CN115896737A - High-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and preparation method thereof - Google Patents
High-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and preparation method thereof Download PDFInfo
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical group [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 77
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 75
- 239000000835 fiber Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 33
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims description 60
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 56
- 229910052786 argon Inorganic materials 0.000 claims description 28
- 229910052721 tungsten Inorganic materials 0.000 claims description 22
- 239000010937 tungsten Substances 0.000 claims description 22
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 16
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 16
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000012495 reaction gas Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 9
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 8
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005086 pumping Methods 0.000 claims description 7
- 238000004804 winding Methods 0.000 claims description 7
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 238000000151 deposition Methods 0.000 abstract description 14
- 238000000576 coating method Methods 0.000 abstract description 13
- 239000011248 coating agent Substances 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- 230000008021 deposition Effects 0.000 description 13
- 239000011358 absorbing material Substances 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 5
- 238000011161 development Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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Abstract
The invention provides a high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and a preparation method thereof, belonging to the technical field of materials. Depositing a carbon layer with a certain thickness between the tungsten core and the silicon carbide coating by a direct chemical vapor deposition method to prepare the tungsten/carbon core silicon carbide fiber. The tungsten/carbon core silicon carbide fiber has stronger dielectric loss capability and good high temperature resistance.
Description
Technical Field
The invention relates to a high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and a preparation method thereof, belonging to the technical field of materials.
Background
The high-speed aircraft flies in the atmosphere with high Mach number, the surface temperature of the aircraft is rapidly raised by pneumatic heating, the temperature generally exceeds 600 ℃, and the local temperature can even reach thousands of ℃, so that a plurality of electromagnetic wave absorbing materials cannot normally perform the functions. With the demand of technical development, low detectability is the development trend of future high-speed aircrafts, and the wave-absorbing material is the most main and effective technical way for inhibiting the strong scattering of radar under the condition that the application of the shape stealth technology is limited. Therefore, the development of high temperature resistant electromagnetic wave absorbent is very important for the development of high temperature stealth technology.
The silicon carbide material is a high-temperature resistant ceramic material which is widely applied and developed at present, and is widely considered as a high-temperature resistant wave-absorbing material with great application potential in the future. However, silicon carbide as a semiconductor material has relatively low conductivity and low dielectric loss, and cannot meet the requirement of strong electromagnetic wave absorption. Compared with silicon carbide materials, the silicon carbide-based composite material has the advantages of improving the electrical conductivity, strengthening the polarization loss and optimizing the impedance matching characteristic, and has become a hotspot of research in the field of high-temperature-resistant wave-absorbing materials. The invention relates to a high-temperature-resistant wave-absorbing fiber, namely tungsten/carbon core silicon carbide fiber, which is one of silicon carbide-based composite materials, relevant units in China currently adopt a radio frequency heating or direct current heating mode to realize the deposition of a silicon carbide coating on a continuous tungsten filament, such as patents CN1146428A, CN101121577A, CN112481601A and the like, the methods need radio frequency heating equipment or direct current heating equipment, the device is complex, the production condition is severe, the energy consumption is large, the process control is complicated, and the method is not suitable for the preparation of laboratory-level or small-batch samples.
Disclosure of Invention
The invention aims to provide a high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber and a preparation method thereof, aiming at the defects of the prior art. The invention adopts a direct chemical vapor deposition approach to prepare the high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber, and provides technical support for the research of high-temperature-resistant stealth materials.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber comprises the following steps:
1) Winding a tungsten filament on a carbon rod;
2) Placing the tungsten filament wound with the carbon rod in the step 1) in a high-temperature tube furnace, introducing mixed gas containing hydrogen and argon, heating, and then naturally cooling;
3) Placing the tungsten filament treated in the step 2) in a silicon carbide chemical vapor deposition system, and pumping out air in the silicon carbide chemical vapor deposition system;
4) Selecting acetylene gas as a reaction gas, mixing the acetylene gas with argon gas, introducing the mixture into a chemical vapor deposition system, starting a temperature-raising program to raise the temperature after the relative pressure and flow rate of the mixed gas in the silicon carbide chemical vapor deposition system reach a stable state, reacting after reaching a specified temperature, and keeping for a certain time;
5) Selecting one or more of methyl trichlorosilane, dimethyl dichlorosilane and trimethyl chlorosilane as reaction gas, and then introducing argon, hydrogen and the reaction gas into the silicon carbide chemical vapor deposition system to keep the reaction temperature unchanged;
6) And (3) when the relative pressure and the flow rate of the mixed gas reach a stable state, reacting for a period of time, and then naturally cooling to obtain the high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber.
