CN115216153A - High-performance heat-conducting silicone grease and preparation method and application thereof - Google Patents
High-performance heat-conducting silicone grease and preparation method and application thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- 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
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- 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
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- 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
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
- C08K3/28—Nitrogen-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention provides a high-performance heat-conducting silicone grease, which comprises: a matrix and a filler; the matrix is selected from one or more of dimethyl silicone oil, benzyl silicone oil, alkoxy silicone oil and hydroxyl silicone oil; the filler is a heat-conducting filler; the filler is selected from one or more of aluminum, silver, zinc oxide, aluminum nitride, boron nitride, silicon nitride, diamond, carbon nano tube and nano graphite. The invention provides the heat-conducting silicone grease with the isotropic, dynamically uniform and stable matrix-filler composite structure, and the heat-conducting silicone grease provided by the invention has good wire drawing property and thixotropy on the basis of realizing high heat conduction, low heat resistance, low viscosity and high reliability, and realizes the application of the heat-conducting silicone grease in ultrathin and deformable interfaces. The invention also provides application of the high-performance heat-conducting silicone grease.
Description
Technical Field
The invention belongs to the technical field of heat-conducting silicone grease, and particularly relates to high-performance heat-conducting silicone grease as well as a preparation method and application thereof.
Background
With the development of modern electronic information technology and the continuous increase of packaging density, the problem of overheating has become a bottleneck limiting the development of electronic technology. The ideal state of the heat sink for optimum heat dissipation is to achieve close surface contact with the heat source. However, due to the limitation of the machining accuracy, there are actually many gaps between the contact surfaces of the two. The thermal resistance of the air filling these gaps is large, which can greatly reduce the heat dissipation effect. The high thermal conductivity thermal interface material can well fill the gaps, and the heat dissipation effect is obviously improved. The heat-conducting silicone grease is used as a paste thermal interface material, can realize ultrathin interface thickness and ultralow interface thermal resistance, and is widely applied between electronic components and heat dissipation plates or radiators.
On the one hand, the further miniaturization and high efficiency of the current electronic products put forward higher requirements on the heat-conducting performance of the heat-conducting silicone grease; on the other hand, it is desirable that the thermally conductive silicone grease be suitable for use in thinner application interfaces (< 100 μm, even thinner). In the practical application scene, the heat-conducting silicone grease needs to meet the following performance requirements: (1) The viscosity is low, so that the interface gap can be fully filled, and the ultralow interface thermal resistance is realized; (2) The heat conducting silicone grease has certain thixotropy, can keep the thickness of the heat conducting silicone grease matched with the thickness of an interface unchanged in long-term use, can ensure the long-term stability of a formed heat conducting channel, and can avoid polluting surrounding components; (3) The heat-conducting silicone grease has certain wire drawing property, and when the upper surface and the lower surface of an application interface deform, the heat-conducting silicone grease can avoid material breakage through self wire drawing deformation to influence the formation of a heat-conducting path. In addition, at present, the heat-conducting silicone grease is generally coated between an electronic component and a radiator by a screen printing mode, the low viscosity and the wire drawing property of the heat-conducting silicone grease are key performances which are not negligible in the screen printing, and the blade coating difficulty is caused by the overhigh viscosity; poor wire drawability easily causes the shortage or breakage of materials in blade coating, and influences the stability and the blade coating efficiency of the blade coating process.
However, in order to achieve higher heat conductivity of the heat conductive silicone grease, it is necessary to fill the silicone grease with a heat conductive filler having a larger particle size and increase the filling amount of the heat conductive filler, but the product may be applied with an increase in interface thickness, a sharp increase in viscosity, a loss of wire drawability, and a decrease in long-term stability. Therefore, how to prepare the heat-conducting silicone grease which can be applied to ultrathin and deformable interfaces and has high heat conduction, low thermal resistance, low viscosity and high reliability becomes the technical difficulty of the current industry.
Disclosure of Invention
In view of this, an object of the embodiments of the present invention is to provide a high-performance thermal grease and an application thereof, where the thermal grease provided by the present invention has high thermal conductivity, low thermal resistance, low viscosity, high reliability, wire-drawing property, and thixotropy, and can be applied to an ultrathin and deformable interface.
The invention provides a high-performance heat-conducting silicone grease, which comprises:
a matrix and a filler;
the matrix is selected from one or more of dimethyl silicone oil, benzyl silicone oil, alkoxy silicone oil and hydroxyl silicone oil;
the filler is a heat-conducting filler and is selected from one or more of aluminum, silver, zinc oxide, aluminum nitride, boron nitride, silicon nitride, diamond, carbon nano tubes and nano graphite.
Preferably, the phenyl content in the benzyl silicone oil is 5-25 mol%; the mass content of the benzyl silicone oil in the matrix is 0-30 wt%;
the alkoxy silicone oil is one or two of methoxy and ethoxy; the mass content of the alkoxy silicone oil in the matrix is 0-50 wt%;
the mass content of hydroxyl in the hydroxyl silicone oil is 0.1-8 wt%; the mass content of the hydroxyl silicone oil in the matrix is 0-5 wt%.
Preferably, the kinematic viscosity of the matrix at 25 ℃ is 10 to 500mm 2 S; the surface tension of the substrate at 25 ℃ is 20-26 mN/m.
Preferably, the volume content of the filler in the high-performance heat-conducting silicone grease is more than or equal to 70vol%.
Preferably, the filler comprises a first heat-conducting filler, a second heat-conducting filler and a third heat-conducting filler;
the granularity D50 of the first heat-conducting filler is 0.1-1 mu m, and D100 is less than or equal to 60 mu m; the volume content of the first heat-conducting filler in the filler is 10-30 vol%;
the granularity D50 of the second heat-conducting filler is 1.5-5 mu m, and D100 is less than or equal to 60 mu m; the appearance of the second heat-conducting filler is spherical or spheroidal; the volume content of the second heat-conducting filler in the filler is 20-40 vol%;
the granularity D50 of the third heat-conducting filler is 8-20 mu m, D100 is less than or equal to 60 mu m, and D90-D10 is less than or equal to D50; the shape of the third heat-conducting filler is spherical or spheroidal; the volume content of the third heat-conducting filler in the filler is 40-70 vol%.
