CN106565263A - Preparation method for carbon nano-tube/silicon carbide heat-conducting composite material - Google Patents

Preparation method for carbon nano-tube/silicon carbide heat-conducting composite material Download PDF

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CN106565263A
CN106565263A CN201610967909.3A CN201610967909A CN106565263A CN 106565263 A CN106565263 A CN 106565263A CN 201610967909 A CN201610967909 A CN 201610967909A CN 106565263 A CN106565263 A CN 106565263A
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composite material
silicon carbide
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CN106565263B (en
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封伟
尹晓东
陈松超
冯奕钰
秦盟盟
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Tianjin University
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Abstract

The invention relates to a preparation method for a silicon carbide/carbon nano-tube heat-conducting composite material. The preparation method comprises the following steps: placing silicon carbide particles in a tubular furnace; charging argon and hydrogen; heating to 750-850 DEG C; charging a mixed solution of a carbon source and a catalyst, and growing carbon nano-tubes on the silicon carbide; impregnating a polycarbosilane solution and the silicon carbide growing the carbon nano-tubes in a state that a vacuum degree is less than or equal to 0.1MPa; drying to form blocks; and carrying out pre-pressing and hot-pressing forming on the obtained blocks to obtain the silicon carbide/carbon nano-tube heat-conducting composite material. The bending strength of the composite material can achieve more than 125MPa, and the compressive strength thereof can achieve more than 500MPa via a test. The composite material is high in oxidation resistance, and tolerant to high-temperature ablation at 800-1200 DEG C for a long time in air. The thermal conductivity of the composite material can achieve more than 30W/(m.K).

Description

A kind of preparation method of CNT/carborundum heat-conductive composite material
Technical field
The present invention relates to a kind of preparation method of CNT/carborundum heat-conductive composite material.
Background technology
With the high speed development of science and technology, efficient heat conduction becomes the key issue of field of heat management and by people with radiating Extensive concern.With the volume of the fast development of microelectronics integrated technology and package technique, logic circuit and electronic devices and components It is less and less, and operating frequency sharply increases the heat abruptly increase for producing system, if no sufficient heat management guarantee, easily Cause related device premature aging or damage.Microelectronic chip surface temperature is must be maintained at relatively low temperature (such as silicon device 100 DEG C of part ﹤) just can ensure that its high performance operation, many electronic units need at a temperature of 40～60 DEG C could normal work, For ensure electronic devices and components can long-time reliably normal work, heat-sinking capability just become the restriction of its service life length because Element.Traditional metal heat-conducting material (such as aluminum, copper etc.) has that density is larger, specific heat conductance (thermal conductivity coefficient and material volume density Ratio) defect such as relatively low, thermal coefficient of expansion is higher, oxidizable, it is difficult to meet thermal management requirements growing at present.Carbon materials Material, with higher heat conductivity, relatively low density and preferable chemical resistance, is most with prospects in recent years One class Heat Conduction Material.But the aerial use temperature upper limit of material with carbon element is relatively low, is easily oxidized at high temperature.Therefore it is serious Limit application of the heat conduction material with carbon element under high temperature aerobic environment.
CNT/carborundum 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, it is a series of with high temperature resistant, low-density, Gao Biqiang, antioxidation, anti-yaw damper and high-heating radiation rate etc. Excellent properties, while have the non-oxidizability that do not have of carbon carbon composite (C/C), thus in Aero-Space, the energy, lead to The fields such as news, electronics have broad application prospects.But CNT is weak with silicon carbide substrate Interface adhesive strength.Interface lacks Fall into the mechanical property for having had a strong impact on composite.Additionally, CNT and silicon carbide-based body interface easily produce gap, hinder The propagation of phonon, greatly reduces the heat conductivility of composite.
