CN115260770B - Thermal management material, preparation method and application thereof - Google Patents
Thermal management material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of thermal management materials, and provides a thermal management material, a preparation method and application thereof, wherein the thermal management material comprises the following raw materials in parts by weight: low viscosity vinyl silicone oils; a thermally conductive filler; the multi-hydrogen silicone oil is microcapsule coated multi-hydrogen silicone oil; and, terminal hydrogen silicone oil; the sum of the amounts of Si-H in the polyhydrogenated silicone oil and the terminal hydrogen-containing silicone oil being equal to CH in the low-viscosity vinyl silicone oil 2 The ratio R of the amounts of substances=ch-is 1:1.2 to 1:2.2; the ratio r of the amount of Si-H in the hydrogen-containing silicone oil at the end to the amount of Si-H in the hydrogen-containing silicone oil at the end is 0.75-1.25; the thermal management material has the advantages of high thermal conductivity, low hardness, low interface thermal resistance and no oil seepage.
Description
Technical Field
The invention relates to the technical field of thermal management materials, relates to the technical field of thermal management materials capable of being used for preparing heat-conducting gaskets, heat-conducting gel and heat-conducting pouring sealant, and particularly discloses a thermal management material, a preparation method and application thereof.
Background
With the increase of chip power density and the development of electric automobiles, the design of thermal management has become one of the core contents of these fields. The heat-conducting composition prepared by compounding the liquid organic silicon material with the heat-conducting filler such as aluminum oxide, aluminum nitride, boron nitride and the like is always favored and widely used because of the outstanding advantages of the heat-conducting composition in the aspects of temperature resistance, insulation, cost and the like. The organic silicon material has poor heat conduction performance, which is only about 0.2W/(m.k), and can not be used as a heat conduction material alone, but after the heat conduction filler is compounded, the heat conduction filler forms a heat conduction path in a system taking the liquid organic silicon material as a continuous phase, so that higher heat conductivity can be realized. The higher the filler loading (i.e., the volume or mass ratio of thermally conductive filler to silicone material), the more thermally conductive paths, and the higher the thermal conductivity of the thermally conductive composition.
When the liquid organosilicon is filled with the heat-conducting filler, the viscosity of the mixture can rise with the increase of the filling amount, and the subsequent operation is difficult. Alleviating this problem can generally be initiated from two aspects:
one is powder optimization, namely, the interaction between hydroxyl groups on the surface of the filler and other materials is reduced by selecting a heat-conducting filler with specific shape and particle size or carrying out surface treatment on the filler.
On the other hand, vinyl silicone oil with lower viscosity is selected; however, because of the relatively small molecular weight of the low viscosity vinyl silicone oils, several crosslinks are often required to form larger molecules or network molecular structures; the heat-conducting composition often contains a large number of parts with smaller molecular weight or insufficient crosslinking degree after curing, and the components have larger activity, so that the heat-conducting composition has oil seepage phenomenon after curing. Oil bleeding can not only contaminate the application environment, but also cause deterioration of the thermal and mechanical properties of the material itself, such as hardening, embrittlement, cracking, etc.
To solve the problem of oil bleeding, it is often necessary to increase the amount of the hydrogen-containing silicone oil so that the system forms a denser space network structure after crosslinking to suppress the production of low molecular weight products. However, due to the high vinyl content of the low-viscosity vinyl silicone oil, too many crosslinking points of the space network structure after crosslinking and the large addition amount of the filler, the hardness of the thermal management material after heat curing is too high, which is often higher than 80Shore OO. Too high hardness not only can cause the material to be too brittle and easy to break, but also can cause the interface bonding degree among the thermal management material product (such as a heat conduction gasket), the heating element (such as a chip) and the radiating fin to be insufficient, thereby causing the interface thermal resistance to be too large and affecting the overall heat conduction performance and the radiating effect.
Disclosure of Invention
In view of the above-mentioned drawbacks or deficiencies of the prior art, the present invention is directed to a thermal management material, a method of making, and uses thereof, having the advantages of high thermal conductivity, low hardness, low thermal interface resistance, and no oil bleed.
One of the purposes of the present invention is to provide a thermal management material comprising the following raw materials:
low viscosity vinyl silicone oils;
a thermally conductive filler;
the multi-hydrogen silicone oil is microcapsule coated multi-hydrogen silicone oil; and
terminal hydrogen silicone oil.
The sum of the amounts of Si-H in the polyhydrogenated silicone oil and the terminal hydrogen-containing silicone oil being equal to CH in the low-viscosity vinyl silicone oil 2 The ratio R of the amounts of the substances=ch-is 1:1.2 to 1:2.2.
The ratio r of the amount of Si-H in the terminal hydrogen-containing silicone oil to the amount of Si-H in the multi-hydrogen-containing silicone oil is 0.75-1.25.
The low-viscosity vinyl silicone oil is vinyl silicone oil with the viscosity of 50-65000 MPa.S.
The heat management material is characterized in that the mass of the heat conduction filler is 100-2500 parts based on 100 parts of the mass of the low-viscosity vinyl silicone oil.
Preferably, the thermal management material further comprises an inhibitor, the inhibitor being 0.01 to 0.1 parts by mass based on 100 parts by mass of the low viscosity vinyl silicone oil.
Preferably, the thermal management material further comprises a platinum catalyst, and the mass of the platinum element in the platinum catalyst is 3-20 ppm of the total mass of the thermal management material.