Preferably, the tungsten wire has a diameter of 10 to 20 μm.
Preferably, the volume of the hydrogen in the step 2) accounts for 3-7%.
Preferably, the heating temperature in the step 2) is 700-900 ℃, and the heating time is 1-3 h.
Preferably, the volume ratio of the acetylene gas in the step 4) is 5-20%, and the flow rate of the mixed gas is 0.5-2L/min.
Preferably, the specified temperature in the step 4) is 1000-1200 ℃, and the reaction time is 1-5 h.
Preferably, in the step 5), the volume ratio of the argon gas in the mixed gas is at least 50%, the volume ratio of the hydrogen gas in the mixed gas is 20-40%, and the volume ratio of the reaction gas in the mixed gas is 10-30%.
Preferably, the flow rate of gas introduced in the step 5) is 1-3L/min,
preferably, the reaction time in step 6) is 1 to 10 hours.
The high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber is prepared by the preparation method and comprises a tungsten core, a carbon layer and a silicon carbide layer, wherein the carbon layer is coated on the tungsten core, and the silicon carbide layer is coated outside the carbon layer.
Compared with the reported preparation of continuous tungsten core silicon carbide fiber by adopting a radio frequency heating or direct current heating mode in the current domestic related units, the method disclosed by the invention is prepared by a direct chemical vapor deposition method, and the preparation of the fiber is completed by using a silicon carbide chemical vapor deposition system (a chemical vapor deposition furnace), so that the characteristics of complex synthesis device, severe production conditions, large energy consumption and fussy process control in the production mode are avoided, and the method is suitable for preparing laboratory-level or small-batch samples. In addition, the tungsten/carbon core silicon carbide fiber synthesized by the invention deposits a carbon layer with a certain thickness between the tungsten core and the silicon carbide coating, and has stronger dielectric loss capability under the influence of the dielectric property of the middle carbon layer compared with the reported tungsten core silicon carbide. The synthesized tungsten/carbon core silicon carbide fiber can be used for synthesizing wave-absorbing materials and provides technical support for the research of high-temperature resistant stealth materials.
Drawings
FIG. 1 is a schematic representation of the structure of a tungsten/carbon core silicon carbide fiber made in accordance with the present invention.
FIG. 2 is a scanning electron microscope image of the wave-absorbing fiber of tungsten/carbon core silicon carbide fiber prepared in example 1.
Fig. 3 is a scanning electron microscope picture of the tungsten/carbon core silicon carbide fiber wave-absorbing fiber prepared in example 2.
FIG. 4 is a scanning electron microscope image of a tungsten core silicon carbide wave-absorbing fiber prepared by a comparative example.
Detailed Description
In order to make the aforementioned and other features and advantages of the invention more comprehensible, embodiments accompanied with figures are described in detail below.
The invention provides a preparation method of a high-temperature-resistant wave-absorbing fiber, which is prepared by a direct chemical vapor deposition method and comprises the following steps:
the first step is as follows: selecting a tungsten wire and winding the tungsten wire on a carbon rod.
According to some embodiments, the diameter of the tungsten wire can be selected from 10 to 20 μm, and the tungsten wire is wound on a carbon rod to facilitate the deposition and collection of a sample after preparation;
the second step: placing the tungsten filament wound on the carbon rod in a high-temperature tube furnace, introducing mixed gas containing hydrogen and argon, heating, and then naturally cooling.
According to some embodiments, the hydrogen gas is present in a proportion of 3% to 7% by volume.
According to some embodiments, the heating temperature may be selected to be between 700 and 900 ℃, and the holding temperature may be selected to be between 1 and 3 hours.
