CN115386232A - Bi-component heat-conducting silica gel and preparation process thereof - Google Patents

Bi-component heat-conducting silica gel and preparation process thereof Download PDF

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CN115386232A
CN115386232A CN202211242852.2A CN202211242852A CN115386232A CN 115386232 A CN115386232 A CN 115386232A CN 202211242852 A CN202211242852 A CN 202211242852A CN 115386232 A CN115386232 A CN 115386232A
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heat
conducting
gel
fumed silica
stirring
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林伟毅
林武城
张财根
谭承业
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Fujian Zhenjing New Material Technology Co ltd
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Fujian Zhenjing New Material Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K5/00Heat-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
    • C09K5/08Materials not undergoing a change of physical state when used
    • C09K5/14Solid materials, e.g. powdery or granular
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/005Additives being defined by their particle size in general
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives

Abstract

The invention discloses a bi-component heat-conducting silica gel and a preparation process thereof, and the bi-component heat-conducting silica gel and the preparation process thereof have the following working principles: alpha, omega-divinyl dimethyl silicone polymer (the viscosity is 100-2000 mPa.s) is taken as basic silicone oil, hydrogen-containing silicone oil (the active hydrogen mass fraction is 0.06-7.5), inhibitor (ethynyl cyclohexanol) and catalyst (3200 ppm platinum catalyst); heat conductive filler (Al) 2 O 3 ) Alumina, alumina: purity not less than 99%, average particle diameter 5 μm, spherical oxidationAluminum: purity is more than or equal to 99.8%, and average grain size is 20 μm aluminum hydroxide: purity is more than or equal to 99%, average grain diameter is 20 mu m, and white carbon black by a gas phase method: YH-200. The invention adopts spherical Al 2 O 3 The heat-conducting performance of the heat-conducting filler and the heat-conducting silica gel is obviously improved, and the spherical Al 2 O 3 After high filling is realized, the fluidity of the heat-conducting gel is good, the heat-conducting gel can be gradually vulcanized after assembly, the assembly thickness can be very low, the thermal resistance is relatively low, the heat-conducting gel has high thixotropy, and the vulcanized state is stable.

Description

Bi-component heat-conducting silica gel and preparation process thereof
Technical Field
The invention relates to the technical field of food, in particular to a bi-component heat-conducting silica gel and a preparation process thereof.
Background
The power loss of electronic devices during operation is mainly converted into heat energy, so that the temperature of electronic equipment is increased, the thermal stress is increased, the reliability and the service life of the electronic devices are seriously influenced, and the excess heat energy needs to be dissipated as soon as possible. In the heat dissipation process, the thermal interface material plays a vital role, and is mainly used for filling up micro-gaps and holes with uneven surfaces generated when an electronic device is in contact with a heat radiator, and reducing the heat resistance of heat transfer.
Compared with 4G wireless mobile terminal equipment, the chip processing capacity of the 5G wireless mobile terminal equipment is greatly improved to 4 and 5 times of that of 4G, so that the power consumption is greatly improved, and the generated heat is also obviously improved; the number of networking devices is greatly increased, and the number of antennas of the 5G wireless mobile terminal is 5 times or 10 times that of antennas of the 4G wireless mobile terminal. The 5G wireless mobile terminal also adopts new materials such as ceramic and glass shells which do not generate shielding effect on 5G signals, but the heat dissipation performance of the materials is weaker than that of metal, so that the materials with more excellent heat conduction performance are required. Meanwhile, a large amount of thermal interface materials are needed for quick heat dissipation in the construction of the 5G communication base station. Therefore, on one hand, the latest development of electronic technology opens up a brand-new application field for thermal interface materials, so that the thermal interface materials have more and more important functions in various electronic products and become important materials in electronic heat dissipation engineering, and the usage amount is continuously and greatly increased in the future; on the other hand, the continuous upgrade of electronic products poses new performance requirements and technical challenges for the thermal interface materials associated in the industry chain.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides the bi-component heat-conducting silicone gel and the preparation process thereof, and the heat conductivity of the heat-conducting gel is improved and the tensile strength of the gel is improved by optimizing the heat conductivity and the fluidity of the heat-conducting silicone gel.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: the working principle of the bi-component heat-conducting silica gel and the preparation process thereof is as follows: alpha, omega-divinyl dimethyl silicone polymer (the viscosity is 100-2000 mPa s) is used as basic silicone oil, hydrogen-containing silicone oil (the active hydrogen mass fraction is 0.06-7.5), inhibitor (ethynyl cyclohexanol) and catalyst (3200 ppm platinum catalyst); heat conductive filler (Al) 2 O 3 ) Alumina, alumina: purity is more than or equal to 99%, average grain diameter is 5 μm, spherical alumina: purity is more than or equal to 99.8%, and average grain size is 20 μm aluminum hydroxide: purity is more than or equal to 99%, average grain diameter is 20 mu m, and white carbon black by a gas phase method: YH-200.
