CN112143232B - High-strength ultralow-dielectric-property foaming heat-conducting silica gel gasket and preparation method thereof - Google Patents
High-strength ultralow-dielectric-property foaming heat-conducting silica gel gasket and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength ultralow-dielectric-property foamed heat-conducting silica gel gasket and a preparation method thereof, wherein the foamed heat-conducting silica gel gasket mainly comprises the following heat-conducting interface materials: liquid base glue, heat conduction filler, foaming agent, cross-linking agent, catalyst and retarder. The heat-conducting silica gel gasket is filled with specific heat-conducting filler, obtains high heat conductivity coefficient based on a specific process preparation means, has the characteristics of ultralow dielectricity and small density, adopts the glass fiber cloth with low dielectricity to enhance the overall toughness of the product, and has wide prospect in the communication industry of the times of 5G or more than 5G.
Description
Technical Field
The invention relates to a heat-conducting interface material applied to the field of high-speed communication, in particular to a foamed heat-conducting silica gel gasket and a preparation method thereof.
Background
In recent years, miniaturization and integration have become the trend of electronic devices. With the increasing of the power of electronic devices, the heat generated by the operation of the devices increases rapidly, which directly affects the functional stability and the service life of the electronic products, so that the solution of the good heat problem is the key for the rapid development of the electronic products, especially with the commercial spread of the 5G era, 5G devices will be produced in large quantities, but based on the characteristics of faster transmission speed and poorer transmission signal strength of 5G signals, the interference of the materials to the signals is more obvious.
Wherein Td is a signal transmission delay time, and L is a signal transmission length; and c is the speed of light. The above formula shows that the higher the dielectric constant value of the material is, the more significant the delay of the electromagnetic signal is, so that the 5G era has higher requirements on heat conduction, and simultaneously, the heat conduction material is required to have a lower dielectric constant, thereby ensuring the smooth transmission of the 5G signal.
The approach for obtaining a composite material with both thermal conductivity and ultra-low dielectric property has two aspects: firstly, carrying out micro-foaming modification on a substrate, and secondly, adopting a heat-conducting filler with low dielectric property. However, the heat conducting gasket in the current market generally adopts alumina, aluminum nitride, zinc oxide, metal powder or graphite powder as a filler, and the emphasis is on improving the heat conductivity coefficient, but the dielectric constant is usually large and is more than 5.5. Some enterprises are also researching the foaming heat-conducting gasket, but the main focus is on the characteristic of low density, and the foaming heat-conducting gasket mainly aims at the field of new energy automobiles. At present, no composite product aiming at high heat conduction and low dielectric property exists in the market, but the composite product is a necessary product for 5G commercial use.
Chinese patent application publication No. CN108977105A discloses a method for preparing a heat-conducting silica gel sheet, which comprises preparing a foamed sheet from ethylene-vinyl acetate copolymer, heat-conducting graphite flakes, EPS foam particles and vinyl ester resin, mixing and heating the ethylene-vinyl acetate copolymer, glass fiber and expanded graphite powder to obtain glass fiber resin, coating the glass fiber resin on the surface of the foamed sheet, hot-pressing and vulcanizing to obtain the heat-conducting silica gel sheet, using polar groups and active groups in epoxidized soybean oil to make acrylate matrix resin show excellent adhesive strength, electric insulation performance and high temperature resistance, using benzene ring structure of the EPS foam particles to endow matrix resin with heat resistance and rigidity, achieving the effect that viscosity is not reduced at high temperature, improving compatibility of the graphite flakes and the ethylene-vinyl acetate copolymer through coupling effect, expanding and relaxing the heat-conducting graphite flakes, the heat conducting area of the silica gel sheet is improved. The heat-conducting silica gel sheet prepared by the related technology is structurally insufficient for operation of calendaring equipment, so that the heat-conducting silica gel sheet cannot be prepared in a continuous coiling manner, the production efficiency is poor, and the product characteristics cannot meet the requirements of high strength and ultralow dielectric property.
The Chinese patent application publication No. CN108366511A discloses a heat-conducting gasket and a preparation method thereof, wherein a heat-conducting gasket body is prepared by uniformly mixing glass fiber cloth and silica gel, and adding the following raw materials: the heat conducting gasket comprises divinyl-terminated polydimethylsiloxane, methyl silicone oil, hydrogen-containing silicone oil, a retarder, a platinum catalyst and heat conducting powder, and has good heat conductivity, elasticity and restorability. The heat conducting gasket manufactured by the related art pursues heat conductivity and elasticity, and does not consider the balance of the heat conductivity and the dielectric property. If the adhesive tape is attached to an electronic product, there is a risk of electric leakage or electric interference.
