CN111040380A - Heat-conducting modified epoxy resin-based composite material and preparation method thereof - Google Patents
Heat-conducting modified epoxy resin-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a heat-conducting modified epoxy resin-based composite material and a preparation method thereof. Compared with the prior art, the composite material can obviously reduce the amount of heat-conducting fillers on the premise of reaching the same heat conductivity and can also obviously improve the high-temperature resistance and the thermal stability of the epoxy resin.
Description
Technical Field
The invention relates to a heat-conducting modified epoxy resin-based composite material added with a heat-conducting filler and taking an epoxy resin/thermoplastic resin incompatible two-phase blend as a matrix and a preparation method thereof.
Background
With the continuous development of industrial production, higher and higher requirements are put forward on the comprehensive thermal mechanical property of heat conduction materials, and the traditional metal heat conduction materials represented by copper have high density, are easy to corrode, have low mechanical property and large thermal deformation, and cannot meet the use requirements of certain special occasions. The polymer matrix composite material added with the high heat conduction filler can effectively overcome the defects of the metal heat conduction material. However, the thermal conductivity of the polymer matrix in these composites is poor, and their potential as a metal substitute is therefore limited in cases where higher demands are made on the thermal conductivity. Generally, the thermal conductivity of the composite material can be enhanced by increasing the amount of filler, with the greater the amount of thermally conductive filler added to the resin matrix, the better the thermal conductivity of the resulting composite material. However, an increase in the amount of filler inevitably leads to an increase in the cost of the composite material and a decrease in mechanical properties. Therefore, there is a need to solve the problem of how to obtain polymer matrix composites with higher thermal conductivity at lower filler content.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a heat-conducting modified epoxy resin-based composite material which is low in filler content and good in heat-conducting property and is based on a double percolation effect.
The purpose of the invention can be realized by the following technical scheme: a heat-conducting modified epoxy resin-based composite material is characterized in that a blend with a two-phase double-percolation structure and incompatible epoxy resin/thermoplastic resin is used as a matrix, and a heat-conducting filler compatible with the two-phase resin matrix is added to obtain the three-phase double-percolation structure heat-conducting modified composite material of epoxy resin/thermoplastic resin/heat-conducting filler. Compared with pure epoxy resin, the composite material can obviously reduce the amount of heat-conducting filler on the premise of reaching the same heat conductivity, and can also obviously improve the high-temperature resistance and the thermal stability of the epoxy resin.
The thermoplastic resin used to blend with the epoxy resin to form a double percolation structure may be any thermoplastic resin that is soluble in the liquid epoxy resin and incompatible with the epoxy resin when cured at high temperatures, thereby separating from the epoxy resin. In a further preferred embodiment of the present invention, the thermoplastic resin is one of phenolphthalein polyaryletherketone, polyetherimide and polypropylene.
The viscosity of the epoxy resin is less than 100 Pa.s at 25 ℃.
The epoxy resin/thermoplastic resin/heat-conducting filler composite material forms a double-percolation structure by adjusting the weight ratio, the curing temperature and the curing time of the epoxy resin and the thermoplastic resin.
More preferably, the mass ratio of the epoxy resin to the thermoplastic resin is 50-84: 50-16.
More preferably, the heat conductive filler is selected from one of graphene and carbon nanotubes, and the addition amount of the heat conductive filler is 0.1-5 wt% of the mass of the matrix.
The preparation method of the heat-conducting modified epoxy resin-based composite material is characterized by comprising the following specific steps of:
(a) adding thermoplastic resin into a solvent while stirring, completely dissolving the thermoplastic resin, then adding a heat-conducting filler into a solution system, dispersing, adding epoxy resin into the solution system, stirring for 5-10 minutes, and then dispersing the solution system;
(b) placing the mixture in a vacuum oven to remove the solvent, adjusting the pressure of the vacuum oven to air pressure, opening the vacuum oven to take out the material, quickly adding the curing agent and fully stirring, then, heating the temperature to 150 ℃ in the vacuum oven, adjusting the pressure to 0.1MPa, keeping the vacuum degree for about 15 minutes to continue defoaming;
(c) pouring the mixture into a preheated mold for curing, wherein the curing conditions are as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
And a step a, adopting an ultrasonic disperser as an instrument for twice dispersion, wherein the power of the ultrasonic disperser is 75W, the vibration frequency is 22 +/-1 KHz, and the dispersion time is 1-2 h.