Preferably, the component A: taking 100 parts of alpha, omega-divinyl dimethyl polysiloxane, 0.5g of catalyst, 0.1g of catalyst and 400-1200 parts of heat conducting filler, uniformly mixing, stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, adding 100g of aluminum hydroxide, stirring for 15min, vacuumizing to remove bubbles after uniform stirring, adding 200g of spherical alumina, stirring for 0.5h, vacuumizing to remove bubbles, and finally adding fumed silica to adjust the viscosity to 50 multiplied by 10 4 ~100×10 4 mPa·s。
Preferably, the component B: taking 100 parts of alpha, omega-divinyl polydimethylsiloxane, 01g of inhibitor and stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, adding 100g of aluminum hydroxide, stirring for 15min, vacuumizing to remove bubbles, adding 200g of spherical alumina, stirring for 0.5h, vacuumizing to remove bubbles, and finally adding fumed silica to adjust the viscosity to 50 x 10 4 ~100×10 4 mPa·s。
Preferably, the alpha, omega-divinyl polydimethylsiloxane is one of the main components of addition type mailing silica gel, and the alpha, omega-divinyl polydimethylsiloxane is synthesized by adding octamethylcyclotetrasiloxane into a dry reaction bottle, stirring and heating to 90 ℃, adding tetramethyl divinyl disiloxane, fully stirring, adding tetramethyl ammonium hydroxide silicon alkoxide, introducing nitrogen at 110 ℃ until the viscosity of reactants is not changed, increasing the gas amount of introduced nitrogen, decomposing residual catalyst at 200 ℃, stopping the decomposition reaction when the discharged tail gas is pH =8, removing low-boiling substances under reduced pressure, mixing activated adsorbent and synthesized alpha, omega-divinyl polydimethylsiloxane, fully stirring at a certain temperature, standing after keeping the temperature for several hours, precipitating the adsorbent, filtering under reduced pressure to remove the adsorbent, and obtaining colorless and transparent alpha, omega-divinyl polydimethylsiloxane.
Preferably, each component of the heat-conducting gel is in a solid-liquid mixed state, the larger the crosslinking density of the heat-conducting gel is, the smaller the oil leakage amount of the heat-conducting gel is, and the influence of oil leakage is delayed by adding a certain amount of fumed silica to increase the stability of the system.
Preferably, the fumed silica has small particle size of 8-19 nm and specific surface area of 130-480 2 The DBP oil absorption value is 1.50-2.00 c 3 The fumed silica has the advantages of high purity and good reinforcing effect, and when the specific surface area of the fumed silica is 200m 2 The heat-conducting gel has the lowest consistency and the highest extrudability, and the specific surface area of the fumed silica is 100m 2 In the case of the specific surface area of the added white carbon black, the consistency of the heat-conducting gel is highest, the extrudability is worst, the consistency of the gel is reduced along with the increase of the specific surface area of the white carbon black, the extrudability is better, the proportion of the white carbon black in the heat-conducting gel by a gas phase method is 5-30%, the mechanical properties of the heat-conducting gel are greatly influenced by different proportions, and the specific surface area of the added white carbon black is 200m 2 The tensile strength performance of the/g heat-conducting gel is best, the increase of the using amount of the fumed silica can cause that the fumed silica is difficult to disperse in a system, powder agglomeration occurs, the formation of a heat-conducting gel network structure is hindered, the fracture elongation of the silica gel is reduced, the heat storage time of the fumed silica has great influence on the storage period of the sealant, the storage period of the prepared heat-conducting gel can be increased along with the increase of the heat storage time of the fumed silica, when the heat storage time of the fumed silica is higher than 12h, the storage period of the heat-conducting gel can be prolonged, and the increase of the gas storage time of the fumed silicaThe hot storage time of the fumed silica can effectively reduce the water content of the heat-conducting gel, the vulcanization speed of the heat-conducting gel is reduced, the consistency of the heat-conducting gel using the fumed silica with the high specific surface area can be effectively reduced, the extrusion performance of the heat-conducting gel is improved, the mechanical performance of the heat-conducting gel can be improved by adding the fumed silica, the white silica with the same addition amount is selectively added, the tensile strength of the fumed silica with the high specific surface area can be higher, the white silica with the high specific surface area is added, the heat-conducting gel has the best elongation at break, and the storage period of the heat-conducting gel can be prolonged by adding the fumed silica after baking treatment.
