WO2016208846A1 - Procédé de production d'une fibre de carbure de silicium, fibre de carbure de silicium et élément chauffant à fibre de carbure de silicium produit à l'aide de celle-ci, et dispositif de chauffage l'utilisant - Google Patents

Procédé de production d'une fibre de carbure de silicium, fibre de carbure de silicium et élément chauffant à fibre de carbure de silicium produit à l'aide de celle-ci, et dispositif de chauffage l'utilisant Download PDF

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WO2016208846A1
WO2016208846A1 PCT/KR2016/002609 KR2016002609W WO2016208846A1 WO 2016208846 A1 WO2016208846 A1 WO 2016208846A1 KR 2016002609 W KR2016002609 W KR 2016002609W WO 2016208846 A1 WO2016208846 A1 WO 2016208846A1
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Prior art keywords
silicon carbide
heating element
carbide fiber
fiber
fibers
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PCT/KR2016/002609
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English (en)
Korean (ko)
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이형석
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Omnicera Co Ltd
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Omnicera Co Ltd
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Priority claimed from KR1020150090437A external-priority patent/KR101684600B1/ko
Priority claimed from KR1020150150501A external-priority patent/KR101732573B1/ko
Priority claimed from KR1020160006913A external-priority patent/KR101734472B1/ko
Application filed by Omnicera Co Ltd filed Critical Omnicera Co Ltd
Publication of WO2016208846A1 publication Critical patent/WO2016208846A1/fr
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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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • 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
    • H05B6/00—Heating by electric, magnetic or electromagnetic fields
    • H05B6/64—Heating using microwaves
    • 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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/97—Preparation from SiO or SiO2
    • 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
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/956—Silicon carbide
    • C01B32/963—Preparation from compounds containing silicon
    • C01B32/984—Preparation from elemental silicon
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
    • 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—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating 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
    • 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—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor
    • H05B3/12—Heating 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—Heating 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
    • 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
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater
    • H05B3/34—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater flexible, e.g. heating nets or webs

Definitions

  • the present invention relates to a method for producing silicon carbide fibers (SiCf) and the application of the silicon carbide fibers,
  • carbon fibers may be formed by sublimation of a sublimation raw material selected from, for example, silicon or silicon dioxide, or a mixture thereof at a high temperature, by a sublimation gas infiltration reaction.
  • a sublimation raw material selected from, for example, silicon or silicon dioxide, or a mixture thereof at a high temperature
  • a sublimation gas infiltration reaction Provides a method for producing silicon carbide fibers (SiCf), silicon carbide fibers and silicon carbide fiber heating elements, and other applications,
  • Further sublimation further comprises a doping source to provide nano-doped silicon carbide fibers and heating elements using the same,
  • the present invention relates to a rapid heating highly efficient silicon carbide fiber heating element capable of minimizing the loss of thermal heat energy and a heating device using the same.
  • Silicon carbide (SiC) fiber is a representative non-oxide-based ceramic material and has excellent physicochemical stability at high temperatures, and is being used in composite materials fields such as aerospace, energy, and defense.
  • the existing SiC fiber manufacturing process is made by three methods, powder extrusion (Carborundum), CVD (Chemical Vapor Deposition), precursor method.
  • SiC Powders submicron SiC powder
  • a sintering aid were mixed together with a suitable polymer to make a compound capable of melt spinning, and then extruded to a desired diameter and sintered at 2,000 oC to prepare SiC fibers.
  • creep resistance is the most excellent fiber.
  • the CVD method transfers core wire (tungsten wire or carbon fiber) through the Mercury Contact at a constant speed into the quartz reaction tube, and flows current through the injected core wire and heats it by 1,000 ⁇ 1,300 oC by self-heating, and is a raw material of methyldichlorosilane It is prepared by depositing SiC by adding silane gas such as (Methyl Dichlorosilane) and Ar, H2 gas, which are atmospheric gases.