So the present invention is using CNT is grown on sic, then impregnates Polycarbosilane hot pressing and obtain carbon nanometer Pipe/carborundum heat-conductive composite material.This composite has high temperature resistant, low-density, Gao Biqiang, antioxidation, anti-yaw damper and height A series of excellent properties such as thermal emissivity rate, while comparing traditional carbon carbon composite, enhance the knot of CNT and carborundum Cooperation is used, and mechanical performance is excellent, and process is simple, Heat Conduction Material products pure, without other impurity, therefore thermal conductivity also compared with It is high.
The content of the invention
The present invention is directed to CNT/composite material of silicon carbide boundary defect seriously and the shortcoming of low thermal conductivity, there is provided one Plant the preparation method that CNT heat-conductive composite material is grown on carborundum.
The present invention is employed the following technical solutions：
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 and hydrogen；It is warming up to 750-850 DEG C；Be passed through carbon source and Catalyst mixed solution, grows CNT on sic；
2) in the state of vacuum is less than or equal to 0.1MPa, by Polycarbosilane solution and the carborundum for growing CNT Dipping；Block is formed after drying；
3) by gained block precompressed, hot-forming, that is, obtain silicon carbide/carbon nanotube heat-conductive composite material.
Optimum condition is as follows：
Argon flow amount is passed through for 300-500sccm；Hydrogen flowing quantity is passed through for 30-50sccm.
Carbon source be ethanol, dimethylbenzene mixed solution, ethanol：Dimethylbenzene volume ratio is=1:1.
Catalyst is ferrocene, and ferrocene is dissolved in carbon source mixed solution, and its concentration is 0.02-0.03g/ml.
The CNT time is grown on sic for 10-60min.Polycarbosilane concentration is 0.3-0.6g/ml.
Step 2) dip time 20-40min.
Step 3) pre-molding is less than or equal to pre-molding at 50MPa pressure and 180-200 DEG C.It is hot-forming be by Obtained by pre-molding, base substrate is placed in mould, carries out high temperature hot pressing in being placed in vacuum hotpressing stove, hot pressing temperature 1300 DEG C with On, hot pressing pressure is 5～50MPa, and heat-insulation pressure keeping 1～4 hour obtain silicon carbide/carbon nanotube heat-conductive composite material.
It is described as follows：
1. array carbon nano tube is grown：Silicon-carbide particle is placed in tube furnace, the carborundum of CNT is not grown Grain is as shown in Figure 1；It is passed through the hydrogen that the argon and flow that flow is 300-500sccm is 30-50sccm；It is warming up to 750-850 ℃；Carbon source and catalyst mixed solution are passed through, injection speed is 15-20ml/h, and growth time is 10-60min；After growth terminates Close H2；Length is taken out after cooling the carborundum of CNT, and growth has the carborundum of CNT as shown in Figure 2；
2. Polycarbosilane (PCS) is impregnated：In the state of vacuum is less than or equal to 0.1MPa, by the poly- of 0.3-0.6g/ml Carbon silane (PCS) solution and the SiC dipping 20-40min for growing CNT；Block is formed after drying；
3. hot-forming：By gained carborundum block less than or equal to pre-molding at 50MPa pressure and 180-200 DEG C, Subsequently gained base substrate is placed in mould, one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature is 1300 More than DEG C, hot pressing pressure is 5～50MPa, and heat-insulation pressure keeping 1～4 hour obtain silicon carbide/carbon nanotube heat-conductive composite material, As shown in Figure 3.
CNT/carborundum the heat-conductive composite material obtained by this method has good mechanical property, and bending is strong , up to more than 125MPa, comprcssive strength is up to more than 500MPa for degree.This composite has good antioxygenic property, can be Tolerate 800-1200 DEG C of high temperature ablation in air for a long time.The thermal conductivity of this composite can reach 30W/ (mK) with On.The inventive method is simple, and prepared CNT/composite material of silicon carbide has excellent high temperature resistant, antioxidation, hyperpyrexia The performances such as conductance.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of the carborundum for not growing CNT；
Fig. 2 is the scanning electron microscopic picture of the carborundum that growth has array carbon nano tube；
Photos of the Fig. 3 for CNT/composite material of silicon carbide.
Specific embodiment
Embodiments of the invention are given below, are that the present invention is further illustrated, rather than limit the scope of the present invention.
