CN106565263B - A kind of preparation method of carbon nanotube/silicon carbide heat-conductive composite material - Google Patents
A kind of preparation method of carbon nanotube/silicon carbide heat-conductive composite material Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of silicon carbide/carbon nanotube heat-conductive composite material, and silicon-carbide particle is placed in tube furnace；It is passed through argon gas and hydrogen；It is warming up to 750-850 DEG C；It is passed through carbon source and catalyst mixed solution, grows carbon nanotube on sic；In the state that vacuum degree is less than or equal to 0.1MPa, by the SiC dipping of Polycarbosilane solution and growth carbon nanotube；Block is formed after drying；By the precompressed of gained block, it is hot-forming to get arrive silicon carbide/carbon nanotube heat-conductive composite material.After tested, this composite material bending strength is up to 125MPa or more, and compression strength is up to 500MPa or more.This composite material has good antioxygenic property, can be resistant to 800-1200 DEG C of high temperature ablation for a long time in air.The thermal conductivity of this composite material can reach 30W/ (mK) or more.
Description
Technical field
The present invention relates to a kind of carbon nanotube/silicon carbide heat-conductive composite material preparation methods.
Background technique
With the high speed development of science and technology, efficient thermally conductive and heat dissipation becomes the critical issue of field of heat management and by people
Extensive concern.With the fast development of microelectronics integrated technology and package technique, the volume of logic circuit and electronic component
It is smaller and smaller, and working frequency sharply increases the heat abruptly increase for generating system, if without sufficient heat management guarantee, easily
Lead to related device premature aging or damage.Microelectronic chip surface temperature must be maintained at lower temperature (such as silicon device
100 DEG C of part ﹤) just can ensure that its high performance operation, many electronic components need 40~60 DEG C at a temperature of could work normally,
To guarantee that electronic component can be worked normally reliably for a long time, heat-sinking capability just become the restriction of its service life length because
Element.Traditional metal thermal conductive material (such as aluminium, copper) there are density larger, specific heat conductance (thermal conductivity coefficient and material volume density
The ratio between) it is lower, thermal expansion coefficient is higher, oxidizable the defects of, be difficult to meet growing thermal management requirements at present.Carbon materials
Expect thermal coefficient, lower density and preferable chemical corrosion resistance with higher, is most with prospects in recent years
A kind of Heat Conduction Material.But the aerial use temperature upper limit of carbon material is lower, is easily oxidized at high temperature.Therefore serious
Limit application of the thermally conductive carbon material under high temperature aerobic environment.
Carbon nanotube/silicon carbide heat-conductive composite material (C/SiC) is that one kind is answered modern space flight and aviation development in science and technology and emerged in large numbers
Advanced composite material (ACM) out has high temperature resistant, low-density, Gao Biqiang, anti-oxidant, anti-ablation and high-heating radiation rate etc. a series of
Excellent properties, while the inoxidizability that there is carbon carbon composite (C/C) not have, thus in the aerospace, energy, logical
The fields such as news, electronics have broad application prospects.But carbon nanotube and silicon carbide substrate Interface adhesive strength are weak.Interface lacks
Fall into the mechanical property for having seriously affected composite material.In addition, carbon nanotube and silicon carbide-based body interface are easy to produce gap, hinder
The propagation of phonon greatly reduces the heating conduction of composite material.
So the present invention, which using carbon nanotube is grown on sic, then impregnates Polycarbosilane hot pressing, obtains carbon nanometer
Pipe/silicon carbide heat-conductive composite material.This composite material has high temperature resistant, low-density, Gao Biqiang, anti-oxidant, anti-ablation and height
A series of excellent properties such as thermal emissivity rate, while compared to traditional carbon carbon composite, enhance the knot of carbon nanotube and silicon carbide
Cooperation use, mechanical performance is excellent, and simple process, Heat Conduction Material products pure, be free of other impurity, therefore thermal conductivity also compared with
It is high.