Preferably, the filler is a filler modified by a modifier;
the modifier is selected from one or more of silane coupling agent, silane coupling agent oligomer, alkoxy polymer, modified silane coupling agent oligomer and modified alkoxy polymer.
Preferably, the modified filler comprises a first modified thermally conductive filler, a second modified thermally conductive filler, and a third thermally conductive modified filler;
the first modified heat-conducting filler contains a first heat-conducting filler interface layer, the effective grafting rate of the first heat-conducting filler interface layer is 0.01-5%, the thickness of the first heat-conducting filler interface layer is 0.5-300 nm, the D50 particle size retention rate of the first modified heat-conducting filler is 110-220%, and the surface energy reduction rate of the first heat-conducting modified heat-conducting filler is 50-95%;
the second modified heat-conducting filler contains a second heat-conducting filler interface layer, the effective grafting rate of the second heat-conducting filler interface layer is 0.01-5%, and the thickness of the second heat-conducting filler interface layer is 0.5-300 nm; the D50 granularity retention rate of the second modified heat-conducting filler is 100.1-160%, and the surface energy reduction rate of the second modified heat-conducting filler is 40-80%;
the third modified heat-conducting filler contains a third heat-conducting filler interface layer, the effective grafting ratio of the third heat-conducting filler interface layer is 0.01-5%, and the thickness of the third heat-conducting filler interface layer is 0.5-300 nm; the D50 particle size retention rate of the third modified heat-conducting filler is 100.1-115%, and the surface energy reduction rate of the third modified heat-conducting filler is 20-60%.
The invention provides a preparation method of high-performance heat-conducting silicone grease, which comprises the following steps:
mixing a matrix and a filler to obtain high-performance heat-conducting silicone grease;
the mixing equipment is selected from one or more of a planetary mixer, a high-speed mixer and a three-roll grinder.
Preferably, the preparation method of the high-performance heat-conducting silicone grease specifically comprises the following steps:
mixing the matrix, and mixing the obtained mixed solution with the filler;
the adding sequence of the filler is a first modified heat-conducting filler, a second modified heat-conducting filler and a third modified heat-conducting filler.
Preferably, when a high-speed mixer is adopted for mixing, the stirring speed in the mixing process is 500-4000 rpm;
when the three-roller grinder is adopted for mixing, the grinding gap in the mixing process is 20-100 mu m;
when the mixing adopts a planetary stirrer, the linear speed in the mixing process is 1-8 m/s.
The present invention provides a deformable interface comprising:
a first surface;
a second surface;
high-performance heat-conducting silicone grease filled between the first surface and the second surface;
the filling mode is selected from dispensing, coating or printing;
the high-performance heat-conducting silicone grease is the high-performance heat-conducting silicone grease in the technical scheme.
Preferably, the thickness of the gap between the first surface and the second surface is less than or equal to 100 μm;
the deformation rate of the interface of the first surface and the second surface is less than or equal to 200 percent.
The research on the heat-conducting silicone grease in the prior art generally focuses on how to obtain a high heat conductivity coefficient and simultaneously reduce the viscosity of a product as much as possible, but few references and researches are made on the stringiness, thixotropy and the thickness of an applicable interface which are very critical in practical application; in addition, most of researches on the heat-conducting silicone grease are carried out on the components of a formula system, and the researches on the structure of a matrix, a filler and a matrix-filler interface and the correlation between the structure and the product performance are very few.
The invention provides a heat-conducting silicone grease with a matrix-filler composite structure which is isotropic, uniform and stable in dynamic state and a preparation method thereof. According to the invention, the matrix structure, the filler accumulation structure and the matrix-filler interface structure are innovatively and accurately regulated by a multi-dimensional regulation technology, an isotropic, dynamically uniform and stable matrix-filler composite structure is designed, and the preparation of the high-performance heat-conducting silicone grease applied to an ultrathin and deformable interface is realized.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides high-performance heat-conducting silicone grease, which comprises the following components:
a matrix and a filler.
In the present invention, the matrix may be selected from one or more of dimethicone, benzyl silicone oil, alkoxy silicone oil, and hydroxy silicone oil.
In the present invention, the phenyl group content in the benzyl silicone oil may be 5 to 25mol%, may be 10 to 20 mol%, and may be 15 mol%. In the present invention, the content of the benzyl silicone oil in the matrix may be 0 to 30wt%, 5 to 25wt%, 10 to 20wt%, or 15wt%.
In the invention, the alkoxy silicone oil can be selected from one or two of methoxy and ethoxy as alkoxy. In the present invention, the content of the alkoxy silicone oil in the matrix may be 0 to 50wt%, 10 to 40wt%, 20 to 30wt%, or 25wt%.
In the present invention, the hydroxyl group content in the hydroxyl silicone oil may be 0.1 to 8wt%, or 0.5 to 7wt%, or 1 to 6wt%, or 2 to 5wt%, or 3 to 4wt%. In the invention, the mass content of the hydroxyl silicone oil in the matrix can be 0-5 wt%, also can be 1-4 wt%, also can be 2-3 wt%.
In the present invention, the kinematic viscosity of the matrix at 25 ℃ may be 10 to 500mm 2 The thickness of the coating layer may be 50 to 400mm 2 The thickness of the coating layer may be 100 to 300mm 2 And/s, can also be 200mm 2 S; the surface tension of the substrate at 25 ℃ may be 20 to 26mN/m, may be 21 to 25mN/m, may be 22 to 24mN/m, and may be 23mN/m.
In the present invention, the filler may be a thermally conductive filler; the filler may be selected from one or more of aluminium, silver, zinc oxide, aluminium nitride, boron nitride, silicon nitride, diamond, carbon nanotubes, nano graphite.
In the present invention, the filler may include a first thermally conductive filler, a second thermally conductive filler, and a third thermally conductive filler; the granularity D50 of the first heat-conducting filler can be 0.1-1 mu m, also can be 0.2-0.8 mu m, also can be 0.3-0.6 mu m; d100 can be less than or equal to 60 mu m; the volume content of the first heat-conducting filler in the filler can be 10-30 vol%, 15-25 vol% and 20vol%; the first heat conductive filler may be formed by using fillers of different compositions.