The solvent adopted in the step a is any solvent which can dissolve the epoxy resin and the thermoplastic resin at the same time and has a boiling point of 60-70 ℃. In a further preferred embodiment of the present invention, the solvent is one of tetrahydrofuran, acetone, and chloroform.
And c, controlling the vacuum degree of the vacuum oven in the step b to be 0.01-0.1 MPa, controlling the temperature to be normal temperature-120 ℃, and controlling the time for removing the solvent to be 5-15 h. The solvent can be removed within the vacuum range and temperature range and with a holding time, such as standing at 60 deg.C under 0.06MPa for 10 hours to remove most of the solvent. Then, the temperature was raised to 120 ℃ and the degree of vacuum was continuously adjusted during the process to further remove the solvent and bubbles in the system. Maintaining at 120 deg.C and 0.1MPa vacuum degree for 10 min.
And the curing agent in the step b is diamino diphenyl sulfone, and the molar ratio of the epoxy resin to the diamino diphenyl sulfone is 100: 55.
The critical value of the filler that causes the composite to form a continuous conductive path on the substrate is called the percolation value. By dual percolation effect, it is meant that when the filler is selectively distributed in one of the incompatible two phase matrices and this phase is a continuous structure throughout the material matrix, once the filler reaches the percolation value in that phase, a continuous conduction path is formed throughout the material matrix, i.e., the filler reaches the percolation value throughout the matrix.
Thermosetting resins represented by epoxy resins have excellent mechanical properties, chemical resistance, weather resistance, electrical insulation and dimensional stability, which cannot be replaced by thermoplastic resins. The epoxy resin/thermoplastic resin incompatible two-phase double-percolation structure blend is used as a matrix, and the heat-conducting filler compatible with the two-phase resin matrix is added to prepare the epoxy resin/thermoplastic resin/heat-conducting filler three-phase double-percolation structure heat-conducting modified composite material.
Compared with the prior art, the invention can obtain the following beneficial effects:
(1) the invention prepares the epoxy resin/thermoplastic resin/heat-conducting filler three-phase double-percolation structure heat-conducting modified composite material, and compared with pure epoxy resin, the composite material can obviously reduce the amount of the heat-conducting filler on the premise of reaching the same heat conductivity.
(2) The epoxy resin/thermoplastic resin/heat-conducting filler three-phase double-percolation structure heat-conducting modified composite material prepared by the invention has good interface compatibility between the epoxy resin and the thermoplastic resin, and the two-phase interface blocks the movement of molecular chains and molecular chain segments, thereby obviously improving the high temperature resistance and the thermal stability of the epoxy resin.
(3) The material preparation method adopted by the invention is a solution method, the resin is dissolved in the low-viscosity solvent, the overall viscosity of the material system is reduced, and then the graphene is ultrasonically dispersed in the solution system, so that the graphene is uniformly dispersed, and the processing performance of the material is improved.
Drawings
FIG. 1 shows that the composite material respectively takes epoxy resin as a matrix and the weight ratio of the epoxy resin to phenolphthalein polyaryletherketone is 81: 19 is used as a matrix, and the thermal conductivity change curve is changed along with the change of the addition amount of the graphene.
FIG. 2 shows that the weight ratio of epoxy resin to epoxy resin/phenolphthalein polyaryletherketone/graphene is 81: 19: the 0.5 composite (81EP19PEK-C0.5GR) has a heat flow curve measured under Differential Scanning Calorimetry (DSC) with glass transition temperatures of 213.1 ℃ and 227.2 ℃.
