A thermally conductive potting adhesive material and a preparation method thereof

Abstract

The invention relates to a heat-conducting potting glue material and a preparation method thereof, and belongs to the technical field of composite materials. The invention uses vinyl silicone oil, hydrogen-containing silicone oil, self-made modified hollow glass microbeads, silicon micropowder, graphene powder, ethynyl cyclohexanol and platinum catalyst as raw materials to prepare a heat-conducting potting glue material. The invention prepares a heat-conducting potting glue material by firstly stirring and mixing the vinyl silicone oil and the modified hollow glass microbeads, cooling the mixture and adding the hydrogen-containing silicone oil for stirring and mixing to obtain a silicone potting glue component A, and simultaneously stirring and mixing the vinyl silicone oil, silicon micropowder and graphene powder, cooling the mixture and adding the platinum catalyst for stirring and mixing to obtain a component B. The preparation method of the invention mixes the hydrogen-containing silicone oil and the platinum catalyst into the A and B components of the silicone potting glue respectively, so that the components of the prepared potting glue can be made more uniform. In addition, the invention adds the graphene powder with good thermal conductivity in the preparation process, so that the prepared heat-conducting potting glue has excellent thermal conductivity.

Description

Technical Field

[0001] The present invention belongs to the technical field of composite materials, and in particular, relates to a thermal conductive potting glue material and a preparation method thereof. Background Art

[0002] As a composite colloid material designed specifically for electronic devices and power equipment, thermal conductive potting glue has the advantages of low density and good thermal conductivity. It is widely used in new energy vehicles, electronic power supplies, high-frequency transformers, connectors, sensors, electric heating parts and circuit boards. Thermal conductive potting glue can fill the tiny gaps between electronic components, provide solid mechanical support and protection, and through its excellent thermal conductivity, transfer heat from the heat source to the heat dissipation system, thereby effectively preventing performance degradation or damage caused by overheating.

[0003] With the continuous development of electronic equipment, the requirements for heat dissipation are also constantly increasing. The heat dissipation performance of the thermally conductive potting materials in the prior art can no longer meet the needs of electronic equipment. Adding inorganic materials with excellent thermal conductivity to the thermally conductive potting materials can obtain better thermal conductivity, but it also increases the solid particle content in the potting glue, and the flow resistance between the colloids will also increase, thereby causing the viscosity to increase, which is not conducive to use. Based on this, the present invention provides a thermally conductive potting glue material and a preparation method thereof, and prepares a thermally conductive potting glue material with high thermal conductivity and low viscosity. Summary of the invention

[0004] The object of the present invention is to provide a thermally conductive potting material and a preparation method thereof, so as to solve the problems mentioned in the above background technology.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A thermally conductive potting material, comprising the following raw materials in parts by mass: 180-200 parts of vinyl silicone oil, 25-35 parts of hydrogen-containing silicone oil, 30-42 parts of modified hollow glass microspheres, 42-60 parts of silicon micropowder, 24-30 parts of graphene powder, 0.004-0.005 parts of ethynyl cyclohexanol, and 0.6-0.7 parts of platinum catalyst;

[0007] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0008] The first step is to weigh the raw materials according to their mass proportions: 180-200 parts of vinyl silicone oil, 25-35 parts of hydrogenated silicone oil, 30-42 parts of modified hollow glass microspheres, 42-60 parts of silicon micropowder, 24-30 parts of graphene powder, 0.004-0.005 parts of ethynyl cyclohexanol, and 0.6-0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0009] Step 2: Add the first portion of vinyl silicone oil and modified hollow glass microspheres into a ball mill and heat-stir for 2-3 hours, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours to obtain silicone potting compound component A;

[0010] Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and heat and stir for 2 hours, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 hours to obtain component potting glue B;

[0011] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0012] Furthermore, the vinyl silicone oil is formed by mixing terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.4-0.6wt%, and the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%.

