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WO2024088062A1 - Composition d'organosilicium de type à addition thermoconductrice pour l'enrobage - Google Patents

Composition d'organosilicium de type à addition thermoconductrice pour l'enrobage Download PDF

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Publication number
WO2024088062A1
WO2024088062A1 PCT/CN2023/123962 CN2023123962W WO2024088062A1 WO 2024088062 A1 WO2024088062 A1 WO 2024088062A1 CN 2023123962 W CN2023123962 W CN 2023123962W WO 2024088062 A1 WO2024088062 A1 WO 2024088062A1
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Prior art keywords
thermally conductive
conductive filler
polysiloxane
parts
composition according
Prior art date
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Ceased
Application number
PCT/CN2023/123962
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English (en)
Chinese (zh)
Inventor
雷丽娟
郭鹏
申晶
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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Jiangxi Bluestar Xinghuo Silicone Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure

Definitions

  • the present application relates to a heat-conductive addition-type silicone composition for potting, a method for preparing the silicone composition, and a product made from the silicone composition.
  • the silicone composition of the present invention can be used in the field of new energy.
  • Thermally conductive addition-type silicone potting compound has been used for heat dissipation management in the new energy field. It can be deeply potted and no low molecular weight substances are produced during the curing process. The shrinkage rate is extremely low, and it can also be heated and cured quickly. Thermally conductive silicone potting compound can improve the thermal management performance of high-power equipment by quickly dissipating heat, protecting fragile components and reducing stress.
  • the first aspect of the present application relates to a thermally conductive addition-type silicone composition for potting, comprising:
  • a thermally conductive filler the particles of which are treated with oligomers or hydrolysates of vinyltrialkoxysilane and have a D50 particle size in the range of 0.5-50 ⁇ m, preferably 1-40 ⁇ m, for example 5-30 ⁇ m.
  • the addition-type silicone potting composition containing the component can have improved thermal conductivity and excellent flowability.
  • the thermal conductivity of such a potting composition can reach 0.6W/m ⁇ K-2.0W/m ⁇ K, and the thixotropic index is 1.0-1.5, thus having good flowability.
  • component E) an anti-settling agent comprising white carbon treated with at least one polysiloxane and silazane compound containing at least two vinyl groups bonded to silicon atoms per molecule may be added.
  • the silicone composition for encapsulation prepared by the present invention can further have excellent storage stability. After long-term storage (e.g., ⁇ 6 months), it has excellent anti-settling performance and no lumps on the bottom, thus being able to give the material excellent comprehensive properties such as electrical insulation, flame retardancy and mechanical properties after curing.
  • the thermally conductive addition-type silicone composition according to the present invention is particularly suitable for thermally conductive potting of thermal management components or electronic components in new energy fields such as wind power generation motor systems, photovoltaic energy storage systems, new energy vehicle battery modules, and on-board chargers.
  • the second aspect of the present application relates to a product comprising a thermally conductive potting compound formed from the organic silicon composition of the present invention.
  • the product is preferably a thermal management component or electronic component in the new energy field such as a wind power generation motor system, a photovoltaic energy storage system, a new energy vehicle battery module, and an on-board charger.
  • the third aspect of the present application relates to an anti-settling agent, which comprises at least one White carbon treated with polysiloxane and silazane compounds containing at least two vinyl groups bonded to silicon atoms.
  • the fourth aspect of the present application relates to the use of the above-mentioned thermally conductive filler and anti-settling agent in a thermally conductive silicone composition for potting, for improving the thermal conductivity, thixotropy, flowability and/or storage stability of the potting compound.
  • Component A) in the present application is a vinyl-containing polysiloxane, wherein the vinyl group may be located at any position on the main chain of the polysiloxane, for example, at the end or in the middle of the molecular chain or at both ends and in the middle.
  • the vinyl-containing polysiloxane comprises:
  • R 1 represents a C 2-12 , preferably a C 2-6 alkenyl group, most preferably a vinyl group or an allyl group,
  • Z may identically or differently represent a monovalent hydrocarbon group having 1 to 30, preferably 1 to 12, carbon atoms, preferably selected from C 1-8 alkyl groups, including alkyl groups optionally substituted by at least one halogen atom, and also preferably selected from aryl groups, especially C 6-20 aryl groups,
  • a is 1 or 2
  • b is 0, 1 or 2
  • the sum of a+b is 1, 2 or 3
  • Z has the meaning as described above and c is 0, 1, 2 or 3.
