CN108751159A - A kind of compound carbon foam of CVI-SiC nano wires enhancing - Google Patents
A kind of compound carbon foam of CVI-SiC nano wires enhancing Download PDFInfo
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- CN108751159A CN108751159A CN201810591706.8A CN201810591706A CN108751159A CN 108751159 A CN108751159 A CN 108751159A CN 201810591706 A CN201810591706 A CN 201810591706A CN 108751159 A CN108751159 A CN 108751159A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/90—Carbides
- C01B32/914—Carbides of single elements
- C01B32/956—Silicon carbide
- C01B32/963—Preparation from compounds containing silicon
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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Abstract
The present invention, which is a kind of CVI-SiC nano wires, enhances compound carbon foam and preparation method thereof, it is made of three-dimensional netted carbon foam and the SiC nanowire being grown in carbon foam, the steep that wall section of the carbon foam is round, ellipse or triangle, its porosity 95~99.5%, 10-50 μm of pore size；The SiC nanowire is that the tip of purity >=99% carries the beta-SiC nano-wire of metal ball, 10~80nm of nanowire diameter, and length is 0.5~50 μm.The advantages that composite foam has density low, and large specific surface area, temperature tolerance is good, and crushing resistance is good, can be used for ultracapacitor, energy storage material, catalyst carrier etc..
Description
Technical field
The present invention relates to a kind of carbon foams, enhance compound carbon foam material more particularly to a kind of CVI-SiC nano wires
Material and preparation method thereof.
Background technology
It is light porous with tridimensional network that carbon foam is that a kind of hole steep that wall steeped and be connected with each other by hole is formed
Material.Other than the traditional performance with carbon material, also have density is small, intensity is high, anti-thermal shock, it is anti-oxidant and it is good every
Heat inhales the physical and chemical properties such as wave.It can be widely applied to energy storage, aerospace, shipping industry, communication electronics work
Many technical fields such as industry, building field.Nowadays carbon foam mainly uses pitch, mesophase pitch, coal, thermosetting resin etc.
It as raw material, is prepared using sintered and foamed method and atmosphere protection pyrolysismethod, and controls it by controlling technique and be graphitized journey
It spends to realize the heat-insulated and heat conduction of carbon foam.But since carbon foam antioxygenic property is poor, can not use under hot environment again, it is more
Nian Lai prepares carbon foam to thermosetting resin both at home and abroad and enters deeper research again.
The Chinese patent of Patent No. ZL200680056163.5 provides a kind of composite foam, by two kinds of Material claddings
It forms, one of which is the carbon foam material comprising porous network and multiple discontinuity surfaces；Another kind is to be deposited on carbon foam
Multiple discontinuity surfaces of material it is at least some on the second material.The carbon foam structure can be used for lead-acid battery, inhibit electricity
Pole is damaged, and battery life is improved.
The Chinese patent of Patent No. ZL201510018971.3 provides a kind of silicon carbide foam ceramic material, the foam
Ceramic material indicates by mass percentage, including silicon carbide micro-powder 40%~60%, hydrogen peroxide 4%~10%, calcium carbonate are micro-
Powder 5%~15%, polyvinyl alcohol 3%~6% and Ludox 5%~15%.It can be seen that silicon carbide purity is low, it is unable to give full play carbon
Every excellent properties of SiClx.
The Chinese patent of Patent No. ZL201410743407.3 provides a kind of high temperature resistance and high strength SiC claddings carbon foam
Composite heat-insulated material and preparation method thereof, the carbon foam composite heat-insulated material are made of carbon foam and carbonization silica aerogel.This is multiple
The apparent density for closing foam is 0.4~0.6g/cm3, compression strength is 11~15MPa, and room temperature thermal conductivity is in 0.4~0.6W/
(m·K).The prepared composite foam heat-barrier material has anti-oxidant, and temperature tolerance is good, while its materials is simple and technique is simple and direct
The advantages of, and technical process is easy to operate, large-scale production easy to implement.
Application No. is the Chinese patents of CN201710604378.6 to provide a kind of three-dimensional CVD carbonizations with hollow member
Silicon ceramic foam material, β-three-dimensional netted skeleton of type silicon carbide by purity higher than 99% are constituted, 1~20 μ of skeleton radial dimension
M, draw ratio are 5~10, and the voidage of the ceramic foam is 90~99.5%, and three-dimensional netted pore size is 10~100 μm, carbon
SiClx skeleton is in hollow form, constitutes pore passage structure, and duct cross sectional shape is round, ellipse or triangle, and size is 0.5~
10 μm, silicon carbide skeleton wall thickness is 0.1~10 μm.The material gap rate is high, and density is low, can be used for ultracapacitor, also can be used for
Catalytic industries, while material can use under high temperature environment.
