WO2020199353A1 - Préparation et utilisation de fibre électrothermique résistante à haute température - Google Patents

Préparation et utilisation de fibre électrothermique résistante à haute température Download PDF

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WO2020199353A1
WO2020199353A1 PCT/CN2019/091444 CN2019091444W WO2020199353A1 WO 2020199353 A1 WO2020199353 A1 WO 2020199353A1 CN 2019091444 W CN2019091444 W CN 2019091444W WO 2020199353 A1 WO2020199353 A1 WO 2020199353A1
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Prior art keywords
fiber
electric heating
temperature resistant
high temperature
resistant electric
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PCT/CN2019/091444
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English (en)
Chinese (zh)
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李辰宇
汪威
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碳翁(北京)科技有限公司
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Publication of WO2020199353A1 publication Critical patent/WO2020199353A1/fr

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    • 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
    • C23C16/26—Deposition of carbon only
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/10—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material
    • H05B3/14—Heater elements characterised by the composition or nature of the materials or by the arrangement of the conductor characterised by the composition or nature of the conductive material the material being non-metallic
    • H05B3/145—Carbon only, e.g. carbon black, graphite
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H05B3/54—Heating elements having the shape of rods or tubes flexible

Definitions

  • the invention belongs to the field of materials, and specifically relates to a method for preparing high-temperature resistant electric heating fibers by using a chemical vapor deposition technology (CVD) method and its application in the field of electric heating components.
  • CVD chemical vapor deposition technology
  • Electric heating materials are used in the manufacture of heating elements in various resistance heating equipment. At present, the electric heating method has been widely used because of its advantages such as easy control and adjustment, no pollution to the environment, and good product quality. Among them, the resistance heating method using the resistance heating element as the electrothermal conversion medium is the most convenient and widely used.
  • Common electric heating materials include metal electric heating materials and non-metal electric heating materials. The main disadvantage of metal electric heating materials is that they are expensive and demanding on the conditions of use. Among them, refractory metal electric heating materials must be used in a vacuum or protective atmosphere. Metallic electric heating materials are usually processed into a wire spiral or wave structure, which is prone to inductive reactance effect and energy loss when energized.
  • non-metallic electric heating materials Compared with metal electric heating materials, non-metallic electric heating materials have the advantages of high temperature resistance, corrosion resistance, oxidation resistance, and high electrothermal conversion efficiency. No matter in the field of high temperature heating or medium and low temperature heating, non-metallic electric heating materials are gradually replacing metal electric heating materials.
  • non-metallic electric heating elements are generally processed into rods, strips, plates or U shapes through biscuit and sintering processes, which cannot solve the problems of large resistance dispersion and poor mechanical properties. Therefore, the research and development of new high-performance electrothermal materials not only has important scientific research significance, but also has important practical application value.
  • the purpose of the present invention is to provide a method for preparing a high-temperature resistant electrothermal fiber material.
  • the present invention prepares the electrothermal material by directly growing microcrystalline graphite, which can effectively optimize the performance of the electrothermal material and reduce the preparation cost.
  • Microcrystalline graphite is a carbon nanomaterial with a disordered structure formed by hexagonal carbon atoms composed of sp 2 hybrid orbitals and randomly distributed on the substrate in a honeycomb lattice.
  • the infrared emissivity of the electrothermal fiber prepared by the invention is as high as 0.95, which can effectively improve the heat conversion rate and reduce the power consumption; it has outstanding advantages such as high temperature resistance, flexibility, easy configuration, and adjustable resistivity, and has low thermal inertia and is heated The advantages of close body contact and low heat conduction loss.
  • the range of use of traditional electric heating materials can be expanded, making it used in many fields such as household appliances, electronics, medical treatment, transportation, and aerospace.
  • the present invention provides a method for preparing a high-temperature resistant electric heating fiber, which is characterized in that the method includes the following steps:
  • Step 1 Prepare insulating fiber material
  • Step 2 Perform surface coating treatment on the fiber material, and the coating layer contains a carbon source cracking catalytic material (a material that has a catalytic cracking effect on the carbon source);
  • Step 3 Place the coated fiber material in a vacuum reaction chamber
  • Step 4 Pass protective gas and reducing gas into the vacuum reaction chamber, and then pass in a carbon source to grow microcrystalline graphite;
  • Step 5 cooling the fiber material under a protective gas and reducing gas atmosphere to obtain a high-temperature resistant electric heating fiber.
  • the fiber material is a clean fiber material.
  • the carbon source cracking catalytic material is a metal carbon source cracking catalytic material.
