CN105970185A - Preparation method for carbon nanotube-SiC film - Google Patents
Preparation method for carbon nanotube-SiC film Download PDFInfo
- Publication number
- CN105970185A CN105970185A CN201610281612.1A CN201610281612A CN105970185A CN 105970185 A CN105970185 A CN 105970185A CN 201610281612 A CN201610281612 A CN 201610281612A CN 105970185 A CN105970185 A CN 105970185A
- Authority
- CN
- China
- Prior art keywords
- carbon nanotube
- hydrogen
- nanotube powder
- preparation
- argon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention provides a preparation method for a carbon nanotube-SiC film. The preparation method comprises the following steps of placing a transition metal substrate and carbon nanotube powder in a vacuum reaction system, wherein the particle size of the carbon nanotube powder is 10-20 nanometers; adopting argon to be the carrier gas of the carbon nanotube powder and the carrier gas of trichloromethylsilane, using hydrogen as reaction gas, under the situation that oxygen in a vacuum cavity is removed, maintaining the indoor vacuum degree to be 1-1000 Pa, performing heating to 800-1200 DEG C, and injecting the hydrogen into the vacuum cavity, wherein the flow capacity of the hydrogen is 100-500mL/min; separately injecting the argon loaded with the carbon nanotube powder and the argon loaded with the trichloromethylsilane into the vacuum cavity, wherein the flow capacity of the argon loaded with the carbon nanotube powder is 10-100 ml/min, the flow capacity of the argon loaded with the trichloromethylsilane is 100-500ml/min, and the feeding speed of the carbon nanotube powder is 10-100 mg/min; and maintaining the flow capacity of the hydrogen, and performing heat preservation for 1-5 h, wherein the cooling rate is 5-20 DEG C/min. The preparation method disclosed by the invention has the main beneficial effects that the high-temperature oxidation resistance and the ablation resistance of a SiC film are improved.
Description
Technical field
The present invention relates to the preparation method of a kind of SiC thin film, particularly relate to the preparation method of a kind of CNT-SiC thin film.
Background technology
CNT has good mechanical property, and CNTs tensile strength reaches 50～200GPa, is 100 times of steel, and density is but only
Have the 1/6 of steel, at least higher an order of magnitude than ordinary graphite fiber；Its elastic modelling quantity is up to 1TPa, with the springform of diamond
Amount is suitable, about 5 times of steel.The hardness of CNT is suitable with diamond, but has good pliability, can stretch.
In industrially conventional enhanced fiber, determine that a key factor of intensity is draw ratio, i.e. length and diameter ratio.
At aerospace field, coat of silicon carbide is utilized as the high temperature coating of material with carbon element and carbon/carbon composite, opposing
The combustion gas stream of 2500-3000 DEG C, shows excellent antioxidation, anti-yaw damper feature.The fusing point of CNT is in known materials simultaneously
In be the highest, therefore at aerospace field, there is the highest practical value.
Patent application publication number a kind of carbon/carbon composite SiC/ZrB2-SiC/SiC that has been the disclosure of the invention of CN 102417375 A
Coating and preparation method thereof.Including undercoating, external coating and inter coat, internally coated thickness is 20～50 μm, outer painting
The thickness of layer is 30～80 μm, and the thickness of inter coat is 50～80 μm.Send out method by embedding and prepare SiC undercoating,
Reduce the thermal stress of intermediate layer ZrB2-SiC and C/C composite.Prepared in the middle of ZrB2-SiC by Supersonic Plasma Spraying
Layer, ZrB2-SiC provides good high temperature ablation, middle low temperature antioxidation and heat-proof quality for C/C composite.By deposition
Method prepares SiC external coating, and effectively healing coating surface defect, stops the infiltration of oxygen, provides good for C/C composite
High-temperature oxydation is protected.Simultaneously in middle low temperature oxidization process, the oxidation product B 2O3 of ZrB2 can effectively heal the defect in coating,
Good middle temperature oxidation protection is provided for coating sample.