1) silicon-carbide particle is placed in tube furnace；It is 30- to be passed through the argon and flow that flow is 300-500sccm 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 that ethanol, dimethylbenzene are mixed Close solution, ethanol：Dimethylbenzene volume ratio is=1:1, 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, and growth time is 10-60min；Growth is closed after terminating H2；Length is taken out after cooling the carborundum of CNT；
2) in the state of vacuum 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 CNT；Block is formed after drying；
3) gained base substrate is subsequently put by gained block less than or equal to pre-molding at 50MPa pressure and 180-200 DEG C In mould, one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, more than 1300 DEG C, hot pressing pressure is hot pressing temperature 5～50MPa, heat-insulation pressure keeping 1～4 hour obtain silicon carbide/carbon nanotube heat-conductive composite material.
Embodiment 1
Silicon-carbide particle is placed in tube furnace；It is passed through the hydrogen that the argon and flow that flow is 300sccm is 30sccm； It is warming up to 750 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethanol, dimethylbenzene mixed solution, ethanol：Diformazan Benzene volume ratio is=1:1, catalyst is ferrocene, is dissolved in carbon source mixed solution, and its concentration is 0.02g/ml, and injection speed is 15ml/h, growth time are 10min；Growth closes H after terminating2；Length is taken out after cooling the carborundum of CNT；In vacuum In the state of spending for 0.1MPa, by Polycarbosilane (PCS) solution of 0.3g/ml and the SiC dipping for growing CNT 20min；Block is formed after drying；By gained carborundum block at 35MPa pressure and 180 DEG C pre-molding, subsequently by gained Base substrate is placed in mould, and one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature at 1350 DEG C, hot pressing pressure For 10MPa, heat-insulation pressure keeping 2 hours, CNT/carborundum heat-conductive composite material is obtained, its 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 hydrogen that the argon and flow that flow is 350sccm is 40sccm； It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethanol, dimethylbenzene mixed solution, ethanol：Diformazan Benzene volume ratio is=1:1, catalyst is ferrocene, is dissolved in carbon source mixed solution, and its concentration is 0.02g/ml, and injection speed is 18ml/h, growth time are 30min；Growth closes H after terminating2；Length is taken out after cooling the carborundum of CNT；In vacuum In the state of spending for 0.1MPa, by Polycarbosilane (PCS) solution of 0.35g/ml and the SiC dipping for growing CNT 30min；Block is formed after drying；By gained carborundum block at 35MPa pressure and 180 DEG C pre-molding, subsequently by gained Base substrate is placed in mould, and one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature at 1400 DEG C, hot pressing pressure For 20MPa, heat-insulation pressure keeping 2 hours, CNT/carborundum heat-conductive composite material is obtained, its 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 hydrogen that the argon and flow that flow is 400sccm is 40sccm； It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethanol, dimethylbenzene mixed solution, ethanol：Diformazan Benzene volume ratio is=1:1, catalyst is ferrocene, is dissolved in carbon source mixed solution, its concentration be 0.025g/ml, injection speed For 18ml/h, growth time is 30min；Growth closes H after terminating2；Length is taken out after cooling the carborundum of CNT；True In the state of reciprocal of duty cycle is 0.1MPa, by Polycarbosilane (PCS) solution of 0.4g/ml and the SiC dipping for growing CNT 40min；Block is formed after drying；By gained carborundum block at 40MPa pressure and 180 DEG C pre-molding, subsequently by gained Base substrate is placed in mould, and one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature at 1400 DEG C, hot pressing pressure For 30MPa, heat-insulation pressure keeping 2 hours, CNT/carborundum heat-conductive composite material is obtained, its 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 hydrogen that the argon and flow that flow is 450sccm is 50sccm； It is warming up to 800 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethanol, dimethylbenzene mixed solution, ethanol：Diformazan Benzene volume ratio is=1:1, catalyst