The low-viscosity vinyl silicone oil is one or more of compounds with structures shown as A-1, A-2 or A-3;
the terminal hydrogen-containing silicone oil is a compound with a structure shown as B-1;
the polyhydrogen silicone oil is a compound having a structure as shown in B-2 and/or B-3;
the total hydrogen content of the terminal hydrogen-containing silicone oil and the multi-hydrogen-containing silicone oil is 0.05% -1.0%, and preferably 0.1% -0.5%.
The microcapsule coated type multi-hydrogen silicone oil comprises a capsule wall material and a capsule core, wherein the capsule core is the multi-hydrogen silicone oil.
Preferably, the wall material is a thermoplastic material, preferably one or more of polymethyl methacrylate PMMA, polystyrene PSt, acrylonitrile modified polystyrene PSt-AN, polycarbonate PC, cyclodextrin or thermoplastic silicone, and in order to ensure compatibility after curing and heat resistance after curing of the thermal management material composition, preferably thermoplastic silicone, and further preferably thermoplastic methylphenyl silicone.
If the softening point of the capsule wall material is too low, the microcapsules may be damaged due to local heating caused by friction during stirring; if the softening point of the capsule wall material is too high, the capsule wall is difficult to soften and release the hydrogen-containing silicone oil at the common curing temperature, which is unfavorable for the curing process; if the curing temperature is too high, the PET used for calendaring can deform, which is unfavorable for obtaining products with better appearance. Therefore, the microcapsule-coated multi-hydrogen-containing silicone oil is preferably a thermoplastic silicone resin with a softening point of 60-120 ℃, and preferably a thermoplastic silicone resin with a softening point of 70-100 ℃.
Preferably, the mass ratio of the capsule core to the capsule wall material is 2:8-4:6.
Preferably, the microcapsule coated type hydrogen-containing silicone oil is spherical microcapsule.
Preferably, the microcapsule-coated hydrogen-containing silicone oil has an average particle diameter of 0.8 μm to 1.5 μm.
The heat conducting filler comprises one or more of aluminum oxide, magnesium oxide, aluminum hydroxide, magnesium hydroxide, aluminum nitride, silicon dioxide or silicon carbide.
Preferably, the thermally conductive filler is spherical and/or non-spherical in shape, preferably spherical.
Preferably, the heat conductive filler is a heat conductive filler having an average particle diameter of 0.1 to 120 μm.
Preferably, the heat conducting filler is a heat conducting filler subjected to surface modification, preferably a heat conducting filler subjected to surface modification by hexadecyltrimethoxysilane.
Preferably, the platinum catalyst is one or more of Karstedt catalyst, speier catalyst, ashby catalyst, lamoreaux catalyst or capsule platinum catalyst, preferably Karstedt catalyst.
Preferably, the inhibitor is one or more of alkynol inhibitors, fumarate esters, maleate esters, butynedioate esters, carbene inhibitors or phosphite esters, preferably alkynol inhibitors, and more preferably acetylene cyclohexanol.
The second object of the present invention is to provide a method for preparing a thermal management material, the method comprising the steps of:
uniformly mixing low-viscosity vinyl silicone oil, terminal hydrogen-containing silicone oil, heat-conducting filler, microcapsule coated multi-hydrogen-containing silicone oil, optional inhibitor and optional platinum catalyst to obtain the thermal management material;
preferably, firstly, uniformly mixing low-viscosity vinyl silicone oil, terminal hydrogen-containing silicone oil and heat-conducting filler, adding an optional inhibitor, an optional platinum catalyst and microcapsule coated multi-hydrogen-containing silicone oil, uniformly mixing, and defoaming to obtain the thermal management material;
it is a further object of the present invention to provide the use of a thermal management material that can be used for the preparation of thermally conductive gaskets, thermally conductive gels and thermally conductive potting adhesives.
The beneficial effects of the invention include:
the thermal management material is prepared by polymerization reaction of low-viscosity vinyl silicone oil, multi-hydrogen silicone oil and terminal hydrogen silicone oil. In the invention, microcapsule coated multi-hydrogen-containing silicone oil is used, the multi-hydrogen-containing silicone oil with relatively low activity is singly coated into microcapsules by thermoplastic materials, and the terminal hydrogen-containing silicone oil with high activity for adjusting hardness does not carry out any coating treatment, so that the temperature difference of the reaction of the two hydrogen-containing silicone oils is enlarged. After heating, firstly, chain extension reaction is carried out on the hydrogen-containing silicone oil at the end and the low-viscosity vinyl silicone oil to form long-chain or vinyl silicone oil mainly with long chain, and the long-chain structure is beneficial to realizing better flexibility under the condition of high filling and solving the problem of oil seepage. After the end hydrogen-containing reaction is finished, the temperature is raised until the wrapping material is melted, and the multi-hydrogen-containing silicone oil is released to participate in the reaction to form a space reticular structure, so that the strength and the rebound resilience of the material are endowed. Therefore, the microcapsule coated multi-hydrogen-containing silicone oil is used for controlling the curing process and creating conditions, so that the end hydrogen-containing silicone oil and the low-viscosity vinyl silicone oil firstly undergo chain extension reaction, and then the multi-hydrogen-containing silicone oil is interposed for crosslinking and curing. Can effectively solve the problem of oil seepage, and has low hardness, low interface thermal resistance and good heat conduction performance.
Detailed Description
The technical features in the technical scheme provided by the invention are further and clearly described below in combination with the specific embodiments, and the protection scope is not limited.
