CN112408857A - High-thermal-conductivity epoxy resin composite material and preparation method thereof - Google Patents
High-thermal-conductivity epoxy resin composite material and preparation method thereof Download PDFInfo
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- CN112408857A CN112408857A CN202011400485.5A CN202011400485A CN112408857A CN 112408857 A CN112408857 A CN 112408857A CN 202011400485 A CN202011400485 A CN 202011400485A CN 112408857 A CN112408857 A CN 112408857A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/10—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B26/14—Polyepoxides
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1018—Coating or impregnating with organic materials
- C04B20/1029—Macromolecular compounds
- C04B20/1037—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention belongs to the technical field of epoxy resin composite material preparation, and particularly relates to a preparation method of a high-thermal-conductivity epoxy resin composite material. The carbon nano tubes are directionally arranged to form a three-dimensional framework by adopting a directional freezing method, and then are immersed in a mixture of aluminum oxide powder, a curing agent and epoxy resin, and the composite material is obtained after segmented heating and curing. The preparation process is simple, the preparation conditions are mild, and the obtained epoxy resin composite material has excellent heat conductivity.
Description
Technical Field
The invention belongs to the technical field of epoxy resin composite material preparation, and particularly relates to a preparation method of a high-thermal-conductivity epoxy resin composite material.
Background
Due to the rapid development of modern electronic product industry and the trend of miniaturization of electronic devices, rapid heat dissipation, long-term packaging and environmental adaptability of electronic equipment are increasingly urgently required. Epoxy resins are widely used for preparing composite materials with high thermal conductivity by using epoxy resins as a matrix, because they can widely accommodate different types of fillers. Many studies have shown that temperature has a decisive influence on the use of electronic devices. When a large amount of heat is accumulated and the temperature inside the equipment is too high, irreversible damage can occur inside the equipment, and the service life of the equipment can be greatly shortened. Except that a large amount of heat that produces in the operation in the equipment of in time leading-out, make equipment operating temperature maintain a reasonable moderate scope, the life of extension electronic equipment, heat conduction epoxy composite material can also be with the inseparable encapsulation bonding of the little device in the electronic equipment, guarantees that electronic equipment's whole is complete and long-term operation. At present, various problems exist in a plurality of heat-conducting epoxy resin composite materials, such as complicated preparation process, expensive and difficult acquisition of used fillers, insufficient heat-conducting property and the like. Therefore, the development of epoxy resin composite materials with high thermal conductivity has important practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-thermal-conductivity epoxy resin composite material aiming at the defects of complex preparation and low thermal conductivity of the existing thermal-conductivity epoxy resin composite material. The method has the advantages of simple operation flow, cheap and easily obtained raw materials, mild preparation conditions, and excellent heat conductivity of the obtained high-heat-conductivity epoxy resin composite material, and is a method with important practical significance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a high-thermal-conductivity epoxy resin composite material comprises the following steps:
(1) adding 1 part of polyoxyethylene-8-octyl phenyl ether into 300 parts of deionized water, carrying out ultrasonic treatment on the mixture for 30-60 minutes, then adding 3 parts of carbon nano tubes, and continuing the ultrasonic treatment for 45-60 minutes.
(2) Transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a precooled copper block, and keeping the copper block to be cooled at the temperature of-50 DEG CoC~-70oAnd C, cooling and freezing the dispersion liquid from bottom to top, freezing for 60-120 minutes, freeze-drying the frozen solid for 48-72 hours, and finally sintering for 4-6 hours.
(3) And (3) immersing the sintered carbon nanotube framework in the step (2) in a mixture of pre-mixed spherical aluminum oxide powder, a curing agent and diphenol propane epoxy resin, and placing the mixture in a vacuum oven for 6-8 hours to fully wrap the carbon nanotube framework.
(4) And (4) placing the mixture obtained in the step (3) in a forced air drying oven for heating and curing to obtain a final product.
The power of ultrasonic treatment in the step (1) is 800-1200 w, and the frequency is 30-40 KHz.
And (3) keeping the copper block to be cooled at a low temperature by adopting a mixture of ethyl acetate and liquid nitrogen in the step (2). And mixing ethyl acetate and liquid nitrogen according to the volume ratio of 1: 2-1: 5.
The condition of freeze-drying in the step (2) is-60 to-40oC, 1-5 Pa, the sintering condition is nitrogen atmosphere, and the temperature is 200-300 DEG CoC。
And (3) mixing the spherical aluminum oxide powder, the curing agent, the diphenol propane epoxy resin and the carbon nano tube skeleton according to the mass ratio of 28:1:10: 3-32: 1:10: 3. Wherein the grain diameter of the aluminum oxide is 2-10 mu m, the curing agent is a mixture of dicyandiamide, 3-phenyl-1, 1-dimethyl urea and 2, 4-diaminodiphenylmethane, and the mass ratio is 6: 3: 1 and mixing.