In the present invention, the particle size D50 of the second heat conductive filler may be 1.5 to 5 μm, 2 to 4 μm, 2.5 to 3.5 μm, or 3 μm; d100 can be less than or equal to 60 mu m; the morphology of the second heat-conducting filler can be spherical or spheroidal; the volume content of the second heat-conducting filler in the filler can be 20-40 vol%, 25-35 vol% and 30vol%; the second thermally conductive filler may be formed by using fillers of different compositions.
In the present invention, the particle size D50 of the third thermal conductive filler may be 8 to 20 μm, 10 to 15 μm, or 12 to 13 μm; d100 can be less than or equal to 60 mu m; D90-D10 is more than or equal to D50 (the granularity span of the filler is less than or equal to 1); the shape of the third heat-conducting filler can be spherical or spheroidal; the volume content of the third heat-conducting filler in the filler can be 40-70 vol%, 50-60 vol% and 55vol%; the third thermally conductive filler may be formed by using fillers of different compositions.
In the present invention, the filler may be a filler modified with a modifier; the modifier and different heat-conducting fillers can form a heat-conducting filler interface layer with special space conformation through the synergistic effect of physical adsorption and chemical bonding.
In the present invention, the modifying agent may be selected from one or more of a silane coupling agent, a silane coupling agent oligomer, an alkoxy polymer, a modified silane coupling agent oligomer, and a modified alkoxy polymer.
In the present invention, the modified filler may be prepared by modifying the filler with a modifier by a wet method or a dry method. The present invention is not particularly limited to the specific method of the wet modification treatment or the dry modification treatment, and the modification treatment may be performed by a method of the wet modification treatment or the dry modification treatment known to those skilled in the art.
In the present invention, the method of the dry modification treatment may include:
dripping the modifier and the organic solvent into the filler, fully and uniformly stirring the filler by a stirrer, and drying the filler.
In the present invention, the method of the wet modification treatment may include:
soaking the filler in a dilute solution of a modifier, an organic solvent and water, fully and uniformly stirring, and filtering and drying.
In the invention, the first heat-conducting filler is treated by a modifier to form a first modified heat-conducting filler, the first modified heat-conducting filler contains a first heat-conducting filler interface layer, and the effective grafting ratio of the first heat-conducting filler interface layer can be 0.01-5%, also can be 0.05-4%, also can be 0.1-3%, also can be 0.5-2%, and also can be 1-1.5%; the thickness of the first heat-conducting filler interface layer can be 0.5-300 nm, also can be 1-250 nm, also can be 10-200 nm, also can be 50-150 nm, also can be 80-120 nm, also can be 100nm; the D50 particle size retention rate of the first modified heat-conducting filler can be 110-220%, can also be 150-200%, and can also be 160-180%; the first modified heat conductive filler may have a surface energy reduction rate of 50 to 95%, or 60 to 90%, or 70 to 80%, or 75%.
In the invention, the second heat-conducting filler is treated by a modifier to form a second modified heat-conducting filler, the second modified heat-conducting filler contains a second heat-conducting filler interface layer, and the effective grafting ratio of the second heat-conducting filler interface layer can be 0.01-5%, also can be 0.05-4%, also can be 0.1-3%, also can be 0.5-2%, and also can be 1-1.5%; the thickness of the second heat-conducting filler interface layer can be 0.5-300 nm, also can be 1-250 nm, also can be 10-200 nm, also can be 50-150 nm, also can be 80-120 nm, also can be 100nm; the retention rate of the D50 particle size of the second modified heat-conducting filler can be 100.1-160%, 110-150%, 120-140% or 130%; the surface energy reduction rate of the second modified heat conductive filler may be 40 to 80%, or 50 to 70%, or 60%.
In the present invention, the third heat conductive filler is treated with a modifier to form a third modified heat conductive filler, the third modified heat conductive filler contains a third heat conductive filler interface layer, and the effective grafting ratio of the third heat conductive filler interface layer may be 0.01 to 5%, or 0.05 to 4%, or 0.1 to 3%, or 0.5 to 2%, or 1 to 1.5%; the thickness of the third heat-conducting filler interface layer can be 0.5-300 nm, also can be 1-250 nm, also can be 10-200 nm, also can be 50-150 nm, also can be 80-120 nm, also can be 100nm; the D50 particle size retention rate of the third modified heat-conducting filler can be 100.1-115%, can also be 105-110%, and can also be 106-108%; the surface energy reduction rate of the third modified heat conductive filler may be 20 to 60%, or 30 to 50%, or 40%.
In the invention, the effective grafting rate refers to the ratio of the grafting amount of the modifier to the modified heat-conducting filler multiplied by 100 percent; the effective grafting rate can be calculated by measuring the carbon content of the heat-conducting filler before and after modification and according to the difference value of the carbon content of the heat-conducting filler before and after modification and the molecular weight of the modifier.
In the invention, the thickness of the interface layer of the heat-conducting filler can be obtained by detecting the modified heat-conducting filler by a high-power spherical aberration transmission electron microscope.
In the invention, the retention rate of the D50 particle size of the modified heat conductive filler refers to the ratio of the D50 particle size of the modified heat conductive filler to the D50 particle size of the modified heat conductive filler, and can be detected by a scanning electron microscope and a particle size analyzer.
In the invention, the surface energy reduction rate of the modified heat-conducting filler refers to the ratio of the surface energy of the modified heat-conducting filler to the surface energy of the modified heat-conducting filler, and can be detected by a surface energy analyzer.
In the invention, the volume content of the filler in the high-performance heat-conducting silicone grease can be more than or equal to 70vol%.
The invention provides a preparation method of high-performance heat-conducting silicone grease, which comprises the following steps:
and mixing the matrix and the filler to obtain the high-performance heat-conducting silicone grease.
In the invention, the matrix can be mixed firstly, and the obtained mixed liquid is mixed with the filler; the matrix mixing may be performed at room temperature, and the mixing may be performed under stirring; the mixing equipment can be one or more of a planetary mixer, a high-speed mixer and a three-roll grinder; when a high-speed mixer is adopted for mixing, the stirring speed can be 500-4000 rpm, 1000-3000 rpm or 2000rpm; when a planetary stirrer is used for mixing, the linear speed of stirring can be 1-8 m/s, also can be 2-6 m/s, and also can be 3-5 m/s.