  • silane gas such as (Methyl Dichlorosilane) and Ar, H2 gas, which are atmospheric gases.
  • This manufacturing method is a method of coating the SiC on the surface of the core wire is superior in thermal stability than other fibers, but the manufacturing process is difficult and the manufacturing cost is high.
  • coarse fibers are manufactured with a diameter of 150 um or more, which is not suitable for the application of fiber reinforced composite materials.
  • SCS SiC Fibers Process, Properties and Production Technical Data from the Website fo Specialty Materials, www. specmaterials. com]
  • the precursor method is a process for producing SiC fibers having a diameter of 10 to 100 um through melt spinning and pyrolysis of a polycarbosilane (PCS) precursor which is an organosilicon polymer.
  • PCS polycarbosilane
  • the general PCS manufacturing method is mainly a high temperature pressurization reaction using autoclave using dimethyldichlorosilane (DMDS) as a starting material.
  • DMDS dimethyldichlorosilane
  • the Silane-based gas since the Silane-based gas has a property of igniting at a low temperature, when these gases leak during the reaction, there is a problem in safety such as the risk of ignition.
  • the oxygen content in the silicon carbide fiber is mixed by about 10% to form an oxycarbide amorphous in the form of SiCOx, which is thermally decomposed at a high temperature to cause a significant degradation of the physical properties of the fiber.
  • Nippon Carbon manufactures SiC fiber with oxygen content of 1% or less by stabilizing by using electron beam irradiation instead of thermal oxidation method to improve the heat resistance of SiC fiber, so that the tensile strength does not decrease even at high temperature of 1,500 oC.
  • the super heat-resistant silicon carbide fiber was developed.
  • the CVD method is very difficult to fabricate and manufacture a fiber having a diameter of 150 um or more, which is difficult to weave the fiber, and the precursor method has a high oxygen content in silicon carbide fibers, a low production yield, and an oxycarbide amorphous to form a high temperature. This causes a great decrease in the physical properties of the fiber.
  • This patent relates to a ceramic heater for heating a sensor employing a composite electrode type heater electrode formed on a sensor heating heater substrate, which uses a high purity alumina powder and MgO additive of 99.999% or more to form a heater substrate.
  • a ceramic heater for heating a sensor employing a composite electrode type heater electrode formed on a sensor heating heater substrate, which uses a high purity alumina powder and MgO additive of 99.999% or more to form a heater substrate.
  • This patent discloses electrical resistance to a level suitable for heating element use by reacting and sintering a molding sprayed with silicon powder, and then volatilizing the remaining silicon, reacting with silicon which is not volatilized by doping with nitrogen, and completely removing silicon from the heating element. Since the silicon carbide heating element is doped with nitrogen in the silicon carbide lattice, there is a flow charge carrier, so it has a rapid temperature increase characteristic at low temperature, and the resistance increases as the temperature increases, thereby overheating itself. It suggests a technology that has the advantage of suppressing it.
  • This patent relates to a ceramic heating element composition, a dielectric heating device and a dielectric heating method using the same, in particular, a ceramic heating element that can reduce the occurrence of hot spots (hot spots) and increase the temperature increase rate and heat storage time
  • a ceramic heating element that can reduce the occurrence of hot spots (hot spots) and increase the temperature increase rate and heat storage time
  • high-efficiency heaters can be widely used throughout the industry, such as individual heating, industrial and agricultural dryers, industrial annealing furnaces, cooking cooking ovens.
  • the heating device adopts an eco-friendly or high-efficiency method that utilizes solar, wind, and midnight electricity.
  • This patent relates to a ceramic heater for heating a sensor employing a composite electrode type heater electrode formed on a sensor heating heater substrate, which uses a high purity alumina powder and MgO additive of 99.999% or more to form a heater substrate.