  • the carbon source cracking catalytic material has volatility under low pressure (for example, less than 100 Pa).
  • the carbon source cracking catalytic material is a volatile material under reaction temperature and low pressure conditions.
  • the growth time of the microcrystalline graphite is controlled after all the attached film layer is volatilized, for example, after the volatilization amount of the film layer exceeds 99.9%.
  • the fiber material is selected from at least one of a single fiber, a single fiber, and a fiber cloth.
  • the thickness of the coated film layer is 10-100 ⁇ m, more preferably 40-60 ⁇ m.
  • the protective gas includes an inert gas
  • the reducing gas includes H 2
  • the step 4 further includes the step of introducing the carbon source after the gas flow of the protective gas and the reducing gas is stabilized.
  • the present invention provides a high temperature resistant electric heating fiber, characterized in that the high temperature resistant electric heating fiber includes a fiber layer and a microcrystalline graphite layer covering the fiber layer.
  • the microcrystalline graphite layer is wrapped outside the fiber layer in the following manner:
  • Step 1 Prepare insulating fiber material
  • Step 2 Perform surface coating treatment on the fiber material, and the coating layer contains a carbon source cracking catalytic material;
  • Step 3 Place the coated fiber material in a vacuum reaction chamber
  • Step 4 Pass protective gas and reducing gas into the vacuum reaction chamber, and then pass in a carbon source to grow microcrystalline graphite;
  • Step 5 cooling the fiber material under a protective gas and reducing gas atmosphere to obtain a high-temperature resistant electric heating fiber.
  • the present invention provides an application of the high-temperature resistant electric heating fiber, and the application includes applying a voltage across the high-temperature resistant electric heating fiber to perform electrothermal conversion.
  • the application includes applying the high temperature resistant electrothermal fiber to a high temperature environment with or generating 200-1200 degrees Celsius, and performing electrothermal conversion based on infrared radiation.
  • Step 1 may include a process of cleaning the fibers: sequentially placing the fibers in cyclohexane, ethanol, and deionized water, ultrasonically cleaning them for a predetermined time, such as 10 minutes, and drying with nitrogen to complete the cleaning of the fibers.
  • the fiber may be selected from at least one of high-temperature resistant quartz fiber, glass fiber, asbestos fiber, metal fiber, nitrile boron fiber, ceramic fiber, and other fibers that can be used above 300°C. That is, the selected fibers are all insulating and heat-resistant fiber materials.
  • the metal coating process is preferably performed through a metal coating process, and the thickness of the metal film is not greater than 100 m.
  • the coating metal is selected from at least one of metals that can catalyze the cracking of carbon sources, such as copper, nickel, and platinum.
  • the attached film layer needs to meet the temperature conditions of 300°C-1100°C and the pressure conditions during the reaction in step 4 to have a volatilization effect.
  • the metal coating process is selected from at least one of electroplating, electroless plating, sol-gel, magnetron sputtering, and direct spraying of the metal coating, preferably a direct spraying method of nano metal particles.
  • the flow into the reaction chamber can be 800-1000sccm Ar and 800-1000sccm H2.
  • the growth time can be controlled within 10-300 minutes, preferably 40-300 minutes, and the growth process is set at 300°C-1100°C, thereby forming a microcrystalline graphite layer with a controllable thickness on the surface of the metal-clad fiber.
  • the carbon source is selected from gaseous (methane, ethylene, acetylene), solid (polyaniline, polystyrene, etc.), liquid (toluene, benzoic acid, chlorobenzene, ethanol, acetonitrile, etc.) carbon sources At least one.
  • Step 5 specifically includes: after the growth of microcrystalline graphite, turn off the carbon source vapor, set the flow distribution of Ar and H2 to 100-300sccm/100-300sccm, start the cooling process, turn off Ar/H2 after the temperature drops to room temperature, and take out the sample , Complete the entire preparation process.
  • reaction temperature various gas flow rates, and reaction time involved in the above preparation process can be adjusted according to process requirements.
  • the applicant of the present application has discovered a method for preparing electrothermal fibers that can achieve high infrared emissivity, low surface resistance, and high temperature resistance.
  • the prepared electric heating material can achieve high temperature resistance of 1200 degrees, realize the surface resistance value is lower than 100 ⁇ /sq (even as low as 10 ⁇ /sq in embodiment 1), and the infrared radiation rate is higher than 90%, basically reaching 95% (corresponding to the present invention Best Practice).
  • the surface resistance value can be prepared Electric heating fiber with lower than 100/sq, 95% infrared radiation rate and high temperature resistance of 1200 degrees.
