CN103061112A - Composite material of silicon carbide and carbon nanotube and preparation method thereof - Google Patents
Composite material of silicon carbide and carbon nanotube and preparation method thereof Download PDFInfo
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- CN103061112A CN103061112A CN2012105154609A CN201210515460A CN103061112A CN 103061112 A CN103061112 A CN 103061112A CN 2012105154609 A CN2012105154609 A CN 2012105154609A CN 201210515460 A CN201210515460 A CN 201210515460A CN 103061112 A CN103061112 A CN 103061112A
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Abstract
The invention relates to a composite material of silicon carbide and carbon nanotube and a preparation method thereof. Macroscopic bodies of the carbon nanotubes are used as performs, a chemical vapor deposition method is used for pyrolysis of a silicon-containing precursor, and then the silicon carbide is deposited on the carbon nanotube to prepared the composite material of the silicon carbide and the carbon nanotube, with a mass percent of the carbon nanotube being 0.5-90 %. By selecting the macroscopic bodies of the carbon nanotubes of various orientations and arrangements as performs, the composite material of the silicon carbide and the carbon nanotube with high dispersion, high volume content and various orientations and arrangements can be obtained. By designing fiber performs, the composite material of the silicon carbide and the carbon nanotube with various forms such as fibers and blocks and various sizes can be constructed and prepared. The composite material of the silicon carbide and the carbon nanotube with various mechanical and electrical properties can be obtained, and may be used as high-performance composite materials, conductive and thermal conductivity materials and functional materials in fields of aerospace, national defense equipment, functional material devices, etc.
Description
Technical field
The present invention relates to composite of a kind of carborundum and CNT and preparation method thereof, specifically take carbon nano-tube macroscopic body as precast body, adopt the chemical vapour deposition technique pyrolysis to contain silicon precursor carborundum is deposited on carbon nano-tube macroscopic body, the composite of preparation carborundum and CNT belongs to field of nanometer material technology.
Background technology
Composite material of silicon carbide has lightweight, high-strength, high tenacity, high temperature resistant, anti-thermal shock, Deng excellent mechanics and high-temperature behavior, and have physical properties such as high conduction, high heat conduction, be widely used in the high-tech sectors such as Aero-Space, defence equipment, also be widely used in fields such as machinery, chemical industry, electronics industries.
CNT (CNT) has one-dimensional nano structure, high specific area, has high strength, high-modulus, high tenacity and the performances such as high conduction, high-termal conductivity and electric field transmitted.These excellent structures, mechanics, physics and functional performance make CNT become the ideal material of Development of Novel high-performance, electric-conductivity heat-conductivity high composite and functional material.
CNT is carried out the compound performances such as the high specific area of CNT, high strength, high-modulus and high tenacity of utilizing and can be combined with the good interface of silicon carbide substrate coupling formation as strengthening body and carborundum, have little interfacial stress, be expected to obtain high-strength, shock resistance, high-performance fiber high temperature resistant and anti-thermal shock strengthens composite material of silicon carbide.
Utilize the one-dimensional nano structure of CNT uniqueness, high conduction and high thermal conductivity, can in silicon carbide substrate, form interconnective conduction and heat conduction network, realize the Real-Time Monitoring of composite carrying, military service and actual effect stress, development has the novel silicon carbide based composites of intelligent characteristic.
Chinese patent CN201010540199.9A discloses the silicon carbide fibre stereo fabric that a kind of growth in situ has CNT, this silicon carbide fibre stereo fabric is mainly formed by the silicon carbide fibre braiding, the even carbon nanotube of growth in situ is distributed in the silicon carbide fibre surface, and CNT is wound in network structure mutually.Its preparation method may further comprise the steps: at first the silicon carbide fibre stereo fabric is carried out preliminary treatment; Adopt again catalyst precursor vacuum impregnation-reducing process to load the Ni-La-Al composite catalyst; Carry out at last chemical vapour deposition (CVD), make that growth in situ goes out CNT on the silicon carbide fibre stereo fabric.The method has been used catalyst, and complex process, condition are comparatively harsh, and cost is higher.