  • a ceramic heater for heating a sensor employing a composite electrode type heater electrode formed on a sensor heating heater substrate, which uses a high purity alumina powder and MgO additive of 99.999% or more to form a heater substrate.
  • This patent discloses electrical resistance to a level suitable for heating element use by reacting and sintering a molding sprayed with silicon powder, and then volatilizing the remaining silicon, reacting with silicon which is not volatilized by doping with nitrogen, and completely removing silicon from the heating element. Since the silicon carbide heating element is doped with nitrogen in the silicon carbide lattice, there is a flow charge carrier, so it has a rapid temperature increase characteristic at low temperature, and the resistance increases as the temperature increases, thereby overheating itself. It suggests a technology that has the advantage of suppressing it.
  • the present patent relates to a ceramic heating element composition, a dielectric heating apparatus and a dielectric heating method using the same, in particular, the ceramic heating element composition, dielectric that can reduce the occurrence of hot spots and increase the temperature increase rate and heat storage time A heating heater and a dielectric heating method using the same.
  • This patent discloses a method of manufacturing a porous silicon carbide heating element that is excellent in infrared radiation efficiency, high temperature stability and durability, and can be applied economically and easily to a radiator heater.
  • porous silicon carbide having excellent thermal efficiency is used by using a porous polymer foam that is easy to process and cut without directly processing a silicon carbide material having high hardness, which is difficult to process such as cutting or polishing.
  • the heating element can be manufactured easily and economically in an optimized form.
  • the porous silicon carbide heating element manufactured according to the present invention has a pore structure, which enables instant heating by flame when burning fuel gas, induces complete combustion of fuel gas, and prevents backfire of flame in pores. Combustion takes place, resulting in very good thermal efficiency.
  • metal heating elements As a heating element of the heating method using electricity, metal heating elements have been mainly used, and inexpensive nichrome wire, iron chromium wire, and cantal wire (Fe-Cr-Al) are used as the metal heating material, but power consumption is high. Due to its high and brittleness due to heat, its structural stability is weak at high temperatures.
  • a thick ceramic heating element that is relatively stable at high temperature is widely used.
  • Ceramic heating elements made of molybdenum disilicide (MoSi2) or silicon carbide (SiC) are used as industrial heating elements.
  • MoSi2 molybdenum disilicide
  • SiC silicon carbide
  • the inrush current is very high under the household line voltage (110V or 220V).
  • line voltage 110V or 220V.
  • conventional ceramic heating elements have been required to use expensive transformers that drop voltage from line voltage.
  • the conventional thick ceramic heating element is to directly use the commercial power (110V or 220V) as a home heating device, it is necessary to increase the length or reduce the cross-sectional area based on the basic resistance formula below.
  • R ⁇ * L / A, ( ⁇ : resistivity, L: length, A: cross-sectional area)
  • the present invention in a simpler method, the ceramic heating element is stripped from various ceramic powder molding methods such as sintering, and the silicon carbide fibers and the metal doped carbonization by a gas infiltration reaction. It is an object of the present invention to provide a method for directly producing silicon fibers, and to provide applications such as silicon carbide fibers and fibrous ceramic heating elements using the same, and further, heating devices.
  • the present invention relates to a method of manufacturing a fibrous ceramic heating element by a gas infiltration reaction sublimated at a high temperature, in particular, a method of manufacturing a fibrous ceramic heating element through a process of directly manufacturing silicon carbide fibers from carbon fibers and thereby It is an object to provide an application such as a heating element.
  • an object of the present invention is to provide a method for producing a low-oxygen, dense crystalline silicon carbide fibers in order to improve the high temperature thermal stability of the silicon carbide fibers to provide a method for producing a fibrous ceramic heating element and thereby a heating element.
  • the present invention is to produce a nano-doped silicon carbide fiber including a doping source in the gas permeation reaction in order to improve the oxidation resistance, heat resistance and the like of the silicon carbide fiber, and a method for producing a fibrous ceramic heating element using the same It is an object to provide an application such as a heating element.