Preferably, the Al is 2 O 3 The appearance, the dosage and the grain diameter of the heat-conducting filler also have influence on the performance of the heat-conducting silica gel, and the spherical Al 2 O 3 Has a relatively high fillable amount of spherical Al 2 O 3 After high filling is realized, the fluidity of the rubber material is good, and Al with the granularity of 32-45 mu m and 18-30 mu m is used 2 O 3 The composite heat-conducting silica gel is compounded, when the using amount of the heat-conducting filler is the same, the grain size of the heat-conducting filler is larger, the heat conductivity of the silica gel is better, and Al is contained 2 O 3 The smaller the particle size, the larger the specific surface area and the larger the contact area with the substrate, and the smaller the particle size Al 2 O 3 The prepared heat-conducting silica gel has higher mechanical property and better crosslinking density of a system, and two kinds of Al with different grain diameters 2 O 3 The heat-conducting silica gel has good heat-conducting property and high tensile strength.
Preferably, the bi-component silica gel is used as a base material, alumina is added as a heat conducting filler, and contact denaturation is adjusted by fumed silica, so that the prepared bi-component heat conducting gel has the advantages that the oil extraction amount, the heat conductivity and the hardness of the heat conducting gel are increased along with the increase of storage events, and the shelf life of the heat conducting gel is more reasonably positioned for 3-5 months.
Preferably, the adhesive force of the heat-conducting silicone gel is in a trend of decreasing after increasing along with the increase of the viscosity of the vinyl silicone oil, the adhesive force of the alpha, omega-divinyl polydimethylsiloxane with the viscosity of 500 is the best, the adhesive force of the heat-conducting silicone gel is in a trend of increasing and then decreasing along with the increase of the hydrogen content of the hydrogen-containing silicone oil, the hydrogen-containing silicone oil with the hydrogen content of 0.1 is selected, and the adhesive force is the best
(III) advantageous effects
The invention provides a bi-component heat-conducting silica gel and a preparation process thereof, and the bi-component heat-conducting silica gel has the following beneficial effects:
(1) The invention adopts Al 2 O 3 A thermally conductive filler, al 2 O 3 The Al-based heat-conducting filler is low in price, large in filling amount, relatively small in influence on system viscosity, is a common heat-conducting filler at present, and is Al with different grain diameters 2 O 3 Surface modified Al capable of improving heat conductivity of material by compounding 2 O 3 When the spherical Al-Si-Al heat-conducting silica gel is used as a heat-conducting filler, the heat-conducting performance of the heat-conducting silica gel is obviously improved, and the spherical Al 2 O 3 After high filling is achieved, the flowability is better.
(2) The fumed silica is a reinforcing filler and has good tensile strength and tear strength, because the fumed silica black particles have small size effect and large specific surface area, the surfaces of the fumed silica black particles contain a plurality of silicon hydroxyl groups, the particles can form a network structure through the action of hydroxyl bonds and van der waals force, meanwhile, the silica particles also generate strong interaction with polysiloxane molecules, and the interface cohesiveness is improved.
(3) The heat-conducting gel is a common heat-conducting interface material, can be gradually vulcanized after being assembled, has low assembly thickness, relatively low thermal resistance, high thixotropy and stable state after vulcanization.