The composite that the macroscopic body that adopts chemical vapour deposition technique to form take CNT is prepared carborundum and CNT as precast body has no report.
Summary of the invention
The object of the present invention is to provide composite of a kind of carborundum and CNT and preparation method thereof.The macroscopic body that forms take CNT adopts chemical vapour deposition technique to prepare the composite of carborundum and CNT as precast body.Electrical heating can realize that as efficient local heating means the efficient carborundum deposition of Fast Heating is for the preparation of the composite of carborundum and CNT.The present invention can prepare the composite of various content of carbon nanotubes and homodisperse carborundum and CNT.And can prepare CNT and have the carborundum of various CNTs orientations of the carborundum of unidirectional array and CNT and the composite of CNT.
Chemical vapour deposition technique can form uniform silicon carbide layer in carbon nano tube surface, have the advantages such as the controlled and depositing silicon carbide of reaction is controlled, can regulate and control content and the thickness of carborundum by parameters such as control depositing temperature, time and air pressure, that these composites with the carborundum of even silicon carbide layer enveloped carbon nanometer tube structure and CNT have is high-strength, electric-conductivity heat-conductivity high and the performance such as anti-oxidant, is used for association area as high performance structures and functional material.
The composite of carborundum provided by the invention and CNT is take CNT and contains silicon precursor as raw material, carbon nano-tube macroscopic body is precast body in the electrical heating precipitation equipment, contain silicon precursor by chemical vapor deposition pyrolytic, carborundum is deposited on carbon nano-tube macroscopic body, forms the carborundum of different content of carbon nanotubes and carbon nanotube architecture and the composite of CNT.The mass fraction of CNT can be 0.5-90%.Alternatively, the mass fraction of CNT can be 5-85%,
Described CNT is Single Walled Carbon Nanotube, double-walled carbon nano-tube, the mixture of one or more of multi-walled carbon nano-tubes.
Described carbon nano-tube macroscopic body is the precast body that carbon nano-tube fibre or carbon nano-tube fibre consist of.
Describedly contain one or more the mixing that silicon precursor is methylchlorosilane, methyl-monosilane, silicon-containing compound or carbon compound mixture.
The used temperature of described carborundum deposition is 1000-1200 oC.
The used carrier gas of described carborundum deposition is one or more the mixing in hydrogen, argon gas, the nitrogen.
The used air pressure of described carborundum deposition is 10-101 kPa.
The step that the concrete preparation method of the composite of carborundum provided by the invention and CNT comprises:
Carbon nano-tube fibre is processed into the carbon nano-tube macroscopic body of definite shape according to a conventional method as precast body, precast body places between interior two electrodes of electrical heating precipitation equipment, logical argon gas 1-2 h gets rid of the air in the quartz ampoule, opening power, voltage is set to 15-22 V, to precast body energising heating, and control preform temperatures 900-1400 oC, adopt hydrogen, argon gas, nitrogen are carrier gas (flow 20-40 sccm), preferred argon gas, to contain silicon precursor and be written into quartz ampoule, air pressure in the quartz ampoule is 1-101 kPa, and the silicon precursor pyrolysis is deposited on precast body with carborundum, and sedimentation time is 15-45 min, outage is stopped the supple of gas or steam, and naturally cools to room temperature.
The step that the concrete preparation method of the composite of carborundum provided by the invention and CNT comprises:
Carbon nano-tube fibre is processed into according to a conventional method the precast body of determining shape, precast body places between interior two electrodes of electrical heating precipitation equipment, logical argon gas 1-2 h gets rid of the air in the quartz ampoule, opening power, voltage is set to 15-19 V, to precast body energising heating, control preform temperatures 1000-1100 oC, the employing argon gas is carrier gas (flow 20-40 sccm), and trichloromethyl silane is written into quartz ampoule, air pressure in the quartz ampoule is 30-101 kPa, pyrolysis is deposited on precast body with carborundum, and sedimentation time is 15-35 min, outage is stopped the supple of gas or steam, and naturally cools to room temperature.