Chinese patent application publication No. CN104497574A discloses a multifunctional organic silicon thermal interface material, which is compounded by the following components in percentage by weight: 10 to 40 portions of silicon rubber, 1 to 10 portions of heat-resistant agent, 1 to 20 portions of flame retardant, 1 to 10 portions of vulcanizing agent and 55 to 85 portions of functional filler. The thermal interface material is a sheet material formed by mixing the silicone rubber, the heat-resistant agent, the flame retardant, the vulcanizing agent and the functional filler in the proportion and coating or rolling the mixture on a glass fiber cloth or a polyimide film. The heat conducting gasket manufactured by the related art does not achieve the balance of heat conductivity and dielectric property.
The applicant discloses a high-heat-conductivity flexible silica gel gasket and a preparation method thereof in Chinese invention patent application publication number CN103059576A, wherein the high-heat-conductivity flexible silica gel gasket comprises the following raw materials in parts by weight: 1000 parts of modified spherical alumina powder, 60-100 parts of vinyl silicone oil, 30-50 parts of dimethyl silicone oil, 1.5-4 parts of hydrogen-containing silicone oil and 0.2-0.8 part of catalyst, and the modified spherical alumina powder is prepared by the steps of (1) alumina particle modification, (2) stirring, (3) vacuumizing, (4) vulcanization and the like. The high-heat-conductivity flexible silica gel gasket increases the internal heat-conducting channel of the silica gel gasket by modifying spherical alumina powder, selecting raw materials and controlling the using amount of the raw materials, thereby realizing the improvement of the flexibility and the heat-conducting property of the silica gel gasket.
The applicant discloses a high-thermal-conductivity insulating heat-conducting silica gel gasket and a preparation method thereof in Chinese invention patent application publication No. CN103436019A, wherein the high-thermal-conductivity insulating heat-conducting silica gel gasket comprises the following raw materials in parts by weight: 1000 parts of spherical alumina 600-containing material, 5-15 parts of methyl vinyl silicone rubber, 30-70 parts of dimethyl silicone oil, 2-15 parts of hydrogen-containing silicone oil and 0.5-1.5 parts of catalyst, and the catalyst is prepared by the steps of screening and sintering alumina particles, grinding methyl vinyl silicone rubber and dimethyl silicone oil, stirring, vacuumizing, vulcanizing and forming and the like. The high-heat-conductivity insulating heat-conducting silica gel gasket realizes reasonable distribution of alumina particles in a silica gel matrix and improvement of the heat conductivity coefficient of the alumina particles by screening and sintering spherical alumina particles; the base material is fully ground, so that the silica gel base body and the alumina heat-conducting particles are fully fused, and the heat-conducting property of the silica gel gasket is improved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a high-strength ultralow-dielectric foaming heat-conducting silica gel gasket which can simultaneously meet the dual effects of high heat conduction and ultralow dielectric constant, and meanwhile, a structural tensile layer of low-dielectric glass fiber cloth is used as a calendering carrier, so that the overall toughness is improved, and better operability is provided.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the utility model provides a foaming heat conduction silica gel gasket of ultralow dielectricity of high strength, the heat conduction interface material main component of use includes: liquid-based glue, heat-conducting filler, foaming agent, crosslinking agent, catalyst, delay agent and silane coupling agent. The composite material comprises the following components in parts by mass: 80-150 parts of liquid-based adhesive, 700-950 parts of heat-conducting filler, 5-12 parts of foaming agent, 0.05-0.3 part of retarder, 5-20 parts of cross-linking agent and 3-5 parts of catalyst, and specifically, the middle part of the material is reinforced by glass fiber cloth with low dielectric property. The foaming heat-conducting silica gel gasket comprises a structural tensile layer which is located in the middle and is made of a material selected from glass fiber cloth or carbon fiber cloth, wherein a first foaming silica gel layer and a second foaming silica gel layer are respectively formed on the upper surface and the lower surface of the structural tensile layer by a heat-conducting interface material, the tensile strength of the foaming heat-conducting silica gel gasket is more than or equal to 2.5Mpa, and the heat conductivity coefficient of the foaming heat-conducting silica gel gasket is controlled to be more than 3.0W/m.k and the dielectric constant is controlled to be less than 3.0@1MHz by utilizing multi-section foaming of a foaming agent which is heated, stirred and roasted and solidified after being rolled before being rolled.