In the invention, the adding sequence of the fillers in the mixed filler can be that the first heat-conducting filler (or the first modified heat-conducting filler), the second heat-conducting filler (or the second modified heat-conducting filler) and the third heat-conducting filler (or the third modified heat-conducting filler) are sequentially added in the order for fully mixing; mixing after adding each thermally conductive filler, which may be performed at room temperature; the mixing may be carried out under stirring; the mixing equipment can be one or more of a planetary mixer, a high-speed mixer and a three-roll grinder; when a high-speed mixer is adopted for mixing, the stirring speed can be 500-4000 rpm, 1000-3000 rpm or 2000rpm; when a planetary stirrer is used for mixing, the linear speed of stirring can be 1-8 m/s, also can be 2-6 m/s, and also can be 3-5 m/s.
In the invention, the mixing of the matrix and the filler can be fully mixed by mixing equipment, and the volume filling fraction of the filler in the mixing equipment can be more than or equal to 70vol%; the mixing equipment can be selected from one or more of a planetary mixer, a high-speed mixer and a three-roll grinder. In the invention, the mixing uniformity can be controlled by adjusting the mixing speed, temperature, time, vacuum degree and grinding clearance in the mixing process.
In the present invention, the method of mixing the matrix and the filler may also include:
mixing at room temperature, vacuumizing, mixing, and grinding.
In the present invention, the mixing at room temperature may be performed under stirring, and the mixing may be selected from one or more of a planetary mixer, a high-speed mixer, and a three-roll mill; when a high-speed mixer is adopted for mixing, the stirring speed can be 500-4000 rpm, 1000-3000 rpm or 2000rpm; when a planetary stirrer is used for mixing, the linear speed of stirring can be 1-8 m/s, also can be 2-6 m/s, and also can be 3-5 m/s. In the invention, the temperature of the vacuumizing mixing can be 40-60 ℃, also can be 45-55 ℃ and also can be 50 ℃; the vacuum-pumping mixing can be carried out under the condition of stirring, and the vacuum-pumping mixing can be selected from one or more of a planetary stirrer, a high-speed mixer and a three-roll grinder; when a high-speed mixer is adopted for mixing, the stirring speed can be 500-4000 rpm, 1000-3000 rpm or 2000rpm; when a planetary stirrer is used for mixing, the linear speed of stirring can be 1-8 m/s, also can be 2-6 m/s, and also can be 3-5 m/s. In the present invention, the grinding may be performed using a three-roll grinder; the polishing gap in the polishing process may be 20 to 100 μm, or 30 to 80 μm, or 40 to 60 μm.
The present invention provides a deformable interface comprising:
a first surface;
a second surface;
high-performance heat-conducting silicone grease filled between the first surface and the second surface;
the high-performance heat-conducting silicone grease is the high-performance heat-conducting silicone grease in the technical scheme.
In the invention, the high-performance heat-conducting silicone grease can be applied to an ultrathin and deformable interface; the ultrathin deformable interface is composed of a first surface, a second surface and a gap between the two surfaces, and the high-performance heat-conducting silicone grease is filled in the gap between the two surfaces in a certain mode. In the invention, the thickness of the gap between the first surface and the second surface is the interface thickness, and the first surface and the second surface have a certain deformation.
In the present invention, the method for filling the gap between the first surface and the second surface with the high performance heat conductive silicone grease preferably includes:
and arranging the high-performance heat-conducting silicone grease on one surface, and applying pressure to the other surface to enable the other surface to extrude the surface provided with the high-performance heat-conducting silicone grease, so that the high-performance heat-conducting silicone grease is filled in a gap between the first surface and the second surface.
In the present invention, the method of disposing the high-performance heat-conductive silicone grease on one surface (filling method) is preferably selected from the means of dispensing, coating, or printing.
In the present invention, the interface thickness is preferably 100 μm or less; the interface deformation rate is preferably less than or equal to 200%, and the interface deformation rate refers to the ratio of the thickness of the interface after deformation to the thickness of the interface before deformation.
The key point of the invention is the application scene and the glue applying mode of the high-performance heat-conducting silicone grease: an ultra-thin, deformable interface; dispensing, coating and printing; "multidimensional regulation and control technique": regulation and control of matrix structure, filler stacking structure and matrix-filler interface structure; an isotropic, dynamically uniform and stable matrix-filler composite structure; the heat-conducting silicone grease product provided by the invention is applied to an ultrathin and deformable interface, and has low thermal resistance, low viscosity and high reliability on the basis that the heat conductivity coefficient is more than or equal to 3W/mK.
Example 1
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix consists of 72wt% of dimethyl silicone oil (50 mm) 2 S), 25 wt.% of benzyl silicone oil (150 mm) 2 S) and 3 wt.% of a hydroxy silicone oil (500 mm) 2 /s) compounding; wherein the phenyl content in the benzyl silicone oil is 10mol%, and the hydroxyl content in the hydroxyl silicone oil is 8wt%.
The first heat-conducting filler is composed of zinc oxide and aluminum oxide, the D50 granularity is 1 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the first heat-conducting filler in the filler is 30vol%; the second heat-conducting filler is composed of alumina and aluminum nitride, the D50 granularity is 4 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the second heat-conducting filler in the filler is 25vol%; the third heat-conducting filler is made of alumina, the D50 granularity is 17 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the third heat-conducting filler in the filler is 45vol%.
The first heat-conducting filler, the second heat-conducting filler and the third heat-conducting filler are respectively subjected to dry modification treatment by using a silane coupling agent, and the specific method comprises the following steps: dripping a silane coupling agent and an organic solvent into the heat-conducting filler, fully and uniformly stirring the heat-conducting filler by a stirrer, and drying the heat-conducting filler for later use; the silane coupling agent is octyl trimethoxy silane; the organic solvent is absolute ethyl alcohol; the mass ratio of the silane coupling agent to the organic solvent to the first heat-conducting filler is 2; the mass ratio of the silane coupling agent to the organic solvent to the second heat-conducting filler is 3; the mass ratio of the silane coupling agent to the organic solvent to the third thermally conductive filler is 0.8.