  • an object of the present invention is to provide a silicon carbide fiber having a diameter of 5 to 100 um from the gas permeation reaction, a method of manufacturing a fibrous ceramic heating element using the same, and a heating element thereby.
  • an object of the present invention is to provide a method for producing silicon carbide fibers including a batch or continuous process, a method for producing a fibrous ceramic heating element using the same, and a heating element by the process of directly converting the silicon carbide fibers.
  • the present invention is a fibrous ceramic heating element produced by the gas infiltration reaction (Gas Infiltration Reaction), in addition to silicon carbide fibers (SiCf), glass, alumina, silica, Si3N4, silicate, boron, SiCO, Si-CNO It is an object to provide a silicon carbide fiber, a manufacturing method, a method for producing a fibrous ceramic heating element thereof, and a heating element thereby, which may be a fiber and manufacture these nano-doped fibers.
  • the present invention provides a structure in which a carbon fiber having a predetermined diameter (hereinafter referred to as a 'core carbon fiber') remains in the center (core) portion, and the silicon carbide fiber described above wraps the core carbon fiber in a predetermined thickness on an outer circumferential surface thereof. It aims to do it.
  • a carbon fiber having a predetermined diameter hereinafter referred to as a 'core carbon fiber'
  • the silicon carbide fiber described above wraps the core carbon fiber in a predetermined thickness on an outer circumferential surface thereof. It aims to do it.
  • the present invention is a high efficiency that can generate heat through the resonance within the fiber is absorbed by silicon carbide fibers generated from the magnetron or heat generated by the electrical resistance method, particularly rapid heat generation and can minimize the loss of thermal energy
  • An object of the present invention is to provide a silicon carbide fiber heating element and a heating device using the same.
  • the present invention is to solve the problems as described above, and to directly produce the silicon carbide fibers and nano-doped silicon carbide fibers by the gas infiltration reaction (Gas Infiltration Reaction) by removing from the heating device or the heating element heating device.
  • a heater, heating device or the like having an average diameter of 50 um or less, preferably 50 um or less, more preferably 10 um or less, in which the silicon carbide fiber heating element and the electric resistance or the wavelength of the microwave generated in the magnetron generate heat. It is an object to provide a heat generating device.
  • an object of the present invention is to provide a heat generating apparatus including a heat conductor which is in contact with a silicon carbide fiber heating element and may be a conduit through which a fluid such as heating water flows, and has a power source for stimulating silicon carbide fiber heating element to generate heat. .
  • Sublimation raw material and carbon fiber selected from silicon or silicon dioxide, or mixtures thereof are placed in a vacuum or inert gas atmosphere and at a high temperature so that sublimation of the sublimation raw material is carried out from the carbon carbide from the carbon carbide by gas infiltration reaction. By making fibers.
  • Sublimation raw materials and fibrous materials are placed in a vacuum or inert gas atmosphere and at a high temperature, and then the glass, alumina, silica, Si3N4, silicate, boron, It is made of SiCO, Si-CNO fiber and used as heating element.
  • the nano-doped silicon carbide fibers are prepared by placing the doping source together with the carbon fibers at a higher temperature.
  • the metal is selected from the group consisting of titanium, aluminum, zirconium, molybdenum, boron, halogen, or combinations thereof,
  • Gas permeation reaction temperature is made by heating to 1,000 ⁇ 2,000 oC at a temperature increase rate of 5 ⁇ 20 oC / min,
  • Si / C element content of the prepared silicon carbide fiber is 0.01 ⁇ 2.0
  • Oxygen content of the manufactured silicon carbide fiber is less than 2.0%
  • Carbon fiber refers to carbon fiber made of a precursor of a fiber such as polyacrylonitrile, pitch or rayon,
  • the monofilament diameter of this carbon silicon fiber is 5-100um.