[0013] Furthermore, the viscosity of the vinyl silicone oil is 1000 MPa·s, and the viscosity of the hydrogen-containing silicone oil is 150 MPa·s.

[0014] Furthermore, in the second step, the temperature condition of the first ball milling stirring is 100° C., the rotation speed condition is 900-1000 rpm, and the rotation speed condition of the second ball milling stirring is 400-600 rpm.

[0015] Furthermore, in the third step, the temperature condition of the first ball milling stirring is 120° C., the rotation speed condition is 600-800 rpm, and the time condition of the second ball milling stirring is 400-600 rpm.

[0016] Furthermore, in the fourth step, the mass ratio of the organic silicon component A and the organic silicon potting adhesive B used for mixing is 1:0.8-1.

[0017] Furthermore, the modified hollow glass microspheres are prepared by the following steps:

[0018] Step 1, mixing hollow glass microspheres and sodium hydroxide solution in a three-necked flask, installing a thermometer, turning on magnetic stirring, reacting at a temperature of 60° C. for 1-1.5 hours, then cooling and filtering, and washing the hollow glass microspheres with deionized water and drying to obtain surface-treated hollow glass microspheres;

[0019] Step 2, allyltriethoxysilane, p-trifluoromethylaniline, and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene were mixed in a three-necked flask, equipped with a condenser and a thermometer, and magnetic stirring was turned on. The mixture was reacted at a temperature of 40-60° C. for 20-24 hours. After the reaction was completed, the mixture was washed with a saturated sodium bicarbonate solution and extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated to obtain intermediate 1;

[0020] Step 3, the surface treated hollow glass microspheres, nano-aluminum nitride, and ethanol solution are mixed in a beaker, the pH value of the solution is adjusted to 2 with a 10% by mass dilute nitric acid solution, and then ultrasonically dispersed for 1.5-2.5 hours, and then the system temperature is raised to 40-60 ° C and the intermediate 1 is added to the beaker, and the reaction is carried out at a temperature of 40-60 ° C for 1.5 hours. After the reaction is completed, vacuum filtration is performed, and the surface treated hollow glass microspheres are washed with anhydrous ethanol and dried to obtain modified hollow glass microspheres.

[0021] Furthermore, the sodium hydroxide solution used in step 1 is a sodium hydroxide aqueous solution with a concentration of 0.3 mol / L, and the mass ratio of the hollow glass microspheres to the sodium hydroxide aqueous solution is 10g:15-25g.

[0022] Furthermore, the mass ratio of allyltriethoxysilane, p-trifluoromethylaniline, and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene used in step 2 is 4g:1.7-2g:0.057-0.06g.

[0023] Furthermore, the ethanol solution in step 3 is an ethanol solution with a mass fraction of 90%.

[0024] Furthermore, the mass ratio of the surface treated hollow glass microspheres, nano-aluminum nitride, ethanol solution, and intermediate 1 used in step 3 is 10g: 1g: 30-45g: 1.2-1.8g.

[0025] Beneficial effects of the present invention:

[0026] 1) The present invention uses vinyl silicone oil, hydrogenated silicone oil, homemade modified hollow glass microspheres, silicon micropowder, graphene powder, ethynyl cyclohexanol and platinum catalyst as raw materials to prepare a thermally conductive potting glue material. The present invention first heats and stirs the vinyl silicone oil and the modified hollow glass microspheres, cools the mixture and adds the hydrogenated silicone oil to stir and mix to obtain the silicone potting glue component A. Meanwhile, the vinyl silicone oil, silicon micropowder and graphene powder are heat and stirred to mix, and then the mixture is cooled and the platinum catalyst is added to stir and mix to obtain the component B. The preparation method of the present invention mixes the hydrogenated silicone oil and the platinum catalyst into the silicone potting glue components A and B respectively, so that the components of the prepared potting glue can be made more uniform. In addition, the present invention adds the graphene powder with good thermal conductivity in the preparation process, so that the prepared thermally conductive potting glue has excellent thermal conductivity.