The present invention utilizes carbon nano-tube macroscopic body to be precast body, by carbon nano-tube fibre being carried out the braiding of various orientations, form the carbon nano-tube macroscopic body of different carbon nanotube architecture, have various content of carbon nanotubes, the composite of specific orientation and homodisperse carborundum and CNT by the chemical vapor deposition of silicon carbide preparation.
Composite of carborundum provided by the invention and CNT and preparation method thereof, adopt chemical vapour deposition technique to form uniform silicon carbide layer in carbon nano tube surface, have the advantages such as the controlled and depositing silicon carbide of reaction is controlled, can regulate and control content and the thickness of carborundum by parameters such as control depositing temperature, time and air pressure, electrical heating can realize the efficient carborundum deposition of Fast Heating as efficient local heating means.Thereby can prepare the composite of various content of carbon nanotubes and homodisperse carborundum and CNT.And can prepare CNT and have the carborundum of various CNTs orientations of the carborundum of unidirectional array and CNT and the composite of CNT.The present invention prepares the composite of carborundum and CNT.That these composites with the carborundum of even silicon carbide layer enveloped carbon nanometer tube structure and CNT have is high-strength, electric-conductivity heat-conductivity high and the performance such as anti-oxidant, can be used as high performance structures conductive heat conducting material and functional material, be used for association area, be expected to especially as high-performance composite materials, be used for the fields such as Aero-Space, defence equipment and function material component.
Description of drawings
Fig. 1 is electrical heating precipitation equipment schematic diagram of the present invention.
Fig. 2 is the optical photograph of example 1 electrical heating carbon nano-tube fibre precast body.
Fig. 3 is the surface sweeping electromicroscopic photograph of example 1 carborundum and carbon nano tube compound material.
Fig. 4 is the surface sweeping electromicroscopic photograph of example 1 carborundum and carbon nano tube compound material.
Fig. 5 is the high magnification stereoscan photograph of example 1 carborundum and carbon nano tube compound material.
Fig. 6 is the infared spectrum of example 1 carborundum and carbon nano tube compound material.
Fig. 7 is the Raman collection of illustrative plates of example 1 carborundum and carbon nano tube compound material.
The specific embodiment
Be further described below in conjunction with embodiment, but do not limit protection scope of the present invention with this:
Fig. 1 electrical heating precipitation equipment schematic diagram, wherein, 1 flowmeter; 2 switches; 3 contain silicon precursor; 4 quartz ampoules; 5 carbon nano-tube macroscopic bodies; 6 graphite electrodes; 7 wires; 8 polytetrafluoro flanges.
The electrical heating precipitation equipment is comprised of reactor, power supply and pipeline.Reactor is that quartz ampoule 4 two ends seal with polytetrafluoro flange 8, and two graphite electrodes 6 are installed at the middle part, are used for fixedly carbon nano-tube macroscopic body 5 and on-load voltage, and electrode connects outside voltage stabilization and current stabilization dc source.Regulate carrier gas flux by flowmeter 1.Infrared radiation thermometer signal receive window aligned carbon nanotubes macroscopic body 5 middle parts are used for monitoring temperature.