  • the silicon carbide fiber heating element according to the present invention in order to achieve the above object
  • Any sublimation raw material and carbon fiber selected from silicon or silicon dioxide, or mixtures thereof are placed in a vacuum or inert gas atmosphere and a high temperature state,
  • Heat is generated by applying a microwave, or heat generated by the electrical resistance method.
  • the heat conductor is a pipeline through which a fluid flows
  • the power supply unit preferably includes a magnetron for generating microwaves for resonance and heat generation of the silicon carbide fiber heating element.
  • the carbon fiber is directly converted into silicon carbide fiber by sublimation gas permeation reaction at high temperature (other glass, alumina, silica, Si3N4, silicate, boron, SiCO, Si-CNO fibers are also available).
  • the heating element can be continuously produced, it is possible to produce crystalline silicon carbide fibers with excellent physical properties by controlling the reaction conditions, in particular, to produce doped source doped silicon carbide fibers with improved oxidation resistance, heat resistance, etc. It has excellent heat resistance, corrosion resistance and electrical characteristics, so it can be used in high-tech electrical, electronic, chemical, physics and other industrial fields,
  • heating element that can be utilized in a furnace, a power plant, an industrial / agricultural drying furnace, a household heating device or a cooking heating device (hot plate, electric range, etc.) and various heating devices using the same.
  • the silicon carbide fiber heating element and the heating device using the same according to the present invention the wavelength of the microwave generated from the magnetron is absorbed by the silicon carbide fiber and can be rapidly generated within a short time through the resonance in the fiber or through the electrical resistance method In addition, the loss of thermal energy can be minimized to provide high efficiency characteristics.
  • the heating device uses a rapid heating highly efficient silicon carbide fiber heating element, thereby providing a rapid heating characteristic that can be minimized with loss of thermal energy.
  • High-efficiency silicon carbide fiber heating element that can be applied to various heating elements regardless of the shape of various heaters or heaters, and can be heated while minimizing the loss of thermal energy by allowing heat to be rapidly generated and heated in a short time. It is possible to provide a heating device using.
  • FIG. 1 is a schematic diagram showing a process of forming a silicon carbide layer from the surface of the carbon fiber by the gas permeation reaction by the method for producing a silicon carbide fiber heating element according to the present invention.
  • FIG. 2 is an enlarged photograph of a silicon carbide fiber heating element generated by microwaves.
  • FIG. 3 is a conceptual diagram of a heating device having a magnetron according to the present invention.
  • Figure 4 is a schematic diagram of a heating device using a silicon carbide fiber heating element according to the present invention.
  • heating device 110 casing
  • first and / or second may be used to describe various components, but the components are not limited to the terms. The terms are only for the purpose of distinguishing one component from other components, for example, without departing from the scope of the rights according to the inventive concept, the first component may be called a second component, and For example, the second component may also be referred to as a first component.
  • Sublimation of any sublimation raw material selected from silicon or silicon dioxide, or a mixture thereof is made from carbon fibers disposed together by a sublimated gas infiltration reaction. .
  • This gas permeation reaction is preferably carried out in a vacuum or inert gas atmosphere.
  • the silicon carbide fiber, the heating element and the heating device using the same according to the present invention to further arrange a doping source to produce a silicon carbide fiber doped with the doping source to the physical properties such as oxidation resistance and heat resistance It is desirable to produce improved silicon carbide fibers and heating elements thereof.
  • the doping source is preferably selected from the group consisting of titanium, aluminum, zirconium, molybdenum, boron, halogen or combinations thereof.
  • These doped source particles may be disposed on the SiC surface or may be disposed in the SiC particles.
  • the method for producing the silicon carbide fiber and the heating element according to the present invention is a step of converting the silicon carbide fiber directly into a batch or continuous process.