Detailed Description
All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The invention provides a technical scheme that: a two-component heat-conducting silica gel and a preparation process thereof have the following working principle: alpha, omega-divinyl dimethyl silicone polymer (the viscosity is 100-2000 mPa.s) is taken as basic silicone oil, hydrogen-containing silicone oil (the active hydrogen mass fraction is 0.06-7.5), inhibitor (ethynyl cyclohexanol) and catalyst (3200 ppm platinum catalyst); heat conductive filler (Al) 2 O 3 ) Alumina, alumina: purity is more than or equal to 99%, average grain diameter is 5 μm, spherical alumina: purity is more than or equal to 99.8%, and average grain size is 20 μm aluminum hydroxide: purity is more than or equal to 99%, average grain diameter is 20 mu m, and white carbon black by a gas phase method: YH-200.
Further component A: uniformly mixing 100 parts of alpha, omega-divinyl polydimethylsiloxane, 0.5g of catalyst, 0.1g of catalyst and 400-1200 parts of heat-conducting filler, stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, adding 100g of aluminum hydroxide, stirring for 15min, vacuumizing to remove bubbles after stirring uniformly, adding 200g of spherical alumina, stirring for 0.5h, vacuumizing to remove bubbles, and finally adding fumed silica to adjust the viscosity to 50 multiplied by 10 4 ~100×10 4 mPa·s。
And further B component: taking 100 parts of alpha, omega-divinyl polydimethylsiloxane, 01g of inhibitor and stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, adding 100g of aluminum hydroxide, stirring for 15min, vacuumizing to remove bubbles, adding 200g of spherical alumina, stirring for 0.5h, vacuumizing to remove bubbles, and finally adding fumed silica to adjust the viscosity to 50 x 10 4 ~100×10 4 mPa·s。
The synthesis method of the alpha, omega-divinyl dimethyl silicone comprises the steps of adding octamethylcyclotetrasiloxane into a dry reaction bottle, stirring and heating to 90 ℃, adding tetramethyl divinyl disiloxane into the reaction bottle, fully stirring, adding tetramethyl ammonium hydroxide silicon alkoxide, introducing nitrogen into the reaction bottle at 110 ℃ until the viscosity of reactants is unchanged, increasing the amount of the introduced nitrogen, decomposing residual catalyst at 200 ℃, stopping decomposition reaction when discharged tail gas ph =8, removing low-boiling-point substances under reduced pressure, mixing activated adsorbent with the synthesized alpha, omega-divinyl dimethyl silicone, fully stirring at a certain temperature, standing the mixture after heat preservation for several hours, precipitating the adsorbent, filtering under reduced pressure to remove the adsorbent, and obtaining colorless and transparent alpha, omega-divinyl dimethyl silicone.
Each component of the further heat-conducting gel is in a solid-liquid mixed state, the larger the crosslinking density of the heat-conducting gel is, the smaller the oil leakage amount of the heat-conducting gel is, and the phenomenon of silicone oil precipitation can occur after the heat-conducting gel is placed for a period of time, and the stability of the system is improved by adding a certain amount of fumed silica so as to delay the influence of oil precipitation.