Summary of the invention
The present invention provides one for the disadvantage that carbon nanotube/composite material of silicon carbide boundary defect is serious and thermal conductivity is low
The preparation method of carbon nanotube heat-conductive composite material is grown on kind silicon carbide.
The invention adopts the following technical scheme:
A kind of preparation method of silicon carbide/carbon nanotube heat-conductive composite material, its step are as follows:
1) silicon-carbide particle is placed in tube furnace；It is passed through argon gas and hydrogen；It is warming up to 750-850 DEG C；Be passed through carbon source and
Catalyst mixed solution, grows carbon nanotube on sic；
2) in the state that vacuum degree is less than or equal to 0.1MPa, by the silicon carbide of Polycarbosilane solution and growth carbon nanotube
Dipping；Block is formed after drying；
3) by the precompressed of gained block, it is hot-forming to get arrive silicon carbide/carbon nanotube heat-conductive composite material.
Optimum condition is as follows:
Being passed through argon flow is 300-500sccm；Being passed through hydrogen flowing quantity is 30-50sccm.
Carbon source is ethyl alcohol, dimethylbenzene mixed solution, and ethyl alcohol: dimethylbenzene volume ratio is=1:1.
Catalyst is ferrocene, and ferrocene is dissolved in carbon source mixed solution, concentration 0.02-0.03g/ml.
The growth carbon nanotube time is 10-60min on sic.Polycarbosilane concentration is 0.3-0.6g/ml.
The dip time 20-40min of step 2).
Step 3) pre-molding is the pre-molding in the case where being less than or equal to 50MPa pressure and 180-200 DEG C.It is hot-forming be by
Green body obtained by pre-molding is placed in mold, is placed in vacuum hotpressing stove and is carried out high temperature hot pressing, hot pressing temperature 1300 DEG C with
On, hot pressing pressure is 5~50MPa, and heat-insulation pressure keeping 1~4 hour is to get arriving silicon carbide/carbon nanotube heat-conductive composite material.
It is described as follows:
1. growth array carbon nano tube: silicon-carbide particle being placed in tube furnace, does not grow the silicon carbide of carbon nanotube
Grain is as shown in Figure 1；It is passed through the argon gas that flow is 300-500sccm and the hydrogen that flow is 30-50sccm；It is warming up to 750-850
℃；It is passed through carbon source and catalyst mixed solution, injection speed 15-20ml/h, growth time 10-60min；After growth
Close H2；The silicon carbide with carbon nanotube is taken out after cooling, growth has the silicon carbide of carbon nanotube as shown in Figure 2；
2. impregnating Polycarbosilane (PCS): in the state that vacuum degree is less than or equal to 0.1MPa, by the poly- of 0.3-0.6g/ml
The SiC dipping 20-40min of carbon silane (PCS) solution and growth carbon nanotube；Block is formed after drying；
3. hot-forming: by gained silicon carbide block in the case where being less than or equal to 50MPa pressure and 180-200 DEG C pre-molding,
Then gained green body is placed in mold, one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, hot pressing temperature is 1300
DEG C or more, hot pressing pressure is 5~50MPa, heat-insulation pressure keeping 1~4 hour to get arriving silicon carbide/carbon nanotube heat-conductive composite material,
As shown in Figure 3.
There is good mechanical property by carbon nanotube/silicon carbide heat-conductive composite material that this method obtains, bending is strong
It spends up to 125MPa or more, compression strength is up to 500MPa or more.This composite material has good antioxygenic property, can be
800-1200 DEG C of high temperature ablation is resistant in air for a long time.The thermal conductivity of this composite material can reach 30W/ (mK) with
On.The method of the present invention is simple, and prepared carbon nanotube/composite material of silicon carbide has excellent high temperature resistant, anti-oxidant, high fever
The performances such as conductance.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture for not growing the silicon carbide of carbon nanotube；
Fig. 2 makes a living the scanning electron microscopic picture of the silicon carbide with array carbon nano tube；
Fig. 3 is carbon nanotube/composite material of silicon carbide photo.