The present invention prepares CVI-SiC nano wires using CVI techniques enhances compound carbon foam, and prepared enhancing is compound
SiC nanowire rule is filled in inside abscess and supports foam structure in carbon foam, and obtained compound carbon foam is close
Spend low, skeleton is elongated and structure uniform, controllable, has excellent specific property.
Invention content
The technical solution adopted to achieve the purpose of the present invention is a kind of compound carbon foam material of CVI-SiC nano wires enhancing
Material and preparation method thereof, it is characterised in that be made of three-dimensional netted carbon foam and the SiC nanowire being grown in carbon foam, carbon
The steep that wall section of foam is round, ellipse or triangle, and size is 1-10 μm, and the porosity of carbon foam is 95~99.5%,
The pore size of carbon foam is 10-50 μm, and draw ratio is 5~20, and compressive strength is 20~50kPa；The SiC nanowire is point
Beta-SiC nano-wire of the end with metal ball, purity >=99%, a diameter of 10~80nm of nano wire, length are 0.5~50 μm.
The CVI-SiC nano wires enhance the preparation method of compound carbon foam, it is characterised in that including suitable below
Sequence step：
(1) it is configured to the catalyst solution that molar concentration is 0.001~0.5mol/L using ethyl alcohol and catalyst；
(2) carbon foam is sequentially placed into acetone and ethyl alcohol to drying at room temperature after carrying out 10~20min of ultrasonic cleaning；
(3) by the carbon foam after cleaning in step (2) be put into dipping 5 in the catalyst solution prepared by step (1)~
After 60min, at 30~80 DEG C dry 5~for 24 hours, be made supported catalyst carbon foam；
(4) carbon foam of supported catalyst in step (3) is put into CVI stoves, and after being evacuated to 0.1MPa pressure, to anti-
It answers and is passed through reaction source gas in stove, at a temperature of 800~1300 DEG C, CVI-SiC nano wires are grown in carbon foam；Wherein, instead
Answer source gas for argon gas, hydrogen, trichloromethyl silane mixed gas, argon gas: hydrogen: the ratio of trichloromethyl silane is 10:
0.1~10: 0.01~5；
(5) after reacting 0.5~10h under the conditions of step (4), source gas is closed, and after cooling to room temperature with the furnace, be made
CVI-SiC nano wires enhance compound carbon foam.
The density that the prepared CVI-SiC nano wires obtained of the step (5) enhance compound carbon foam is 5~20mg/
cm3, SiC mass fractions are 10~30%, and compressive strength is 0.4~0.8MPa.
Present invention has the advantages that (1) enhances the low (5~20mg/cm of density of compound carbon foam3), crushing resistance significantly carries
It is high；(2) material can be used for ultracapacitor, and the porous compound skeleton structure that nano wire interlocks can store energy particle,
Greatly improve energy storage efficiency；(3) material makes it have the ratio table of superelevation due to nano wire and the compound skeleton structure of carbon
Area also can be used for catalytic industries.
Description of the drawings
Fig. 1, which is a kind of CVI-SiC nano wires, enhances compound carbon foam shape appearance figure.
Specific implementation mode
With reference to specific embodiment, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate the present invention
Rather than limit the scope of the invention, after having read the present invention, various equivalences of the those skilled in the art to the present invention
It is as defined in the appended claims that the modification of form falls within the application.
Embodiment 1
Compound carbon foam of a kind of CVI-SiC nano wires enhancing and preparation method thereof, it is characterised in that by three-dimensional netted
Carbon foam and the SiC nanowire that is grown in carbon foam constitute, the steep that wall section of carbon foam is triangle, and size is 5 μm, carbon
The porosity of foam is 95%, and the pore size of carbon foam is 15 μm, draw ratio 20, compressive strength 30kPa；The SiC
Nano wire is the beta-SiC nano-wire that tip carries metal ball, and purity >=99%, a diameter of 10nm of nano wire, length is 15 μm.