The effective grafting rate of the obtained first heat-conducting filler interface layer is 2%, the thickness of the first heat-conducting filler interface layer is 150nm, the D50 particle size retention rate of the first modified heat-conducting filler is 135%, and the surface energy reduction rate of the first modified heat-conducting filler is 90%; the effective grafting rate of the second heat-conducting filler interface layer is 1.6%, the thickness of the second heat-conducting filler interface layer is 90nm, the D50 retention rate of the second modified heat-conducting filler is 120%, and the surface energy reduction rate of the second modified heat-conducting filler is 60%; the effective grafting rate of the interface layer of the third heat-conducting filler is 0.9%, the thickness of the interface layer of the third heat-conducting filler is 40nm, the D50 retention rate of the third modified heat-conducting filler is 105%, and the surface energy reduction rate of the third modified heat-conducting filler is 30%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat-conducting filler is 76vol%;
sequentially adding the matrixes into a high-speed mixer according to the mass ratio, and fully mixing at room temperature at 1000rpm to obtain a mixed solution; adding the first modified heat-conducting filler into the mixed solution, and fully mixing at room temperature and 2000rpm to obtain a first mixture; adding the second modified heat-conducting filler into the first mixture, and fully mixing at room temperature and 2000rpm to obtain a second mixture; adding the third modified heat-conducting filler into the second mixture, fully mixing at room temperature of 2000rpm, vacuumizing at 50 ℃ of 2000rpm, and fully mixing to obtain a third mixture; and grinding the obtained third mixture by a three-roll grinder (the grinding gap is 60 mu m) to obtain a heat-conducting silicone grease product.
Example 2
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix consists of 96wt% of dimethyl silicone oil (200 mm) 2 S) and 4 wt.% of a hydroxy silicone oil(400mm 2 /s) compounding; wherein the hydroxyl content in the hydroxyl silicone oil is 6wt%.
The first heat-conducting filler is composed of zinc oxide and aluminum oxide, the D50 granularity is 0.5 mu m, the D100 granularity is controlled to be less than or equal to 50 mu m, and the percentage of the D100 granularity in the filler is 20vol%; the second heat-conducting filler is composed of alumina and aluminum, the D50 granularity is 3 mu m, the D100 granularity is controlled to be less than or equal to 50 mu m, and the proportion of the second heat-conducting filler in the filler is 28vol%; the third heat-conducting filler is composed of alumina and aluminum, the D50 granularity is 14 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 50 mu m, and the percentage of the third heat-conducting filler in the filler is 52vol%.
The method comprises the following steps of performing wet modification treatment on the first heat-conducting filler, the second heat-conducting filler and the third heat-conducting filler by using a silane coupling agent, wherein the specific method comprises the following steps: soaking the heat-conducting filler in a diluted solution of a silane coupling agent, an organic solvent and water with the pH value adjusted, fully and uniformly stirring, and filtering and drying for later use; the pH value is 4.5, and the silane coupling agent is decyl trimethoxy silane; the organic solvent is isopropanol; the mass ratio of the silane coupling agent to the organic solvent to the water to the first heat-conducting filler is 3:200:20:100, respectively; the mass ratio of the silane coupling agent to the organic solvent to the water to the second heat-conducting filler is 1:180:5:100, respectively; the mass ratio of the silane coupling agent to the organic solvent to the water to the third heat-conducting filler is 2:200:5:100.
the effective grafting rate of the obtained first heat-conducting filler interface layer is 2.4%, the thickness of the first heat-conducting filler interface layer is 200nm, the D50 particle size retention rate of the first modified heat-conducting filler is 145%, and the surface energy reduction rate of the first modified heat-conducting filler is 95%; the effective grafting rate of the second heat-conducting filler interface layer is 1.2%, the thickness of the second heat-conducting filler interface layer is 80nm, the D50 retention rate of the second modified heat-conducting filler is 115%, and the surface energy reduction rate of the second modified heat-conducting filler is 55%; the effective grafting rate of the third heat-conducting filler interface layer is 0.6%, the thickness of the third heat-conducting filler interface layer is 30nm, the D50 retention rate of the third modified heat-conducting filler is 103%, and the surface energy reduction rate of the third modified heat-conducting filler is 40%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat-conducting filler is 81vol%;
sequentially adding the base bodies into a planetary stirrer according to the mass ratio, and fully mixing at the room temperature and the linear speed of 5m/s to obtain a mixed solution; adding the first modified heat-conducting filler into the mixed solution, vacuumizing at the linear speed of 5m/s at room temperature, and fully mixing to obtain a first mixture; adding a second modified heat-conducting filler into the first mixture, and fully mixing at a room temperature and a linear speed of 5m/s to obtain a second mixture; adding the third modified heat-conducting filler into the second mixture, fully mixing at the room temperature with the linear speed of 5m/s, vacuumizing at the 50 ℃ with the linear speed of 5m/s, and fully mixing to obtain a third mixture; and grinding the obtained third mixture by a three-roll grinder (the grinding gap is 50 mu m) to obtain a heat-conducting silicone grease product.
Example 3
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix consists of 80wt% of dimethyl silicone oil (100 mm) 2 S) and 20% by weight of an alkoxysilaneoil (100 mm) 2 /s) compounding; wherein the alkoxy silicone oil is trimethoxy terminated.
The first heat-conducting filler is composed of zinc oxide and carbon nano tubes, the D50 granularity is 0.3 mu m, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the first heat-conducting filler in the filler is 15vol%; the second heat-conducting filler is composed of alumina and aluminum nitride, the D50 granularity is 2 mu m, the D100 granularity is controlled to be less than or equal to 60 mu m, and the proportion of the second heat-conducting filler in the filler is 40vol%; the third heat-conducting filler is composed of alumina and aluminum, the D50 granularity is 20 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the third heat-conducting filler in the filler is 45vol%.
The first heat conductive filler, the second heat conductive filler and the third heat conductive filler are respectively modified by silane coupling agents, and the modification method is the same as that of example 2.