Specific embodiment
The embodiment of the present invention is given below, is not intended to limit the scope of the invention to further explanation of the invention.
1) silicon-carbide particle is placed in tube furnace；Being passed through argon gas that flow is 300-500sccm and flow is 30-
The hydrogen of 50sccm；It is warming up to 750-850 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixes
Close solution, ethyl alcohol: dimethylbenzene volume ratio is=1:1, and catalyst is ferrocene, and ferrocene is dissolved in carbon source mixed solution,
Its concentration is 0.02-0.03g/ml；Injection speed is 15-20ml/h, growth time 10-60min；It is closed after growth
H2；The silicon carbide with carbon nanotube is taken out after cooling；
2) in the state that vacuum degree is less than or equal to 0.1MPa, by Polycarbosilane (PCS) solution of 0.3-0.6g/ml and life
The SiC dipping 20-40min of long carbon nanotube；Block is formed after drying；
3) by gained block in the case where being less than or equal to 50MPa pressure and 180-200 DEG C pre-molding, then gained green body is set
In mold, one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, hot pressing temperature is in 1300 DEG C or more, hot pressing pressure
5~50MPa, heat-insulation pressure keeping 1~4 hour is to get arriving silicon carbide/carbon nanotube heat-conductive composite material.
Embodiment 1
Silicon-carbide particle is placed in tube furnace；It is passed through the argon gas that flow is 300sccm and the hydrogen that flow is 30sccm；
It is warming up to 750 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixed solution, ethyl alcohol: diformazan
Benzene volume ratio is=1:1, and catalyst is ferrocene, is dissolved in carbon source mixed solution, concentration 0.02g/ml, and injection speed is
15ml/h, growth time 10min；H is closed after growth2；The silicon carbide with carbon nanotube is taken out after cooling；In vacuum
In the state that degree is 0.1MPa, by the SiC dipping of Polycarbosilane (PCS) solution of 0.3g/ml and growth carbon nanotube
20min；Block is formed after drying；By gained silicon carbide block at 35MPa pressure and 180 DEG C pre-molding, then by gained
Green body is placed in mold, and one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, and hot pressing temperature is at 1350 DEG C, hot pressing pressure
For 10MPa, heat-insulation pressure keeping 2 hours, carbon nanotube/silicon carbide heat-conductive composite material is obtained, bending strength resists up to 132MPa
Compressive Strength reaches 550MPa, and thermal conductivity reaches 34.2W/ (mK).
Embodiment 2
Silicon-carbide particle is placed in tube furnace；It is passed through the argon gas that flow is 350sccm and the hydrogen that flow is 40sccm；
It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixed solution, ethyl alcohol: diformazan
Benzene volume ratio is=1:1, and catalyst is ferrocene, is dissolved in carbon source mixed solution, concentration 0.02g/ml, and injection speed is
18ml/h, growth time 30min；H is closed after growth2；The silicon carbide with carbon nanotube is taken out after cooling；In vacuum
In the state that degree is 0.1MPa, by the SiC dipping of Polycarbosilane (PCS) solution of 0.35g/ml and growth carbon nanotube
30min；Block is formed after drying；By gained silicon carbide block at 35MPa pressure and 180 DEG C pre-molding, then by gained
Green body is placed in mold, and one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, and hot pressing temperature is at 1400 DEG C, hot pressing pressure
For 20MPa, heat-insulation pressure keeping 2 hours, carbon nanotube/silicon carbide heat-conductive composite material is obtained, bending strength resists up to 135MPa
Compressive Strength reaches 543MPa, and thermal conductivity reaches 36.1W/ (mK).