The temperature of the vacuum oven in the step (3) is 50-70 DEGoC, the pressure is-100 to-60 KPa.
In the step (4), the temperature rise and solidification process in the air-blast drying oven is 70-90 DEGoC, curing for 3 hours, and then 90-110oC, curing for 2 hours, and finally, 110-130oC, curing for 1 h.
The invention has the advantages that:
1. according to the invention, polyoxyethylene-8-octyl phenyl ether is simultaneously used as a dispersing agent and a binder, after the carbon nano tubes are wrapped and dispersed in the aqueous solution, when the whole is cooled from bottom to top, water is frozen firstly, so that two ends of the carbon nano tubes wrapped by the ethylene-8-octyl phenyl ether are extruded, and the wrapped carbon nano tubes have a vertical arrangement trend, therefore, a three-dimensional framework obtained after the carbon nano tubes are directionally frozen has a directionally arranged three-dimensional structure, and the prepared composite material has better heat conductivity.
2. According to the invention, the carbon nanotube three-dimensional framework, the spherical aluminum oxide and the epoxy resin are fully mixed and wrapped, so that the obtained composite material has higher internal filling rate and better heat conductivity.
3. The composite material has low curing temperature requirement and mild conditions. The uncured composite material mixture can be preserved for a long time at normal temperature, and has wide application range.
Drawings
FIG. 1. thermal conductivity of composite and neat resin composite after non-orientation and orientation of example 1;
FIG. 2 thermal conductivity of the composite of examples 2, 3, 4 and 5;
FIG. 3. Young's modulus of composite with neat resin composite for unoriented and oriented example 1;
FIG. 4 Young's modulus of the composite material of examples 2, 3, 4 and 5;
FIG. 5. impact strength of composite with neat resin after unoriented and oriented in example 1;
FIG. 6 impact strength of composites of examples 2, 3, 4, 5;
FIG. 7 is an electron microscope image of the skeletal structure of the composite material in example 5.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 30 minutes under the conditions that the power is 800 w and the frequency is 30 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 45 minutes.
(2) And (3) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block. Immersing the lower part of the copper block in ethyl acetate and liquid nitrogen according to the volume ratio of 1:2 to mixIn the mixture of (1). After directional freezing for 60 minutes, the mixture is placed at-60 DEG CoFreeze-drying in a freeze-dryer at C, 1Pa for 48 hr, and then under nitrogen atmosphere, 200oAnd C sintering for 4 hours.
(3) Mixing 2.8 g of spherical aluminum oxide (diameter 2 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, immersing the three-dimensional framework obtained in the step (2) in the mixture, and placing the mixture in a container with the diameter of 50 DEG CoC, 6 hours in a vacuum oven of-100 KPa.
(4) Placing the mixture obtained in (3) in a forced air drying oven, 70oC cured for 3 h, then 90oC curing for 2h, finally 110oC, curing for 1 hour to obtain a final product. The thermal conductivity of the oriented and unoriented epoxy resin composites obtained under the conditions of this example is shown in FIG. 1.
Example 2
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 40 minutes under the conditions that the power is 900 w and the frequency is 35 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 45 minutes.
(2) And (3) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block. The lower part of the copper block is immersed in a mixture of ethyl acetate and liquid nitrogen in a volume ratio of 1: 3. After directional freezing for 90 minutes, the mixture was placed at-55oFreeze-drying in freeze-dryer of C, 2 Pa for 60 hr, and then under nitrogen atmosphere, 200oAnd C, sintering for 5 hours.
(3) Mixing 2.9 g of spherical aluminum oxide (diameter of 4 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, immersing the three-dimensional framework obtained in the step (2) in the mixture, and placing the mixture in a container with the three-dimensional framework in a volume of 55%oC, 6 hours in a vacuum oven at-90 KPa.
(4) Placing the mixture obtained in (3) in a forced air drying oven, 75oC cured for 3 h, then 95oC curing for 2h, finally 115oC, curing for 1 hour to obtain a final product.
Example 3
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 50 minutes under the conditions that the power is 1000 w and the frequency is 35 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 60 minutes.
(2) And (3) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block. The lower part of the copper block is immersed in a mixture of ethyl acetate and liquid nitrogen in a volume ratio of 1: 3. After directional freezing for 100 minutes, the mixture is placed at-50oFreeze-drying in a freeze-dryer at C, 3 Pa for 72 hr, and then under nitrogen atmosphere, 250oAnd C, sintering for 5 hours.