Patent application publication number a kind of SiC/Ta/C/Ta/SiC that has been the disclosure of the invention of CN 103722849 A
Multilayer antioxidant high-temperaure coating and preparation method thereof.It is made up of SiC layer, Ta layer and C layer laminate, it is characterised in that lamination
Order be followed successively by SiC layer, Ta layer, C layer, Ta layer, SiC layer, circulate 1～3 time, C layer both sides are Ta layer,
Innermost layer and outermost layer are SiC layer, are sequentially depositing Ta layer, C by chemical vapour deposition technique in prepared SiC layer
Layer, Ta layer and SiC layer, obtain SiC/Ta/C/Ta/SiC multilayer anti-oxidation high-temperaure coating.Outer layer SiC
In high temperature aerobic environment, form one layer of SiO2 film, can effectively stop the diffusion of oxygen atom, simultaneously connecing at Ta layer and C layer
Contacting surface, can form TaC layer and improve antioxygenic property further.The alternating deposit of coating can effectively alleviate thermal expansion between coating
Difference of coefficients, is remarkably improved the thermal shock performance of coating, by control sedimentation time and frequency of depositing can control matrix thickness and
The number of plies, can realize the control to composite coating microstructure.
Summary of the invention
The purpose of the present invention is intended to improve the high-temperature oxidation resistant of SiC thin film, anti-yaw damper performance, it is provided that one can be effectively improved matrix
Surface high-temp antioxidation, the preparation method of CNT-SiC thin film of anti-yaw damper performance.
For realizing the purpose of the present invention, be the technical scheme is that the preparation method of a kind of CNT-SiC thin film, it is special
Levying and be to be placed in vacuum response system transition metal substrate and carbon nanotube dust, carbon nanotube powder particle size is 10 to receive
Rice-20 nanometers, use argon respectively as carbon nanotube dust gas carrier and trichloromethyl silane gas carrier, and hydrogen is as reaction
Gas, in removing vacuum chamber in the case of oxygen, maintains house vacuum degree 1-1000Pa, and is warming up to 800-1200 DEG C, will
Hydrogen injects in vacuum chamber, and flow is 100-500mL/min, will be loaded with the argon of carbon nanotube powder and trichloromethyl silane respectively
Gas is passed through in vacuum chamber, and flow is respectively 10-100ml/min and 100-500ml/min, and carbon nanotube powder feed speed is
10-100mg/min, keeps hydrogen flowing quantity simultaneously, is incubated 1-5h, and rate of temperature fall is 5-20 DEG C/min.
Beneficial effects of the present invention: 1. technique is simple, can realize large area deposition；2. the carbon nano-tube film prepared by has superelevation
High-temperature oxidation resistant and anti-yaw damper performance；3. the carbon nano-tube film prepared by, while hardness strength is higher, has higher
Toughness 4. has preferable heat conductivility.
Detailed description of the invention
Below in conjunction with specific embodiment, it is further elucidated with the present invention, it should be understood that these embodiments are merely to illustrate the present invention and need not
In limiting the scope of the present invention, after having read the present invention, those skilled in the art repair the various equivalent form of values of the present invention
Change and all fall within the application claims and limited.
Embodiment 1
The preparation method of a kind of CNT-SiC thin film, it is characterised in that transition metal substrate and carbon nanotube dust are placed in very
In empty response system, carbon nanotube powder particle size is 10 nanometers, use argon respectively as carbon nanotube dust gas carrier and
Trichloromethyl silane gas carrier, hydrogen, as reacting gas, in removing vacuum chamber in the case of oxygen, maintains house vacuum degree
1Pa, and it is warming up to 800 DEG C, hydrogen being injected in vacuum chamber, flow is 100mL/min, will be loaded with carbon nanotube powder respectively
Being passed through in vacuum chamber with the argon gas of trichloromethyl silane, flow is respectively 10ml/min and 100ml/min, carbon nanotube powder
Feed speed is 10mg/min, keeps hydrogen flowing quantity simultaneously, is incubated 1h, and rate of temperature fall is 5 DEG C/min.
Prepared carbon nano-tube film has high-temperature oxidation resistant and the anti-yaw damper performance of superelevation；While hardness strength is higher,
There is higher toughness, there is preferable heat conductivility.