The thermal management material is prepared by polymerization reaction of hydrogen-containing silicone oil and low-viscosity vinyl silicone oil, and therefore, the specific scheme of the invention is as follows:
first, a thermal management material is provided, which comprises the following raw materials: low viscosity vinyl silicone oils; a thermally conductive filler; the multi-hydrogen silicone oil is microcapsule coated multi-hydrogen silicone oil; and terminal hydrogen-containing silicone oil.
The sum of the amounts of Si-H in the polyhydrogenated silicone oil and the terminal hydrogen-containing silicone oil being equal to CH in the low-viscosity vinyl silicone oil 2 The ratio R of the amounts of the substances=ch-is 1:1.2 to 1:2.2.
The ratio r of the amount of Si-H in the terminal hydrogen-containing silicone oil to the amount of Si-H in the multi-hydrogen-containing silicone oil is 0.75-1.25.
The low-viscosity vinyl silicone oil is vinyl silicone oil with the viscosity of 50-65000 MPa.S.
In the present invention, the low viscosity vinyl silicone oil means that the molecule contains two or more CH groups bonded to Si 2 Low viscosity vinyl silicone oil =ch-.
In the present invention, the polyhydrogen silicone oil refers to a hydrogen silicone oil having at least 3 or more H atoms (i.e., si-H bonds) connected to Si atoms on a polydimethylsiloxane molecular chain, and functions to crosslink with vinyl silicone oil to form a space network structure, thereby generating rebound and strength.
In the invention, the terminal hydrogen-containing silicone oil refers to hydrogen-containing silicone oil which only has Si-H bonds at two ends of a polydimethylsiloxane molecular chain and does not contain Si-H bonds in the middle of the molecular chain, and the terminal hydrogen-containing silicone oil has the effects of chain extension of low-viscosity vinyl silicone oil, molecular weight increase, oil production inhibition, product hardness reduction after solidification and product flexibility endowing.
In order to control the viscosity, the present invention uses a low-viscosity vinyl silicone oil obtained by polymerization of a multi-hydrogen-containing silicone oil and a terminal hydrogen-containing silicone oil, but if the low-viscosity vinyl silicone oil is directly mixed with the terminal hydrogen-containing silicone oil and the multi-hydrogen-containing silicone oil to react, CH 2 The simultaneous reaction of the =ch-with the terminal Si-H bond and Si-H between the molecular chains, the simultaneous chain extension reaction and the crosslinking reaction, may result in incomplete chain extension, resulting in failure of the product to suppress oil production, high hardness, and poor flexibility.
Therefore, in the invention, the curing process is controlled, namely, the multi-hydrogen-containing silicone oil with relatively low activity is singly coated into microcapsules by thermoplastic materials, and the terminal hydrogen-containing silicone oil with high activity for adjusting the hardness does not carry out any coating treatment, so that the temperature difference of the reaction of the two hydrogen-containing silicone oils is enlarged. After heating, the hydrogen-containing silicone oil at the end reacts with the low-viscosity vinyl silicone oil to form a long chain, or the vinyl silicone oil with the long chain as a main part, and the long chain structure is favorable for realizing better flexibility under the condition of high filling and solving the problem of oil seepage. After the end hydrogen-containing reaction is finished, the temperature is raised until the wrapping material is melted, and the multi-hydrogen-containing silicone oil is released to participate in the reaction to form a space reticular structure, so that the strength and the rebound resilience of the material are endowed.
The hardness of the composition containing the microcapsule coated type multi-hydrogen-containing silicone oil after curing is lower than that of the composition containing only the uncoated multi-hydrogen-containing silicone oil after curing, and the phenomenon of oil seepage is avoided. And the corresponding breaking strength and breaking elongation are better than those of the composition only containing uncoated multi-hydrogen silicone oil, which shows that the composition is more flexible and is not easy to break and damage in the gasket assembly process. In the aspect of heat conduction effect, the composition containing the capsule type multi-hydrogen silicone oil has better heat conduction performance of a sample after being solidified due to lower hardness.
When R <1:2.2 and R >1.25, the thermal management material has too low hardness after curing, no mechanical strength, and severe oil bleeding; when R >1:1.2 and R <0.75, the thermal management material has too high a hardness after curing far beyond the conventional required range of thermally conductive gaskets.
Thus, in the present invention, R is 1:1.2 to 1:2.2, for example 1:1.25, 1:1.4, 1:1.48, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9, 1:2, 1:2.1 or 1:2.15.
In the present invention, r is 0.75 to 1.25, for example, 0.8, 0.85, 0.9, 0.95, 1, 1.05, 1.1, 1.15, 1.2 or 1.23.
In a preferred embodiment of the present invention, the thermal management material has a mass of 100 to 2500 parts of the thermally conductive filler based on 100 parts by mass of the low viscosity vinyl silicone oil.
In the present invention, the heat conductive filler has a mass of 100 to 2500 parts, for example, 100 parts, 200 parts, 500 parts, 800 parts, 1000 parts, 1200 parts, 1500 parts, 1700 parts, 2000 parts, 2300 parts, 2400 parts, 2500 parts.
Preferably, the thermal management material further comprises an inhibitor, the inhibitor being 0.01 to 0.1 parts by mass based on 100 parts by mass of the low viscosity vinyl silicone oil.
In the present invention, the mass of the inhibitor is, for example, 0.01 part, 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part, and 0.1 part.