  • the electrothermal fiber obtained by other methods cannot achieve such excellent performance in all aspects.
  • the middle fiber filament is covered with microcrystalline graphite, not only the toughness and air permeability of the electric heating fiber can be increased, but also the heat radiation area can be increased, and the heat conversion efficiency can be further improved. % Of electrothermal conversion efficiency.
  • the method of the present invention has low cost, high yield, and the prepared electrothermal fiber has excellent properties such as good hydrophobicity and air permeability, and has huge social and economic value.
  • an electrothermal fiber material that can withstand a high temperature of more than 500 degrees and an infrared radiation rate of more than 80%.
  • Figure 1 is a schematic diagram of a chemical vapor deposition (CVD) system.
  • Example 2 is a physical diagram of the high-temperature electric heating fiber cloth prepared in Example 1.
  • Example 3 is an SEM image of the electric heating fiber cloth prepared in Example 1.
  • Example 4 is an electrothermal diagram of the electrothermal fiber cloth prepared in Example 1.
  • 5 and 6 are diagrams showing the hydrophobic properties of the surface of the electric heating fiber cloth prepared in Example 1.
  • Example 7 is a diagram showing the surface air permeability characteristics of the electric heating fiber cloth prepared in Example 1.
  • Example 8 is a graph showing the electrothermal performance of the electrothermal fiber cloth and the metal wire electrothermal film prepared in Example 6.
  • Figure 1 shows a conventional chemical vapor deposition equipment, and the method of the present invention can be implemented by using this equipment.
  • the equipment mainly includes a gas supply part on the left, a high temperature tube furnace in the middle, and a cooling and gas exhaust device on the right.
  • the gas supply part is used to provide protective gas, reducing gas and carbon source to the high-temperature tube furnace.
  • the high-temperature tube furnace is the main reaction equipment in which microcrystalline graphite is grown, and the gas exhaust device is used to react the remaining gas. Processing.
  • the quartz fiber cloth is cleaned by ultrasonic cleaning, and copper is sprayed at room temperature (20% of the mass fraction of nano copper powder (Aladdin-C103844) is ultrasonically dispersed in the ethanol solution to form a mixed solution, and a common paint spray gun is used , You can directly spray the advanced technology of the metal coating, this is the prior art, which will not be described in detail here.)
  • the method of covering the surface of the quartz fiber with copper to form a copper sparse structure film (the same below), and controlling the thickness of the copper film 50 ⁇ m (so that there is no metal residue in the subsequent reaction process, the applicant found that once there is catalyst residue in the fiber, the fiber will be easy to age and break).
  • the carbon material growth process was set to 120 minutes, and the toluene valve was quickly closed after the growth was completed, and the Ar/H 2 was set to 300/300 sccm to start the cooling process.
  • the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • the flow rates of the carbon source, the protective gas, and the reducing gas can be appropriately adjusted as needed, and the values in the embodiment are not necessarily limited.
  • the flow of Ar/H 2 in the early stage can be controlled to 700-1300 sccm; after the growth, the Ar/H 2 can be set to 200-500.
  • the sample By applying 3V DC/AC, the sample can be heated to 100°C in an instant (less than 1 second), showing good rapid heating characteristics and uniform heating surface; JCY- The two-drop contact angle measuring instrument measured the contact angle of the fiber cloth to be 100 degrees, showing the characteristics of hydrophobicity; comparing the sample before and after in a 100 °C water vapor environment, it can be seen that the sample has good air permeability characteristics.
  • the TIR 100-2 rapid emissivity tester is used to make the surface of the sample to be tested receive the infrared radiation radiated by a 100°C hemispherical black body, and then receive the infrared radiation reflected by the sample, measure the infrared radiation reflectivity and obtain the sample according to the calibration value ( The infrared emissivity of the heating fiber cloth), the measurement result is that the infrared emissivity is 0.95.
  • QUANTAX EDS German Bruker X-ray energy spectrometer
  • the high temperature resistance of 1200°C (the same below) or other temperatures mentioned in the fire resistance test mentioned in the present invention is not an absolute limit for embrittlement, but only when the test is carried out to the vicinity of this temperature. When the temperature is raised, obvious embrittlement will be found. The description of this temperature is only used to prove the approximate degree of the high temperature resistance of the product of the present invention.
  • the toluene vapor quickly decomposes into activated carbon species after entering the reaction chamber, and a large amount of activated carbon species adsorbs to the surface of the quartz fiber, migrates and collides on the surface, thereby achieving the nucleation and growth of microcrystalline graphite.
