CN113957702B - Preparation method and application of thermal interface material based on high-graphitization asphalt-based carbon fiber - Google Patents
Preparation method and application of thermal interface material based on high-graphitization asphalt-based carbon fiber Download PDFInfo
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Abstract
The invention belongs to the technical field of thermal interface materials, and relates to a preparation method and application of a thermal interface material based on high-graphitization asphalt-based carbon fibers, wherein the preparation method comprises the following steps: the preparation method comprises the following steps of (1) placing non-glued graphitized pitch-based carbon fibers in a plasma cleaning machine for treatment, (2) adding boric acid and urea into deionized water, stirring to prepare a precursor solution, (3) adding the carbon fibers obtained in the step 1 into the precursor solution, performing ultrasonic impregnation, filtering and drying, (4) performing heat treatment on the carbon fiber material obtained in the step 3 to prepare boron nitride-coated carbon fibers, (5) mixing the boron nitride-coated carbon fibers prepared in the step 4 with a silica gel precursor, and performing curing molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material. The method has simple process and strong universality, and solves the problems of the reduction of the resistivity of the thermal interface material and the like caused by the high-graphitization carbon fiber as the filler.
Description
Technical Field
The invention relates to a preparation method and application of a thermal interface material based on high-graphitization asphalt-based carbon fibers, and belongs to the technical field of thermal interface materials.
Background
With the rapid development of the third generation semiconductor technology, electronic devices are rapidly developing in the direction of miniaturization, intensification and wearable. The power density is rapidly increased due to the intensification of electronic components and the continuous compression of the mounting volume, and the local high temperature caused by the power increase can further improve the power to form a vicious circle, so that the reliability of equipment is reduced. Carbon fiber is a filler with ultrahigh thermal conductivity, and it is a common practice to coat the surface of carbon fiber with an insulating coating in order to maintain the high electrical resistivity of the thermal interface material. The carbon fiber is a filler with ultrahigh heat conductivity, and after the carbon fiber is coated with the boron nitride, the high heat conductivity of the thermal interface material can be kept, and meanwhile, the high insulation property of the thermal interface material is maintained, so that the safe operation of the thermal interface material in a circuit is ensured. In order to be tightly combined with a coating, the surface of the highly inert surface of the highly graphitized asphalt-based carbon fiber needs to be modified, the overall structure of the material is damaged by a common mixed acid oxidation method, the heat conductivity of graphite crystals is affected, and the treatment of waste acid is also a troublesome problem. Plasma treatment is an effective means to effectively etch and modify the surface of a material.
Patent 200810222205.9 discloses a method for coating hexagonal boron nitride on a fiber braided body, which comprises the steps of preparing reaction liquid, dipping, drying and heat treatment to prepare a boron nitride coating. The method does not activate the surface of the fiber and is not suitable for graphitizing asphalt-based carbon fiber. The method has the heat treatment temperature of 850 ℃ at most, and the crystal form of boron nitride is changed along with the rise of the heat treatment temperature, preferably 900-1200 ℃.
Patent 201611028877.7 discloses a preparation method of polyacrylonitrile-based carbon fiber with a boron nitride coating on the surface, which comprises carbon fiber treatment, impregnation liquid preparation, carbon fiber impregnation, pre-oxidation and temperature programming to obtain the boron nitride coating. The method aims at the polyacrylonitrile carbon fiber with more active surface layer, has no surface activation treatment process, and is not suitable for graphitized asphalt-based carbon fiber with higher thermal conductivity. According to the method, ethanol is used as a solvent to prepare the dipping solution, so that the concentration upper limit of the dipping solution is limited, and the thickness of boron nitride is influenced.
Patent 201810362753.5 discloses a preparation method of a hexagonal boron nitride coating on the surface of a carbon material, which comprises the steps of carbon fiber coating removal and air activation, precursor preparation, vacuum impregnation and heat treatment to prepare the hexagonal boron nitride coating. The method uses air to activate the carbon fiber, the activation degree is not easy to control, and the dipping process is complex.
Patent 201410786687.6 discloses a preparation method of a PPT/PET/polyether ester polymer composite material, wherein plasma modification treatment of carbon nanofibers is involved: vacuum degree of 1-0.2mmHg, input voltage of 220V, and atmosphere of O 2 Treatment time 1-3min, then exposure to air for 5-25min, and the method does not mention plasma generation power.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a preparation method and application of a thermal interface material based on high-graphitization asphalt-based carbon fibers. The method successfully prepares the insulating high-thermal-conductivity coating on the surface of the high-graphitization asphalt-based carbon fiber, increases the overall resistivity of the material on the premise of keeping the high-thermal-conductivity framework formed by the carbon fiber, and has the advantages of low cost, simple process, small influence on the carbon fiber structure and better universality.