According to the chemical gaseous phase spin processes preparation of patent CN101665997A report for the preparation of carborundum and the used carbon nano-tube fibre of carbon nano tube compound material.With approximately 40 and length are 4 cm(diameters ~ 150 μ m) carbon nano-tube fibre forward twists and forms the used precast body (carbon nano-tube macroscopic body) of depositing silicon carbide, and precast body is the rod shape.Precast body is sandwiched between quartz ampoule 4 interior two graphite electrodes 6 of electrical heating precipitation equipment, logical argon gas (160 sccm) 2 h get rid of the air in the quartz ampoule, opening power (YH-1718-5, the voltage stabilization and current stabilization dc source, the large magnificent company in Beijing) voltage is set to 19 V, to precast body energising heating, use infrared radiation thermometer (Raytek-Raynger-3i, range 600-3000 oC, U.S. Lei Tai company) thermometric, infrared radiation thermometer shows that preform temperatures reaches 1100 oC, accompanying drawing 2 is electrical heating precast body optical photographs when reaching depositing temperature, adopt argon gas (40 sccm) as carrier gas trichloromethyl silane to be written into quartz ampoule 4, the air pressure in the quartz ampoule 4 is 101 kPa, and the trichloromethyl silane pyrolysis is deposited on precast body with carborundum, deposit 15 min, outage is stopped the supple of gas or steam, and naturally cools to room temperature, makes the composite of carborundum and CNT.Quality before and after the precast body of the weighing deposition, composite CNT mass fraction is 90%.Observe the composite material surface pattern with ESEM (SEM, TDCLS-4800, Toshiba Corp), material surface is evenly fine and close, such as accompanying drawing 3.High magnification is observed the composite cross section, has a large amount of carborundum to be deposited on tube bank and interbank, such as accompanying drawing 4.Observe composite inner, the nanometer silicon carbide uniform particles is distributed in the CNT interfascicular, and diameter 100-120 nm has also coated carborundum, such as accompanying drawing 5 on the carbon nano-tube bundle.Infrared spectrum (Bio-Rad FTS 6000,400-4000 cm
-1, the Beijing Rayleigh Analytical Instrument Co.,Ltd) and COMPOSITE MATERIALS is at 780 cm
-1There is the Si-C characteristic peak at the place, shows that SiC has deposited to precast body, such as accompanying drawing 6.Raman spectrum (DXR, laser 532 nm, 100-3500 cm
-1, the U.S.) and COMPOSITE MATERIALS is at 813 cm
-1There is the SiC characteristic peak at the place, has further confirmed the existence of SiC, such as accompanying drawing 7.
Embodiment 2:
Adopt the identical method of example 1, turn down voltage, make depositing temperature 1100 oC be reduced to the composite that 1050 oC make carborundum and CNT.It is 0.81 g/cm that drainage records composite density
3
Embodiment 3:
Adopt the identical method of example 1, sedimentation time 15 min are extended for the composite that 35 min make carborundum and CNT.Quality before and after the precast body of the weighing deposition, composite CNT mass fraction is 85%.
Embodiment 4:
Adopt the identical method of example 1, turn down voltage, make depositing temperature 1100 oC be reduced to the composite that 1000 oC make carborundum and CNT.
Embodiment 5:
Adopt the identical method of embodiment 1, the carrier gas argon gas is changed into the composite that hydrogen (20 sccm) makes carborundum and CNT.Carborundum evenly wraps up carbon nano-tube bundle in the composite.
Embodiment 6:
Adopt the identical method of embodiment 5, turn down voltage, make depositing temperature 1100 oC be reduced to the composite that 1050 oC make carborundum and CNT.
Embodiment 7:
Adopt the identical method of embodiment 1, quartz ampoule internal gas pressure 101 kPa are reduced to the composite that 30 kPa make carborundum and CNT.
Embodiment 8:
Adopt the identical method of embodiment 1, quartz ampoule internal gas pressure 101 kPa are reduced to the composite that 10 kPa make carborundum and CNT.
Embodiment 9:
Adopt the identical method of embodiment 5, quartz ampoule internal gas pressure 101 kPa are reduced to the composite that 30 kPa make carborundum and CNT.
Embodiment 10:
Adopt the identical method of embodiment 1, change precast body into composite fibre that carbon nano-tube fibre makes carborundum and CNT.Carborundum evenly wraps up carbon nano-tube fibre.
Embodiment 11:
Adopt the identical method of embodiment 10, the carrier gas argon gas is changed into the composite fibre that hydrogen makes carborundum and CNT.
Embodiment 12:
Adopt the identical method of embodiment 10, quartz ampoule internal gas pressure 101 kPa are reduced to the composite fibre that 30 kPa make carborundum and CNT.
Embodiment 13:
Adopt the identical method of embodiment 10, quartz ampoule internal gas pressure 101 kPa are reduced to the composite fibre that 5 kPa make carborundum and CNT.
Claims (9)
1. the composite of a carborundum and CNT, it is take CNT and contains silicon precursor as raw material, it is characterized in that: in the electrical heating precipitation equipment, carbon nano-tube macroscopic body is precast body, contain silicon precursor by chemical vapor deposition pyrolytic, carborundum is deposited on carbon nano-tube macroscopic body, forms the composite of carborundum and CNT; The mass fraction of CNT can be 0.5-90%.