Embodiment 3
Silicon-carbide particle is placed in tube furnace；It is passed through the argon gas that flow is 400sccm and the hydrogen that flow is 40sccm；
It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixed solution, ethyl alcohol: diformazan
Benzene volume ratio is=1:1, and catalyst is ferrocene, is dissolved in carbon source mixed solution, concentration 0.025g/ml, injection speed
For 18ml/h, growth time 30min；H is closed after growth2；The silicon carbide with carbon nanotube is taken out after cooling；True
In the state that reciprocal of duty cycle is 0.1MPa, by the SiC dipping of Polycarbosilane (PCS) solution of 0.4g/ml and growth carbon nanotube
40min；Block is formed after drying；By gained silicon carbide block at 40MPa pressure and 180 DEG C pre-molding, then by gained
Green body is placed in mold, and one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, and hot pressing temperature is at 1400 DEG C, hot pressing pressure
For 30MPa, heat-insulation pressure keeping 2 hours, carbon nanotube/silicon carbide heat-conductive composite material is obtained, bending strength resists up to 138MPa
Compressive Strength reaches 556MPa, and thermal conductivity reaches 34.7W/ (mK).
Embodiment 4
Silicon-carbide particle is placed in tube furnace；It is passed through the argon gas that flow is 450sccm and the hydrogen that flow is 50sccm；
It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixed solution, ethyl alcohol: diformazan
Benzene volume ratio is=1:1, and catalyst is ferrocene, is dissolved in carbon source mixed solution, concentration 0.03g/ml, and injection speed is
20ml/h, growth time 50min；H is closed after growth2；The silicon carbide with carbon nanotube is taken out after cooling；In vacuum
In the state that degree is 0.1MPa, by the SiC dipping of Polycarbosilane (PCS) solution of 0.5g/ml and growth carbon nanotube
45min；Block is formed after drying；By gained silicon carbide block at 45MPa pressure and 190 DEG C pre-molding, so then by institute
Green body is placed in mold, one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, hot pressing temperature is at 1400 DEG C, hot pressing pressure
Power is 35MPa, heat-insulation pressure keeping 2.5 hours, obtains carbon nanotube/silicon carbide heat-conductive composite material, bending strength is reachable
136MPa, compression strength reach 558MPa, and thermal conductivity reaches 33.9W/ (mK).
Embodiment 5
Silicon-carbide particle is placed in tube furnace；It is passed through the argon gas that flow is 500sccm and the hydrogen that flow is 50sccm；
It is warming up to 850 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethyl alcohol, dimethylbenzene mixed solution, ethyl alcohol: diformazan
Benzene volume ratio is=1:1, and catalyst is ferrocene, is dissolved in carbon source mixed solution, concentration 0.03g/ml, and injection speed is
20ml/h, growth time 60min；H is closed after growth2；The silicon carbide with carbon nanotube is taken out after cooling；In vacuum
In the state that degree is 0.1MPa, by the SiC dipping of Polycarbosilane (PCS) solution of 0.6g/ml and growth carbon nanotube
40min；Block is formed after drying；By gained silicon carbide block at 50MPa pressure and 200 DEG C pre-molding, then by gained
Green body is placed in mold, and one is placed in vacuum hotpressing stove and carries out high temperature hot pressing, and hot pressing temperature is at 1350 DEG C, hot pressing pressure
For 50MPa, heat-insulation pressure keeping 4 hours, carbon nanotube/silicon carbide Heat Conduction Material is obtained, bending strength is up to 138MPa, pressure resistance
Degree reaches 552MPa, and thermal conductivity reaches 36.1W/ (mK).
Claims (9)
1. a kind of preparation method of silicon carbide/carbon nanotube heat-conductive composite material, it is characterized in that steps are as follows:
1) silicon-carbide particle is placed in tube furnace；It is passed through argon gas and hydrogen；It is warming up to 750-850 DEG C；It is passed through carbon source and catalysis
Agent mixed solution, grows carbon nanotube on sic；
2) in the state that vacuum degree is less than or equal to 0.1MPa, the silicon carbide of Polycarbosilane solution and growth carbon nanotube is soaked
Stain；Block is formed after drying；
3) by the precompressed of gained block, it is hot-forming to get arrive silicon carbide/carbon nanotube heat-conductive composite material；
The carbon source is ethyl alcohol, dimethylbenzene mixed solution.