is ferrocene, is dissolved in carbon source mixed solution, and its concentration is 0.03g/ml, and injection speed is 20ml/h, growth time are 50min；Growth closes H after terminating2；Length is taken out after cooling the carborundum of CNT；In vacuum In the state of spending for 0.1MPa, by Polycarbosilane (PCS) solution of 0.5g/ml and the SiC dipping for growing CNT 45min；Block is formed after drying；By gained carborundum block at 45MPa pressure and 190 DEG C pre-molding, so subsequently by institute Base substrate is placed in mould, one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature at 1400 DEG C, hot pressing pressure Power is 35MPa, and heat-insulation pressure keeping 2.5 hours obtains CNT/carborundum heat-conductive composite material, and its bending strength is reachable 136MPa, comprcssive 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 hydrogen that the argon and flow that flow is 500sccm is 50sccm； It is warming up to 850 DEG C；It is passed through carbon source and catalyst mixed solution, wherein carbon source is ethanol, dimethylbenzene mixed solution, ethanol：Diformazan Benzene volume ratio is=1:1, catalyst is ferrocene, is dissolved in carbon source mixed solution, and its concentration is 0.03g/ml, and injection speed is 20ml/h, growth time are 60min；Growth closes H after terminating2；Length is taken out after cooling the carborundum of CNT；In vacuum In the state of spending for 0.1MPa, by Polycarbosilane (PCS) solution of 0.6g/ml and the SiC dipping for growing CNT 40min；Block is formed after drying；By gained carborundum block at 50MPa pressure and 200 DEG C pre-molding, subsequently by gained Base substrate is placed in mould, and one is placed in high temperature hot pressing is carried out in vacuum hotpressing stove, hot pressing temperature at 1350 DEG C, hot pressing pressure For 50MPa, heat-insulation pressure keeping 4 hours, CNT/carborundum Heat Conduction Material is obtained, its 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, is characterized in that step is as follows：
1) silicon-carbide particle is placed in tube furnace；It is passed through argon and hydrogen；It is warming up to 750-850 DEG C；It is passed through carbon source and catalysis Agent mixed solution, grows CNT on sic；
2) in the state of vacuum is less than or equal to 0.1MPa, carborundum of the Polycarbosilane solution with growth CNT is soaked Stain；Block is formed after drying；
3) by gained block precompressed, hot-forming, that is, obtain silicon carbide/carbon nanotube heat-conductive composite material.
2. the method for claim 1, is characterized in that being passed through argon flow amount for 300-500sccm；Being passed through hydrogen flowing quantity is 30-50sccm。
3. the method for claim 1, is characterized in that carbon source for ethanol, dimethylbenzene mixed solution, ethanol：Dimethylbenzene volume Than for=1:1.
4. the method for claim 1, is characterized in that catalyst is ferrocene, and ferrocene is dissolved in carbon source mixed solution In, its concentration is 0.02-0.03g/ml.
5. the method for claim 1, is characterized in that growing on sic the CNT time for 10-60min.
6. the method for claim 1, is characterized in that Polycarbosilane concentration is 0.3-0.6g/ml.
7. the method for claim 1, is characterized in that step 2) dipping 20-40min.
8. the method for claim 1, is characterized in that step 3) pre-molding is less than or equal to 50MPa pressure and 180- Pre-molding at 200 DEG C.
9. the method for claim 1, is characterized in that hot-forming is that base substrate obtained by pre-molding is placed in mould, and Being placed in vacuum hotpressing stove carries out high temperature hot pressing, hot pressing temperature more than 1300 DEG C, hot pressing pressure be 5～50MPa, heat-insulation pressure keeping 1～4 hour, that is, obtain silicon carbide/carbon nanotube heat-conductive composite material.
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CN111377750A (en) * 2020-04-15 2020-07-07 齐荟仟 Carbon nanotube sponge reinforced silicon carbide ceramic matrix composite and preparation method thereof
CN112442684A (en) * 2019-09-03 2021-03-05 天津大学 Carbon nanotube array-metal composite heat dissipation material and preparation method thereof
CN114804886A (en) * 2021-01-18 2022-07-29 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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