The effective grafting rate of the obtained first heat-conducting filler interface layer is 1.2%, the thickness of the first heat-conducting filler interface layer is 100nm, the retention rate of the D50 particle size of the first modified heat-conducting filler is 125%, and the surface energy reduction rate of the first modified heat-conducting filler is 85%; the effective grafting rate of the interface layer of the second heat-conducting filler is 1.8%, the thickness of the interface layer of the second heat-conducting filler is 90nm, the D50 retention rate of the second modified heat-conducting filler is 115%, and the surface energy reduction rate of the second modified heat-conducting filler is 50%; the effective grafting rate of the third heat-conducting filler interface layer is 0.5%, the thickness of the third heat-conducting filler interface layer is 30nm, the D50 retention rate of the third modified heat-conducting filler is 102%, and the surface energy reduction rate of the third modified heat-conducting filler is 30%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat-conducting filler is 78vol%;
sequentially adding the base bodies into a planetary stirrer according to the mass ratio, and fully mixing at the room temperature and the linear speed of 4m/s to obtain a mixed solution; adding a first modified heat-conducting filler into the mixed solution, vacuumizing at the linear speed of 4m/s at room temperature, and fully mixing to obtain a first mixture; adding the second modified heat-conducting filler into the first mixture, and fully mixing at a linear speed of 4m/s at room temperature to obtain a second mixture; adding the third modified heat-conducting filler into the second mixture, fully mixing at the offline speed of 4m/s at room temperature, vacuumizing at the offline speed of 4m/s at 50 ℃, and fully mixing to obtain a third mixture; and grinding the obtained third mixture by a three-roll grinder (the grinding gap is 60 mu m) to obtain a heat-conducting silicone grease product.
Example 4
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix is benzyl silicone oil (350 mm) 2 (s), the content of phenyl in the benzyl silicone oil is 30mol percent;
the first heat-conducting filler is composed of zinc oxide and aluminum oxide, the D50 granularity is 1 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the first heat-conducting filler in the filler is 30vol%; the second heat-conducting filler is composed of alumina and aluminum nitride, the D50 granularity is 4 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the second heat-conducting filler in the filler is 25vol%; the third heat-conducting filler is made of alumina, the D50 granularity is 17 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the third heat-conducting filler in the filler is 45vol%.
The first heat conductive filler, the second heat conductive filler and the third heat conductive filler are respectively modified by a silane coupling agent in a dry method, and the modification method is the same as that of example 1.
The effective grafting rate of the obtained first heat-conducting filler interface layer is 2%, the thickness of the first heat-conducting filler interface layer is 150nm, the D50 particle size retention rate of the first modified heat-conducting filler is 135%, and the surface energy reduction rate of the first modified heat-conducting filler is 90%; the effective grafting rate of the second heat-conducting filler interface layer is 1.6%, the thickness of the second heat-conducting filler interface layer is 90nm, the D50 retention rate of the second modified heat-conducting filler is 120%, and the surface energy reduction rate of the second modified heat-conducting filler is 60%; the effective grafting rate of the interface layer of the third heat-conducting filler is 0.9%, the thickness of the interface layer of the third heat-conducting filler is 40nm, the D50 retention rate of the third modified heat-conducting filler is 105%, and the surface energy reduction rate of the third modified heat-conducting filler is 30%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat-conducting filler is 76vol%;
sequentially adding the matrix and the first modified heat-conducting filler into a high-speed mixer, and fully mixing at room temperature and 2000rpm to obtain a first mixture; adding the second modified heat-conducting filler into the first mixture, and fully mixing at room temperature and 2000rpm to obtain a second mixture; adding the third modified heat-conducting filler into the second mixture, fully mixing at room temperature and 2000rpm, vacuumizing at 50 ℃ and 2000rpm, and fully mixing to obtain a third mixture; and grinding the obtained third mixture by a three-roll grinder (the grinding gap is 60 mu m) to obtain a heat-conducting silicone grease product.
Example 5
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix consists of 72wt% of dimethyl silicone oil (50 mm) 2 S), 25 wt.% of benzyl silicone oil (150 mm) 2 S) and 3 wt.% of a hydroxy silicone oil (500 mm) 2 /s) compounding; wherein the phenyl content in the benzyl silicone oil is 10mol%, and the hydroxyl content in the hydroxyl silicone oil is 8wt%;
the first heat-conducting filler is composed of zinc oxide and aluminum oxide, the D50 granularity is 1 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the first heat-conducting filler in the filler is 45vol%; the third heat-conducting filler is made of alumina, the D50 granularity is 17 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the third heat-conducting filler in the filler is 55vol%.
The first heat conductive filler and the third heat conductive filler are respectively modified by a silane coupling agent in a dry method, and the modification method is the same as that of example 1.
The effective grafting rate of the obtained first heat-conducting filler interface layer is 2%, the thickness of the first heat-conducting filler interface layer is 150nm, the D50 particle size retention rate of the first modified heat-conducting filler is 135%, and the surface energy reduction rate of the first modified heat-conducting filler is 90%; the effective grafting rate of the second heat-conducting filler interface layer is 0.9%, the thickness of the second heat-conducting filler interface layer is 40nm, the D50 retention rate of the second modified heat-conducting filler is 105%, and the surface energy reduction rate of the second modified heat-conducting filler is 30%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat-conducting filler is 76vol%;
sequentially adding the matrixes into a high-speed mixer according to the mass ratio, and fully mixing at room temperature at 1000rpm to obtain a mixed solution; adding the first modified heat-conducting filler into the mixed solution, and fully mixing at room temperature and 2000rpm to obtain a first mixture; adding the second modified heat-conducting filler into the first mixture, fully mixing at room temperature and 2000rpm, vacuumizing at 50 ℃ and 2000rpm, and fully mixing to obtain a second mixture; and grinding the obtained second mixture by a three-roll grinder (the grinding gap is 60 mu m) to obtain a heat-conducting silicone grease product.
Example 6
The structural characteristics of the heat-conducting silicone grease are as follows:
the matrix consists of 72wt% of dimethyl silicone oil (50 mm) 2 S), 25 wt.% of benzyl silicone oil (150 mm) 2 S) and 3 wt.% of a hydroxy silicone oil (500 mm) 2 /s) compounding; the phenyl content in the benzyl silicone oil is 10mol%, and the hydroxyl content in the hydroxyl silicone oil is 8wt%.