Further, the white carbon black prepared by the gas phase method has small particle size of 8-19 nm and specific surface area of 130-480 2 The DBP oil absorption value is 1.50-2.00 c 3 The fumed silica has the advantages of high purity and good reinforcing effect, and when the specific surface area of the fumed silica is 200m 2 The density of the heat-conducting gel is lowest, the extrusion performance is highest, and the specific surface area of the fumed silica is 100m 2 In the case of the specific surface area of the added white carbon black, the consistency of the heat-conducting gel is highest, the extrudability is worst, the consistency of the gel is reduced along with the increase of the specific surface area of the white carbon black, the extrudability is better, the proportion of the white carbon black in the heat-conducting gel by a gas phase method is 5-30%, the mechanical properties of the heat-conducting gel are greatly influenced by different proportions, and the specific surface area of the added white carbon black is 200m 2 The tensile strength performance of the heat-conducting gel is best, the use amount of the fumed silica is increased, the fumed silica is difficult to disperse in a system, powder agglomeration occurs, the formation of a mesh structure of the heat-conducting gel is hindered, the fracture elongation rate of the silica gel is reduced, the heat storage time of the fumed silica has great influence on the storage period of the sealant, the storage period of the prepared heat-conducting gel is increased along with the increase of the heat storage time of the fumed silica, when the heat storage time of the fumed silica is higher than 12h, the storage period of the heat-conducting gel is prolonged, the water content of the heat-conducting gel can be effectively reduced by increasing the heat storage time of the fumed silica, the vulcanization speed of the heat-conducting gel is reduced, the consistency of the fumed silica with a high specific surface area can be effectively reduced, the extrusion performance of the heat-conducting gel is improved, and the fumed silica is addedThe carbon black can improve the mechanical property of the heat-conducting gel, the white carbon black with the same addition amount is selected to be added, the tensile strength of the white carbon black with the high specific surface area is higher, the heat-conducting gel has the best elongation at break when the white carbon black with the high specific surface area is added, and the storage period of the heat-conducting gel can be prolonged through the gas-phase white carbon black subjected to baking treatment.
Further Al 2 O 3 The appearance, the dosage and the grain diameter of the heat-conducting filler also have influence on the performance of the heat-conducting silica gel, and the spherical Al 2 O 3 Has a relatively high fillable amount of spherical Al 2 O 3 After high filling is realized, the fluidity of the rubber material is better, and Al with the granularity of 32-45 mu m and 18-30 mu m is added 2 O 3 The silicon gel is compounded, when the dosage of the heat-conducting filler is the same, the particle size of the heat-conducting filler is larger, the heat conductivity of the silicon gel is better, and Al is 2 O 3 The smaller the particle size, the larger the specific surface area and the larger the contact area with the substrate, and the small particle size Al is used 2 O 3 The prepared heat-conducting silica gel has higher mechanical property and better crosslinking density of a system, and two kinds of Al with different grain diameters 2 O 3 The heat-conducting silicone gel has good heat-conducting property and high tensile strength.
And further, the bi-component silica gel is used as a base material, aluminum oxide is added as a heat-conducting filler, and the contact denaturation is adjusted by using fumed silica to prepare the bi-component heat-conducting gel, along with the increase of storage events, the oil precipitation amount, the heat conductivity and the hardness of the heat-conducting gel are increased, and the shelf life of the heat-conducting gel is positioned for 3-5 months more reasonably.
Further, along with the process that the viscosity of the vinyl silicone oil is increased, the adhesive force of the heat-conducting silicone gel tends to be decreased after being increased, the adhesive force of the alpha, omega-divinyl dimethyl silicone oil with the viscosity of 500 is the best, along with the increase of the hydrogen content of the hydrogen-containing silicone oil, the adhesive force of the heat-conducting silicone gel tends to be increased and then decreased, and the adhesive force of the hydrogen-containing silicone oil with the hydrogen content of 0.1 is the best.
In summary, the bi-component heat-conducting silica gel and the preparation process thereof are prepared by Al 2 O 3 And the problem of low heat dissipation performance is solved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. The bi-component heat-conducting silica gel and the preparation process thereof are characterized by comprising the following specific steps: the double-component heat-conducting silica gel and the preparation process thereof have the following working principle: alpha, omega-divinyl dimethyl silicone polymer (the viscosity is 100-2000 mPa.s) is taken as basic silicone oil, hydrogen-containing silicone oil (the active hydrogen mass fraction is 0.06-7.5), inhibitor (ethynyl cyclohexanol) and catalyst (3200 ppm platinum catalyst); heat conductive filler (Al) 2 O 3 ) Alumina, alumina: purity is more than or equal to 99%, average grain diameter is 5 mu m, spherical alumina: purity is more than or equal to 99.8%, and average grain size is 20 μm aluminum hydroxide: purity is more than or equal to 99%, average grain diameter is 20 mu m, and white carbon black by a gas phase method: YH-200.
2. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the component A comprises: uniformly mixing 100 parts of alpha, omega-divinyl polydimethylsiloxane, 0.5g of catalyst, 0.1g of catalyst and 400-1200 parts of heat-conducting filler, stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, adding 100g of aluminum hydroxide, stirring for 15min, vacuumizing to remove bubbles after stirring uniformly, adding 200g of spherical alumina, stirring for 0.5h, vacuumizing to remove bubbles, and finally adding fumed silica to adjust the viscosity to 50 multiplied by 10 4 ~100×10 4 mPa·s。
3. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the component B comprises: taking 100 parts of alpha, omega-divinyl polydimethylsiloxane, 01g of inhibitor, stirring for 15min, vacuumizing to remove bubbles, adding 50g of alumina, stirring for 20min, and stirring againAdding 100g of aluminum hydroxide, stirring for 15min, uniformly stirring, vacuumizing to remove bubbles, adding 200g of spherical aluminum oxide, stirring for 0.5h, vacuumizing to remove bubbles, and adding fumed silica to adjust the viscosity to 50 x 10 4 ~100×10 4 mPa·s。
4. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the alpha, omega-divinyl dimethyl polysiloxane is one of main components of addition type mailing silicone gel, the synthesis method of the alpha, omega-divinyl dimethyl polysiloxane comprises the steps of adding octamethylcyclotetrasiloxane into a dry reaction bottle, stirring and heating to 90 ℃, adding tetramethyl divinyl disiloxane, fully stirring, adding tetramethyl ammonium hydroxide silicon alkoxide, introducing nitrogen at 110 ℃, increasing the amount of introduced nitrogen until the viscosity of reactants is unchanged, decomposing residual catalyst at 200 ℃, stopping decomposition reaction when discharged tail gas ph =8, removing low-boiling-point substances under reduced pressure, mixing activated adsorbent and synthesized alpha, omega-divinyl dimethyl polysiloxane, fully stirring at a certain temperature, standing after keeping the temperature for several hours, precipitating the adsorbent, filtering under reduced pressure to remove the adsorbent, and obtaining colorless and transparent alpha, omega-divinyl dimethyl polysiloxane.
5. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: each component of the heat-conducting gel is in a solid-liquid mixed state, the crosslinking density of the heat-conducting gel is larger and the oil permeation amount of the heat-conducting gel is smaller when the heat-conducting gel is placed for a period of time, and the stability of the system is improved by adding a certain amount of fumed silica so as to delay the influence of oil precipitation.
6. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the white carbon black prepared by the vapor phase method has small particle size of 8-19 nm and specific surface area of 130-480 m 2 G, DBP oil absorption value of 1.50-2.00 cm 3 The white carbon black has the advantages of high purity and reinforcing effectPreferably, when the specific surface area of the fumed silica is 200m 2 The heat-conducting gel has the lowest consistency and the highest extrudability, and the specific surface area of the fumed silica is 100m 2 In the case of the specific surface area of the added white carbon black, the consistency of the heat-conducting gel is highest, the extrudability is worst, the consistency of the gel is reduced along with the increase of the specific surface area of the white carbon black, the extrudability is better, the proportion of the white carbon black in the heat-conducting gel by a gas phase method is 5-30%, the mechanical properties of the heat-conducting gel are greatly influenced by different proportions, and the specific surface area of the added white carbon black is 200m 2 The tensile strength performance of the heat-conducting gel is best, the usage amount of fumed silica is increased, fumed silica is difficult to disperse in a system, powder aggregation occurs, the formation of a heat-conducting gel net structure is hindered, the breaking elongation of silica gel is reduced, the heat storage time of fumed silica has a great influence on the storage period of the sealant, the storage period of the prepared heat-conducting gel is prolonged along with the increase of the heat storage time of the fumed silica, when the heat storage time of the fumed silica is longer than 12h, the storage period of the heat-conducting gel is prolonged, the water content of the heat-conducting gel can be effectively reduced by increasing the heat storage time of the fumed silica, the vulcanization speed of the heat-conducting gel is reduced, the consistency of the fumed silica with high specific surface area can be effectively reduced by using the fumed silica with high specific surface area, the extrusion performance of the heat-conducting gel is improved, the mechanical performance of the heat-conducting gel can be improved by adding the fumed silica, the same amount of the fumed silica is selected, the tensile strength of the fumed silica with high specific surface area is higher, the addition amount of the white silica with high specific surface area, the best breaking elongation of the heat-conducting gel, and the baking time of the fumed silica after treatment.
7. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the Al is 2 O 3 The appearance, the dosage and the particle size of the heat-conducting filler also influence the performance of the heat-conducting silica gel, and the spherical Al 2 O 3 Has a relatively high fillable amount of spherical Al 2 O 3 After high filling is realized, the fluidity of the rubber material is good, and Al with the granularity of 32-45 mu m and 18-30 mu m is used 2 O 3 The silicon gel is compounded, when the dosage of the heat-conducting filler is the same, the particle size of the heat-conducting filler is larger, the heat conductivity of the silicon gel is better, and Al is 2 O 3 The smaller the particle size, the larger the specific surface area and the larger the contact area with the substrate, and the smaller the particle size Al 2 O 3 The prepared heat-conducting silica gel has higher mechanical property and better crosslinking density of a system, and two kinds of Al with different grain diameters 2 O 3 The heat-conducting silicone gel has good heat-conducting property and high tensile strength.
8. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: according to the prepared double-component heat-conducting gel, the oil separation amount, the heat conductivity and the hardness of the heat-conducting gel are increased along with the increase of storage events by using the double-component silica gel as a base material and adding the alumina as a heat-conducting filler and adjusting the contact denaturation through the fumed silica, and the shelf life of the heat-conducting gel is more reasonably positioned for 3-5 months.
9. The two-component heat-conducting silicone gel and the preparation process thereof according to claim 1, wherein: the adhesive force of the heat-conducting silicone gel is the trend of decreasing after increasing along with the process of increasing the viscosity of the vinyl silicone oil, the adhesive force of the alpha, omega-divinyl dimethyl silicone oil with the viscosity of 500 is the best, the adhesive force of the heat-conducting silicone gel is the trend of increasing and then decreasing along with the increase of the hydrogen content of the hydrogen-containing silicone oil, and the adhesive force of the heat-conducting silicone gel is the best when the hydrogen content of the hydrogen-containing silicone oil is 0.1.
CN202211242852.2A 2022-10-11 2022-10-11 Bi-component heat-conducting silica gel and preparation process thereof Pending CN115386232A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115926473A (en) * 2022-12-27 2023-04-07 福建臻璟新材料科技有限公司 Low-oil-yield heat-conducting gel and preparation method thereof
CN116063853A (en) * 2023-01-31 2023-05-05 安徽迈腾新材料有限公司 Platinum vulcanization type heat-conductive silicone rubber composite material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10189838A (en) * 1996-12-25 1998-07-21 Siegel:Kk Heat conductive gel
CN109735112A (en) * 2018-12-28 2019-05-10 广州市白云化工实业有限公司 Additional organosilicon thermally conductive gel and preparation method thereof
CN113444487A (en) * 2020-09-14 2021-09-28 浙江大学山东工业技术研究院 Bi-component addition type heat-conducting silica gel for heat dissipation of LED lighting chip
CN114032063A (en) * 2021-12-06 2022-02-11 深圳联腾达科技有限公司 High-thermal-conductivity low-viscosity bi-component organic silicon pouring sealant and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10189838A (en) * 1996-12-25 1998-07-21 Siegel:Kk Heat conductive gel
CN109735112A (en) * 2018-12-28 2019-05-10 广州市白云化工实业有限公司 Additional organosilicon thermally conductive gel and preparation method thereof
CN113444487A (en) * 2020-09-14 2021-09-28 浙江大学山东工业技术研究院 Bi-component addition type heat-conducting silica gel for heat dissipation of LED lighting chip
CN114032063A (en) * 2021-12-06 2022-02-11 深圳联腾达科技有限公司 High-thermal-conductivity low-viscosity bi-component organic silicon pouring sealant and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115926473A (en) * 2022-12-27 2023-04-07 福建臻璟新材料科技有限公司 Low-oil-yield heat-conducting gel and preparation method thereof
CN116063853A (en) * 2023-01-31 2023-05-05 安徽迈腾新材料有限公司 Platinum vulcanization type heat-conductive silicone rubber composite material

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