FIG. 3 shows that the weight ratio of epoxy resin to epoxy resin/phenolphthalein polyaryletherketone/graphene is 81: 19: the weight-temperature curve of 0.5 composite (81EP19PEK-C0.5GR) tested under a thermogravimetric analyzer (TGA) showed that the temperature T5% at 5% weight decomposition corresponds to 320.1 ℃ and 322.7 ℃ and the char yield is 24.2% and 30.5%, respectively.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
A preparation method of a heat-conducting modified epoxy resin-based composite material based on a double percolation effect comprises the following steps:
1. adding phenolphthalein polyaryletherketone accounting for 19 weight percent of the matrix resin into solvent tetrahydrofuran while stirring, and completely dissolving the phenolphthalein polyaryletherketone. Then, 0.5phr of specific gravity graphene was added to the solution system and dispersed at a frequency of 22 ± 1KHz for 2 hours using an ultrasonic disperser. Next, an epoxy resin having a weight proportion of 81 to the matrix resin was added to the solution system and stirred for 5 minutes. The solution system was then dispersed in an ultrasonic disperser at a frequency of 22 + -1 KHz for two more hours.
2. The mixture was left to stand in a vacuum oven at 60 ℃ under 0.06MPa for 10 hours to remove most of the tetrahydrofuran solvent. Then, the temperature was raised to 120 ℃ and the degree of vacuum was continuously adjusted during the process to further remove the solvent and bubbles in the system. Maintaining at 120 deg.C and 0.1MPa vacuum degree for 10min, adjusting vacuum oven pressure to air pressure, opening oven, taking out material, rapidly adding stoichiometric amount of curing agent diamino diphenyl sulfone (epoxy resin: diamino diphenyl sulfone ═ 100:55) and stirring thoroughly. Then, the temperature was raised to 150 ℃ in a vacuum oven, and the pressure was adjusted to 0.1MPa in vacuum and kept for about 15 minutes to continue the deaeration.
3. Pouring the mixture into a preheated mold for curing, wherein the curing system is as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
Through tests, the weight ratio of the prepared epoxy resin/phenolphthalein polyaryletherketone/graphene is 81: 19: the thermal conductivity of the 0.5 composite (81EP19PEK-C0.5GR) was 0.37 W.m-1·K-1Compared with pure epoxy matrix composite materials, the filler amount reaching the same thermal conductivity coefficient is reduced by half. The results are shown in FIG. 1. Compared with pure epoxy resin, the other thermal properties of the composite material are also improved. After modification, the glass transition temperature of the material is increased from 213.1 ℃ to 227.2 ℃, and the high temperature resistance is improved; the results are shown in FIG. 2. The thermal decomposition temperature is increased from 320.1 ℃ to 322.7 ℃, the carbon residue rate is also increased from 24.2 percent to 30.5 percent, and the thermal stability is improved; the results are shown in FIG. 3.
Example 2
The preparation method of the heat-conducting modified epoxy resin-based composite material comprises the following specific steps:
(a) adding thermoplastic resin into solvent acetone while stirring, completely dissolving the thermoplastic resin, then adding the heat-conducting filler graphene into a solution system, dispersing for 1h by adopting an ultrasonic disperser, then adding epoxy resin into the solution system, stirring for 10min, and then dispersing the solution system for 1h by adopting the ultrasonic disperser; the mass ratio of the epoxy resin to the thermoplastic resin was 50:50, and the amount of the thermally conductive filler added was 0.1 wt% of the mass of the matrix (the sum of the masses of the thermoplastic resin and the epoxy resin). The power of the ultrasonic dispersion instrument is 75W, and the vibration frequency is 22 +/-1 KHz;
(b) the mixture is placed in a vacuum oven to remove the solvent, and the specific steps are as follows: the mixture was allowed to stand at 60 ℃ under a vacuum of 0.06MPa for 10 hours to remove most of the solvent. Then, the temperature was raised to 120 ℃ and the degree of vacuum was continuously adjusted during the process to further remove the solvent and bubbles in the system. Keeping the vacuum degree of 0.1MPa at 120 ℃ for 10min, then adjusting the pressure of a vacuum oven to air pressure, opening the vacuum oven to take out the material, quickly adding a curing agent diaminodiphenyl sulfone (the molar ratio of epoxy resin to diaminodiphenyl sulfone is 100:55) and fully stirring, then, heating the temperature to 150 ℃ in the vacuum oven, adjusting the pressure to 0.1MPa, keeping the vacuum degree for about 15 min and continuing defoaming;