The production process of the tungsten wire is a hot drawing process, a layer of oxide film often exists on the surface of a product, and the oxide film can be effectively removed and reduced into tungsten through high-temperature treatment in an argon/hydrogen mixed atmosphere. If the temperature is too low and the treatment time is too short, the reduction is not easy to be thorough.
The third step: and (4) placing the tungsten filament after the treatment in the previous step into a silicon carbide chemical vapor deposition system, and pumping out air in the silicon carbide chemical vapor deposition system.
The fourth step: selecting acetylene gas as reaction gas, mixing the acetylene gas with argon gas, introducing the mixture into a silicon carbide chemical vapor deposition system, starting a temperature-raising program to raise the temperature after the relative pressure and the flow rate of the mixed gas in the silicon carbide chemical vapor deposition system reach a stable state, reacting after reaching a specified temperature, and keeping for a certain time.
According to some embodiments, the volume ratio of acetylene gas is 5% to 20%, and the flow rate of the mixed gas is 0.5 to 2L/min.
According to some embodiments, the specified temperature of the reaction is between 1000 and 1200 ℃ and the reaction time is between 1 and 5h. The temperature interval is suitable for the growth of the silicon carbide coating, the high temperature is favorable for the rapid growth of the silicon carbide coating, but the too high temperature easily causes the uneven growth of silicon carbide crystal grains, and the too low temperature is not favorable for the reaction.
Acetylene gas is used as a carbon source, can be decomposed through a CVD process and then is deposited on the surface of the tungsten filament to form a carbon layer, and the thickness of the carbon layer can be regulated and controlled through reaction time and is in direct proportion to the reaction time.
The fifth step: introducing high-purity argon, hydrogen and reaction gas into a deposition system according to a certain proportion and flow rate;
according to some embodiments, the high purity argon gas is at least 50% by volume of the mixed gas and functions as a carrier gas; the volume ratio of hydrogen in the mixed gas can be set to 20-40%, which acts as a diluent gas.
According to some embodiments, the reaction gas comprises one or more of monomethyltrichlorosilane, dimethyldichlorosilane and trimethylchlorosilane, and the volume of the reaction gas in the mixed gas is 10-30%. The methyl trichlorosilane is beneficial to the uniform growth of the silicon carbide coating, but the growth speed of the crystal is slow; dimethyldichlorosilane and trimethylchlorosilane facilitate rapid growth of silicon carbide coatings, but tend to form relatively coarse crystal particles, so that the reaction gas can be selected according to actual conditions and test requirements.
According to some embodiments, the flow rate can be set to 1-3L/min, and when the gas flow rate is high, the waste gas is discharged, the growth of the silicon carbide coating is facilitated, but the reaction gas is easily wasted due to the fact that the flow rate is not too high.
And a sixth step: when the relative pressure and flow rate of the mixed gas reach a stable state, keeping for a certain time, and then naturally cooling.
According to some embodiments, the reaction time can be set to 1 to 10 hours, the reaction time being positively correlated to the silicon carbide coating thickness, the longer the reaction time, the greater the silicon carbide coating thickness.
The structure of the synthetic tungsten/carbon core silicon carbide fiber prepared by the invention is shown in figure 1, and the synthetic tungsten/carbon core silicon carbide fiber comprises a tungsten core, a carbon layer and a silicon carbide layer, wherein the carbon layer is coated on the tungsten core, and the silicon carbide layer is coated outside the carbon layer.
Specific examples are listed below:
example 1
The first step is as follows: selecting a tungsten wire with the diameter of about 10 mu m, and winding the tungsten wire on a carbon rod;
the second step: placing a tungsten filament wound on a carbon rod in a high-temperature tube furnace, introducing high-purity argon containing 3% of volume fraction hydrogen, keeping the argon at 800 ℃ for 3 hours, and then naturally cooling;
the third step: placing the tungsten filament treated in the previous step in a silicon carbide chemical vapor deposition system, and pumping out air in the deposition system;
the fourth step: mixing acetylene gas and argon gas, introducing the mixture into a chemical vapor deposition system, wherein the volume of the acetylene gas accounts for 10%, the flow rate of the mixed gas is 1L/min, starting a temperature rise program to start temperature rise after the relative pressure and the flow rate of the mixed gas in the chemical vapor deposition system reach stable states, setting the reaction temperature to be 1050 ℃, and keeping the reaction temperature for 3 hours;
the fifth step: introducing high-purity argon, hydrogen and methyl trichlorosilane into a deposition system at a flow rate of 2L/min according to the proportion of 50 percent, 20 percent and 30 percent;
and a sixth step: and after the relative pressure and the flow rate of the mixed gas in the chemical vapor deposition system reach a stable state, keeping for 6h, and then naturally cooling to obtain the tungsten/carbon core silicon carbide fiber.