Embodiment 2
The preparation method of a kind of CNT-SiC thin film, it is characterised in that transition metal substrate and carbon nanotube dust are placed in very
In empty response system, carbon nanotube powder particle size is 20 nanometers, use argon respectively as carbon nanotube dust gas carrier and
Trichloromethyl silane gas carrier, hydrogen, as reacting gas, in removing vacuum chamber in the case of oxygen, maintains house vacuum degree
1000Pa, and it is warming up to 1200 DEG C, hydrogen being injected in vacuum chamber, flow is 500mL/min, will be loaded with CNT respectively
The argon gas of powder and trichloromethyl silane is passed through in vacuum chamber, and flow is respectively 100ml/min and 500ml/min, carbon nanometer
Pipe powder feed speed is 100mg/min, keeps hydrogen flowing quantity simultaneously, is incubated 5h, and rate of temperature fall is 20 DEG C/min.
Prepared carbon nano-tube film has high-temperature oxidation resistant and the anti-yaw damper performance of superelevation；While hardness strength is higher,
There is higher toughness, there is preferable heat conductivility.
Above are only two detailed description of the invention of the present invention, but the design concept of the present invention is not limited thereto, all utilize this structure
Think the present invention is carried out the change of unsubstantiality, the behavior invading the scope of protection of the invention all should be belonged to.In every case it is without departing from this
The content of inventive technique scheme, any type of simple modification above example made according to the technical spirit of the present invention, etc.
With change and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (1)
1. the preparation method of a CNT-SiC thin film, it is characterised in that transition metal substrate and carbon nanotube dust are placed in
In vacuum response system, carbon nanotube powder particle size is 10 nanometer-20 nanometers, uses argon respectively as carbon nanotube powders
Body gas carrier and trichloromethyl silane gas carrier, hydrogen, as reacting gas, in removing vacuum chamber in the case of oxygen, maintains
House vacuum degree 1-1000Pa, and it is warming up to 800-1200 DEG C, hydrogen being injected in vacuum chamber, flow is 100-500mL/min,
Being passed through in vacuum chamber by the argon gas being loaded with carbon nanotube powder and trichloromethyl silane respectively, flow is respectively 10-100ml/min
And 100-500ml/min, carbon nanotube powder feed speed is 10-100mg/min, keeps hydrogen flowing quantity simultaneously, is incubated 1-5h,
Rate of temperature fall is 5-20 DEG C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610281612.1A CN105970185B (en) | 2016-04-22 | 2016-04-22 | A kind of preparation method of carbon nanotubes-SiC films |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610281612.1A CN105970185B (en) | 2016-04-22 | 2016-04-22 | A kind of preparation method of carbon nanotubes-SiC films |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105970185A true CN105970185A (en) | 2016-09-28 |
| CN105970185B CN105970185B (en) | 2018-05-08 |
Family
ID=56993505
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610281612.1A Active CN105970185B (en) | 2016-04-22 | 2016-04-22 | A kind of preparation method of carbon nanotubes-SiC films |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105970185B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107354447A (en) * | 2017-07-24 | 2017-11-17 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of low heat conduction boron nitride carborundum films |
| CN109594060A (en) * | 2018-10-19 | 2019-04-09 | 中国科学院上海应用物理研究所 | A kind of preparation method of fine grain silicon carbide clad |
| 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 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834287A (en) * | 2005-03-18 | 2006-09-20 | 西北工业大学 | Method of preparing carbon-carbon composite material surface silicon carbide nano wire |
| CN103061112A (en) * | 2012-12-05 | 2013-04-24 | 天津大学 | Composite material of silicon carbide and carbon nanotube and preparation method thereof |
| JP2014114509A (en) * | 2012-12-06 | 2014-06-26 | Industry-Academic Cooperation Foundation Yonsei Univ | FORMATION METHOD AND DEVICE OF C/SiC INCLINATION COATING FILM |
| CN104150939A (en) * | 2014-07-24 | 2014-11-19 | 西北工业大学 | Preparation method of electrophoretic deposition CNTs (carbon nano tubes) reinforced ceramic matrix composite material |
-
2016
- 2016-04-22 CN CN201610281612.1A patent/CN105970185B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834287A (en) * | 2005-03-18 | 2006-09-20 | 西北工业大学 | Method of preparing carbon-carbon composite material surface silicon carbide nano wire |
