silicon electronic pouring sealant has the heat conduction coefficient of 1.6-2.8W.m-1.K-1, the linear thermal expansion coefficient of 25-113 mu m/(m DEG C) and the hardness of adjustable, and the fluidity is convenient to adjust.
The experimental methods used in the examples below are as described without any particular limitation. Are all conventional methods.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
Example 1:
100 parts by mass of linear vinyl siloxane with the viscosity of 43mPa.s and the vinyl content of 1.85wt% are mixed with 1150 parts by mass of aluminum oxide heat conduction powder, stirred and blended for 60 minutes at 30 ℃, heated, dehydrated and stirred and blended for 120 minutes at 110 ℃, and cooled to obtain a base material;
15 parts by mass of hydrogen-containing silicone oil crosslinking agent with hydrogen content of 0.55%, 201 parts by mass of methyl silicone oil with viscosity of 50mPa.s, a proper amount of crosslinking inhibitor and 100 parts by mass of base material are fully stirred and mixed for 30 minutes to obtain a component A;
fully stirring and mixing a proper amount of platinum catalyst and 100 parts by mass of base material for 30 minutes to obtain a component B;
and (3) uniformly blending the component A and the component B in equal parts by mass at room temperature, and defoaming for 20 minutes under the vacuum degree of 0.1MPa to obtain the high-heat-conductivity organic silicon electronic pouring sealant.
The heat conductivity coefficient of the cured pouring sealant of example 1 was 2.3w..m -1 .K -1 The linear thermal expansion coefficient was 113 μm/(m..degree.C.).
Example 2:
100 parts by mass of linear vinyl siloxane with the viscosity of 43mPa.s and the vinyl content of 1.85wt% are mixed with 1150 parts by mass of aluminum oxide heat conduction powder, stirred and blended for 60 minutes at 30 ℃, heated, dehydrated and stirred and blended for 120 minutes at 110 ℃, and cooled to obtain a base material;
15 parts by mass of a hydrogen-containing silicone oil crosslinking agent with the hydrogen content of 0.55%, 201 parts by mass of methyl silicone oil with the viscosity of 50mPa.s, a proper amount of crosslinking inhibitor and 100 parts by mass of base material are fully stirred and mixed for 30 minutes to obtain a component A;
fully stirring and mixing a proper amount of platinum catalyst and 100 parts by mass of base material for 30 minutes to obtain a component B;
and (3) uniformly blending the component A and the component B in equal parts by mass at room temperature, and defoaming for 20 minutes under the vacuum degree of 0.1MPa to obtain the high-heat-conductivity organic silicon electronic pouring sealant.
Example 2 Heat conductivity coefficient of the cured pouring sealant was 2.8W.m -1 .K -1 The linear thermal expansion coefficient was 70. Mu.m/(m..degree.C.))。
Example 3:
100 parts by mass of linear vinyl siloxane with the viscosity of 43mPa.s and the vinyl content of 1.85wt% are mixed with 1150 parts by mass of aluminum oxide heat conduction powder, stirred and blended for 60 minutes at 30 ℃, heated, dehydrated and stirred and blended for 120 minutes at 110 ℃, and cooled to obtain a base material;
15 parts by mass of hydrogen-containing silicone oil crosslinking agent with hydrogen content of 0.55%, 201 100 parts by mass of methyl silicone oil with viscosity of 50mPa.s, a proper amount of crosslinking inhibitor and 100 parts by mass of base material are fully stirred and mixed for 30 minutes to obtain a component A;
fully stirring and mixing a proper amount of platinum catalyst and 100 parts by mass of base material for 30 minutes to obtain a component B;
and (3) uniformly blending the component A and the component B in equal parts by mass at room temperature, and defoaming for 20 minutes under the vacuum degree of 0.1MPa to obtain the high-heat-conductivity organic silicon electronic pouring sealant.