(c) pouring the mixture into a preheated mold for curing, wherein the curing conditions are as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
Example 3
The preparation method of the heat-conducting modified epoxy resin-based composite material comprises the following specific steps:
(a) adding thermoplastic resin into solvent acetone while stirring, completely dissolving the thermoplastic resin, then adding the heat-conducting filler graphene into a solution system, dispersing for 1.5 hours by adopting an ultrasonic disperser, then adding epoxy resin into the solution system, stirring for 8 minutes, and then dispersing for 1.5 hours by adopting the ultrasonic disperser; the mass ratio of the epoxy resin to the thermoplastic resin was 70:30, and the amount of the thermally conductive filler added was 5 wt% of the mass of the matrix (the sum of the masses of the thermoplastic resin and the epoxy resin). The power of the ultrasonic dispersion instrument is 75W, and the vibration frequency is 22 +/-1 KHz;
(b) the mixture is placed in a vacuum oven to remove the solvent, and the specific steps are as follows: the mixture was allowed to stand at 60 ℃ under a vacuum of 0.06MPa for 10 hours to remove most of the solvent. Then, the temperature was raised to 120 ℃ and the degree of vacuum was continuously adjusted during the process to further remove the solvent and bubbles in the system. Keeping the vacuum degree of 0.1MPa at 120 ℃ for 10min, then adjusting the pressure of a vacuum oven to air pressure, opening the vacuum oven to take out the material, quickly adding a curing agent diaminodiphenyl sulfone (the molar ratio of epoxy resin to diaminodiphenyl sulfone is 100:55) and fully stirring, then, heating the temperature to 150 ℃ in the vacuum oven, adjusting the pressure to 0.1MPa, keeping the vacuum degree for about 15 min and continuing defoaming;
(c) pouring the mixture into a preheated mold for curing, wherein the curing conditions are as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
Example 4
The preparation method of the heat-conducting modified epoxy resin-based composite material comprises the following specific steps:
(a) adding thermoplastic resin into solvent acetone while stirring, completely dissolving the thermoplastic resin, then adding the heat-conducting filler graphene into a solution system, dispersing for 2 hours by adopting an ultrasonic disperser, then adding epoxy resin into the solution system, stirring for 5 minutes, and then dispersing for 2 hours by adopting the ultrasonic disperser; the mass ratio of the epoxy resin to the thermoplastic resin was 84:16, and the amount of the thermally conductive filler added was 3 wt% of the mass of the matrix (the sum of the masses of the thermoplastic resin and the epoxy resin). The power of the ultrasonic dispersion instrument is 75W, and the vibration frequency is 22 +/-1 KHz;
(b) the mixture is placed in a vacuum oven to remove the solvent, and the specific steps are as follows: the mixture was allowed to stand at 60 ℃ under a vacuum of 0.06MPa for 10 hours to remove most of the solvent. Then, the temperature was raised to 120 ℃ and the degree of vacuum was continuously adjusted during the process to further remove the solvent and bubbles in the system. Keeping the vacuum degree of 0.1MPa at 120 ℃ for 10min, then adjusting the pressure of a vacuum oven to air pressure, opening the vacuum oven to take out the material, quickly adding a curing agent diaminodiphenyl sulfone (the molar ratio of epoxy resin to diaminodiphenyl sulfone is 100:55) and fully stirring, then, heating the temperature to 150 ℃ in the vacuum oven, adjusting the pressure to 0.1MPa, keeping the vacuum degree for about 15 min and continuing defoaming;
(c) pouring the mixture into a preheated mold for curing, wherein the curing conditions are as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
Claims (10)
1. A heat-conducting modified epoxy resin-based composite material is characterized in that a blend with a two-phase double-percolation structure and incompatible epoxy resin/thermoplastic resin is used as a matrix, and a heat-conducting filler compatible with the two-phase resin matrix is added to obtain the three-phase double-percolation structure heat-conducting modified composite material of epoxy resin/thermoplastic resin/heat-conducting filler.