According to the invention, the foaming agent and the low-dielectric heat conduction filler are combined on the upper surface and the lower surface of the structural tensile layer by combining a multi-section foaming process, so that the foaming heat conduction silica gel gasket with the heat conductivity coefficient of more than 3.0W/m.k, the dielectric constant of less than or equal to 3.0, the density of less than 2.0g/cc and the tensile strength of more than or equal to 2.5MPA is obtained. The thermal conductivity was measured by ASTM D5470, and the dielectric constant was measured by ASTM D150.
In the alternative of the foamed heat-conducting silica gel gasket, the liquid-based adhesive comprises any one or more of vinyl silicone oil, vinyl silicone resin and vinyl phenyl silicone resin with different viscosities;
preferably, the vinyl silicone oil contained in the liquid-based adhesive is subjected to fine suction filtration treatment, the small molecular volatile component D3-D20 is less than or equal to 150ppm, and the viscosity is controlled within 300-10000mpa.s, particularly within 500-800 mpa.s.
By utilizing the technical characteristics of the preferable scheme, the vinyl silicone oil contained in the liquid-based adhesive has the micromolecule volatile matter D3-D20 of less than or equal to 150ppm, the viscosity is controlled to be 300-10000mpa.s, and the powder is better filled.
In the alternative of the foamed heat-conducting silica gel gasket, the heat-conducting filler is heat-conducting powder with low dielectric property, such as one or more of BN, silicon carbide, silicon micropowder and the like;
preferably, the heat-conducting filler is boron nitride powder, the particle size is mainly selected from 1-3 microns, 40 microns, 70 microns and 120 microns, and the specific matching specific gravity is 1-3 microns: 40 microns: 70 microns: 120 microns in the ratio of 4: 1: 1: 5 or 4: 0.5: 0.5: 5, but not limited to the above proportion, other combinations and combinations are also possible.
The invention utilizes the technical characteristics of the above alternatives, the heat-conducting filler is a matching combination of various particle size selections, and is matched with the proper proportion of individual particle sizes, when the heat-conducting filler with 1-3 microns or fine particle size is more, the heat-conducting filler is seriously thickened and is easy to agglomerate, so that the heat conductivity coefficient is reduced, the phenomenon of serious thickening can be prevented by properly selecting the heat-conducting filler with 70 microns or 120 microns or coarse particle size, the heat conduction can be effectively improved, and the balance of the particle size proportion can be obtained.
Preferably, the boron nitride powder is subjected to surface coating treatment by a coupling agent;
preferably, the boron nitride powder is subjected to baking treatment for removing water before use, and the baking temperature can be 120-150 ℃ and the baking time is 1-3H.
According to the invention, by utilizing the technical characteristics of the alternative scheme, the boron nitride powder is used as the heat-conducting filler, so that the heat conductivity is good, and the low dielectric property is also good; when the baking temperature after rolling is close to or slightly higher than the decomposition temperature of the foaming agent, the rolling forming can increase the foaming effect of the foaming agent which is continuously played by baking at the rear section, and the low dielectric stability in use is maintained.
In the alternative of the foaming heat-conducting silica gel gasket, the type of the coupling agent mainly comprises any one or any combination of long-chain alkyl siloxane, a titanate coupling agent, an aluminate coupling agent, a vinyl silane coupling agent and an epoxy silane coupling agent;
preferably, the coupling agent of the coated boron nitride powder is hexadecyl trimethoxy siloxane.
According to the invention, by utilizing the technical characteristics of the alternative, the coupling agent changes the surface characteristics of the heat-conducting filler, so that the heat-conducting filler is more uniformly dispersed in the first foaming silica gel layer and the second foaming silica gel layer.
In the alternative of the foaming heat-conducting silica gel gasket, the foaming agent mainly comprises any one or any combination of azo compounds, sulfonyl hydrazine compounds, nitroso compounds, carbonates, water glass and carbon black;
preferably, the foaming agent used for the foamed heat-conducting silica gel gasket specifically includes azobisisobutyronitrile, the decomposition temperature of which may be between 90 ℃ and 115 ℃, but is not limited to the collocation of azobisisobutyronitrile with other foaming agents. For example, the foaming agent is of the composite type. Other blowing agents are used in combination to adjust the decomposition temperature of the blowing agent.