  • Z may be selected from methyl, ethyl, propyl, 3,3,3-trifluoropropyl, phenyl, xylyl and tolyl, etc.
  • at least 60 mol% (or by number) of the groups Z are methyl.
  • Preferred vinyl-containing polysiloxanes suitable for the present invention may have a viscosity of at least 50 mPa ⁇ s and preferably less than 1200 mPa ⁇ s, for example 100-500 mPa ⁇ s. They are also commonly referred to as vinyl silicone oils. In the present application, all viscosities are related to dynamic viscosity values and can be measured, for example, in a known manner at 25° C. using conventional equipment such as a TA rheometer.
  • the vinyl content of the component is 0.1-2 wt%, more preferably 0.37 wt-1.2 wt%.
  • the vinyl group-containing polysiloxane (a1) may be formed only of the unit of formula (I-1) or may additionally contain the unit of formula (I-2).
  • the vinyl group-containing polysiloxane may be linear, branched or cyclic.
  • siloxy unit of formula (I-1) examples are vinyldimethylsiloxy, vinylphenylmethylsiloxy, vinylmethylsiloxy and vinylsiloxy units.
  • siloxy unit of formula (I-2) examples are SiO 4/2 unit, dimethylsiloxy, methylphenylsiloxy, diphenylsiloxy, methylsiloxy and phenylsiloxy.
  • vinyl-containing polysiloxane examples include linear or cyclic compounds such as dimethyl polysiloxane (having dimethyl vinyl silyl terminal groups), (methyl vinyl) (dimethyl) polysiloxane copolymers (having trimethyl silyl terminal groups), (methyl vinyl) (dimethyl) polysiloxane copolymers (having dimethyl vinyl silyl terminal groups) and cyclic methyl vinyl polysiloxanes.
  • the vinyl polysiloxane may be vinyl-terminated polydimethylsiloxane (Vi-PDMS) or vinyl-terminated polymethylvinylsiloxane (Vi-PMVS).
  • component B) is a hydrogen-containing polysiloxane which must have at least two hydrogen atoms bonded to the same or different silicon atoms in order to undergo a crosslinking reaction with the vinyl polysiloxane of component A). Therefore, as the hydrogen-containing polysiloxane component, at least one hydrogen-containing polysiloxane having at least two hydrogen atoms bonded to the same or different silicon atoms per molecule or a mixture of at least two hydrogen-containing polysiloxanes having at least one hydrogen atom bonded to the same or different silicon atoms per molecule can be used.
  • the silicon hydride groups may be located at any position on the polysiloxane main chain, for example, at the ends or in the middle of the molecular chain or at both ends and in the middle.
  • the hydrogen-containing polysiloxane having SiH groups can undergo a crosslinking reaction with component A), i.e., a cured product is formed by reacting the SiH groups in the component with the vinyl groups in component A).
  • component B at least one hydrogen-containing polysiloxane having two, three or more SiH groups per molecule is used.
  • the hydrogen-containing polysiloxane comprises
  • R2 may be identical or different and represent a monovalent hydrocarbon group, which is preferably selected from C1-8 alkyl groups, including alkyl groups optionally substituted by at least one halogen atom, and is also preferably selected from aryl groups, especially C6-20 aryl groups,
  • d is 1 or 2
  • e is 0, 1 or 2
  • the sum of d+e is 1, 2 or 3
  • R 3 has the meaning as described above and f is 0, 1, 2 or 3.
  • R 3 can be selected from methyl, ethyl, propyl, 3,3,3-trifluoropropyl, phenyl, xylyl and tolyl.
  • the dynamic viscosity of the component B) or the hydrogen-containing polysiloxane or the mixture thereof is at least 1 mPa ⁇ s and preferably between 3 and 1000 mPa ⁇ s, more preferably 5-100 mPa ⁇ s.
  • the hydrogen-containing polysiloxane may be formed only of the unit of formula (I-3) or may additionally contain the unit of formula (I-4).