[0027] 2) The present invention modifies the hollow glass microspheres with sodium hydroxide solution to obtain surface-treated hollow glass microspheres with rough surfaces, and at the same time, modifies allyltriethoxysilane with trifluoromethylaniline, and uses the amino group of trifluoromethylaniline and the double bond of allyltriethoxysilane to undergo Michael addition reaction under the catalytic action of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene to obtain a modified silane coupling agent intermediate 1, and finally uses the intermediate 1 to modify the surface-treated hollow glass microspheres. The modified hollow glass microspheres are prepared by coating aluminum nitride on the surface of the surface-treated hollow glass microspheres through ultrasonic dispersion to obtain modified hollow glass microspheres. The surface of the modified hollow glass microspheres has a rough structure and a low surface F-containing group, so that the modified hollow glass microspheres have good hydrophobicity and can reduce the viscosity of the finished thermal conductive potting glue. At the same time, the aluminum nitride structure coated on the surface can also improve the thermal conductivity of the modified hollow glass microspheres. When the modified hollow glass microspheres are added to the thermal conductive potting glue, the density of the thermal conductive potting glue can be reduced while having better thermal conductivity.

[0028] 3) The thermally conductive potting adhesive of the present invention has uniform components, stable properties, low viscosity, low density, and good thermal conductivity, and can be widely used in the fields of electronic components and communication components. DETAILED DESCRIPTION

[0029] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0030] Example 1

[0031] A modified hollow glass microsphere is prepared by the following steps:

[0032] Step 1, 10g of hollow glass microspheres and 15g of 0.3mol / L sodium hydroxide solution were mixed in a three-necked flask, a thermometer was installed, magnetic stirring was turned on, the reaction was carried out at a temperature of 60°C for 1h, and then the hollow glass microspheres were cooled and filtered, and the hollow glass microspheres were washed with deionized water and dried to obtain surface-treated hollow glass microspheres;

[0033] Step 2, 4 g of allyltriethoxysilane, 1.7 g of p-trifluoromethylaniline, and 0.057 g of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 40° C. for 20 h. After the reaction was completed, the mixture was washed with a saturated sodium bicarbonate solution and extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated to obtain intermediate 1;

[0034] Step 3, 10g of surface treated hollow glass microspheres, 1g of nano-aluminum nitride, and 30g of ethanol solution are mixed in a beaker, and the pH value of the solution is adjusted to 2 with a 10% by mass dilute nitric acid solution, followed by ultrasonic dispersion for 1.5h, and then the system temperature is raised to 40°C and 1.2g of intermediate 1 is added to the beaker, and the reaction is carried out at a temperature of 40°C for 1.5h. After the reaction is completed, vacuum filtration is performed, and the surface treated hollow glass microspheres are washed with anhydrous ethanol and dried to obtain modified hollow glass microspheres.

[0035] Example 2

[0036] A modified hollow glass microsphere is prepared by the following steps:

[0037] Step 1, 10g of hollow glass microspheres and 20g of 0.3mol / L sodium hydroxide solution were mixed in a three-necked flask, a thermometer was installed, magnetic stirring was turned on, the reaction was carried out at a temperature of 60°C for 1.25h, and then the hollow glass microspheres were cooled and filtered, and the hollow glass microspheres were washed with deionized water and dried to obtain surface-treated hollow glass microspheres;

[0038] Step 2, 4 g of allyltriethoxysilane, 1.8 g of p-trifluoromethylaniline, and 0.058 g of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 50° C. for 22 h. After the reaction was completed, the mixture was washed with a saturated sodium bicarbonate solution and extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated to obtain intermediate 1;

[0039] Step 3, 10g of surface treated hollow glass microspheres, 1g of nano-aluminum nitride, and 38g of ethanol solution were mixed in a beaker, and the pH value of the solution was adjusted to 2 with a 10% by mass dilute nitric acid solution, followed by ultrasonic dispersion for 2h, and then the system temperature was raised to 50°C and 1.6g of intermediate 1 was added to the beaker, and the reaction was carried out at a temperature of 50°C for 1.5h. After the reaction was completed, vacuum filtration was performed, and the surface treated hollow glass microspheres were washed with anhydrous ethanol and dried to obtain modified hollow glass microspheres.