Preferably, the thermal management material further comprises a platinum catalyst, and the mass of the platinum element in the platinum catalyst is 3-20 ppm of the total mass of the thermal management material.
In the present invention, the mass of the platinum element is, for example, 3ppm, 5ppm, 8ppm, 10ppm, 11ppm, 13ppm, 15ppm, 17ppm, 18ppm, 19ppm, 20ppm.
In a preferred embodiment of the present invention, the low viscosity vinyl silicone oil is one or more of compounds having a structure as shown in A-1, A-2 or A-3;
the molecular structures shown in A-1, A-2 and A-3 only show the relative positions of the vinyl groups (at both ends or in the middle of the molecular chain), but not the actual positions of the vinyl groups in the molecular chain, and do not suggest the presence of block-like structural units.
In the present invention, the A-1 is a molecular chain of CH 2 ＝CH-Si(CH 3 ) 2 O-blocked polydimethylsiloxanes which do not contain other unsaturated bonds in the molecule; the A-2 is a molecular Chain (CH) 3 ) 3 SiO-end-capped, the molecular chain contains two or more Si and-CH=CH 2 Linked polydimethylsiloxanes; the A-3 is a molecular chain of CH 2 ＝CH-Si(CH 3 ) 2 O-end capping with one or more Si and-ch=ch in the middle of the molecular chain 2 Linked polydimethylsiloxanes.
In a preferred embodiment of the present invention, the hydrogen-terminated silicone oil is a compound having a structure as shown in B-1;
in the present invention, the B-1 is a metal compound obtained by reacting H-Si (CH) 3 ) 2 End-capping, a polydimethylsiloxane containing Si-H bonds only at the ends of the molecular chain, whereas a polydimethylsiloxane containing no Si-H bonds in the middle of the molecular chain.
In a preferred embodiment of the present invention, the polyhydrogenated silicone oil is a compound having a structure represented by B-2 and/or B-3.
The molecular structures shown in B-2 and B-3 merely illustrate the relative positions of Si-H bonds, and not the actual positions of Si-H bonds in the molecular chain, nor do they suggest the presence of block-like building blocks.
The multi-hydrogen silicone oil is polydimethylsiloxane containing at least 3 Si-H bonds; the B-2 is represented by (CH) 3 ) 3 Si-terminated polydimethyl siloxane with at least 3 Si-H bonds in the molecular chain; the B-3 is H-Si (CH) 3 ) 2 -end-capping, polydimethylsiloxanes (B-3) containing at least 1 Si-H bond in the middle of the molecular chain.
In a preferred embodiment of the invention, the hydrogen content of the end hydrogen containing silicone oil and the multi-hydrogen containing silicone oil after mixing is 0.05% to 1.0%, for example 0.05%, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, 0.55%, 0.6%, 0.65%, 0.7%, 0.75%, 0.8%, 0.85%, 0.9%, 0.95% or 1%.
The hydrogen content of the terminal hydrogen-containing silicone oil and the multi-hydrogen-containing silicone oil after mixing is preferably 0.1 to 0.5%, for example, 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45% or 0.5%.
In a preferred embodiment of the present invention, the microcapsule coated type hydrogen-containing silicone oil comprises a wall material and a core, and the core is hydrogen-containing silicone oil.
Preferably, the wall material is a thermoplastic material, preferably one or more of polymethyl methacrylate, PMMA, polystyrene, acrylonitrile-modified polystyrene, PSt-AN, polycarbonate, PC, cyclodextrin or thermoplastic silicone, such as PMMA, PSt, PSt-AN, PC, cyclodextrin, thermoplastic silicone, PMMA and PSt, PSt-AN and PC, cyclodextrin and thermoplastic silicone, PMMA, PSt and PSt-AN, PMMA, PSt and thermoplastic silicone, PC, cyclodextrin and thermoplastic silicone, or PMMA, PSt, PSt-AN and thermoplastic silicone.
The wall material is preferably thermoplastic silicone, preferably thermoplastic phenyl silicone and/or thermoplastic methylphenyl silicone, and more preferably thermoplastic methylphenyl silicone.
Preferably, the microcapsule coated type multi-hydrogen silicone oil has a wall material of thermoplastic silicone resin with a softening point of 60-120 ℃, such as 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃, 110 ℃ or 120 ℃.
The microcapsule-coated multi-hydrogen-containing silicone oil is preferably thermoplastic silicone resin with softening point of 70-100deg.C, such as 70deg.C, 75deg.C, 80deg.C, 85deg.C, 90deg.C, 95deg.C, 100deg.C
Preferably, the mass ratio of the capsule core to the capsule wall material is 2:8-4:6, for example 2.2:7.8, 2.5:7.5, 2.7:7.3, 3:7, 3.3:6.7, 3.5:6.5, 3.7:6.3 or 4:6.
Preferably, the microcapsule coated type hydrogen-containing silicone oil is spherical microcapsule.
Preferably, the microcapsule-coated polyhydrogenated silicone oil has an average particle size of 0.8 μm to 1.5 μm, for example, 0.8 μm, 0.9 μm,1 μm, 1.1 μm, 1.2 μm, 1.3 μm, 1.4 μm, or 1.5 μm.
Specifically, in the invention, the preparation method of the microcapsule coated type multi-hydrogen silicone oil comprises the following steps:
the wall material is dissolved in an organic solvent comprising one or more of toluene, methylene chloride, xylene, ethyl acetate, butyl acetate, chloroform or dichloroethane, preferably toluene and/or methylene chloride, more preferably a mixture of toluene and methylene chloride.