In order to achieve the purpose of the invention and solve the problems existing in the prior art, the invention adopts the technical scheme that: a preparation method of a thermal interface material based on high-graphitization asphalt-based carbon fibers comprises the following steps:
step 1, placing 1-3g of non-rubberized graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 5-30W, the air pressure at 0-100Pa, the temperature at 15-30 ℃, the time at 400-1200s, and replacing the atmosphere with oxygen for 1-3 times to obtain the carbon fiber treated by the plasma cleaning machine;
step 2, adding boric acid and urea into 80-100mL of deionized water according to the mass ratio of 1-5 to prepare a water solution, and stirring at 60-95 ℃ for 10-60min to prepare a precursor solution;
step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 5-120min, filtering the carbon fiber material, drying at 20-110 ℃, and repeating the drying for 1-3 times;
step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate to be 1-10 ℃/min, heating to 900-1200 ℃, preserving heat for 1-5h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber;
and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 10-70%, and the vacuum defoaming time is 5-10min.
The thermal interface material based on the highly graphitized asphalt-based carbon fiber prepared by the preparation method is applied to the aspect of heat dissipation of electronic components.
The invention has the beneficial effects that: a preparation method and application of a thermal interface material based on high-graphitization asphalt-based carbon fibers are disclosed, wherein the preparation method comprises the following steps: the preparation method comprises the following steps of (1) placing non-glued graphitized pitch-based carbon fibers in a plasma cleaning machine for treatment, (2) adding boric acid and urea into deionized water to prepare an aqueous solution, stirring to prepare a precursor solution, (3) adding carbon fibers treated by the plasma cleaning machine obtained in the step (1) into the precursor solution prepared in the step (2) for ultrasonic impregnation, filtering and drying the carbon fiber materials, and (4) carrying out heat treatment on the carbon fiber materials obtained in the step (3) in a nitrogen atmosphere, and taking out a sample when the temperature is reduced to room temperature to prepare boron nitride-coated carbon fibers; (5) And (4) mixing the boron nitride coated carbon fiber prepared in the step (4) with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material. Compared with the prior art, the method overcomes the defects that the structure of the carbon fiber is damaged due to mixed acid oxidation in the surface modification of the high-graphitization asphalt-based carbon fiber at the present stage, and the resistivity of the thermal interface material is greatly reduced due to the carbon fiber as a filler, better maintains the mechanical property of the carbon fiber while enhancing the interface effect, and can promote the wide application of the carbon fiber in the field of electronic packaging.
Drawings
FIG. 1 is a scanning electron microscope image of boron nitride-coated carbon fibers prepared in example 1.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Step 1, placing 1g of non-glued graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 5W, the air pressure at 20pa, the temperature at 20 ℃, the time at 800s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 10g of boric acid and 30g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 60 ℃ for 30min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 10min, filtering the carbon fiber material, drying at 50 ℃, and repeating the drying times for 2 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 950 ℃, preserving heat for 4h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 70%, and the vacuum defoaming time is 5min. Scanning electron microscope images of the boron nitride-coated carbon fibers are obtained, and are shown in figure 1.
The prepared thermal interface material is subjected to resistance test, and the overall resistivity of the material is 1 multiplied by 10 5 The electrical resistivity of omega cm is 332 times higher than that of a thermal interface material taking untreated carbon fibers as fillers with the same filling proportion, and the thermal interface material embodies better insulation, and the thermal conductivity of the material is 18.23W/m.K.
Example 2
Step 1, placing 1.5g of non-glued graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 10W, the air pressure at 30pa, the temperature at 20 ℃, the time at 400s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 5g of boric acid and 10g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 70 ℃ for 20min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 20min, filtering the carbon fiber material, drying at the temperature of 80 ℃, and repeating the drying for 2 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 950 ℃, preserving heat for 4h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 50%, and the vacuum defoaming time is 5min.
The resistance test is carried out on the prepared thermal interface material, and the overall resistivity of the material is 3.01 multiplied by 10 8 Omega cm, the specific resistance of the thermal interface material which takes untreated carbon fiber as the filler in the same filling proportion is 5.02 multiplied by 10 4 Omega cm is improved by 6000 times, good insulativity is embodied, and the thermal conductivity of the material is 10.77W/m.K.
Example 3
Step 1, placing 1.8g of non-rubberized graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 20W, the air pressure at 30pa, the temperature at 25 ℃, the time at 600s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 10g of boric acid and 30g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 80 ℃ for 20min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 25min, filtering the carbon fiber material, drying at the temperature of 80 ℃, and repeating the drying times for 3 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 1000 ℃, preserving heat for 4h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 40%, and the vacuum defoaming time is 5min.
The resistance test is carried out on the prepared thermal interface material, and the overall resistivity of the material is 7.54 multiplied by 10 12 Omega cm, the specific resistance of the thermal interface material which takes untreated carbon fiber as the filler with the same filling proportion is 1 multiplied by 10 5 Omega cm is improved by 7.5 multiplied by 10 7 The material has good insulation property, and the thermal conductivity of the material is 6.93W/mK.