[0040] Example 3

[0041] A modified hollow glass microsphere is prepared by the following steps:

[0042] Step 1, 10g of hollow glass microspheres and 25g of 0.3mol / L sodium hydroxide solution were mixed in a three-necked flask, a thermometer was installed, magnetic stirring was turned on, the reaction was carried out at a temperature of 60°C for 1.5h, and then the hollow glass microspheres were cooled and filtered, and the hollow glass microspheres were washed with deionized water and dried to obtain surface-treated hollow glass microspheres;

[0043] Step 2, 4 g of allyltriethoxysilane, 2 g of p-trifluoromethylaniline, and 0.06 g of 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene were mixed in a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, and the reaction was carried out at a temperature of 60° C. for 24 h. After the reaction was completed, the mixture was washed with a saturated sodium bicarbonate solution and extracted with dichloromethane. The organic layer was then separated with a separatory funnel, and the organic layer was rotary evaporated to obtain intermediate 1;

[0044] Step 3, 10g of surface treated hollow glass microspheres, 1g of nano-aluminum nitride, and 45g of ethanol solution were mixed in a beaker, and the pH value of the solution was adjusted to 2 with a 10% by mass dilute nitric acid solution, followed by ultrasonic dispersion for 2.5h, and then the system temperature was raised to 60°C and 1.8g of intermediate 1 was added to the beaker, and the reaction was carried out at a temperature of 60°C for 1.5h. After the reaction was completed, vacuum filtration was performed, and the surface treated hollow glass microspheres were washed with anhydrous ethanol and dried to obtain modified hollow glass microspheres.

[0045] Example 4

[0046] A thermally conductive potting material, comprising the following raw materials in parts by mass: 180 parts of vinyl silicone oil, 25 parts of hydrogen-containing silicone oil, 30 parts of modified hollow glass microspheres obtained in Example 1, 42 parts of silicon micropowder, 24 parts of graphene powder, 0.004 parts of ethynyl cyclohexanol, and 0.6 parts of a platinum catalyst;

[0047] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0048] The first step is to weigh the raw materials by mass: 180 parts of vinyl silicone oil, 25 parts of hydrogenated silicone oil, 30 parts of the modified hollow glass microspheres obtained in Example 1, 42 parts of silicon micropowder, 24 parts of graphene powder, 0.004 parts of ethynyl cyclohexanol, and 0.6 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0049] Step 2: Add the first portion of vinyl silicone oil and the modified hollow glass microspheres obtained in Example 1 into a ball mill and stir for 2-3 hours at a temperature of 100° C. and a speed of 900 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours at a speed of 400 rpm to obtain a silicone potting compound component A;

[0050] Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and stir for 2 h at 120°C and 600 rpm, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 h at 400 rpm to obtain component potting glue B;

[0051] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0052] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:0.8.

[0053] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.4wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0054] Example 5

[0055] A thermally conductive potting material, comprising the following raw materials in parts by mass: 190 parts of vinyl silicone oil, 30 parts of hydrogen-containing silicone oil, 36 parts of modified hollow glass microspheres obtained in Example 2, 51 parts of silicon micropowder, 27 parts of graphene powder, 0.0045 parts of ethynyl cyclohexanol, and 0.65 parts of a platinum catalyst;

[0056] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0057] The first step is to weigh the raw materials by mass: 190 parts of vinyl silicone oil, 30 parts of hydrogenated silicone oil, 36 parts of modified hollow glass microspheres obtained in Example 2, 51 parts of silicon micropowder, 27 parts of graphene powder, 0.0045 parts of ethynyl cyclohexanol, and 0.65 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0058] Step 2: Add the first portion of vinyl silicone oil and the modified hollow glass microspheres obtained in Example 2 into a ball mill and stir for 2.5 hours at a temperature of 100° C. and a speed of 950 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours at a speed of 500 rpm to obtain a silicone potting compound component A;

[0059] Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and stir for 2 h at 120°C and 700 rpm, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 h at 500 rpm to obtain component potting glue B;

[0060] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0061] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:0.9.