  • the hydrogen-containing polysiloxane may have a linear, branched or cyclic structure.
  • Examples of units of formula (I-3) are H(CH 3 ) 2 SiO 1/2 , HCH 3 SiO 2/2 and H(C 6 H 5 )SiO 2/2 .
  • Examples of the unit of formula (I-4) may be the same as those given above for the unit of formula (I-2).
  • Examples of usable hydrogen-containing polysiloxanes include linear or cyclic compounds such as dimethylpolysiloxane (having hydrodimethylsilyl terminal groups), copolymers having (dimethyl)(hydrogenmethyl)polysiloxane units (having trimethylsilyl terminal groups), copolymers having (dimethyl)(hydrogenmethyl)polysiloxane units (having hydrodimethylsilyl terminal groups), hydromethylpolysiloxanes having trimethylsilyl terminal groups, and cyclic hydromethylpolysiloxanes.
  • linear or cyclic compounds such as dimethylpolysiloxane (having hydrodimethylsilyl terminal groups), copolymers having (dimethyl)(hydrogenmethyl)polysiloxane units (having trimethylsilyl terminal groups), copolymers having (dimethyl)(hydrogenmethyl)polysiloxane units (having hydrodimethylsilyl terminal groups), hydromethylpolysi
  • the hydrogen-containing polysiloxane may be a dimethylpolysiloxane containing a hydrogenated dimethylsilyl terminal group and an organopolysiloxane containing at least three hydrogenated silyl groups. mixture.
  • the component B) is at least one of hydrogen-terminated polydimethylmethylhydrogensiloxane H1, polydimethylmethylhydrogensiloxane H2 and hydrogenated Q resin H3. More preferably, the hydrogen content of H1 is 0.2wt-0.8wt%, the molar percentage of methylhydrogen chain segments in H2 is 3-50% and its viscosity ranges from 10-35mPa ⁇ s. Hydrogenated Q resin H3 can be commercially obtained, such as HQM-105 or HQM-107 from Gelest.
  • the catalyst C) of at least one platinum group metal may be composed of at least one platinum group metal or compound, and its amount should be sufficient to promote the addition reaction of the alkenyl group in component A) and the silyl hydrogen in component B) to cure.
  • the amount of the catalyst may be in the range of 0.1-1,000 ppm, preferably 1-50 ppm, based on the weight of the metal.
  • Platinum group metals include ruthenium, rhodium, palladium, osmium and iridium in addition to platinum.
  • the catalyst may be composed of the following components: platinum group metals or compounds thereof or combinations thereof.
  • Such catalysts include, but are not limited to: platinum black, chloroplatinic acid, platinum dichloride, chloroplatinic acid monohydric alcohol reactant.
  • a compound of platinum and rhodium is used. Platinum is generally the preferred catalyst.
  • a key component of the composition of the present invention is a thermally conductive filler, the particles of which are treated with oligomers or hydrolysates of vinyltrialkoxysilane and have a D50 particle size range of 0.5-50 microns, preferably 1-40 microns, such as 5-30 microns.
  • oligomers or hydrolyzates of vinyltrialkoxysilane as powder treatment agents for thermally conductive fillers is more suitable for improving the flowability of silicone compositions than other conventional treatment agents such as ⁇ -glycidyloxypropyltrimethoxysilane, ⁇ -methacryloxypropyltrimethoxysilane or other alkoxysilanes such as n-octyltrimethoxysilane, n-decyltrimethoxysilane and hexadecyltrimethoxysilane.
  • the "alkoxy" in the oligomer or hydrolyzate of the vinyl trialkoxysilane can be an alkoxy group including C1-C12, such as C2-C8. Therefore, preferred oligomers or hydrolyzates of vinyl trialkoxysilane include oligomers or hydrolyzates of vinyl trimethoxysilane, vinyl triethoxysilane and vinyl tripropoxysilane.
  • the vinyl content of the oligomer or hydrolyzate of the vinyltrialkoxysilane is It is 8-16 wt %, and preferably has a viscosity of 2-25 mPa ⁇ s, such as 5-15 mPa ⁇ s.