Adding the multi-hydrogen silicone oil, uniformly mixing, and drying into powder by a spray dryer.
Preferably, the powder is dried using a spray dryer whose drying conditions meet at least one of the following conditions: a dual-channel nozzle; nitrogen inlet temperature 90-100 deg.c and nitrogen outlet temperatureThe temperature is 40-50 ℃ and the nitrogen flow is 1.1-1.5 m 3 /min。
In the present invention, the nitrogen inlet temperature is, for example, 90 ℃, 91 ℃, 92 ℃, 93 ℃, 94 ℃, 95 ℃, 96 ℃, 97 ℃, 98 ℃, 99 ℃ or 100 ℃.
In the present invention, the nitrogen outlet temperature is, for example, 40 ℃, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, or 50 ℃.
In the present invention, the nitrogen flow rate is, for example, 1.1m 3 /min、1.2m 3 /min、1.3m 3 /min、1.4m 3 /min or 1.5m 3 /min。
Preferably, the mass ratio of the polyhydrogen silicone oil to the wall material is 2:8 to 4:6, for example, 2.2:7.8, 2.5:7.5, 2.7:7.3, 3:7, 3.3:6.7, 3.5:6.5, 3.7:6.3 or 4:6; the microcapsule-coated hydrogen-containing silicone oil obtained is spherical microcapsule having an average particle diameter of 0.8 μm to 1.5 μm, for example, 0.8 μm, 0.9 μm,1 μm, 1.1 μm, 1.2 μm, 1.3 μm, 1.4 μm or 1.5 μm.
In a preferred embodiment of the present invention, the heat conductive filler includes one or more of alumina, magnesia, aluminum hydroxide, magnesium hydroxide, aluminum nitride, silica, or silicon carbide, for example, alumina, magnesia, aluminum hydroxide, magnesium hydroxide, aluminum nitride, silica, silicon carbide, alumina and magnesia, alumina and aluminum hydroxide, alumina and aluminum nitride, magnesia and magnesium hydroxide, silica and silicon carbide, alumina, aluminum hydroxide and aluminum nitride, magnesia, aluminum hydroxide, magnesium hydroxide and aluminum nitride, or alumina, aluminum hydroxide, magnesium hydroxide, aluminum nitride and silicon carbide.
Preferably, the thermally conductive filler is spherical and/or non-spherical in shape, preferably spherical.
Preferably, the heat conductive filler is a heat conductive filler having an average particle diameter of 0.1 to 120 μm, for example, 0.1 μm,1 μm,10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm, 100 μm, 110 μm or 120 μm.
Preferably, the heat conducting filler is a heat conducting filler subjected to surface modification, preferably a heat conducting filler subjected to surface modification by hexadecyltrimethoxysilane.
Specifically, the mass of hexadecyltrimethoxysilane was 0.5% of the mass of the thermally conductive filler.
Preferably, the heat conductive filler is prepared from the following components in percentage by mass: 2:4, spherical alumina having an average diameter of 1 μm,10 μm and 80 μm.
The platinum catalyst is selected so as not to affect the hardness, heat conduction effect and mechanical property of the heat management material composition after being cured. The platinum catalyst is one or more of Karstedt catalyst, speier catalyst, ashby catalyst, lamoreaux catalyst or capsule platinum catalyst, preferably Karstedt catalyst.
Specifically, the Karstedt catalyst is as disclosed in USP3715334, the Speier catalyst is as disclosed in USP2823218, the Ashby catalyst is as disclosed in USP3159662, the Lamoreaux catalyst is as disclosed in USP3220972, the capsule type platinum catalyst is as disclosed in USP4481341a, USP4874667a, USP5009957a, USP5015716A, USP5017654A, EP0661349A2, USP2019100649A1 and USP 5789334A.
The selection, collocation and dosage of the inhibitor mainly influence the storage stability, the curing temperature and the curing time of the composition, and do not obviously influence the hardness, the heat conduction effect and the mechanical property of the heat management material composition after curing. The inhibitor is one or more of alkynol inhibitors, fumaric acid esters, maleic acid esters, butynedioic acid esters, carbene inhibitors or phosphite inhibitors, preferably alkynol inhibitors, and more preferably ethynyl cyclohexanol.
Specifically, the alkynol inhibitors such as the disclosures of USP3445420A, USP3989666 and USP4336364, the alkynol inhibitors such as the disclosures of USP2012-0328787A1, and of the alkynol inhibitors, ethynyl cyclohexanol, methylbutynol, etc., the fumaric acid esters, the maleic acid esters inhibitors such as the disclosures of USP4256870 and USP4533575A, the butynedioic acid esters inhibitors such as the disclosures of USP4533575A and USP4347346a, the carbene inhibitors such as the disclosures of Science 2002,298,204-206, the phosphite inhibitors such as the disclosures of USP4593084A and USP4256616, and mixtures of two or more inhibitors such as the disclosures of USP5945475A are commercially available.
Secondly, the invention provides a preparation method of the thermal management material, which comprises the following steps:
and uniformly mixing the low-viscosity vinyl silicone oil, the terminal hydrogen-containing silicone oil, the heat conducting filler, the microcapsule coated multi-hydrogen-containing silicone oil, the optional inhibitor and the optional platinum catalyst to obtain the thermal management material.