[0062] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.5wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0063] Example 6

[0064] A thermally conductive potting material, comprising the following raw materials in parts by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogen-containing silicone oil, 42 parts of modified hollow glass microspheres obtained in Example 3, 60 parts of silicon micropowder, 30 parts of graphene powder, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of a platinum catalyst;

[0065] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0066] The first step is to weigh the raw materials by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogenated silicone oil, 42 parts of modified hollow glass microspheres obtained in Example 3, 60 parts of silicon micropowder, 30 parts of graphene powder, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0067] Step 2: Add the first portion of vinyl silicone oil and the modified hollow glass microspheres obtained in Example 3 into a ball mill and stir for 3 h at a temperature of 100° C. and a speed of 1000 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 h at a speed of 600 rpm to obtain a silicone potting compound component A;

[0068] Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and stir for 2 h at 120°C and 800 rpm, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain component potting glue B;

[0069] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0070] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:1.

[0071] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0072] Comparative Example 1

[0073] A thermally conductive potting material, comprising the following raw materials in parts by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogen-containing silicone oil, 42 parts of hollow glass microspheres, 60 parts of silicon micropowder, 30 parts of graphene powder, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of a platinum catalyst;

[0074] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0075] The first step is to weigh the raw materials by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogenated silicone oil, 42 parts of hollow glass microspheres, 60 parts of silicon micropowder, 30 parts of graphene powder, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0076] Step 2: Add the first portion of vinyl silicone oil and hollow glass microbeads into a ball mill and stir for 3 hours at 100°C and 1000 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours at 600 rpm to obtain silicone potting compound component A;

[0077] Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and stir for 2 h at 120°C and 800 rpm, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain component potting glue B;

[0078] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0079] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:1.

[0080] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0081] Comparative Example 2

[0082] A thermally conductive potting material, comprising the following raw materials in parts by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogen-containing silicone oil, 42 parts of hollow glass microspheres, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of a platinum catalyst;

[0083] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0084] The first step is to weigh the raw materials according to their mass fractions: 200 parts of vinyl silicone oil, 35 parts of hydrogenated silicone oil, 42 parts of hollow glass microspheres, 0.005 parts of ethynyl cyclohexanol, and 0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0085] Step 2: Add the first portion of vinyl silicone oil and hollow glass microbeads into a ball mill and stir for 3 hours at 100°C and 1000 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours at 600 rpm to obtain silicone potting compound component A;

[0086] Step 3: Add the second portion of vinyl silicone oil into a ball mill and stir for 2 h at 120°C and 800 rpm, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain component potting glue B;

[0087] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0088] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:1.

[0089] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0090] Comparative Example 3

[0091] A thermally conductive potting adhesive material, comprising the following raw materials in parts by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogen-containing silicone oil, 42 parts of hollow glass microspheres, and 0.7 parts of a platinum catalyst;

[0092] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0093] The first step is to weigh the raw materials according to their mass fractions: 200 parts of vinyl silicone oil, 35 parts of hydrogenated silicone oil, 42 parts of hollow glass microspheres, and 0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass;

[0094] Step 2: Add the first portion of vinyl silicone oil and hollow glass microbeads into a ball mill and stir for 3 hours at 100°C and 1000 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours at 600 rpm to obtain silicone potting compound component A;

[0095] Step 3: Add the second portion of vinyl silicone oil into a ball mill and stir for 2 h at 120°C and 800 rpm, then cool to room temperature, add platinum catalyst to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain component potting glue B;

[0096] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0097] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:1.