Example 3 Heat conductivity coefficient of the cured pouring sealant was 1.6W.m -1 .K -1 The linear thermal expansion coefficient was 49 μm/(m..degree.C.).
Example 4:
100 parts by mass of linear vinyl siloxane with the viscosity of 43mPa.s and the vinyl content of 1.85wt% are mixed with 1150 parts by mass of aluminum oxide heat conduction powder, stirred and blended for 60 minutes at 30 ℃, heated, dehydrated and stirred and blended for 120 minutes at 110 ℃, and cooled to obtain a base material;
15 parts by mass of hydrogen-containing silicone oil crosslinking agent with hydrogen content of 0.55%, 201 200 parts by mass of methyl silicone oil with viscosity of 50mPa.s, a proper amount of crosslinking inhibitor and 100 parts by mass of base material are fully stirred and mixed for 30 minutes to obtain a component A;
fully stirring and mixing a proper amount of platinum catalyst and 100 parts by mass of base material for 30 minutes to obtain a component B;
and (3) uniformly blending the component A and the component B in equal parts by mass at room temperature, and defoaming for 20 minutes under the vacuum degree of 0.1MPa to obtain the high-heat-conductivity organic silicon electronic pouring sealant.
Example 4 Heat conductivity coefficient of the cured pouring sealant was 1.6W.m -1 .K -1 The linear thermal expansion coefficient is 25 μm +.(m.℃)。
Example 5:
100 parts by mass of linear vinyl siloxane with the viscosity of 43mPa.s and the vinyl content of 1.85wt% are mixed with 1150 parts by mass of aluminum oxide heat conduction powder, stirred and blended for 60 minutes at 30 ℃, heated, dehydrated and stirred and blended for 120 minutes at 110 ℃, and cooled to obtain a base material;
15 parts by mass of hydrogen-containing silicone oil crosslinking agent with hydrogen content of 0.55%, 201 300 parts by mass of methyl silicone oil with viscosity of 50mPa.s, a proper amount of crosslinking inhibitor and 100 parts by mass of base material are fully stirred and mixed for 30 minutes to obtain a component A;
fully stirring and mixing a proper amount of platinum catalyst and 100 parts by mass of base material for 30 minutes to obtain a component B;
and (3) uniformly blending the component A and the component B in equal parts by mass at room temperature, and defoaming for 20 minutes under the vacuum degree of 0.1MPa to obtain the high-heat-conductivity organic silicon electronic pouring sealant.
The heat conductivity coefficient of the cured pouring sealant in example 5 was 1.6W.m -1 .K -1 The linear thermal expansion coefficient was 66. Mu.m/(m..degree.C.).
The results of the performance test of the above examples are shown in table 1.
TABLE 1
From the table above, the high-heat-conductivity organic silicon electronic pouring sealant has excellent heat conduction performance and thermal fatigue resistance, and the hardness can be regulated and controlled according to the requirement. The thermal conductivity coefficient is 1.6-2.8 W.m. according to the different dosages of the methyl silicone oil 201 -1 .K -1 The temperature is adjustable, the linear thermal expansion coefficient is adjustable between 25 and 113 mu m/(m DEG C), and the Shore hardness A is adjustable between 5 and 84.
According to the figures 2-4, the defects of low heat conductivity and poor thermal fatigue performance of the traditional electronic pouring sealant can be overcome, the application field of the organic silicon electronic pouring sealant is widened, and the electronic pouring sealant has good market prospect.
Through the high-heat-conductivity addition type organic silicon electronic pouring sealant and the preparation method thereof, the performances of colloid heat conductivity coefficient, linear heat expansion coefficient, hardness and the like can be regulated and controlled, the application field of the organic silicon pouring sealant is widened, and the organic silicon electronic pouring sealant has good market prospect.
The above embodiments are only exemplary embodiments of the present application and are not intended to limit the present application, the scope of which is defined by the claims. Various modifications and equivalent arrangements may be made to the present application by those skilled in the art, which modifications and equivalents are also considered to be within the scope of the present application.