(3) Mixing 3 g of spherical aluminum oxide (diameter 6 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, immersing the three-dimensional framework obtained in the step (2) in the mixture, and placing the mixture in a container with the three-dimensional framework in a volume of 60 goC, a vacuum oven of-80 KPa for 7 hours.
(4) Placing the mixture obtained in (3) in a forced air drying oven, 80oC cured for 3 h, then 100oC curing for 2h, and finally 120oC, curing for 1 hour to obtain a final product.
Example 4
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 60 minutes under the conditions that the power is 1100 w and the frequency is 40 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 60 minutes.
(2) And (3) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block. The lower part of the copper block is immersed in a mixture of ethyl acetate and liquid nitrogen in a volume ratio of 1: 4. After directional freezing for 120 minutes, the mixture is placed at-45 DEG CoFreeze-drying in a freeze-dryer at C, 4 Pa for 72 hr, and then under nitrogen atmosphere 300 deg.CoAnd C, sintering for 5 hours.
(3) Mixing 3.1 g of spherical aluminum oxide (diameter 8 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, immersing the three-dimensional framework obtained in the step (2) in the mixture, and placing the mixture in a container 65oC, -70 KPa vacuum oven for 8 hours.
(4) Obtained in (3)The resulting mixture was placed in a forced air drying oven, 85oC cured for 3 h, then 105oC curing for 2h, finally 125oC, curing for 1 hour to obtain a final product.
Example 5
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 60 minutes under the conditions that the power is 1200 w and the frequency is 40 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 60 minutes.
(2) And (3) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block. The lower part of the copper block is immersed in a mixture of ethyl acetate and liquid nitrogen in a volume ratio of 1: 5. After directional freezing for 120 minutes, the mixture is placed at-40oFreeze-drying in a freeze-dryer at C, 5 Pa for 72 hr, and then under nitrogen atmosphere 300 deg.CoAnd C, sintering for 6 hours.
(3) Mixing 3.2 g of spherical aluminum oxide (diameter 10 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, immersing the three-dimensional framework obtained in the step (2) in the mixture, and placing the mixture in a container of 70 DEG CoC, 8 hours in a vacuum oven at-60 KPa.
(4) Placing the mixture obtained in (3) in a forced air drying oven, 90oC is cured for 3 h, then 110oC curing for 2h, finally 130oC, curing for 1 hour to obtain a final product.
Example 6
(1) 0.1g of polyoxyethylene-8-octyl phenyl ether is added into 30 g of deionized water, ultrasonic treatment is carried out for 30 minutes under the conditions that the power is 800 w and the frequency is 30 KHz, then 0.3 g of carbon nano tube is added, and the ultrasonic treatment is continued for 45 minutes.
(2) Transferring the carbon nanotube dispersion liquid obtained after the treatment in the step (1) to a refrigerator, and performing treatment at-10 oC after freezing for 60 minutes, placing at-60 DEG CoFreeze-drying in a freeze-dryer at C, 1Pa for 48 hr, and then under nitrogen atmosphere, 200oAnd C sintering for 4 hours.
(3) Mixing 2.8 g of spherical aluminum oxide (diameter 2 μm), 0.1g of dicyandiamide and 1g of diphenol propane epoxy resin, and mixing(2) The three-dimensional skeleton obtained in (1) is immersed in the mixture and then placed at 50 deg.CoC, 6 hours in a vacuum oven of-100 KPa.
(4) Placing the mixture obtained in (3) in a forced air drying oven, 70oC cured for 3 h, then 90oC curing for 2h, finally 110oC, curing for 1 hour to obtain a final product. The unoriented epoxy composite was obtained under the conditions of the present example.
As can be seen from fig. 1 and 2, the thermal conductivity of the composite material obtained by the oriented arrangement is significantly improved compared with that of the pure resin composite material, and as can be seen from fig. 1, under the same preparation conditions, the thermal conductivity of the composite material obtained by the oriented arrangement is better than that of the composite material obtained by the unoriented arrangement.
The Young's modulus reaction material resists external force and keeps the shape of the material. As can be seen from fig. 3 and 4, the young's modulus of the composite material obtained after alignment is significantly higher than that of the composite material obtained from the pure resin, and, under the same production conditions, as can be seen from fig. 3, the young's modulus of the composite material obtained without alignment is lower than that of the composite material obtained with alignment.