In the present invention, the optional means optional.
Preferably, firstly, uniformly mixing low-viscosity vinyl silicone oil, terminal hydrogen-containing silicone oil and a heat-conducting filler, adding an inhibitor, a platinum catalyst and microcapsule coated type multi-hydrogen-containing silicone oil, uniformly mixing, and defoaming to obtain the heat management material;
preferably, after the addition of the microcapsule-coated polyhydrogenated silicone oil, slow agitation is maintained in order to prevent capsule rupture.
Specifically, in the present invention, the preparation method is as follows: firstly, uniformly mixing a heat-conducting filler surface treating agent with low-viscosity vinyl silicone oil and hydrogen-containing silicone oil at the end, adding the heat-conducting filler at room temperature, and stirring to ensure that powder is slowly mixed into the silicone oil to form clusters; stirring for 10-20 min at room temperature, and adding inhibitor; and after continuously mixing uniformly, adding a platinum catalyst, uniformly mixing again, adding microcapsule coated multi-hydrogen silicone oil, slowly stirring for 5-15 min, and continuously stirring for 5-20 min under a vacuum condition for defoaming to obtain the target thermal management material composition.
The invention further provides application of the thermal management material as a heat conduction gasket, a heat conduction gel or a heat conduction pouring sealant. Specifically, the composition of the thermal management material is rolled, heated and cured to obtain the heat-conducting gasket, the heat-conducting gel or the heat-conducting pouring sealant.
Examples
The present invention will be described in further detail with reference to examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other. The present invention will be described in detail with reference to examples.
The raw materials used in the examples:
1) Low viscosity vinyl silicone oil: vinyl silicone oil with viscosity of 100 MPa.s and structure shown as A-1;
2) Terminal hydrogen silicone oil: the hydrogen content is 0.1 percent, and the structure is as shown in B-1;
3) Microcapsule coated multi-hydrogen silicone oil: the capsule wall material is methyl phenyl silicone resin, the capsule core is multi-hydrogen silicone oil with the viscosity of 50 MPa.s, the hydrogen content of 0.25% and the structure of B-2, the mass ratio of the capsule core to the capsule wall material is 3:7, and the microcapsule is a spherical capsule with the average particle diameter of 1.1 microns;
4) Platinum catalyst: selecting Karstedt catalyst, wherein the dosage of the platinum catalyst is fixed to 20ppm of the total mass of the thermal management material;
5) Inhibitors: acetylene cyclohexanol, with mass fixed at 0.1% of the total mass of the thermal management material;
6) And (3) a heat conducting filler: the mass ratio is 1:2:4, spherical alumina having an average diameter of 1 μm,10 μm and 80 μm, and a mass of 1500g of the heat conductive filler, and surface-treated with 7.5g of hexadecyltrimethoxysilane.
7) Uncoated polyhydrogenated silicone oils: the viscosity is 50 MPa.s, the hydrogen content is 0.25%, and the structure is shown as B-2.
Performance test:
1) Hardness: shore OO durometer measurement, 3 seconds reading after the durometer handle was pressed;
2) Oil bleeding performance: the sample pieces were cut out by a prototype cutter having a diameter of 3 cm. And controlling the deformation rate of the sample wafer by using a clamp for testing the compression deformation rate of the rubber, and laying printing paper under the sample wafer. Placing the clamp, the sample and the white paper in a baking oven at 120 ℃ for 72 hours, taking out, opening the clamp, observing the size of the oil seal on the white paper contacted with the sample, and if the size of the oil seal is the same as that of the sample, judging that oil seepage exists; if the oil seal is obviously larger than the sample, the oil seal is regarded as oil seepage;
3) Tensile strength and elongation at break: a sample piece having a thickness of 1mm was cut into dumbbell-shaped test pieces, and the tensile strength and tensile elongation were measured at a speed of 50mm/min using a SUNS UTM4104 universal material tester.
4) Thermal resistance: a coupon of 1mm thickness was cut into square pieces of 28mm side length with a die knife, and the thermal resistance of the thermal management sheet was characterized by Longwin9389 compliant with ASTM5470 standard, with a pressure set at 10psi.
The preparation process of microcapsule coated type multi-hydrogen silicone oil comprises the following steps:
70g of methyl phenyl silicone resin with a softening point of 92℃are dissolved in 40mL of toluene and 300mL of methylene chloride with stirring at room temperature, 30g of polyhydrogenated silicone oil are added and stirring is continued for 5 minutes until a homogeneous solution is formed. Drying the solution into powder by a spray dryer, wherein the specific conditions are as follows: double-channel nozzle, nitrogen inflow temperature of 95 ℃, outlet temperature of 45 ℃ and nitrogen flow of 1.3m 3 And/min. Spherical microcapsule coated type polyhydrogenated silicone oil with a coating rate of 30% and an average particle diameter of 1.1 μm was obtained.
The preparation process of the thermal management material comprises the following steps:
firstly, uniformly mixing hexadecyl trimethoxy silane, low-viscosity vinyl silicone oil and hydrogen-containing silicone oil at the end in a planetary mixer, adding a heat conducting filler at room temperature, and stirring to enable powder to be slowly mixed into the silicone oil to form clusters; stirring at room temperature for 15min, and adding inhibitor; and (3) adding a platinum catalyst after continuously mixing uniformly, uniformly mixing again, adding microcapsule coated multi-hydrogen silicone oil, slowly stirring for 10min, continuously stirring for 10min under vacuum condition, and discharging after defoaming, thus obtaining the thermal management material composition.