[0098] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0099] Comparative Example 4

[0100] A thermally conductive potting adhesive material, comprising the following raw materials in parts by mass: 200 parts of vinyl silicone oil, 35 parts of hydrogen-containing silicone oil, and 0.7 parts of a platinum catalyst;

[0101] A method for preparing a thermally conductive potting adhesive material comprises the following steps:

[0102] The first step is to weigh 200 parts of vinyl silicone oil, 35 parts of hydrogenated silicone oil and 0.7 parts of platinum catalyst according to their mass fractions, and divide the vinyl silicone oil into two parts of equal mass;

[0103] Step 2: Add the first portion of vinyl silicone oil into a ball mill and stir for 3 h at 100°C and 1000 rpm, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain silicone potting compound component A;

[0104] Step 3: Add the second portion of vinyl silicone oil into a ball mill and stir for 2 h at 120°C and 800 rpm, then cool to room temperature, add platinum catalyst to the mixture, and continue stirring for 0.5 h at 600 rpm to obtain component potting glue B;

[0105] Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

[0106] The mass ratio of the organic silicone potting adhesive A to the organic silicone potting adhesive B in this embodiment is 1:1.

[0107] Among them, the vinyl silicone oil used in this embodiment is a mixture of terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

[0108] Comparative Example 5

[0109] This comparative example is the thermal conductive potting glue sold by Suzhou Tolmai Electronic Technology Co., Ltd.

[0110] The viscosity of the thermally conductive potting materials in Examples 4-6 and Comparative Examples 1-4 and the commercially available thermally conductive potting material in Comparative Example 5 were tested with reference to GB / T 2794-2013, and the thermal conductivity was tested with reference to ISO 22007-2. The density of the thermally conductive potting materials in each Example and Comparative Example was calculated. The test results are shown in Table 1:

[0111] Table 1

[0112]

[0113]

[0114] It can be seen from Table 1 that the thermally conductive potting glue material of the present invention has better thermal conductivity and lower density than commercially available thermally conductive potting glue, and has lower viscosity and is easy to use. Comparative Examples 1-3 carried out control tests on other raw materials used in the present invention. Although the addition of unmodified hollow glass microspheres can also reduce the density of a potting glue material, it will lead to a decrease in thermal conductivity and an increase in viscosity. The addition of silicon micropowder and graphene powder can effectively improve the thermal conductivity of a thermally conductive potting glue material. The addition of the inhibitor vinyl cyclohexanol can reduce the viscosity of a potting glue material. In summary, the thermally conductive potting glue material of the present invention has excellent thermal conductivity, lower density, low viscosity, is easy to use, and can be widely used in the fields of electronic components and communication components.

[0115] The above is a detailed introduction to a thermally conductive potting material and a preparation method thereof provided by the present invention. The principle and implementation method of the present invention are described in detail using specific examples. The description of the above embodiments is only used to help understand the method and core idea of ​​the present invention, including the best mode, and also enables any technician in the field to practice the present invention, including manufacturing and using any device or system, and implementing any combination method. It should be pointed out that for ordinary technicians in this technical field, the present invention can also be improved and modified without departing from the principle of the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed in the present invention can be used in combination with each other in any way. The fact that these combinations are not exhaustively described in this specification is only for the consideration of omitting space and saving resources. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions within the scope of the claims.