The scanning electron microscope picture of the tungsten/carbon core silicon carbide wave-absorbing fiber prepared in this embodiment is shown in fig. 2, and it can be seen that a carbon layer with a thickness of about 700nm is formed on the surface of the tungsten filament, and the SiC coating with a thickness of about 3 μm is coated on the periphery of the carbon layer.
Example 2
The first step is as follows: selecting a tungsten wire with the diameter of about 12 mu m, and winding the tungsten wire on a carbon rod;
the second step is that: placing a tungsten filament wound on a carbon rod in a high-temperature tube furnace, introducing high-purity argon containing 7% of volume fraction hydrogen, keeping the argon at 900 ℃ for 2 hours, and then naturally cooling;
the third step: placing the tungsten filament treated in the previous step in a silicon carbide chemical vapor deposition system, and pumping out air in the deposition system;
the fourth step: mixing acetylene gas and argon gas, introducing the mixture into a chemical vapor deposition system, wherein the volume of the acetylene gas accounts for 20%, the flow rate of the mixed gas is 2L/min, starting a temperature-raising program to raise the temperature after the relative pressure and the flow rate of the mixed gas in the chemical vapor deposition system reach stable states, setting the reaction temperature to 1200 ℃, and keeping the temperature for 1h;
the fifth step: introducing high-purity argon, hydrogen, monomethyl trichlorosilane and dimethyl dichlorosilane into a deposition system at the flow rate of 3L/min according to the proportion of 55%, 25%, 10% and 10%;
and a sixth step: and after the relative pressure and flow rate of the mixed gas in the chemical vapor deposition system reach a stable state, keeping for 10 hours, and naturally cooling to obtain the tungsten/carbon core silicon carbide fiber.
The scanning electron microscope picture of the tungsten/carbon core silicon carbide wave-absorbing fiber prepared by the embodiment is shown in fig. 3, and it can be seen that the SiC coating is further thickened, and the diameter of the fiber reaches 19 μm.
Example 3
The first step is as follows: selecting a tungsten wire with the diameter of about 20 mu m, and winding the tungsten wire on a carbon rod;
the second step is that: placing a tungsten filament wound on a carbon rod in a high-temperature tube furnace, introducing high-purity argon containing 5% of volume fraction hydrogen, keeping the argon at 700 ℃ for 1h, and then naturally cooling;
the third step: placing the tungsten filament treated in the previous step in a silicon carbide chemical vapor deposition system, and pumping out air in the deposition system;
the fourth step: mixing acetylene gas and argon gas, introducing the mixture into a chemical vapor deposition system, wherein the volume of the acetylene gas accounts for 5%, the flow rate of the mixed gas is 0.5L/min, starting a temperature-raising program to raise the temperature after the relative pressure and the flow rate of the mixed gas in the chemical vapor deposition system reach stable states, setting the reaction temperature to be 1000 ℃, and keeping the temperature for 5 hours;
the fifth step: introducing high-purity argon, hydrogen and methyl trichlorosilane into a deposition system at a flow rate of 1L/min according to the proportion of 50 percent, 40 percent and 10 percent;
and a sixth step: and after the relative pressure and the flow rate of the mixed gas in the deposition system reach a stable state, setting the reaction time to be 1h, and then naturally cooling to obtain the tungsten/carbon core silicon carbide fiber.
The fiber diameter of the tungsten/carbon core silicon carbide wave-absorbing fiber prepared by the embodiment is 28 μm, and a carbon layer is arranged between a tungsten filament and a SiC layer.