Test sample preparation:
preparing a sample block from the composition of the thermal management material by using a stainless steel mold with square holes with side length of 30mm and height of 6 mm; a sample sheet 1mm thick was rolled by a calender. Both the coupon and the coupon were cured by heating to 120℃for 1h and then allowed to stand in a standard atmosphere at 25℃and 50% RH for 24h.
The amounts of the raw materials of the respective components are shown in table 1, and the test samples obtained after curing the thermal management materials of example 1, example 2 and example 3 are designated as T1, T2 and T3, respectively, and the test samples obtained of comparative example 1, comparative example 2, comparative example 3 and comparative example 4 are designated as DB1, DB2, DB3 and DB4, respectively.
Table 1 shows the amounts of the components used in examples 1 to 3 and comparative examples 1 to 4 and the hardness and oil bleeding test data of the prepared samples.
TABLE 1 examples 1 to 3 and comparative examples 1 to 4
In table 1: the microcapsule coated type multi-hydrogen silicone oil is the mass of the capsule core, and does not comprise the mass of the capsule wall; r is the sum of the amounts of Si-H in the polyhydrogenated silicone oil and the terminal hydrogen-containing silicone oil and CH in the low-viscosity vinyl silicone oil 2 Ratio of amounts of substance of =ch-; r is the ratio of the amount of Si-H in the terminal hydrogen containing silicone oil to the amount of Si-H in the polyhydrogen containing silicone oil.
As shown in table 1, R <1:2.2 and R >1.25 of comparative example 1, the thermal management material was too low in hardness after curing, had no mechanical strength, and was severe in oil bleeding; when R >1:1.2 and R <0.75 of comparative example 2, the thermal management material after curing had a hardness of 80Shore OO, which was too high, far outside the conventional requirements of thermally conductive gaskets.
As shown in table 1, the test results of comparative examples 2 and 3, and examples 3 and 4, examples 2 and 3 obtained cured samples T2 and T3 using the microcapsule-coated polyhydrogen silicone oil, T2 having a hardness of 15Shore OO and T3 having a hardness of 20Shore OO; comparative example 3 and comparative example 4 cured samples DB3 and DB4 were obtained using uncoated polyhydrogenated silicone oil, DB3 having a hardness of 40Shore OO and db4 having a hardness of 50Shore OO; as can be seen from comparison of the performance test data, the hardness of the composition containing the microcapsule coated type multi-hydrogen-containing silicone oil after curing is lower than that of the composition only without the coating type multi-hydrogen-containing silicone oil, and the T2 and T3 have no oil seepage phenomenon.
Table 2 shows the test data of the tensile strength, elongation at break and thermal resistance of examples 2 to 3 and comparative examples 3 to 4.
Table 2: examples 2 to 3 and comparative examples 3 to 4
As shown in table 2, T2 had a breaking strength of 0.25 and a breaking elongation of 320%, and DB3 had a breaking strength of 0.28 and a breaking elongation of 260%; the breaking strength of T3 is 0.18, the breaking elongation is 180 percent, and the breaking strength of DB4 is 0.2, the breaking elongation is 120 percent; the sample cured by the microcapsule coated multi-hydrogen silicone oil thermal management material has better flexibility, and is not easy to break and damage in the gasket assembly process. In terms of heat conduction effect, it is known from the comparison of the thermal resistances of T2 and DB3 and the comparison of the thermal resistances of T3 and DB4 that the sample heat conduction performance after the heat management material cured by the microcapsule-coated multi-hydrogen-containing silicone oil is better due to lower hardness.
The above description is only illustrative of the preferred embodiments of the present invention and of the principles of the technology employed. It will be appreciated by persons skilled in the art that the scope of the invention referred to in the present invention is not limited to the specific combinations of the technical features described above, but also covers other technical features formed by any combination of the technical features described above or their equivalents without departing from the inventive concept. Such as the above-mentioned features and the technical features disclosed in the present invention (but not limited to) having similar functions are replaced with each other.
Claims (26)
1. A thermal management material, comprising the following raw materials:
low viscosity vinyl silicone oils;
a thermally conductive filler;
the multi-hydrogen silicone oil is microcapsule coated multi-hydrogen silicone oil; and
end hydrogen silicone oil;
the sum of the amounts of Si-H in the polyhydrogenated silicone oil and the terminal hydrogen-containing silicone oil being equal to CH in the low-viscosity vinyl silicone oil 2 =ch-, andthe ratio R of the amounts of substances is 1:1.2-1:2.2;
the ratio r of the amount of Si-H in the hydrogen-containing silicone oil at the end to the amount of Si-H in the hydrogen-containing silicone oil at the end is 0.75-1.25;
the low-viscosity vinyl silicone oil is vinyl silicone oil with the viscosity of 50-65000MPa.S;
the thermal management material further comprises a platinum catalyst, wherein the mass of platinum element in the platinum catalyst is 3-20 ppm of the total mass of the thermal management material;
the mass of the heat conducting filler is 100-2500 parts based on 100 parts of the mass of the low-viscosity vinyl silicone oil;
the microcapsule coated type multi-hydrogen-containing silicone oil comprises a capsule wall material and a capsule core, wherein the capsule core is the multi-hydrogen-containing silicone oil, and the capsule wall material of the microcapsule coated type multi-hydrogen-containing silicone oil is thermoplastic silicone resin with a softening point of 60-120 ℃.