Claims (10)
1. The high-heat-conductivity addition type organic silicon electronic pouring sealant is characterized by comprising an A component and a B component in equal parts by mass;
the component A comprises the following components in parts by weight: 100 parts of base material, 1-50 parts of hydrogen-containing silicone oil, 0.1-50 parts of methyl silicone oil and 0.002-0.01 part of crosslinking inhibitor;
the component B comprises the following components in parts by weight: 100 parts of base material and 0.01-2.0 parts of catalyst;
the base material comprises the following components in parts by weight: 100 parts of vinyl polydimethylsiloxane and 900-1200 parts of heat conducting powder;
wherein the vinyl polydimethylsiloxane is a linear chain or branched chain organopolysiloxane containing at least two silicon-bonded alkenyl groups in a molecule;
the hydrogen-containing silicone oil is polysiloxane with more than two silicon-bonded hydrogen groups in the molecule.
2. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the methyl silicone oil is conventional methyl silicone oil 201, and the viscosity of the methyl silicone oil 201 at 25 ℃ is 10-10000 Pa.s.
3. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the vinyl polydimethylsiloxane is any one or more of linear vinyl polydimethylsiloxane or branched vinyl polydimethylsiloxane;
wherein the vinyl content of the vinyl polydimethylsiloxane is 0.3-3.0%, and the viscosity at 25 ℃ is 10-1100mPa.s.
4. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the form of the heat conducting powder is any one or more of particles, fibers, whiskers and wafers.
5. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the heat conducting powder is any one or more of aluminum oxide, boron nitride, silicon carbide and zirconium boride.
6. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the hydrogen content of the active hydrogen of the hydrogen-containing silicone oil is 0.3-0.8 percent (mass), and the hydrogen content is the mass percentage of hydrogen atoms in the silicon-hydrogen bond of polysiloxane;
wherein the dynamic viscosity value of the hydrogen-containing silicone oil at 25 ℃ is 5-300 mPa.s;
wherein the dynamic viscosity value of the hydrogen-containing silicone oil at 25 ℃ is 10-100 mPa.s.
7. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the crosslinking inhibitor is an alkynol compound;
wherein the crosslinking inhibitor is any one or more of 2-methyl-3-butynyl-2-alcohol, 2-methyl-1-hexynyl-3-alcohol, 3, 5-dimethyl-1-hexynyl-3-alcohol and 1-ethynyl-1-cyclohexanol.
8. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 1, wherein,
the catalyst is a platinum catalyst or dibutyl tin dilaurate.
9. The high thermal conductivity addition type organic silicon electronic pouring sealant according to claim 8, wherein,
the platinum catalyst is any one or more of chloroplatinic acid, platinum tetrachloride, an alcohol solution of chloroplatinic acid, a platinum-olefin complex, a platinum-alkenyl siloxane complex and a platinum-carbonyl complex.
10. A method for preparing the high-thermal-conductivity addition type organic silicon electronic pouring sealant according to any one of claims 1 to 9, which is characterized by comprising the following steps:
mixing vinyl polydimethylsiloxane into heat conducting powder, stirring and blending at 20-35 ℃ for 60-120 minutes, heating, dehydrating and stirring and blending at 100-150 ℃ for 120-180 minutes, and cooling to obtain a base material;
adding a hydrogen-containing silicone oil cross-linking agent, methyl silicone oil and a cross-linking inhibitor into the base material, and stirring for 30-60 minutes to prepare a component A;
adding a catalyst into the base material at normal temperature, and stirring for 30-60 minutes to prepare a component B;
and uniformly mixing the component A and the component B in equal weight, and defoaming for 5-30 minutes under the vacuum degree of 0.06-0.1MPa to obtain the addition type high-heat-conductivity organic silicon electronic pouring sealant.
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