According to the invention, by utilizing the technical characteristics of the alternatives, the foaming agent has a specific decomposition temperature which is matched with the preheating temperature before calendering and the curing heat treatment temperature of the silica gel after calendering, so that the foaming agent can be decomposed and foamed in the preheating process before calendering and the curing heat treatment process of the silica gel after calendering.
In the alternative of the foaming heat-conducting silica gel gasket, glass fiber cloth is clamped in the material to serve as the structural tensile layer, so that the supporting and toughening effects are achieved; preferably, the structural tensile layer is glass fiber cloth with the thickness of less than or equal to 0.02mm, the glass fiber cloth has low dielectric property, and the dielectric constant of the glass fiber cloth is less than 3.2@1 MHz.
According to the invention, by utilizing the technical characteristics of the alternative, the glass fiber cloth enables the structural tensile layer to have the functions of supporting, toughening and low dielectric of the gasket, and the technical effect that the product dielectric property of the foamed heat-conducting silica gel gasket is lower than that of the middle layer of the structural tensile layer is realized by matching with the foaming gases of the first foaming silica gel layer and the second foaming silica gel layer on the upper surface and the lower surface. The thickness of the structural tensile layer can be designed to be extremely thin, and more configuration thicknesses for forming the first foaming silica gel layer and the second foaming silica gel layer are reserved.
In the alternative of the foaming heat-conducting silica gel gasket, the density of the foaming heat-conducting silica gel gasket is less than or equal to 2.0g/cc, and the foaming heat-conducting silica gel gasket also has the tensile strength of more than or equal to 3.0 Mpa; the tensile strength of the first foaming silica gel layer or/and the second foaming silica gel layer is less than 0.2 Mpa.
The invention utilizes the technical characteristics of the alternative schemes, the density of the foaming heat-conducting silica gel gasket can reach less than or equal to 2.0G/cc, the foaming heat-conducting silica gel gasket has the tensile strength of more than or equal to 3.0MPa by virtue of the structural tensile layer, the integral foaming heat-conducting silica gel gasket has good balance of high heat conduction, low dielectric and high strength, and the foaming heat-conducting silica gel gasket is suitable for heat conduction devices of high-speed communication electronic device products of 5G or more than 5G times.
The invention further provides a preparation method of the foaming heat-conducting silica gel gasket, which comprises the following specific implementation operations:
step S1, dispersing and mixing uniformly vinyl silicone oil with different viscosities and MQ silicone resin contained in the liquid base adhesive, sequentially adding a cross-linking agent and a foaming agent, continuously stirring and mixing uniformly, heating at 120 +/-5 ℃ for 3-20min, and cooling to obtain a rubber material A;
step S2, sequentially adding a delay agent, a heat-conducting filler and a catalyst into the rubber material A, mixing the mixture fully and uniformly by open kneading to obtain rubber material B, and preferably drying and dehumidifying the rubber material B at a high temperature of 120 +/-5 ℃ for 3 +/-1H before the heat-conducting filler is used;
step S3, after the sizing material B is vacuumized, the sizing material B is added on the upper surface and the lower surface of the structural tensile layer at the same time, so that the structural tensile layer such as glass fiber cloth is clamped in the middle of the gasket, and the gasket is calendered into a rubber sheet with a specific thickness by a calender;
and step S4, baking the rolled film in an oven at the temperature of 120-150 ℃ for 15-30min to obtain the final foamed heat-conducting silica gel gasket product.
In the basic scheme of the process, the vacuumizing operation in the step S3 is used for eliminating the influence of air in the material, the heat-conducting interface material which is before being cured in the step S2 and is uniformly stirred can smoothly contact the surface of the structure tensile layer without forming air traps when being calendered in the step S3, and the calendering operation after the vacuumizing in the step S3 prevents the heat-conducting interface material from foaming at the surface of the structure tensile layer, so that the heat-conducting interface material is in closer contact with the structure tensile layer, and the whole product after the silica gel is cured is closer and inseparable in structure. The post-rolling heating of step S4 at a sufficient temperature also causes the foaming agent to continue foaming, but the pre-heating of step S1 can cause the foaming effect to be more sufficient, and the micro-bubbles formed by the foaming agent to be more uniformly dispersed in the thermal interface material, i.e., pre-foaming.
In the optional step of the preparation method of the foaming heat-conducting silica gel gasket, in step S1, the heating pretreatment time is 10-30min, specifically 10 +/-1 min, so that the foaming agent can be foamed normally, the decomposition temperature of the foaming agent is 90-115 ℃, in step S4, the baking temperature is 120-150 ℃, and the baking time is 15-30min, specifically 20 +/-2 min.