| CN103061112A (en) * | 2012-12-05 | 2013-04-24 | 天津大学 | Composite material of silicon carbide and carbon nanotube and preparation method thereof |
| JP2014114509A (en) * | 2012-12-06 | 2014-06-26 | Industry-Academic Cooperation Foundation Yonsei Univ | FORMATION METHOD AND DEVICE OF C/SiC INCLINATION COATING FILM |
| CN104150939A (en) * | 2014-07-24 | 2014-11-19 | 西北工业大学 | Preparation method of electrophoretic deposition CNTs (carbon nano tubes) reinforced ceramic matrix composite material |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107354447A (en) * | 2017-07-24 | 2017-11-17 | 苏州宏久航空防热材料科技有限公司 | A kind of preparation method of low heat conduction boron nitride carborundum films |
| CN109594060A (en) * | 2018-10-19 | 2019-04-09 | 中国科学院上海应用物理研究所 | A kind of preparation method of fine grain silicon carbide clad |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105970185B (en) | 2018-05-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6446175B2 (en) | Thermal spray coated reinforced polymer composites | |
| Yang et al. | High-temperature protective coatings for C/SiC composites | |
| CN103567374B (en) | Coating material for aluminium die casting and the method for preparing the coating material | |
| Xiong et al. | HfC/ZrC ablation protective coating for carbon/carbon composites | |
| Wang et al. | Preparation and ablation properties of Hf (Ta) C co-deposition coating for carbon/carbon composites | |
| Lee et al. | Ablation characteristics of carbon fiber reinforced carbon (CFRC) composites in the presence of silicon carbide (SiC) coating | |
| Li et al. | SiC nanowires toughed HfC ablative coating for C/C composites | |
| CN105970185A (en) | Preparation method for carbon nanotube-SiC film | |
| CN103952660B (en) | Composite material with a nitride film as well as preparation method and application of composite material | |
| CN102277560A (en) | Method for improving oxidation resistance of graphite electrode by obtaining SiC/C gradient surface coating through chemical vapor deposition | |
| Li et al. | Improving the oxidation resistance of carbon/carbon composites at low temperature by controlling the grafting morphology of carbon nanotubes on carbon fibres | |
| Yin et al. | Cold-sprayed metal coatings with nanostructure | |
| Shan et al. | Improvement of the bonding strength and the oxidation resistance of SiC coating on C/C composites by pre-oxidation treatment | |
| CN104150938B (en) | The preparation method of one dimension hafnium carbide HfC material modification carbon/carbon composite | |
| CN103722785B (en) | A kind of porous C/C is the preparation method of the lightweight anti-oxidation materials structure of liner | |
| CN106319518B (en) | Diamond/metal carbides composite coating and its preparation method and application | |
| Qiang et al. | Oxidation resistance of SiC nanowires reinforced SiC coating prepared by a CVD process on SiC‐coated C/C composites | |
| CN106915975A (en) | The preparation method of carbon materials surface SiC-C coatings in graphite heater stove | |
| JP6110852B2 (en) | Carbon material with thermal spray coating | |
| Zhang et al. | Oxidation behaviors of C–ZrB2–SiC composite at 2100 C in air and O2 | |
| CN107354447A (en) | A kind of preparation method of low heat conduction boron nitride carborundum films | |
| Peng et al. | Effect of traceable nitrogen from low-pressure plasma nitriding on diamond growth over WC-co cemented carbides | |
| Kim et al. | Thermal shock resistance of TaC/SiC coatings on carbon/carbon composites by the CVD process | |
| Zhu et al. | Oxidation behavior of titanium carbonitride coating deposited by atmospheric plasma spray synthesis | |
| EP2933353B1 (en) | Method for producing fiber-reinforced composites |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 215400 No. 162 Renmin South Road, Jiangsu, Taicang Applicant after: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. Address before: 215400 No. 162 Renmin South Road, Jiangsu, Taicang Applicant before: Suzhou Oupai Technology Consulting Services Co., Ltd. |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Chen Zhaofeng Inventor after: Pan Ying Inventor after: Yu Shengjie Inventor after: Wang Yang Inventor before: Chen Zhaofeng Inventor before: Pan Ying Inventor before: Wang Yang Inventor before: Yu Shengjie |
|
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20180612 Address after: 215400 No. 162 Renmin South Road, Chengxiang Town, Taicang City, Suzhou, Jiangsu Patentee after: Suzhou Hongjiu Aviation Heat Proof Materials Technology Co., Ltd. Address before: 215400 people south road, Taicang, Jiangsu Province, No. 162 Patentee before: TAICANG PAIOU TECHNOLOGY CONSULTATION SERVICE CO., LTD. |