  • the thermally conductive filler itself includes, but is not limited to: spherical alumina, quasi-spherical alumina, angular alumina, aluminum hydroxide, aluminum nitride, boron nitride, silicon carbide, magnesium oxide, zinc oxide, spherical silica, rounded crystalline silicon powder, crystalline silicon powder, etc., preferably one or more of spherical alumina, quasi-spherical alumina, spherical silica, and rounded crystalline silicon powder.
  • the D50 particle size of thermal conductive fillers should be in the range of 0.5-50 microns to ensure the best thixotropic index and viscosity.
  • the D50 particle size refers to the particle size value corresponding to the cumulative distribution percentage reaching 50%. It is one of the important indicators reflecting the particle size characteristics of powders, also known as the median diameter or median particle size.
  • the measurement equipment for D50 is a laser particle size detector.
  • the volume percentage of the thermally conductive filler with a D50 particle size range of 15 ⁇ m or more is 80-95%, preferably 82-92%
  • the volume percentage of the thermally conductive filler with a D50 particle size range of 6 ⁇ m to less than 15 ⁇ m is 5-20%, preferably 8-16%
  • the volume percentage of the thermally conductive filler with a D50 particle size range of less than 6 ⁇ m is 0-2%, for example 0.5-1.6%.
  • the treatment of the thermally conductive filler can be achieved by fully mixing the oligomer or hydrolyzate of vinyltrialkoxysilane with the particles of the thermally conductive filler under stirring. This mixing can be performed alone or in situ, and can be performed in the presence of other components such as anti-settling agents or catalysts, thereby achieving the treatment of the thermally conductive particles.
  • the treated thermally conductive particles and the anti-settling agent and/or catalyst can advantageously constitute a single component.
  • the amount of the treating agent, ie, the oligomer or hydrolyzate of vinyltrialkoxysilane is 0.15%-1.5%, preferably 0.20%-1.0%, based on the weight of the thermally conductive filler.
  • the total content of the thermally conductive filler is 65-96 wt %, such as 70-90 wt %, based on the total weight of the composition.
  • composition of the invention may also advantageously comprise an anti-settling agent component E) comprising white carbon treated with at least one polysiloxane and silazane compound comprising at least two vinyl groups bonded to silicon atoms per molecule.
  • an anti-settling agent component E comprising white carbon treated with at least one polysiloxane and silazane compound comprising at least two vinyl groups bonded to silicon atoms per molecule.
  • White carbon black is a general term for powdered products of amorphous silicic acid and silicates, including precipitated silica, fumed silica and ultrafine silica gel.
  • the white carbon black is selected from fumed silica.
  • the white carbon black may generally have, for example, a primary particle size of about 3-50 nanometers and an aggregate particle size of about 150-400 nanometers.
  • the white carbon black suitable for the present invention (such as the preferred fumed silica) may be a single white carbon black or a mixture of a plurality of white carbon blacks having different BET specific surface areas.
  • the white carbon black suitable for the present invention may be hydrophilic or hydrophobic, preferably hydrophilic.
  • the vinyl-containing polysiloxane used for treating white carbon may be those of component A) as described above, and the silazane compound includes, for example, hexamethyldisilazane or hexaphenylcyclotrisilazane.
  • the anti-settling agent can be prepared by mixing a vinyl-containing polysiloxane such as a vinyl silicone oil having a viscosity in the range of 100-500 mPa ⁇ s and a silazane compound with white carbon under stirring conditions.
  • the mixing process can be carried out in water and can preferably be carried out under conditions of elevated temperature and/or application of an inert gas such as nitrogen.
  • the content of the anti-settling agent may be in the range of 0.2-1.0%, preferably 0.3-0.8%, based on the total weight of the composition.
  • the potting silicone composition may further contain a polymerization inhibitor.
  • inhibitors for addition-type polysiloxane systems are acetylenic alcohol inhibitors or vinyl inhibitors, or a mixture of these two inhibitors in a specific ratio.
  • vinyl type inhibitor may be: tetramethyldivinylsilane, polyvinyl silicone oil, tetramethyltetravinylcyclotetrasiloxane.