The present invention utilizes the technical features of the aforementioned alternative, the preheating temperature in step S1 is the same as or close to the foaming decomposition temperature in step S4, and the pre-foaming time sufficient to start foaming but not complete foaming is given in step S1, thereby realizing two-stage foaming of the foaming agent before and after calendering.
The invention further provides a heat-conducting interface material for preparing the high-strength ultralow-dielectric foamed heat-conducting silica gel gasket in any technical scheme.
In summary, the present invention includes at least one of the following technical effects that contribute to the prior art:
1. the silica gel gasket achieves the balance of high thermal conductivity (more than or equal to 3.0W/m.k) and low dielectric property (less than or equal to 3.0) at the same time, the thickness range of the silica gel gasket can be controlled within 0.5-5mm, the silica gel gasket is suitable for the attachment heat conduction of a high-speed operation electronic device (such as a 5G component in particular), a structural tensile layer is used as a calendering carrier film before the first foaming silica gel layer and the second foaming silica gel layer on the upper surface and the lower surface are cured and formed, the tensile strength of the foaming heat conduction silica gel gasket of a final product is more than or equal to 2.5Mpa, and the silica gel gasket is suitable for the production process of continuous roll calendering manufacturing equipment;
2. the density of the heat-conducting silica gel gasket is less than or equal to 2.0g/cc, and the heat-conducting silica gel gasket has ideal choice in some occasions with strict requirements on the whole weight;
3. the structural tensile layer is utilized to increase the integral strength, so that the tensile strength of the product is more than or equal to 2.5Mpa, the operability is better in the practical application process, and the method is suitable for the production process of continuous roll rolling manufacturing equipment.
Drawings
FIG. 1 is a cross-sectional view of a high strength ultra-low dielectric foam heat conductive silicone gasket according to some preferred embodiments of the present invention;
fig. 2 is a schematic flow chart illustrating a method for manufacturing a foam heat-conducting silica gel gasket according to some preferred embodiments of the invention.
The reference numbers are 10, a structural tensile layer, 20, a first foaming silica gel layer, 30, a second foaming silica gel layer, 21,31, air bubbles, 22,32 and heat-conducting filler.
Detailed Description
The technical solutions in the embodiments of the present invention will be made clear and fully described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments based on the embodiments of the present invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention.
Referring to fig. 1, a cross-sectional view of a high-strength ultra-low dielectric foamed thermal silica gel gasket according to some preferred embodiments of the invention is shown. A high-strength ultralow-dielectric foaming heat-conducting silica gel gasket mainly comprises the following heat-conducting interface materials: liquid-based glue, heat-conducting filler, foaming agent, crosslinking agent, catalyst, delay agent and silane coupling agent. The composite material comprises the following components in parts by mass: 80-150 parts of liquid-based adhesive, 700-950 parts of heat-conducting filler, 5-12 parts of foaming agent, 0.05-0.3 part of retarder, 5-20 parts of cross-linking agent and 3-5 parts of catalyst, and specifically, the middle part of the material is reinforced by glass fiber cloth with low dielectric property. The foaming heat-conducting silica gel gasket comprises a structural tensile layer 10 which is located in the middle and is made of a material selected from glass fiber cloth or carbon fiber cloth, wherein a first foaming silica gel layer 20 and a second foaming silica gel layer 30 are respectively formed on the upper surface and the lower surface of the structural tensile layer 10 by a heat-conducting interface material, the tensile strength of the foaming heat-conducting silica gel gasket is more than or equal to 2.5Mpa, and the heat conductivity of the foaming heat-conducting silica gel gasket is controlled to be more than 3.0W/m.k and the dielectric constant is controlled to be less than 3.0@1MHz by utilizing multi-stage foaming of heating, stirring and baking and curing of a foaming agent before rolling. Usually, the first foaming silicone rubber layer 20 and the second foaming silicone rubber layer 30 contain the bubbles 21,31 formed by decomposing the foaming agent and the heat conductive fillers 22,32 with different particle sizes, and are sealed by the solidified silicone rubber.
The basic implementation principle of the product is that the foaming heat-conducting silica gel gasket with the heat conductivity coefficient larger than 3.0W/m.k, the dielectric constant smaller than or equal to 3.0, the density smaller than 2.0g/cc and the tensile strength larger than or equal to 2.5MPA is obtained by combining the foaming agent of the multi-section foaming process and the low-dielectric heat-conducting filler on the upper surface and the lower surface of the structural tensile layer.