Example 4
Step 1, placing 2g of non-glued graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 30W, the air pressure at 30pa, the temperature at 25 ℃, the time at 800s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 8g of boric acid and 24g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 90 ℃ for 40min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 40min, filtering the carbon fiber material, drying at 90 ℃, and repeating the drying times for 3 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 1100 ℃, preserving heat for 4 hours, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 30%, and the vacuum defoaming time is 5min.
The prepared thermal interface material is subjected to resistance test, and the overall resistivity of the material is 9.05 multiplied by 10 12 Omega cm, the specific resistance of the thermal interface material which takes untreated carbon fiber as the filler in the same filling proportion is 1.76 multiplied by 10 5 Omega cm is increased by 5.14 multiplied by 10 7 The material has good insulation property, and the thermal conductivity of the material is 4.87W/mK.
Example 5
Step 1, placing 2.5g of non-rubberized graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 30W, the air pressure at 40pa, the temperature at 30 ℃, the time at 1000s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 9g of boric acid and 36g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 90 ℃ for 50min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 50min, filtering the carbon fiber material, drying at 90 ℃, and repeating the drying times for 3 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 1100 ℃, preserving heat for 4 hours, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization asphalt-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 30%, and the vacuum defoaming time is 5min.
The resistance test is carried out on the prepared thermal interface material, and the overall resistivity of the material is 9.94 multiplied by 10 12 Omega cm, the specific resistance of the thermal interface material which takes untreated carbon fiber as the filler in the same filling proportion is 1.76 multiplied by 10 5 Omega cm is increased by 5.65 multiplied by 10 7 The material has good insulation property, and the thermal conductivity of the material is 4.22W/m.K.
Example 6
Step 1, placing 3.0g of non-rubberized graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 30W, the air pressure at 60pa, the temperature at 30 ℃, the time at 1200s, and replacing the atmosphere with oxygen for 3 times to obtain the carbon fiber treated by the plasma cleaning machine. Step 2, adding 11g of boric acid and 44g of urea into 100mL of deionized water to prepare an aqueous solution, and stirring at 90 ℃ for 60min to prepare a precursor solution; step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 60min, filtering the carbon fiber material, drying at 100 ℃, and repeating the drying times for 3 times; step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate at 5 ℃/min, heating to 1200 ℃, preserving heat for 4h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber; and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 10%, and the vacuum defoaming time is 5min.
The resistance test is carried out on the prepared thermal interface material, and the materialBulk resistivity of 1X 10 14 Omega cm, the specific resistance of the thermal interface material which takes untreated carbon fiber as the filler in the same filling proportion is 4.02 multiplied by 10 13 Omega cm is improved by 2.5 times, and the better insulation is embodied, and the thermal conductivity of the material is 1.86W/m.K.
The plasma used in the present invention is a conductive aggregate of charged electrons, ions, and various molecules, atoms, radicals, and the like. The plasma treatment can introduce various active functional groups on the premise of keeping the mechanical property of the material, and improve the interaction with the interface. Analyzing the above embodiment, when the carbon fibers reach a certain amount in the matrix, a conductive network is formed, and at this time, the boron nitride plays a role of an insulating node for separating the carbon fibers. The non-rubberized graphitized asphalt-based carbon fiber used in the invention can be replaced by other carbon fibers after degumming treatment, and has better universality.
Claims (2)
1. A preparation method of a thermal interface material based on high graphitization asphalt-based carbon fiber is characterized by comprising the following steps:
step 1, placing 1-3g of non-rubberized graphitized asphalt-based carbon fiber in a plasma cleaning machine for treatment, controlling the power at 5-30W, the air pressure at 0-100Pa, the temperature at 15-30 ℃, the time at 400-1200s, and replacing the atmosphere with oxygen for 1-3 times to obtain the carbon fiber treated by the plasma cleaning machine;
step 2, adding boric acid and urea into 80-100mL of deionized water according to the mass ratio of 1-5 to prepare a water solution, and stirring at 60-95 ℃ for 10-60min to prepare a precursor solution;
step 3, adding the carbon fiber treated by the plasma cleaning machine obtained in the step 1 into the precursor solution prepared in the step 2, performing ultrasonic impregnation for 5-120min, filtering the carbon fiber material, drying at 20-110 ℃, and repeating the drying for 1-3 times;
step 4, carrying out heat treatment on the carbon fiber material obtained in the step 3 in a nitrogen atmosphere, controlling the heating rate to be 1-10 ℃/min, heating to 900-1200 ℃, preserving heat for 1-5h, and taking out a sample when the temperature is reduced to room temperature to obtain boron nitride coated carbon fiber;
and 5, mixing the boron nitride coated carbon fiber prepared in the step 4 with a silica gel precursor, and curing and molding to prepare the high-graphitization pitch-based carbon fiber-based thermal interface material, wherein the mass fraction of the boron nitride coated carbon fiber in the thermal interface material is 10-70%, and the vacuum defoaming time is 5-10min.
2. The use of the high graphitization pitch-based carbon fiber-based thermal interface material prepared by the preparation method according to claim 1 in the aspect of heat dissipation of electronic components.
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