  • acetylenic alcohol inhibitors include: 3-butyn-2-ol, 1-pentyn-3-ol, 1-hexyn-3-ol, 1-heptyn-3-ol, 5-methyl-1-hexyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, 1-ethynyl-1-cyclopentanol, 1-ethynyl-1-cyclohexanol, 1-ethynyl-1-cycloheptanol, 3-ethyl-1-hexyn-3-ol, 3-ethyl-1-heptyn-3-ol, 3-isobutyl-5-methyl-1-hexyn-3-ol, 3,4-dimethyl-1-hexyn-3-ol.
  • components A) and B) is determined according to the molar ratio of silyl hydride groups to vinyl groups.
  • components A) and B) are used in such amounts in the organosilicon composition that the molar ratio of silyl hydride groups to vinyl groups is in the range of 0.5-5, preferably 0.8-4 and for example 1-3.
  • composition of the present invention may also include other additives, including but not limited to: any one or more of color paste, leveling agent, mildewproof agent, chain extender, wetting agent, etc.
  • the preferred chain extender may be, for example, hydrogen-terminated polydimethylsiloxane, whose hydrogen content is 0.08wt-0.2wt% and viscosity is 8-50mPa ⁇ s.
  • the wetting agent includes but is not limited to at least one of alkoxy-terminated polydimethylsiloxane, polyether-modified silicone oil, dimethyl silicone oil, and hydroxyl-terminated silicone oil.
  • the silicone composition for injection of the present invention can be formulated into multiple parts, preferably two parts.
  • the thermally conductive silicone composition consists of a first part and a second part, wherein the first part includes a vinyl-containing polysiloxane and the second part includes a hydrogen-containing polysiloxane.
  • the thermally conductive filler and anti-settling agent can be distributed in the first or second part or both.
  • other additives can also be formulated into the first or second part according to properties and needs.
  • the first part may include 65-96 parts of thermal conductive filler, 0.15-3.0 parts of wetting agent, 0.2-0.8 parts of anti-settling agent, 3-30 parts of vinyl-containing polysiloxane, 0.005-0.01 parts of catalyst and 0.2-0.8 parts of other auxiliary agents;
  • the second component may include 65-96 parts of thermal conductive filler, 0.2-0.8 parts of anti-settling agent, 2-20 parts of vinyl-containing polysiloxane, 0.5-2 parts of hydrogen-containing polysiloxane, 2-15 parts of chain extender, 0.01-0.1 parts of inhibitor and 0.2-0.8 parts of other auxiliary agents, etc.
  • the two parts may be mixed in equal weight ratios.
  • composition according to the invention can be obtained by mixing the components by mixing and stirring techniques known in the art, using heating and cooling operations as required and applying a vacuum during mixing.
  • Embodiment 1 is a diagrammatic representation of Embodiment 1:
  • the mixture was cooled to below 50°C under vacuum stirring, and 0.2 parts by mass of tetramethyltetravinylcyclotetrasiloxane, 68 parts by mass of hydrogen-terminated polydimethylsiloxane (hydrogen content of 0.2wt%, viscosity of 20mPa ⁇ s) and 9 parts by mass of hydrogen-terminated polydimethylmethylhydrogensiloxane (hydrogen content of 0.5wt%, viscosity of 10mPa ⁇ s) were added to the mixture.
  • the mixture was mixed under vacuum for 30 minutes, and component B-1 was obtained after removing the vacuum.
  • components A-1 and B-1 were mixed evenly in a mass ratio of 1:1, degassed and poured into a mold, and cured at room temperature for 20 hours or heated at 80°C for 30 minutes, and then the product performance was tested.
  • the results are shown in Table 1.
  • Embodiment 2 is a diagrammatic representation of Embodiment 1:
  • A-2 and B-2 were mixed evenly in a mass ratio of 1:1, degassed and poured into a mold, and cured at room temperature for 20 hours or heated at 80°C for 30 minutes, and then the product performance was tested.
  • the results are shown in Table 1.
  • Embodiment 3 is a diagrammatic representation of Embodiment 3
  • the mixture is stirred in vacuum and cooled to below 50°C, 0.1 parts by mass of tetramethyl tetravinyl cyclotetrasiloxane, 53 parts by mass of hydrogen-terminated polydimethylsiloxane (hydrogen content of 0.2wt%, viscosity of 20mPa ⁇ s) and 8 parts by mass of hydrogen-terminated polydimethylmethylhydrogensiloxane (hydrogen content of 0.5wt%, viscosity of 10mPa ⁇ s) are added to the mixture, and the mixture is mixed in vacuum for 30 minutes, and the component B-3 is obtained after the vacuum is released;
  • A-3 and B-3 were mixed evenly in a mass ratio of 1:1, degassed and poured into a mold, and cured at room temperature for 20 hours or heated at 80°C for 30 minutes, and then the product performance was tested.