  • the carbon material growth process is set to 120 minutes.
  • the toluene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started.
  • the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • the surface of the sample to be tested receives the infrared radiation radiated by a 100°C hemispherical black body, and the infrared radiation reflected by the sample is received to measure the reflectivity and obtain the infrared radiation emissivity according to the calibration value.
  • the infrared emissivity was 0.86, which was lower than the structure in Example 1.
  • the German Bruker X-ray energy spectrometer (QUANTAX EDS) system was used to analyze the types of elements in the sample micro-regions, and a small amount of Cu element residue was detected.
  • the applicant found that the metal copper film obtained by magnetron sputtering has a greater bonding force with the fiber surface.
  • the metal copper film obtained by magnetron sputtering has a greater bonding force with the fiber surface.
  • Metal copper is easily oxidized under high temperature conditions in the air, which causes the heat resistance temperature of the sample to drop.
  • the infrared emissivity of metallic copper is much lower than that of microcrystalline graphite, so the infrared emissivity of sample 2 appears to decrease.
  • a large amount of activated carbon material is adsorbed on the surface of the quartz fiber, migrates and collides on the surface, so as to realize the nucleation and growth of microcrystalline graphite.
  • the carbon material growth process is set to 120 minutes. After the growth is completed, the ethylene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started. When the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • Perform performance test on the obtained sample use a liquefied gas torch to conduct a heat resistance test on the prepared electrothermal fiber.
  • the test result is that when the temperature is greater than 1200°C, the fiber begins to crack and has non-combustible characteristics; four probes are used The tester tests the surface resistance value of the sample, and the test result is that the surface resistance value is 100 ⁇ /sq.
  • the surface of the sample to be tested receives the infrared radiation radiated by a 100°C hemispherical black body, and then receives the infrared radiation reflected by the sample, measures the infrared radiation reflectivity and obtains the infrared radiation according to the calibration value Emissivity, the measurement result is that the infrared emissivity is 0.96.
  • the German Bruker X-ray energy spectrometer (QUANTAX EDS) system to analyze the types of elements in the sample micro-area, no nickel residues were detected.
  • the sample prepared in this example has a much lower growth temperature than that in Example 1.
  • the carbon atoms or carbon radicals formed after catalytic cracking on the surface will enter the bulk phase of the nickel metal substrate, and then precipitate from the bulk nickel metal phase to the surface to form a thicker microcrystalline graphite layer when the temperature is lowered.
  • the toluene gas valve After the air flow is stable, open the toluene gas valve and pass in toluene gas to reduce the flow Controlled to 1000sccm, the toluene gas quickly decomposes into activated carbon species after entering the reaction chamber, and a large number of activated carbon species are adsorbed on the surface of the quartz fiber, migrate and collide on the surface, thereby realizing the nucleation and growth of microcrystalline graphite.
  • the carbon material growth process is set to 120 minutes. After the growth is completed, the toluene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started. When the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • Perform performance test on the obtained sample use a liquefied gas torch to conduct a heat resistance test on the prepared electric fiber.
  • the test result is that when the temperature is greater than 1200 °C, the fiber starts to appear brittle and has non-combustible characteristics. Under the following conditions, there is basically no embrittlement after 5 minutes of continuous high temperature; the surface resistance value of the sample is tested with a four-probe tester, and the test result is that the surface resistance value is 150 ⁇ /sq.
  • the surface of the sample to be tested receives the infrared radiation radiated by a 100°C hemispherical black body, and then receives the infrared radiation reflected by the sample, measures the infrared radiation reflectivity and obtains the infrared radiation according to the calibration value Emissivity, the measurement result is that the infrared emissivity is 0.96.
  • the German Bruker X-ray energy spectrometer (QUANTAX EDS) system to analyze the types of elements in the sample micro-area, no nickel residues were detected.
  • Example 3 Compared with the sample in Example 3, the growth temperature of the sample prepared in this example is lowered to 300°. Analysis shows that by controlling toluene under the condition of nickel metal catalysis, low-temperature cracking can be achieved, and there are a large number of benzene ring free radicals. Realize the rapid stacking of hexagonal honeycomb carbon lattice.
  • the carbon material growth process is set to 20 minutes, and the toluene valve is quickly closed after the growth is completed, and the Ar/H 2 flow rate is controlled to 300/300 sccm, and the cooling process is started.
  • the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • Perform performance test on the obtained sample use a liquefied gas torch to conduct a heat resistance test on the prepared electrothermal fiber.