The maximum external impact force which can be resisted by the impact strength reaction material can be seen from fig. 5 and 6, the impact strength of the composite material obtained after the oriented arrangement is obviously higher than that of a pure resin composite material, and also can be seen from fig. 5, under the same preparation condition, the impact strength of the composite material obtained by the oriented arrangement is higher than that of the composite material which is not oriented arrangement.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
1. The preparation method of the high-thermal-conductivity epoxy resin composite material is characterized by comprising the following steps of: the following raw materials are counted according to the weight portion,
(1) adding 1 part of polyoxyethylene-8-octyl phenyl ether into 300 parts of deionized water, carrying out ultrasonic treatment on the mixture for 30-60 minutes, then adding 3 parts of carbon nano tubes, and continuing the ultrasonic treatment for 45-60 minutes;
(2) transferring the carbon nano tube dispersion liquid obtained after the treatment in the step (1) to the top of a pre-cooled copper block, keeping the copper block to be cooled, cooling and freezing the dispersion liquid from bottom to top, freezing for 60-120 minutes, freeze-drying the frozen solid for 48-72 hours, and finally sintering for 4-6 hours;
(3) immersing the sintered carbon nanotube framework in the step (2) in a pre-mixed mixture of spherical alumina powder, a curing agent and diphenol propane epoxy resin, and placing the mixture in a vacuum oven for 6-8 hours to fully wrap the carbon nanotube framework;
(4) and (4) placing the mixture obtained in the step (3) in a forced air drying oven for heating and curing to obtain a final product.
2. The preparation method of the high thermal conductivity epoxy resin composite material according to claim 1, wherein the power of the ultrasonic treatment in the step (1) is 800-1200 w, and the frequency is 30 KHz-40 KHz.
3. The method for preparing a highly thermally conductive epoxy resin composite material as claimed in claim 1, wherein the mixture of ethyl acetate and liquid nitrogen is used to keep the copper block cold at a low temperature of-50 ℃ in step (2)oC~-70oC; and mixing ethyl acetate and liquid nitrogen according to the volume ratio of 1: 2-1: 5.
4. The preparation method of the high thermal conductivity epoxy resin composite material as claimed in claim 1, wherein the freeze-drying conditions in the step (2) are-60 to-40oC，1~5 Pa。
5. The method for preparing the high thermal conductive epoxy resin composite material according to claim 1, wherein the sintering condition in the step (2) is a nitrogen atmosphere, and the temperature is 200-300%oC。
6. The preparation method of the high thermal conductivity epoxy resin composite material according to claim 1, wherein in the step (3), the spherical alumina powder, the curing agent, the diphenol propane epoxy resin and the carbon nanotube skeleton are mixed in a mass ratio of 28:1:10:3 to 32:1:10: 3.
7. The preparation method of the high thermal conductivity epoxy resin composite material according to claim 1, wherein the particle size of the alumina in the step (3) is 2 to 10 μm.
8. The method for preparing a high thermal conductive epoxy resin composite material as claimed in claim 1, wherein the curing agent is a mixture of dicyandiamide, 3-phenyl-1, 1-dimethylurea and 2, 4-diaminodiphenylmethane in a mass ratio of 6: 3: 1 and mixing.
9. The preparation method of the high thermal conductivity epoxy resin composite material according to claim 1, wherein the temperature of the vacuum oven in the step (3) is 50-70%oC, the pressure is-100 to-60 KPa.
10. The preparation method of the high thermal conductive epoxy resin composite material according to claim 1, wherein the temperature rise curing process in the forced air drying oven in the step (4) is 70-90%oC, curing for 3 hours, and then 90-110oC, curing for 2 hours, and finally, 110-130oC, curing for 1 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113121961A (en) * | 2021-04-20 | 2021-07-16 | 安徽大学 | MFS @ CNT epoxy resin composite material and preparation method thereof |
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| CN101239800A (en) * | 2008-03-07 | 2008-08-13 | 哈尔滨工业大学 | Carbon nano-tube enhanced cement-base composite material and preparation method thereof |
| KR20090110597A (en) * | 2008-04-18 | 2009-10-22 | 충북대학교 산학협력단 | Carbon nanotubes functionalized with 4-substituted benzoic acid, carbon nanotubes/polymer nanocomposites |
| CN104788959A (en) * | 2015-03-31 | 2015-07-22 | 中国科学院化学研究所 | Thermal conductive composite material provided with orientation structure and preparation method of thermal conductive composite material |
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| CN101239800A (en) * | 2008-03-07 | 2008-08-13 | 哈尔滨工业大学 | Carbon nano-tube enhanced cement-base composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113121961A (en) * | 2021-04-20 | 2021-07-16 | 安徽大学 | MFS @ CNT epoxy resin composite material and preparation method thereof |
| CN113121961B (en) * | 2021-04-20 | 2022-05-31 | 安徽大学 | MFS @ CNT epoxy resin composite material and preparation method thereof |
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