Fig. 2 is a schematic flow chart illustrating a method for manufacturing a foam heat-conducting silicone gasket according to some preferred embodiments of the invention. The preparation method of the foaming heat-conducting silica gel gasket comprises the following steps:
step S1, dispersing and mixing uniformly vinyl silicone oil with different viscosities and MQ silicone resin contained in the liquid base adhesive, sequentially adding a cross-linking agent and a foaming agent, continuously stirring and mixing uniformly, heating at 120 +/-5 ℃ for 3-20min, and cooling to obtain a rubber material A;
step S2, sequentially adding a retarder, a heat-conducting filler and a catalyst into the rubber material A, mixing the mixture fully and uniformly by open mill kneading to obtain rubber material B, wherein the retarder and the catalyst can be added only after the rubber material A is mixed well, and the catalyst can be added only after the retarder is dispersed uniformly to avoid the rubber material B from being dead, preferably, the heat-conducting filler is dried and dehumidified at a high temperature of 120 +/-5 ℃ for 3 +/-1H before being used;
step S3, after vacuumizing the sizing material B, simultaneously feeding the sizing material B on the upper surface and the lower surface of the structural tensile layer 10 to enable the structural tensile layer 10 such as glass fiber cloth to be clamped in the middle of a gasket, and calendering the gasket into a rubber sheet with a specific thickness through a calender;
step S4, baking the rolled rubber sheet for 15-30min by an oven at the temperature of 120-150 ℃ to obtain a final foamed heat-conducting silica gel gasket product; during actual production, the foamed heat-conducting silica gel gasket obtained after the rubber sheet is rolled and baked can be rolled into a roll.
The basic implementation principle of the process is that the vacuumizing operation in the step S3 is used for eliminating the influence of air in the material, the heat-conducting interface material which is before being cured in the step S2 and is uniformly stirred can smoothly contact the surface of the structure tensile layer without forming air traps when being calendered in the step S3, and the calendering operation after the vacuumizing operation in the step S3 prevents the heat-conducting interface material from foaming at the surface of the structure tensile layer, so that the heat-conducting interface material and the structure tensile layer are in closer contact, and the whole product after the silica gel is cured is structurally tighter and inseparable. The post-rolling heating of step S4 at a sufficient temperature also causes the foaming agent to continue foaming, but the pre-heating of step S1 can cause the foaming effect to be more sufficient, and the micro-bubbles formed by the foaming agent to be more uniformly dispersed in the thermal interface material, i.e., pre-foaming.
Example 1
This embodiment provides a foaming heat conduction silica gel gasket of high strength ultralow dielectricity, and the raw and other materials that prepare are according to the mass fraction: liquid-based adhesive: 65 parts of 500mpa.s double-end vinyl silicone oil, 10 parts of 10000mpa.s double-end vinyl silicone oil and 5 parts of 5000mpa.s MQ silicone resin; 8 parts of H-containing silicone oil; 0.15 parts of a retarder; 3 parts of a platinum catalyst; boron nitride powder (particle size 120 microns 400 parts, 40 microns 80 parts, 70 microns 80 parts, 1-3 microns 320 parts), 5 parts foaming agent. The product was prepared by the following procedure: s1, stirring and mixing 10000mpa.s of double-end vinyl silicone oil, 5000mpa.s of MQ silicone resin and 500mpa.s of double-end vinyl silicone oil uniformly to obtain base glue, adding 5 parts of H-containing silicone oil and 5 parts of foaming agent into the base glue, heating to 120 ℃ for 5min, and cooling to obtain a glue material A; s2, adding 0.1 part of retarder into the sizing material A, and mixing 800 parts of boron nitride powder and 3 parts of platinum catalyst uniformly to obtain a sizing material B; s3, vacuumizing the sizing material B, simultaneously adding the sizing material B on the upper surface and the lower surface of the glass fiber cloth to clamp the glass fiber cloth in the middle of the product, and calendering the product into a product with a specific thickness by a calender; s4, baking the rolled product for 20min by a blast oven at the temperature of 120-150 ℃ to finally obtain the high-strength low-dielectric-property foamed heat-conducting silica gel gasket. The test result of the high-strength low-dielectric-property heat-conducting interface material is as follows: thermal conductivity 3.25W/m.k, dielectric constant 2.85 @1MHZ, density: 1.8 g/cc.