The first heat-conducting filler is composed of zinc oxide and aluminum oxide, the D50 granularity is 1 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the first heat-conducting filler in the filler is 30vol%; the second heat-conducting filler is composed of alumina and aluminum nitride, the D50 granularity is 4 mu m, the D100 is controlled to be less than or equal to 60 mu m, and the proportion of the second heat-conducting filler in the filler is 25vol%; the third heat-conducting filler is made of alumina, the D50 granularity is 17 mu m, the D90 granularity-D10 granularity is controlled to be less than or equal to the D50 granularity, the D100 granularity is controlled to be less than or equal to 60 mu m, and the percentage of the third heat-conducting filler in the filler is 45vol%.
The dry modification treatment is respectively carried out on the first heat-conducting filler, the second heat-conducting filler and the third heat-conducting filler by using a silane coupling agent, and the specific method comprises the following steps: dripping a silane coupling agent and an organic solvent into the heat-conducting filler, fully and uniformly stirring the heat-conducting filler by a stirrer, and drying the heat-conducting filler for later use; the silane coupling agent is propyl trimethoxy silane; the organic solvent is absolute ethyl alcohol; the mass ratio of the silane coupling agent to the organic solvent to the first heat-conducting filler is 2; the mass ratio of the silane coupling agent to the organic solvent to the second heat-conducting filler is 3; the mass ratio of the silane coupling agent to the organic solvent to the third thermally conductive filler is 0.8.
The effective grafting rate of the obtained first heat-conducting filler interface layer is 2%, the thickness of the first heat-conducting filler interface layer is 150nm, the D50 particle size retention rate of the first modified heat-conducting filler is 500%, and the surface energy reduction rate of the first heat-conducting filler is 85%; the effective grafting rate of the interface layer of the second heat-conducting filler is 1.6 percent, the thickness of the interface layer of the second heat-conducting filler is 90nm, the D50 retention rate of the second modified heat-conducting filler is 200 percent, and the surface energy reduction rate of the second modified heat-conducting filler is 60 percent; the effective grafting rate of the third heat-conducting filler interface layer is 0.9%, the thickness of the third heat-conducting filler interface layer is 40nm, the D50 retention rate of the third modified heat-conducting filler is 150%, and the surface energy reduction rate of the third modified heat-conducting filler is 30%.
The preparation method of the heat-conducting silicone grease comprises the following steps:
the volume filling rate of the heat conductive filler was 76vol%.
Sequentially adding the matrixes into a high-speed mixer according to the mass ratio, and fully mixing at room temperature at 1000rpm to obtain a mixed solution; adding the first modified heat-conducting filler into the mixed solution, and fully mixing at room temperature and 2000rpm to obtain a first mixture; adding the second modified heat-conducting filler into the first mixture, and fully mixing at room temperature and 2000rpm to obtain a second mixture; adding a third heat-conducting filler into the second mixture, fully mixing at room temperature of 2000rpm, vacuumizing at 50 ℃ of 2000rpm, and fully mixing to obtain a third mixture; and (4) passing the obtained third mixture through a three-roll grinder (the grinding gap is 60 mu m) to obtain a heat-conducting silicone grease product.
Performance detection
The performance of the heat-conducting silicone grease prepared by the embodiment of the invention is detected, and the detection method comprises the following steps:
coefficient of thermal conductivity: ISO22007-2
Thermal resistance: ASTMD5470
Viscosity: ASTMD2196
Wire drawability: hand feeling
Thixotropy: hand feeling
High temperature resistance, thermal resistance and attenuation: aging at 125 ℃ for 1000H, the rate of change of thermal resistance before and after aging, and damp-heat resistance attenuation of ASTM D5470: 1000H double 85 ℃ aging, thermal resistance change rate before and after aging, ASTM D5470
Temperature resistance and thermal cycling resistance decay: aging at-40-125 ℃ for 1000H, and the rate of change of thermal resistance before and after aging, ASTM D5470
The detection results are as follows:
in the embodiments 1 to 3, the matrix structure, the filler accumulation structure and the matrix-filler interface structure are well regulated and controlled; example 4 the content of the benzyl silicone oil in the matrix structure is too high, so that the silicone grease cannot be prepared; in the embodiment 5, the second heat-conducting filler is not contained in the filler stacking structure, so that the wire drawing performance is seriously influenced; example 6 significant agglomeration was observed after the filler was coated in the matrix-filler interface structure, which severely affected the drawability and reliability.
The invention provides a heat-conducting silicone grease with a matrix-filler composite structure which is isotropic, uniform and stable in dynamic state and a preparation method thereof. According to the invention, the matrix structure, the filler accumulation structure and the matrix-filler interface structure are innovatively and accurately regulated by a multi-dimensional regulation technology, an isotropic, dynamically uniform and stable matrix-filler composite structure is designed, and the preparation of the high-performance heat-conducting silicone grease applied to an ultrathin and deformable interface is realized.
While the invention has been described and illustrated with reference to specific embodiments thereof, such description and illustration are not intended to limit the invention. It will be clearly understood by those skilled in the art that various changes in form and details may be made therein without departing from the true spirit and scope of the invention as defined by the appended claims, to adapt a particular situation, material, composition of matter, substance, method or process to the objective, spirit and scope of this application. All such modifications are intended to be within the scope of the claims appended hereto. Although the methods disclosed herein have been described with reference to particular operations performed in a particular order, it should be understood that these operations may be combined, sub-divided, or reordered to form equivalent methods without departing from the teachings of the present disclosure. Accordingly, unless specifically indicated herein, the order and grouping of the operations is not a limitation of the present application.
Claims (12)
1. A high performance thermally conductive silicone grease comprising:
a matrix and a filler;
the matrix is selected from one or more of dimethyl silicone oil, benzyl silicone oil, alkoxy silicone oil and hydroxyl silicone oil;
the filler is a heat-conducting filler and is selected from one or more of aluminum, silver, zinc oxide, aluminum nitride, boron nitride, silicon nitride, diamond, carbon nano tubes and nano graphite.