  • the test result is that when the temperature is greater than 1200°C, the fiber begins to crack and has non-combustible characteristics; four probes are used The tester tests the surface resistance of the sample, and the test result is that the surface resistance is 1800 ⁇ /sq.
  • the surface of the sample to be tested receives the infrared radiation radiated by a 100°C hemispherical black body, and then receives the infrared radiation reflected by the sample, measures the reflectivity and obtains the infrared radiation of the sample according to the calibration value Emissivity, the measurement result is that the infrared emissivity is 0.96.
  • the German Bruker X-ray energy spectrometer (QUANTAX EDS) system was used to analyze the types of elements in the sample micro-area, and no nickel residue was detected. Compared with the sample of Example 4, the resistance value of the sample of this example is higher.
  • the analysis shows that by controlling the content of the nickel metal catalyst and the growth time, the thickness of the microcrystalline graphite layer on the fiber surface can be controlled. The greater the thickness, the lower the resistance value. .
  • the cavity is quickly decomposed into activated carbon species, a large number of activated carbon species are adsorbed on the surface of the glass fiber, migrate and collide on the surface, so as to realize the nucleation and growth of microcrystalline graphite.
  • the carbon material growth process is set to 120 minutes.
  • the toluene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started.
  • the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • thermoelectric conversion rate of the microcrystalline graphite fiber cloth is 91.4%, and the thermoelectric conversion rate of the metal wire electric heating film is 82.1%.
  • the carbon material growth process is set to 120 minutes. After the growth is completed, the ethylene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started. When the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • Perform performance test on the obtained sample use a liquefied gas torch to conduct a heat resistance test on the prepared electrothermal fiber.
  • the test result is that when the temperature is greater than 1200°C, the fiber begins to crack and has non-combustible characteristics; four probes are used
  • the tester tests the surface resistance value of the sample, and the test result is that the surface resistance value is greater than 10M ⁇ /sq.
  • the surface of the tested sample receives the infrared radiation radiated by a 100°C hemispherical black body, and the infrared radiation reflected by the sample 7 is received to measure the reflectivity and obtain the infrared radiation emissivity according to the calibration value.
  • the measurement result is that the infrared emissivity is 0.48, and the infrared emissivity is greatly reduced.
  • QUANTAX EDS German Bruker X-ray energy spectrometer
  • the carbon material growth process is set to 120 minutes. After the growth is completed, the ethylene valve is quickly closed, and the Ar/H 2 flow rate is controlled to 300/300sccm, and the cooling process is started. When the temperature in the reaction chamber drops to room temperature, turn off Ar/H 2 , open the chamber and take out the sample.
  • the test result is that when the temperature is greater than 600 °C, the fiber begins to crack and has non-combustible characteristics; four probes are used The tester tests the surface resistance of the sample, and the test result is 8 ⁇ /sq.
  • the surface of the sample to be tested receives the infrared radiation radiated by a 100°C hemispherical black body, and the infrared radiation reflected by the sample 8 is received to measure the reflectivity and obtain the infrared radiation emission of the sample according to the calibration value
  • the measurement result is that the infrared emissivity is 0.53.
  • the German Bruker X-ray energy spectrometer (QUANTAX EDS) system was used to analyze the types of constituent elements in the sample micro-area, and a large amount of copper residue was detected.
  • the analysis shows that due to the thick copper film, a large amount of copper remains during the high-temperature growth process, forming a composite material of fiber/copper/microcrystalline graphite. Therefore, the resistance value of the material and the infrared heating rate are reduced. At the same time, the increase in the thickness of the copper film also increases the production cost of the material.

Abstract

L'invention concerne la préparation et l'utilisation d'une fibre électrothermique résistante à haute température. Le procédé comprend : l'étape 1 : la préparation d'un matériau fibreux isolant; l'étape 2 : la soumission du matériau fibreux à un traitement de revêtement de surface, la couche de film revêtue comprenant un matériau issu de la pyrolyse catalytique d'une source de carbone; l'étape 3 : le placement du matériau de fibre revêtu dans une chambre de réaction sous vide; l'étape 4 : l'introduction d'un gaz inerte et de H2 dans la chambre de réaction sous vide, et l'introduction de la source de carbone après que le flux de gaz est stable pour faire croître du graphite microcristallin; et l'étape 5 : le refroidissement du matériau fibreux dans l'atmosphère du gaz inerte et de l'H2, de manière à obtenir la fibre électrothermique résistante à la température élevée.
PCT/CN2019/091444 2019-04-04 2019-06-16 Préparation et utilisation de fibre électrothermique résistante à haute température WO2020199353A1 (fr)

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