2. The thermal management material according to claim 1, further comprising an inhibitor, wherein the inhibitor is 0.01 to 0.1 parts by mass based on 100 parts by mass of the low viscosity vinyl silicone oil.
3. The thermal management material according to claim 1, wherein said low-viscosity vinyl silicone oil is one or more of compounds having a structure shown as a-1, a-2 or a-3;
。
4. the thermal management material according to claim 1, wherein the hydrogen-terminated silicone oil is a compound having a structure as shown in B-1;
。
5. the thermal management material according to claim 1, wherein the hydrogen-rich silicone oil is a compound having a structure as shown in B-2 and/or B-3;
。
6. the thermal management material of claim 1, wherein the terminal hydrogen-containing silicone oil and the multi-hydrogen-containing silicone oil have a total hydrogen content of 0.05% -1.0%.
7. The thermal management material according to claim 6, wherein the total hydrogen content of the terminal hydrogen-containing silicone oil and the multi-hydrogen-containing silicone oil is 0.1 to 0.5%.
8. The thermal management material of claim 1, wherein the wall material is thermoplastic methylphenyl silicone.
9. The thermal management material of claim 1, wherein the microcapsule-coated hydrogen-containing silicone oil has a wall material of thermoplastic silicone resin with a softening point of 70-100 ℃.
10. The thermal management material of claim 1, wherein the mass ratio of the capsule core to the capsule wall material is 2:8-4:6.
11. The thermal management material of claim 1, wherein the microcapsule-coated polyhydrogen silicone oil is spherical microcapsules.
12. The thermal management material of claim 11, wherein the microcapsule-coated hydrogen-containing silicone oil has an average particle diameter of 0.8-1.5 μm.
13. The thermal management material of claim 1, wherein the thermally conductive filler comprises one or more of aluminum oxide, magnesium oxide, aluminum hydroxide, magnesium hydroxide, aluminum nitride, silicon dioxide, or silicon carbide.
14. The thermal management material of claim 1, wherein the thermally conductive filler is spherical and/or non-spherical in shape.
15. The thermal management material of claim 14, wherein the thermally conductive filler is spherical in shape.
16. The thermal management material of claim 15, wherein the thermally conductive filler is a thermally conductive filler having an average particle size of 0.1-120 μm.
17. The thermal management material of claim 1, wherein the thermally conductive filler is a surface modified thermally conductive filler.
18. The thermal management material of claim 17, wherein the thermally conductive filler is a hexadecyltrimethoxysilane surface modified thermally conductive filler.
19. The thermal management material of claim 1, wherein the platinum catalyst is one or more of Karstedt catalyst, speier catalyst, ashby catalyst, lamoreaux catalyst, or encapsulated platinum catalyst.
20. The thermal management material of claim 19, wherein the platinum catalyst is a Karstedt catalyst.
21. The thermal management material of claim 2, wherein the inhibitor is one or more of an acetylenic alcohol inhibitor, a fumarate, a maleate, a butynedioate inhibitor, a carbene inhibitor, or a phosphite inhibitor.
22. The thermal management material of claim 21, wherein the inhibitor is an alkynol inhibitor.
23. The thermal management material of claim 22, wherein the inhibitor is acetylene cyclohexanol.
24. The method of any one of claims 1 to 23, wherein the thermal management material is obtained by uniformly mixing a low viscosity vinyl silicone oil, a terminal hydrogen silicone oil, a thermally conductive filler, a microcapsule coated multi-hydrogen silicone oil, an optional inhibitor, and an optional platinum catalyst.
25. The method for preparing a thermal management material according to claim 24, wherein the thermal management material is prepared by mixing low viscosity vinyl silicone oil, terminal hydrogen-containing silicone oil and heat conductive filler uniformly, adding optional inhibitor, optional platinum catalyst and microcapsule coated multi-hydrogen-containing silicone oil, mixing uniformly, and defoaming.
26. Use of a thermal management material according to any of claims 1-23, wherein the thermal management material is used for the preparation of thermally conductive gaskets, thermally conductive gels and thermally conductive potting gums.
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| JPS6131460A (en) * | 1984-07-25 | 1986-02-13 | Lion Corp | Preparation of solid silicone oil |
| CN105440692A (en) * | 2015-12-14 | 2016-03-30 | 华南理工大学 | Microcapsule-type self-repairing polysiloxane elastomer and preparation method thereof |
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| CN112552691A (en) * | 2020-12-16 | 2021-03-26 | 上海阿莱德实业股份有限公司 | Single-component curing type heat-conducting gel composition and application thereof |
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| US7569625B2 (en) * | 2006-06-02 | 2009-08-04 | The Board Of Trustees Of The University Of Illinois | Self-healing elastomer system |
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| JPS6131460A (en) * | 1984-07-25 | 1986-02-13 | Lion Corp | Preparation of solid silicone oil |
| CN105440692A (en) * | 2015-12-14 | 2016-03-30 | 华南理工大学 | Microcapsule-type self-repairing polysiloxane elastomer and preparation method thereof |
| CN108130040A (en) * | 2017-12-27 | 2018-06-08 | 深圳航美新材料科技有限公司 | A kind of modified double components casting glue and preparation method thereof |
| CN112552691A (en) * | 2020-12-16 | 2021-03-26 | 上海阿莱德实业股份有限公司 | Single-component curing type heat-conducting gel composition and application thereof |
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