Claims

1. A thermally conductive potting material, characterized in that: The invention comprises the following raw materials in parts by weight: 180-200 parts of vinyl silicone oil, 25-35 parts of hydrogen-containing silicone oil, 30-42 parts of modified hollow glass microspheres, 42-60 parts of silicon micropowder, 24-30 parts of graphene powder, 0.004-0.005 parts of ethynyl cyclohexanol, and 0.6-0.7 parts of platinum catalyst; Wherein, the modified hollow glass microspheres are prepared by the following steps: Step 1, mixing hollow glass microspheres and sodium hydroxide solution in a container, stirring evenly, and reacting at a temperature of 60° C. for 1-1.5 hours to obtain surface-treated hollow glass microspheres; Step 2, allyltriethoxysilane, p-trifluoromethylaniline, and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene are mixed in a container, stirred evenly, and reacted at a temperature of 40-60° C. for 20-24 hours to obtain intermediate 1; Step 3, the surface treated hollow glass microspheres, nano-aluminum nitride and ethanol solution are mixed in a container, the pH of the solution is adjusted to 2 with a 10% by mass dilute nitric acid solution, and then ultrasonically dispersed for 1.5-2.5 hours, and then the system temperature is raised to 40-60° C. and the intermediate 1 is added to the container, and the reaction is carried out at a temperature of 40-60° C. for 1.5 hours to obtain modified hollow glass microspheres; Wherein, the sodium hydroxide solution used in step 1 is a sodium hydroxide aqueous solution with a concentration of 0.3 mol / L, and the mass ratio of the hollow glass microspheres to the sodium hydroxide aqueous solution is 10 g:15-25 g; the mass ratio of allyltriethoxysilane, p-trifluoromethylaniline, and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene used in step 2 is 4 g:1.7-2 g:0.057-0.06 g; the ethanol solution in step 3 is an ethanol solution with a mass fraction of 90%, and the mass ratio of the surface-treated hollow glass microspheres, nano-aluminum nitride, ethanol solution, and intermediate 1 used is 10 g:1 g:30-45 g:1.2-1.8 g.

2. A method for preparing the thermally conductive potting material according to claim 1, characterized in that: The method comprises the following preparation steps: The first step is to weigh the raw materials according to their mass proportions: 180-200 parts of vinyl silicone oil, 25-35 parts of hydrogenated silicone oil, 30-42 parts of modified hollow glass microspheres, 42-60 parts of silicon micropowder, 24-30 parts of graphene powder, 0.004-0.005 parts of ethynyl cyclohexanol, and 0.6-0.7 parts of platinum catalyst, and divide the vinyl silicone oil into two parts of equal mass; Step 2: Add the first portion of vinyl silicone oil and modified hollow glass microspheres into a ball mill and heat-stir for 2-3 hours, then cool to room temperature, add hydrogenated silicone oil to the mixture, and continue stirring for 0.5 hours to obtain silicone potting compound component A; Step 3: Add the second portion of vinyl silicone oil, silicon powder and graphene powder into a ball mill and heat and stir for 2 hours, then cool to room temperature, add platinum catalyst and ethynyl cyclohexanol to the mixture, and continue stirring for 0.5 hours to obtain component potting glue B; Step 4: Mix the organic silicone potting glue A and the organic silicone potting glue B in proportion to obtain a thermal conductive potting glue material.

3. The method for preparing a thermally conductive potting material according to claim 2, characterized in that: The vinyl silicone oil is prepared by mixing terminal vinyl silicone oil and side vinyl silicone oil in a mass ratio of 1:1, and the mass fraction of vinyl is 0.4-0.6wt%, the mass fraction of active hydrogen in hydrogen-containing silicone oil is 0.1%, the viscosity of vinyl silicone oil is 1000MPa·s, and the viscosity of hydrogen-containing silicone oil is 150MPa·s.

4. The method for preparing a thermally conductive potting material according to claim 2, characterized in that: In the second step, the temperature condition of the first ball milling stirring is 100° C. and the rotation speed condition is 900-1000 rpm, and the rotation speed condition of the second ball milling stirring is 400-600 rpm.

5. The method for preparing a thermally conductive potting material according to claim 2, characterized in that: In the third step, the temperature condition of the first ball milling stirring is 120° C., the rotation speed condition is 600-800 rpm, and the time condition of the second ball milling stirring is 400-600 rpm.

6. The method for preparing a thermally conductive potting material according to claim 2, characterized in that: In the fourth step, the mass ratio of the organic silicon component A and the organic silicon potting compound B used for mixing is 1:0.8-1.

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