The CVI-SiC nano wires enhance the preparation method of compound carbon foam, it is characterised in that including suitable below
Sequence step：
(1) it is configured to the catalyst solution that molar concentration is 0.5mol/L using ethyl alcohol and catalyst；
(2) carbon foam is sequentially placed into acetone and ethyl alcohol to drying at room temperature after carrying out ultrasonic cleaning 10min；
(3) carbon foam after cleaning in step (2) is put into the catalyst solution prepared by step (1) and impregnates 50min
Afterwards, 5h is dried at 80 DEG C, the carbon foam of supported catalyst is made；
(4) carbon foam of supported catalyst in step (3) is put into CVI stoves, and after being evacuated to 0.1MPa pressure, to anti-
It answers and is passed through reaction source gas in stove, at a temperature of 1300 DEG C, CVI-SiC nano wires are grown in carbon foam；Wherein, reaction source gas
Body is argon gas, hydrogen, trichloromethyl silane mixed gas, argon gas: hydrogen: the ratio of trichloromethyl silane is 10: 10: 5；
(5) under the conditions of step (4) after reaction 0.5, source gas is closed, and after cooling to room temperature with the furnace, CVI-SiC is made
Nano wire enhances compound carbon foam.
The density that the prepared CVI-SiC nano wires obtained of the step (5) enhance compound carbon foam is 8mg/cm3,
SiC mass fractions are 30%, compressive strength 0.7MPa.
Embodiment 2
Compound carbon foam of a kind of CVI-SiC nano wires enhancing and preparation method thereof, it is characterised in that by three-dimensional netted
Carbon foam and the SiC nanowire that is grown in carbon foam constitute, the steep that wall section of carbon foam is circle, and size is 5 μm, carbon bubble
The porosity of foam is 95.5%, and the pore size of carbon foam is 30 μm, draw ratio 5, compressive strength 30kPa；The SiC receives
Rice noodles are the beta-SiC nano-wire that tip carries metal ball, and purity >=99%, a diameter of 20nm of nano wire, length is 35 μm.
The CVI-SiC nano wires enhance the preparation method of compound carbon foam, it is characterised in that including suitable below
Sequence step：
(1) it is configured to the catalyst solution that molar concentration is 0.05mol/L using ethyl alcohol and catalyst；
(2) carbon foam is sequentially placed into acetone and ethyl alcohol to drying at room temperature after carrying out ultrasonic cleaning 20min；
(3) by the carbon foam after cleaning in step (2) be put into dipping 5 in the catalyst solution prepared by step (1)~
After 60min, is dried at 80 DEG C for 24 hours, the carbon foam of supported catalyst is made；
(4) carbon foam of supported catalyst in step (3) is put into CVI stoves, and after being evacuated to 0.1MPa pressure, to anti-
It answers and is passed through reaction source gas in stove, at a temperature of 1200 DEG C, CVI-SiC nano wires are grown in carbon foam；Wherein, reaction source gas
Body is argon gas, hydrogen, trichloromethyl silane mixed gas, argon gas: hydrogen: the ratio of trichloromethyl silane is 10: 8: 0.5；
(5) after reacting 0.5~10h under the conditions of step (4), source gas is closed, and after cooling to room temperature with the furnace, be made
CVI-SiC nano wires enhance compound carbon foam.
The density that the prepared CVI-SiC nano wires obtained of the step (5) enhance compound carbon foam is 10mg/cm3,
SiC mass fractions are 25%, compressive strength 0.75MPa.
Two specific implementation modes of the invention are above are only, but the design concept of the present invention is not limited thereto, all utilizations
This design carries out the present invention change of unsubstantiality, should all belong to the behavior for invading the scope of protection of the invention.In every case it is not
It is detached from the content of technical solution of the present invention, according to the technical essence of the invention to any type of simple made by above example
Modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (3)
1. a kind of CVI-SiC nano wires enhance compound carbon foam, by three-dimensional netted carbon foam and it is grown in carbon foam
SiC nanowire constitute, the steep that wall section of carbon foam is round, ellipse or triangle, and size is 1-10 μm, the hole of carbon foam
Gap rate is 95~99.5%, and the pore size of carbon foam is 10-50 μm, and draw ratio is 5~20, and compressive strength is 20~50kPa；
The SiC nanowire be tip carry metal ball beta-SiC nano-wire, purity >=99%, a diameter of 10~80nm of nano wire,
Length is 0.5~50 μm.