Example 2
This embodiment 2 provides a foaming heat conduction silica gel gasket of ultra-low dielectric property of high strength, and the raw and other materials of preparation are calculated according to the mass fraction: liquid-based adhesive: 75 parts of 500mpa.s double-end vinyl silicone oil and 10 parts of 5000mpa.s MQ silicone resin; 10 parts of silicone oil containing H; 0.15 parts of a retarder; 3 parts of a platinum catalyst; heat conductive filler: 400 parts of 120-micron boron nitride, 80 parts of 40-micron boron nitride, 80 parts of 70-micron boron nitride, 320 parts of 1-3-micron boron nitride) and 8 parts of foaming agent. The specific implementation operation steps refer to those of example 1, and the test result of the high-strength low-dielectric-property thermal interface material is as follows: thermal conductivity 3.11W/m.k, dielectric constant 2.8 @1MHZ, density: 1.65 g/cc.
Example 3
In this example 3, fine adjustment is mainly performed on the basis of the example 2, and the prepared raw materials are as follows in parts by mass: liquid-based adhesive: 75 parts of 500mpa.s double-end vinyl silicone oil and 10 parts of 5000mpa.s MQ silicone resin; 10 parts of H-containing silicone oil; 0.15 parts of a retarder; 3 parts of a platinum catalyst; heat conductive filler: 400 parts of 120-micron boron nitride, 80 parts of 40-micron boron nitride, 80 parts of 70-micron boron nitride, 320 parts of 1-3-micron boron nitride) and 8 parts of foaming agent. The operation was carried out by adjusting the heating time at 120 ℃ to 2min after the blowing agent was added in step S1, and the other steps were completed with reference to the operation in example 1. The test result of the high-strength low-dielectric-property heat-conducting interface material is as follows: thermal conductivity of 3.05W/m.k, dielectric constant of 2.98 @1MHZ, density: 1.89g/cc, the examples mainly demonstrate that the foaming agent must be left to foam for a sufficient time after the foaming agent is added, otherwise the foaming effect cannot be realized.
Comparative example 1
This embodiment provides a foaming heat conduction silica gel gasket of high strength ultralow dielectricity, and the raw and other materials that prepare are according to the mass fraction: liquid-based adhesive: 65 parts of 500mpa.s double-end vinyl silicone oil, 10 parts of 10000mpa.s double-end vinyl silicone oil and 5 parts of 5000mpa.s MQ silicone resin; 8 parts of H-containing silicone oil; 0.15 parts of a retarder; 3 parts of a platinum catalyst; boron nitride powder (particle size 120 micron 400 parts, 40 micron 80 parts, 70 micron 80 parts, 1-3 micron 320 parts), 0 part of foaming agent. Specific implementation procedure reference was made to the procedure in example 1. The test result of the high-strength low-dielectric-property heat-conducting interface material is as follows: thermal conductivity 3.46W/m.k, dielectric constant 3.4 @1MHZ, density: 1.94 g/cc. The results show that the reduction of the foaming agent can improve the heat conductivity of the product to some extent, but the dielectricity is increased, and the influence of the foaming on the product manufacturing process is also explained.
The above embodiments are described in more detail and specifically, but the invention is not limited thereto. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (12)
1. The utility model provides a foaming heat conduction silica gel gasket of ultra-low dielectric property of high strength which characterized in that, the heat conduction interface material's that foaming heat conduction silica gel gasket used constitution mainly includes: the heat-conducting heat-insulating material comprises liquid-based glue, a heat-conducting filler, a foaming agent, a cross-linking agent, a catalyst, a retarding agent and a silane coupling agent, and comprises the following components in parts by mass: 80-150 parts of liquid-based adhesive, 700-950 parts of heat-conducting filler, 5-12 parts of foaming agent, 0.5-2 parts of delay agent, 5-20 parts of cross-linking agent and 3-5 parts of catalyst, wherein the foaming heat-conducting silica gel gasket comprises a structural tensile layer which is positioned in the middle and is made of glass fiber cloth or carbon fiber cloth, a first foaming silica gel layer and a second foaming silica gel layer are respectively formed on the upper surface and the lower surface of the structural tensile layer by the heat-conducting interface material, the tensile strength of the foaming heat-conducting silica gel gasket is more than or equal to 3.0MPa, the heat conductivity coefficient of the foaming heat-conducting silica gel gasket is controlled to be more than 3.0W/m.k and the dielectric constant is less than 3.0@1MHz by utilizing multi-stage foaming of heating stirring before rolling and baking curing after rolling of the foaming agent, the structural tensile layer is used as a rolling carrier, and the foaming heat-conducting silica gel gasket is suitable for the production process of continuous rolling manufacturing equipment, and the multi-stage foaming comprises rolling Pre-foaming by pre-heating and continuous foaming by heating after rolling;
the heat-conducting filler is boron nitride powder, and the particle size is selected from 1-3 microns, 40 microns, 70 microns and 120 microns; the boron nitride powder is subjected to surface coating treatment by a coupling agent; the boron nitride powder is baked to remove moisture before use.