2. The high-performance heat-conducting silicone grease as claimed in claim 1, wherein the phenyl content in the benzyl silicone oil is 5-25 mol%; the mass content of the benzyl silicone oil in the matrix is 0-30 wt%;
the alkoxy silicone oil is one or two of methoxy and ethoxy; the mass content of the alkoxy silicone oil in the matrix is 0-50 wt%;
the mass content of hydroxyl in the hydroxyl silicone oil is 0.1-8 wt%; the mass content of the hydroxyl silicone oil in the matrix is 0-5 wt%.
3. According to claimThe high-performance heat-conducting silicone grease according to claim 1, wherein the kinematic viscosity of the base at 25 ℃ is 10 to 500mm 2 S; the surface tension of the substrate at 25 ℃ is 20-26 mN/m.
4. The high-performance heat-conducting silicone grease as claimed in claim 1, wherein the volume content of the filler in the high-performance heat-conducting silicone grease is not less than 70vol%.
5. The high performance heat conductive silicone grease of claim 1, wherein the filler comprises a first heat conductive filler, a second heat conductive filler and a third heat conductive filler;
the granularity D50 of the first heat-conducting filler is 0.1-1 mu m, and D100 is less than or equal to 60 mu m; the volume content of the first heat-conducting filler in the filler is 10-30 vol%;
the granularity D50 of the second heat-conducting filler is 1.5-5 mu m, and D100 is less than or equal to 60 mu m; the appearance of the second heat-conducting filler is spherical or spheroidal; the volume content of the second heat-conducting filler in the filler is 20-40 vol%;
the granularity D50 of the third heat-conducting filler is 8-20 microns, D100 is less than or equal to 60 microns, and D90-D10 is less than or equal to D50; the shape of the third heat-conducting filler is spherical or spheroidal; the volume content of the third heat-conducting filler in the filler is 40-70 vol%.
6. The high-performance heat-conducting silicone grease as claimed in claim 1, wherein the filler is a modifier-modified filler;
the modifier is selected from one or more of silane coupling agent, silane coupling agent oligomer, alkoxy polymer, modified silane coupling agent oligomer and modified alkoxy polymer.
7. The high performance heat-conducting silicone grease as claimed in claim 6, wherein the modified filler comprises a first modified heat-conducting filler, a second modified heat-conducting filler and a third heat-conducting modified filler;
the first modified heat-conducting filler contains a first heat-conducting filler interface layer, the effective grafting rate of the first heat-conducting filler interface layer is 0.01-5%, the thickness of the first heat-conducting filler interface layer is 0.5-300 nm, the D50 particle size retention rate of the first modified heat-conducting filler is 110-220%, and the surface energy reduction rate of the first heat-conducting modified heat-conducting filler is 50-95%;
the second modified heat-conducting filler contains a second heat-conducting filler interface layer, the effective grafting rate of the second heat-conducting filler interface layer is 0.01-5%, and the thickness of the second heat-conducting filler interface layer is 0.5-300 nm; the D50 granularity retention rate of the second modified heat-conducting filler is 100.1-160%, and the surface energy reduction rate of the second modified heat-conducting filler is 40-80%;
the third modified heat-conducting filler contains a third heat-conducting filler interface layer, the effective grafting rate of the third heat-conducting filler interface layer is 0.01-5%, and the thickness of the third heat-conducting filler interface layer is 0.5-300 nm; the D50 particle size retention rate of the third modified heat-conducting filler is 100.1-115%, and the surface energy reduction rate of the third modified heat-conducting filler is 20-60%.
8. A method for preparing the high-performance heat-conducting silicone grease of claim 1, comprising:
mixing a matrix and a filler to obtain high-performance heat-conducting silicone grease;
the mixing equipment is selected from one or more of a planetary mixer, a high-speed mixer and a three-roll grinder.
9. The method according to claim 8, wherein the preparation method of the high-performance heat-conducting silicone grease specifically comprises:
mixing the matrix, and mixing the obtained mixed solution with the filler;
the adding sequence of the filler is a first modified heat-conducting filler, a second modified heat-conducting filler and a third modified heat-conducting filler.
10. The method of claim 8, wherein when the high-speed mixer is used for mixing, the stirring speed during mixing is 500-4000 rpm;
when the three-roller grinder is adopted for mixing, the grinding gap in the mixing process is 20-100 mu m;
when the planetary stirrer is adopted for mixing, the linear speed in the mixing process is 1-8 m/s.
11. A deformable interface, comprising:
a first surface;
a second surface;
high-performance heat-conducting silicone grease filled between the first surface and the second surface;
the filling mode is selected from dispensing, coating or printing;
the high-performance heat-conducting silicone grease of claim 1.
12. A deformable interface as claimed in claim 11, wherein the thickness of the interstices between the first and second surfaces is ≦ 100 μm;
the deformation rate of the interface of the first surface and the second surface is less than or equal to 200 percent.
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| CN101294067A (en) * | 2008-06-20 | 2008-10-29 | 清华大学 | Heat conductive silicone grease composition |
| CN108624056A (en) * | 2018-05-09 | 2018-10-09 | 华东理工大学 | A kind of High thermal-conductive silicone grease boundary material and preparation method thereof |
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| CN114276789A (en) * | 2021-12-31 | 2022-04-05 | 北京中石伟业科技股份有限公司 | High-thixotropic silicon-based heat-conducting gel and preparation method thereof |
| CN114292442A (en) * | 2021-12-31 | 2022-04-08 | 北京中石伟业科技股份有限公司 | Filler aluminum powder, modification method and application thereof |
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| CN101294067A (en) * | 2008-06-20 | 2008-10-29 | 清华大学 | Heat conductive silicone grease composition |
| CN109206912A (en) * | 2017-07-06 | 2019-01-15 | 河北高富氮化硅材料有限公司 | A kind of insulating heat conductive silicon grease composition |
| CN108624056A (en) * | 2018-05-09 | 2018-10-09 | 华东理工大学 | A kind of High thermal-conductive silicone grease boundary material and preparation method thereof |
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| CN114276789A (en) * | 2021-12-31 | 2022-04-05 | 北京中石伟业科技股份有限公司 | High-thixotropic silicon-based heat-conducting gel and preparation method thereof |
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