2. composite according to claim 1 is characterized in that described CNT is Single Walled Carbon Nanotube, double-walled carbon nano-tube, the mixture of one or more of multi-walled carbon nano-tubes.
3. composite according to claim 1 is characterized in that described carbon nano-tube macroscopic body is the precast body that carbon nano-tube fibre or carbon nano-tube fibre consist of.
4. composite according to claim 1 is characterized in that described one or more the mixing that silicon precursor is methylchlorosilane, methyl-monosilane, silicon-containing compound or carbon compound mixture that contains.
5. composite according to claim 1 is characterized in that the used temperature of described carborundum deposition is 1000-1200 oC.
6. composite according to claim 1 is characterized in that the used carrier gas of described carborundum deposition is hydrogen, argon gas, the mixing of one or more in the nitrogen.
7. composite according to claim 1 is characterized in that the used air pressure of described carborundum deposition is 10-101 kPa.
8. composite manufacture method claimed in claim 1, it is characterized in that the step that comprises: carbon nano-tube fibre is processed into carbon nano-tube macroscopic body according to a conventional method as precast body, precast body places between interior two electrodes of electrical heating precipitation equipment, logical argon gas 1-2 h gets rid of the air in the quartz ampoule, opening power, voltage is set to 15-22 V, to precast body energising heating, control preform temperatures 900-1400 oC, adopt hydrogen, argon gas or nitrogen are that carrier gas will contain silicon precursor and be written into quartz ampoule, air pressure in the quartz ampoule is 1-101 kPa, the silicon precursor pyrolysis is deposited on precast body with carborundum, sedimentation time is 15-45 min, and outage is stopped the supple of gas or steam, and naturally cools to room temperature.
9. the composite manufacture method of a carborundum and CNT is characterized in that the step that comprises:
Carbon nano-tube fibre is processed into carbon nano-tube macroscopic body according to a conventional method as precast body, precast body places between interior two electrodes of electrical heating precipitation equipment, logical argon gas 1-2 h gets rid of the air in the quartz ampoule, opening power, voltage is set to 15-19 V, to precast body energising heating, control preform temperatures 1000-1100 oC, the employing argon gas is carrier gas, and trichloromethyl silane is written into quartz ampoule, air pressure in the quartz ampoule is 30-101 kPa, pyrolysis is deposited on precast body with carborundum, and sedimentation time is 15-35 min, outage is stopped the supple of gas or steam, and naturally cools to room temperature.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103911597A (en) * | 2014-04-22 | 2014-07-09 | 武汉理工大学 | Preparation method of silicon carbide film |
| CN105693263A (en) * | 2016-01-14 | 2016-06-22 | 西北工业大学 | Preparing method for carbon nano tube multi-dimensional woven preform and ceramic matrix composite |
| CN105970185A (en) * | 2016-04-22 | 2016-09-28 | 苏州派欧技术咨询服务有限公司 | Preparation method for carbon nanotube-SiC film |
| CN106631079A (en) * | 2016-12-19 | 2017-05-10 | 中国人民解放军国防科学技术大学 | Carbon nano tube silicon carbide composite material and preparation method thereof |
| CN107311685A (en) * | 2017-06-23 | 2017-11-03 | 西北工业大学 | The preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire |
| CN108598377A (en) * | 2018-01-26 | 2018-09-28 | 河北工业大学 | The preparation method of sulphur-silicon carbide doped carbon nano-tube material |
| CN108863434A (en) * | 2017-05-09 | 2018-11-23 | 天津大学 | A kind of high-content carbon nanotube enhancing PRECURSOR-DERIVED CERAMICS composite material and preparation method |