2. The foamed heat-conducting silica gel gasket of claim 1, wherein the liquid-based adhesive comprises one or more of finely filtered vinyl silicone oil, vinyl silicone resin, and vinyl phenyl silicone resin with different viscosities.
3. The foamed heat-conducting silicone rubber gasket of claim 2, wherein the vinyl silicone oil contained in the liquid-based adhesive is subjected to fine suction filtration and has a small-molecule volatile matter of D3-D20 of 150ppm or less.
4. The foamed heat-conducting silica gel gasket of claim 1, wherein the coupling agent comprises one or any combination of long-chain alkyl siloxane, titanate coupling agent, aluminate coupling agent, vinyl silane coupling agent and epoxy silane coupling agent.
5. The foamed thermal silica gel gasket of claim 4, wherein the coupling agent is hexadecyl trimethoxy siloxane.
6. The foamed thermal silica gel gasket of claim 1, wherein the foaming agent comprises one or any combination of azo compounds, sulfonyl hydrazide compounds, nitroso compounds, carbonates, water glass, and carbon black.
7. The foamed heat-conductive silicone gasket of claim 6, wherein the foaming agent used in the foamed heat-conductive silicone gasket specifically comprises azobisisobutyronitrile.
8. The foamed heat-conducting silica gel gasket of claim 1, wherein the structural tensile layer sandwiched by the foamed heat-conducting silica gel gasket is a glass fiber cloth with a thickness of 0.02mm or less, and the glass fiber cloth has a dielectric constant of < 3.2@1MHz, so that the structural tensile layer sandwiched inside the foamed heat-conducting silica gel gasket plays a role in supporting and toughening.
9. The foamed heat-conducting silicone rubber gasket according to any one of claims 1 to 8, wherein the density of the foamed heat-conducting silicone rubber gasket is less than or equal to 2.0 g/cc; the tensile strength of the first foaming silica gel layer or/and the second foaming silica gel layer is less than 0.2 Mpa.
10. A method for preparing a foamed heat-conducting silica gel gasket, wherein the foamed heat-conducting silica gel gasket is the foamed heat-conducting silica gel gasket with high strength and ultralow dielectric property, which is disclosed in any one of claims 1 to 9, and the method comprises the following steps:
s1, stirring and mixing the liquid base rubber, the cross-linking agent and the foaming agent uniformly in advance, heating to 120 +/-5 ℃, and cooling to obtain a rubber material A;
s2, sequentially adding a retarder, a heat-conducting filler and a catalyst into the rubber material A, and kneading and stirring the mixture in an open mill to be fully and uniformly mixed to obtain rubber material B;
s3, vacuumizing the sizing material B, simultaneously feeding the sizing material B on the upper surface and the lower surface of the structural tensile layer to enable the structural tensile layer to be clamped in the middle of the gasket, and calendering the structural tensile layer into a rubber sheet with a specific thickness by a calender;
s4, baking the rolled film in an oven at the temperature of 120-150 ℃ to obtain the foamed heat-conducting silica gel gasket.
11. The method as claimed in claim 10, wherein the heating pretreatment time is 10-30min at step S1 to allow the foaming agent to be foamed normally, the decomposition temperature of the foaming agent is 90-115 ℃, and the baking temperature is 120-150 ℃ and the baking time is 15-30min at step S4.
12. The method of claim 11, wherein the heating pretreatment time of step S1 is controlled to 10 + -1 min, and the baking time of step S4 is controlled to 20 + -2 min.
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| CN114316607B (en) * | 2022-01-06 | 2023-04-25 | 株洲时代新材料科技股份有限公司 | Fiber-reinforced organic silicon foam material and preparation method and application thereof |
| CN114953653A (en) * | 2022-06-02 | 2022-08-30 | 昆山兆科电子材料有限公司 | Impact-resistant foaming silica gel gasket and preparation method thereof |
| CN116218111B (en) * | 2023-01-10 | 2024-03-26 | 苏州天脉导热科技股份有限公司 | BN low dielectric heat conducting piece |
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