2. the method as described in claim 1, it is characterized in that being passed through argon flow is 300-500sccm；Being passed through hydrogen flowing quantity is
30-50sccm。
3. the method as described in claim 1, it is characterized in that carbon source ethyl alcohol: dimethylbenzene volume ratio is=1:1.
4. ferrocene it is characterized in that catalyst is ferrocene, and is dissolved in carbon source mixed solution by the method as described in claim 1
In, concentration 0.02-0.03g/ml.
5. the method as described in claim 1, it is characterized in that the growth carbon nanotube time is 10-60min on sic.
6. the method as described in claim 1, it is characterized in that Polycarbosilane concentration is 0.3-0.6g/ml.
7. the method as described in claim 1, it is characterized in that the dipping 20-40min of step 2).
8. the method as described in claim 1, it is characterized in that step 3) pre-molding is to be less than or equal to 50MPa pressure and 180-
Pre-molding at 200 DEG C.
9. the method as described in claim 1, it is characterized in that it is hot-forming be green body obtained by pre-molding is placed in mold, and
It is placed in vacuum hotpressing stove and carries out high temperature hot pressing, for hot pressing temperature at 1300 DEG C or more, hot pressing pressure is 5~50MPa, heat-insulation pressure keeping
1~4 hour to get arrive silicon carbide/carbon nanotube heat-conductive composite material.
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| CN112442684A (en) * | 2019-09-03 | 2021-03-05 | 天津大学 | Carbon nanotube array-metal composite heat dissipation material and preparation method thereof |
| CN111377750B (en) * | 2020-04-15 | 2022-06-24 | 齐荟仟 | Carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and preparation method thereof |
| CN114804886B (en) * | 2021-01-18 | 2023-07-18 | 郑州大学 | Preparation method of carbon-modified nano silicon carbide composite material and application of carbon-modified nano silicon carbide composite material as radiation detector material |
| CN115724424A (en) * | 2021-08-25 | 2023-03-03 | 天津大学 | Graphene-oriented carbon nanotube array-based oriented heat conduction and heat dissipation integrated all-carbon material |
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| CN101293772B (en) * | 2008-05-30 | 2011-06-15 | 上海工程技术大学 | Preparation technique for SiC/CNTs composite ceramic |
| CN101774814B (en) * | 2010-01-14 | 2012-11-21 | 天津大学 | Ceramic and carbon nano-fiber composite material and preparation method thereof |
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| CN102021817B (en) * | 2010-11-11 | 2012-03-21 | 中国人民解放军国防科学技术大学 | Silicon carbide fiber solid fabric for in-situ growing carbon nano tubes, composite material and preparation method thereof |
| CN102199872B (en) * | 2011-03-29 | 2013-04-03 | 北京航空航天大学 | Method for in-situ growing carbon nanotubes on fiber surfaces |
| CN102962087B (en) * | 2011-08-31 | 2014-10-22 | 中国科学院金属研究所 | Carbon nanotube/silicon carbide foam catalytic composite material and preparation method thereof |
| CN103754878B (en) * | 2014-01-06 | 2015-10-14 | 上海交通大学 | The method of the spontaneous carbon nanotube of a kind of silicon-carbide particle surface in situ |
| CN104085873B (en) * | 2014-06-03 | 2016-11-02 | 张映波 | A kind of method preparing CNT in fiber surface high density |
| CN105948776B (en) * | 2016-04-28 | 2018-08-28 | 天津大学 | A kind of preparation method of array carbon nano-tube/carbon fiber/silicon carbide heat-conductive composite material |
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