2. a kind of CVI-SiC nano wires enhance the preparation method of compound carbon foam, it is characterised in that walked including following sequence
Suddenly：
(1) it is configured to the catalyst solution that molar concentration is 0.001~0.5mol/L using ethyl alcohol and catalyst；
(2) carbon foam is sequentially placed into acetone and ethyl alcohol to drying at room temperature after carrying out 10~20min of ultrasonic cleaning；
(3) carbon foam after cleaning in step (2) is put into 5~60min of dipping in the catalyst solution prepared by step (1)
Afterwards, at 30~80 DEG C drying 5~for 24 hours, be made supported catalyst carbon foam；
(4) carbon foam of supported catalyst in step (3) is put into CVI stoves, and after being evacuated to 0.1MPa pressure, to reacting furnace
It is inside passed through reaction source gas, at a temperature of 800~1300 DEG C, CVI-SiC nano wires are grown in carbon foam；Wherein, reaction source
Gas is argon gas, hydrogen, trichloromethyl silane mixed gas, argon gas: hydrogen: the ratio of trichloromethyl silane is 10: 0.1~10
: 0.01~5；
(5) after reacting 0.5~10h under the conditions of step (4), source gas is closed, and after cooling to room temperature with the furnace, CVI- is made
SiC nanowire enhances compound carbon foam.
3. according to claim 2, which is characterized in that the prepared CVI-SiC nano wires obtained enhance compound carbon foam
Density be 5~20mg/cm3, SiC mass fractions are 10~30%, and compressive strength is 0.4~0.8MPa.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810591706.8A CN108751159A (en) | 2018-05-27 | 2018-05-27 | A kind of compound carbon foam of CVI-SiC nano wires enhancing |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354022A (en) * | 2018-11-29 | 2019-02-19 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of the high ultralong SiC nanowires of crystallinity |
| CN110065944A (en) * | 2019-04-19 | 2019-07-30 | 苏州宏久航空防热材料科技有限公司 | A kind of method that CVD silicon carbide coating and ultra-long silicon carbide nano-wires are prepared jointly |
| CN111875921A (en) * | 2020-07-14 | 2020-11-03 | 苏州宏久航空防热材料科技有限公司 | High-performance electromagnetic shielding material based on 5G and preparation method thereof |
| CN112144039A (en) * | 2020-09-15 | 2020-12-29 | 西北工业大学 | Method for preparing 3D (three-dimensional) reticular silicon carbide nanowires through nickel-carbon foam |
| CN112457034A (en) * | 2020-11-10 | 2021-03-09 | 中钢南京环境工程技术研究院有限公司 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
| CN113046718A (en) * | 2021-03-09 | 2021-06-29 | 西北工业大学 | Silicon carbide nano heat-insulation wave-absorbing composite material and preparation method thereof |
| CN114276163A (en) * | 2022-01-25 | 2022-04-05 | 西安交通大学 | High-temperature-resistant light high-strength porous ceramic and preparation method thereof |
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| CN103724046A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | SiC foam and preparation method thereof |
| CN105237034A (en) * | 2015-09-11 | 2016-01-13 | 西北工业大学 | Method for preparing porous silicon carbide ceramic based on template |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
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| CN103724046A (en) * | 2013-09-11 | 2014-04-16 | 太仓派欧技术咨询服务有限公司 | SiC foam and preparation method thereof |
| CN105237034A (en) * | 2015-09-11 | 2016-01-13 | 西北工业大学 | Method for preparing porous silicon carbide ceramic based on template |
| CN106747628A (en) * | 2017-02-22 | 2017-05-31 | 南京航空航天大学 | A kind of high temperature resistant foam strengthens SiO2Aerogel insulating material and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109354022A (en) * | 2018-11-29 | 2019-02-19 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of the high ultralong SiC nanowires of crystallinity |
| CN110065944A (en) * | 2019-04-19 | 2019-07-30 | 苏州宏久航空防热材料科技有限公司 | A kind of method that CVD silicon carbide coating and ultra-long silicon carbide nano-wires are prepared jointly |
| CN111875921A (en) * | 2020-07-14 | 2020-11-03 | 苏州宏久航空防热材料科技有限公司 | High-performance electromagnetic shielding material based on 5G and preparation method thereof |
| CN112144039A (en) * | 2020-09-15 | 2020-12-29 | 西北工业大学 | Method for preparing 3D (three-dimensional) reticular silicon carbide nanowires through nickel-carbon foam |
| CN112457034A (en) * | 2020-11-10 | 2021-03-09 | 中钢南京环境工程技术研究院有限公司 | Preparation method of C/SiC composite material with vibrissa-nostril-like structure |
| CN113046718A (en) * | 2021-03-09 | 2021-06-29 | 西北工业大学 | Silicon carbide nano heat-insulation wave-absorbing composite material and preparation method thereof |
| CN113046718B (en) * | 2021-03-09 | 2022-07-22 | 西北工业大学 | Silicon carbide nano heat-insulation wave-absorbing composite material and preparation method thereof |
| CN114276163A (en) * | 2022-01-25 | 2022-04-05 | 西安交通大学 | High-temperature-resistant light high-strength porous ceramic and preparation method thereof |
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