| CN108977795A (en) * | 2017-05-31 | 2018-12-11 | 中国科学院金属研究所 | A kind of device and method for being electrically coupled chemical vapour deposition technique and preparing coat of silicon carbide |
| CN110950323A (en) * | 2019-12-19 | 2020-04-03 | 湖南德智新材料有限公司 | Carbon nanotube-silicon carbide nanowire composite material and preparation method thereof |
| CN113896559A (en) * | 2021-11-19 | 2022-01-07 | 山东建筑大学 | Silicon carbide/carbon nano tube composite material and preparation method thereof |
| CN114436660A (en) * | 2022-02-22 | 2022-05-06 | 合肥工业大学 | Preparation method of carbon nano tube-ceramic composite membrane |
| CN115709996A (en) * | 2022-11-05 | 2023-02-24 | 西北工业大学 | Preparation method of SiC micron tube macroscopic body |
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| CN103911597B (en) * | 2014-04-22 | 2017-01-25 | 武汉理工大学 | Preparation method of silicon carbide film |
| CN103911597A (en) * | 2014-04-22 | 2014-07-09 | 武汉理工大学 | Preparation method of silicon carbide film |
| CN105693263B (en) * | 2016-01-14 | 2018-04-06 | 西北工业大学 | A kind of preparation method of CNT multidimensional braiding precast body ceramic matric composite |
| CN105693263A (en) * | 2016-01-14 | 2016-06-22 | 西北工业大学 | Preparing method for carbon nano tube multi-dimensional woven preform and ceramic matrix composite |
| CN105970185A (en) * | 2016-04-22 | 2016-09-28 | 苏州派欧技术咨询服务有限公司 | Preparation method for carbon nanotube-SiC film |
| CN105970185B (en) * | 2016-04-22 | 2018-05-08 | 太仓派欧技术咨询服务有限公司 | A kind of preparation method of carbon nanotubes-SiC films |
| CN106631079A (en) * | 2016-12-19 | 2017-05-10 | 中国人民解放军国防科学技术大学 | Carbon nano tube silicon carbide composite material and preparation method thereof |
| CN106631079B (en) * | 2016-12-19 | 2019-04-16 | 中国人民解放军国防科学技术大学 | Carbon nanotube composite material of silicon carbide and preparation method thereof |
| CN108863434A (en) * | 2017-05-09 | 2018-11-23 | 天津大学 | A kind of high-content carbon nanotube enhancing PRECURSOR-DERIVED CERAMICS composite material and preparation method |
| CN108977795A (en) * | 2017-05-31 | 2018-12-11 | 中国科学院金属研究所 | A kind of device and method for being electrically coupled chemical vapour deposition technique and preparing coat of silicon carbide |
| CN108977795B (en) * | 2017-05-31 | 2021-01-12 | 中国科学院金属研究所 | Device and method for preparing silicon carbide coating by using electric coupling chemical vapor deposition method |
| CN107311685A (en) * | 2017-06-23 | 2017-11-03 | 西北工业大学 | The preparation method of electrophoresis and thermal evaporation techniques fabricated in situ refractory carbide nano wire |
| CN107311685B (en) * | 2017-06-23 | 2020-05-12 | 西北工业大学 | Preparation method for in-situ synthesis of refractory metal carbide nanowires by electrophoresis and thermal evaporation technology |
| CN108598377A (en) * | 2018-01-26 | 2018-09-28 | 河北工业大学 | The preparation method of sulphur-silicon carbide doped carbon nano-tube material |
| CN108598377B (en) * | 2018-01-26 | 2020-05-12 | 河北工业大学 | Preparation method of sulfur-silicon carbide doped carbon nanotube material |
| CN110950323A (en) * | 2019-12-19 | 2020-04-03 | 湖南德智新材料有限公司 | Carbon nanotube-silicon carbide nanowire composite material and preparation method thereof |
| CN113896559A (en) * | 2021-11-19 | 2022-01-07 | 山东建筑大学 | Silicon carbide/carbon nano tube composite material and preparation method thereof |
| CN114436660A (en) * | 2022-02-22 | 2022-05-06 | 合肥工业大学 | Preparation method of carbon nano tube-ceramic composite membrane |
| CN115709996A (en) * | 2022-11-05 | 2023-02-24 | 西北工业大学 | Preparation method of SiC micron tube macroscopic body |
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