Comparative example
The first step is as follows: selecting a tungsten wire with the diameter of about 10 mu m, and winding the tungsten wire on a carbon rod;
the second step is that: placing a tungsten filament wound on a carbon rod in a high-temperature tube furnace, introducing high-purity argon containing 5% of volume fraction hydrogen, keeping the argon at 700 ℃ for 1h, and then naturally cooling;
the third step: placing the tungsten filament treated in the previous step in a silicon carbide chemical vapor deposition system, and pumping out air in the deposition system; the fourth step: introducing high-purity argon, hydrogen and methyl trichlorosilane into a deposition system at a flow rate of 1L/min according to the proportion of 50 percent, 30 percent and 20 percent;
the fifth step: after the relative pressure and flow rate of the mixed gas in the deposition system reach a stable state, starting a temperature raising program to start raising the temperature, setting the reaction temperature to 1050 ℃ and the reaction time to 3h, and then naturally lowering the temperature;
a scanning electron microscope photograph of the resulting tungsten core silicon carbide fiber is shown in fig. 2. It can be seen that the surface of the tungsten filament directly formed a SiC coating about 1 μm thick.
Although the present invention has been described with reference to the above embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (10)
1. A preparation method of high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber is characterized by comprising the following steps:
1) Winding a tungsten filament on a carbon rod;
2) Placing the tungsten filament wound with the carbon rod in the step 1) in a high-temperature tube furnace, introducing mixed gas containing hydrogen and argon, heating, and then naturally cooling;
3) Placing the tungsten filament treated in the step 2) in a silicon carbide chemical vapor deposition system, and pumping out air in the silicon carbide chemical vapor deposition system;
4) Selecting acetylene gas as a reaction gas, mixing the acetylene gas with argon gas, introducing the mixture into a chemical vapor deposition system, starting a temperature-raising program to raise the temperature after the relative pressure and flow rate of the mixed gas in the silicon carbide chemical vapor deposition system reach a stable state, reacting after reaching a specified temperature, and keeping for a certain time;
5) Selecting one or more of methyl trichlorosilane, dimethyl dichlorosilane and trimethyl chlorosilane as reaction gas, and then introducing argon, hydrogen and the reaction gas into the silicon carbide chemical vapor deposition system to keep the reaction temperature unchanged;
6) And when the relative pressure and the flow rate of the mixed gas reach a stable state, reacting for a period of time, and then naturally cooling to obtain the high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber.
2. The method of claim 1, wherein the tungsten wire has a diameter of 10 to 20 μm.
3. The method according to claim 1, wherein the hydrogen gas in the step 2) is present in an amount of 3 to 7% by volume.
4. The method according to claim 1, wherein the heating temperature in step 2) is 700 to 900 ℃ and the heating time is 1 to 3 hours.
5. The method of claim 1, wherein the acetylene gas in the step 4) is 5 to 20% by volume, and the flow rate of the mixed gas is 0.5 to 2L/min.
6. The method of claim 1, wherein the specified temperature in the step 4) is 1000 to 1200 ℃ and the reaction time is 1 to 5 hours.
7. The method according to claim 1, wherein the argon gas is at least 50% by volume in the mixed gas in the step 5), the hydrogen gas is 20-40% by volume in the mixed gas, and the reaction gas is 10-30% by volume in the mixed gas.
8. The production method according to claim 1 or 7, wherein the gas is introduced at a flow rate of 1 to 3L/min in the step 5).
9. The process according to claim 1, wherein the reaction time in step 6) is from 1 to 10 hours.
10. A high-temperature-resistant wave-absorbing tungsten/carbon core silicon carbide fiber is prepared by the preparation method of any one of claims 1 to 9, and is characterized by comprising a tungsten core, a carbon layer and a silicon carbide layer, wherein the carbon layer is coated on the tungsten core, and the silicon carbide layer is coated outside the carbon layer.
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| CN101121577A (en) * | 2007-05-28 | 2008-02-13 | 魏永芬 | Method and device for realizing double-component coat on SiC fibre surface |
| JP2014133919A (en) * | 2013-01-10 | 2014-07-24 | Shin Etsu Chem Co Ltd | Member coated with thermal decomposition carbon |
| CN105039928A (en) * | 2015-06-17 | 2015-11-11 | 姜辛 | Preparation method of diamond/silicon carbide three-dimensional composite structure and prepared product |
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