  • the results are shown in Table 1.
  • Example 2 was repeated, except that an equal mass portion of ⁇ -glycidyloxypropyltrimethoxysilane was used instead of vinyltrimethoxysilane oligomer (6 mPa ⁇ s), and other components and proportions remained unchanged.
  • the product performance test results are shown in Table 1.
  • Example 2 was repeated, except that an equal mass portion of ⁇ -methacryloxypropyltrimethoxysilane was used instead of vinyltrimethoxysilane oligomer (6 mPa ⁇ s), and other components and proportions remained unchanged.
  • the product performance test results are shown in Table 1.
  • Example 2 was repeated, except that n-decyltrimethoxysilane was used in place of vinyltrimethoxysilane oligomer (6 mPa ⁇ s) in equal parts by mass, and other components and proportions remained unchanged.
  • the product performance test results are shown in Table 1.
  • the other components and proportions remained unchanged.
  • the product performance test results are shown in Table 1.
  • Example 3 was repeated without adding the anti-settling agent AS.
  • the product performance test results are shown in Table 1.
  • Example 3 was repeated, but 1.2 parts of anti-settling agent AS was added.
  • the product performance test results are shown in Table 1.
  • Example 3 using untreated hydrophilic fumed silica
  • the anti-settling agent AS was replaced in equal parts by mass.
  • the product performance test results are shown in Table 1.
  • Thixotropic index Using a Haake rheometer C20/2° rotor product, the ratio of the viscosity at a shear rate of 10.0 s -1 to the viscosity at a shear rate of 1.0 s -1 is taken as the thixotropic index, using the ASTM D1824 standard.
  • Thermal conductivity After mixing the prepared A components and B components in a mass ratio of 1:1, degas and pour into the corresponding mold, and cure at room temperature for 20 hours or heat and cure at 80°C for 30 minutes to obtain a block with a length*width*height of 80mm*80mm*6mm. Use Hotdisk to test the thermal conductivity obtained, using ISO22007-2 standard;
  • Anti-sedimentation pour the prepared A component and B component into two 1L volumes Place the mixture in a round plastic can at room temperature (25°C) for 6 months. Test 3 samples in parallel for each group of samples to observe the oil phase precipitation. Use a tongue depressor to stir the components and observe whether there is powder compaction at the bottom. If it can be easily stirred and the oil phase precipitation is not obvious, the anti-sedimentation performance is OK; if the bottom is compacted and cannot be stirred or is difficult to stir, the anti-sedimentation performance is NG.

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Abstract

La présente invention concerne une composition d'organosilicium de type à addition thermoconductrice pour l'enrobage, un procédé de préparation de la composition d'organosilicium, et un produit préparé à partir de la composition d'organosilicium. La composition d'organosilicium comprend : A) au moins un polysiloxane contenant, par molécule, au moins deux groupes vinyle liés à un atome de silicium ; B) au moins un polysiloxane contenant de l'hydrogène comportant, par molécule, au moins un atome d'hydrogène lié à des atomes de silicium identiques ou différents, à condition que le composant comporte un total d'au moins deux atomes d'hydrogène liés à des atomes de silicium identiques ou différents ; C) au moins un catalyseur métallique du groupe du platine ; et D) une charge thermoconductrice, les particules de la charge thermoconductrice étant traitées à l'aide d'un oligomère ou d'un hydrolysat de vinyltrialcoxysilane et présentant une taille des particules D50 allant de 0,5 à 50 microns.
PCT/CN2023/123962 2022-10-27 2023-10-11 Composition d'organosilicium de type à addition thermoconductrice pour l'enrobage Ceased WO2024088062A1 (fr)

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CN202211329234.1 2022-10-27
CN202211329234.1A CN115612446B (zh) 2022-10-27 2022-10-27 灌封用导热加成型有机硅组合物

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