2. The heat-conducting modified epoxy resin-based composite material as claimed in claim 1, wherein the thermoplastic resin is one of phenolphthalein polyaryletherketone, polyetherimide and polypropylene.
3. A thermally conductive modified epoxy resin based composite material according to claim 1, wherein said epoxy resin has a viscosity of less than 100 Pa-s at 25 ℃.
4. The heat-conducting modified epoxy resin-based composite material as claimed in claim 1, wherein the mass ratio of the epoxy resin to the thermoplastic resin is 50-84: 50-16.
5. The heat-conducting modified epoxy resin-based composite material as claimed in claim 1, wherein the heat-conducting filler is selected from one of graphene and carbon nanotubes, and the addition amount thereof is 0.1-5 wt% of the matrix mass.
6. A preparation method of the heat-conducting modified epoxy resin-based composite material as claimed in any one of claims 1 to 5, characterized by comprising the following specific steps:
(a) adding thermoplastic resin into a solvent while stirring, completely dissolving the thermoplastic resin, then adding a heat-conducting filler into a solution system, dispersing, adding epoxy resin into the solution system, stirring for 5-10 minutes, and then dispersing the solution system;
(b) placing the mixture in a vacuum oven to remove the solvent, adjusting the pressure of the vacuum oven to air pressure, opening the vacuum oven to take out the material, quickly adding the curing agent and fully stirring, then, heating the temperature to 150 ℃ in the vacuum oven, adjusting the pressure to 0.1MPa, keeping the vacuum degree for about 15 minutes to continue defoaming;
(c) pouring the mixture into a preheated mold for curing, wherein the curing conditions are as follows: 150 ℃/0.1MPa vacuum degree/2 hours +180 ℃/0.1MPa vacuum degree/2 hours, then cooling the mixture to room temperature along with the furnace, opening the mold, and obtaining the required product.
7. The preparation method of the heat-conducting modified epoxy resin-based composite material as claimed in claim 6, wherein the instrument used in the step a for twice dispersion is an ultrasonic disperser, the power of the ultrasonic disperser is 75W, the vibration frequency is 22 +/-1 KHz, and the dispersion time is 1-2 h.
8. The method for preparing the heat-conducting modified epoxy resin-based composite material as claimed in claim 6, wherein the solvent used in step a is one of tetrahydrofuran, acetone and chloroform.
9. The preparation method of the heat-conducting modified epoxy resin-based composite material as claimed in claim 6, wherein the vacuum degree of the vacuum oven in the step b is 0.01 MPa-0.1 MPa, the temperature is normal temperature-120 ℃, and the time for removing the solvent is 5-15 h.
10. The method for preparing the heat-conducting modified epoxy resin-based composite material as claimed in claim 6, wherein the curing agent in step b is diaminodiphenyl sulfone, and the molar ratio of the epoxy resin to the diaminodiphenyl sulfone is 100: 55.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114656161A (en) * | 2022-03-24 | 2022-06-24 | 南京航空航天大学 | Preparation method of low-percolation electrothermal-super-hydrophobic film |
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| CN102070876A (en) * | 2010-12-30 | 2011-05-25 | 桂林电子科技大学 | Epoxy resin base polynary conductive composite material with ultra-low threshold value and preparation method thereof |
| CN108841094A (en) * | 2018-04-28 | 2018-11-20 | 武汉工程大学 | A kind of co-continuous, which exceedes, seeps structure thermal conductive polymer composite material and preparation method |
| CN110128825A (en) * | 2019-05-20 | 2019-08-16 | 四川大学 | Polyphenylene sulfide base electro-magnetic screen composite material and preparation method thereof |
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| JP2010132838A (en) * | 2008-12-08 | 2010-06-17 | Mitsubishi Electric Corp | High thermoconductive thermosetting resin composition |
| CN102070876A (en) * | 2010-12-30 | 2011-05-25 | 桂林电子科技大学 | Epoxy resin base polynary conductive composite material with ultra-low threshold value and preparation method thereof |
| CN108841094A (en) * | 2018-04-28 | 2018-11-20 | 武汉工程大学 | A kind of co-continuous, which exceedes, seeps structure thermal conductive polymer composite material and preparation method |
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Application publication date: 20200421 |