  • the silicon carbide fiber and its heating element are manufactured from carbon fibers (Silicon Carbide Fibers, SiCf) in addition to glass, alumina, silica, Si3N4, silicate, boron (Boron Nitride , BNf), etc.), SiCO, Si-CNO fibers, and also a doping source is further arranged to provide these ceramic fibers doped with doping source particles (elements, etc.).
  • the gas permeation reaction temperature is preferably made by heating to 1,000 ⁇ 2,000 oC at a temperature increase rate of 5 ⁇ 20 oC / min.
  • the carbon fiber as the base material means a carbon fiber made of a precursor of a fiber such as polyacrylonitrile, pitch or rayon, and the diameter of the carbon fiber is preferably 5 to 100 um.
  • Silicon carbide fibers and the heating element according to the production method according to the invention is preferably Si / C element content of 0.01 ⁇ 2.0, the oxygen content of silicon carbide fibers is preferably 2.0% or less.
  • the silicon carbide fiber and the heating element of the present invention is preferably used as a heating element, silicon carbide fiber consisting of components such as Si-C, Si-OC, Si-CNO and silicon carbide fibers having a monofilament diameter of 5 to 100 um. Do.
  • silicon carbide fiber heating element of the present invention may be utilized by processing into various shapes such as mesh, plate, rod and the like through secondary processing such as weaving or lamination to apply to various heating devices such as industrial, agricultural, and household.
  • Sublimation raw material and carbon fiber selected from silicon or silicon dioxide, or mixtures thereof are placed in a batch electric furnace equipped with alumina tube, and then carbonized by heating to 1,000 to 2,000 oC at a temperature of 10 oC / min at a temperature of 10 oC / min under nitrogen or argon gas atmosphere.
  • a silicon carbide fiber heating element that can be used as a silicon fiber heating element was prepared.
  • the carbon fibers After placing a sublimation raw material selected from silicon or silicon dioxide or a mixture thereof in a continuous electric furnace equipped with alumina tubes, the carbon fibers are placed in an alumina tube.
  • the winding speed of the fiber winding machine is set to the desired level according to the desired production speed, thereby producing silicon carbide fibers which can be used as a silicon carbide fiber heating element continuously.
  • the diffusion reaction time was varied by 30 minutes (Example 1), 60 minutes (Example 2), 120 minutes (Example 3).
  • 0.1 wt% titanium (Example 4), aluminum 0.1 wt% (Example 5), zirconium 0.1 wt% (Example 6), molybdenum 0.1 wt% (Example 7), 0.1 wt% of boron in the sublimation raw material from Preparation Example 1 % (Example 8) was further mixed with each other to sublimate for 120 minutes at a sublimation temperature of 1750 oC to perform the diffusion reaction of the sublimation gas and carbon fiber, which can be used as a silicon carbide fiber heating element, doped silicon carbide fibers doped with a doping source And the heating element was manufactured.
  • the silicon carbide fiber which can be used as a silicon carbide fiber heating element was continuously manufactured at a sublimation temperature of 1,750 ° C. under a nitrogen or argon gas atmosphere at a speed of 3 cm / min.
  • FIG. 1 is a schematic diagram showing a silicon carbide layer formed from a carbon fiber surface by a sublimation gas infiltration reaction and a SEM analysis photograph of silicon carbide fibers at a specific time period. have),
  • the diameter of the carbon fiber (core shell) is preferably 1 to 3 ⁇ m.
  • a silicon carbide fiber doped with a doping source (Ti) according to Example 4 was prepared and used as a silicon carbide fiber heating element, and an exothermic experiment was performed with a heating element in a heating device equipped with a magnetron.
  • the reticulated silicon carbide fiber heating element (L 150mm ⁇ W 150mm ⁇ H 5mm) generates heat even at low power of 300W or less, and in particular, generates heat at a high temperature of 1,000 ° C. or more within 4 seconds. It was confirmed that.
  • the heating device preferably comprises a silicon carbide fiber heating element manufactured through the sublimation gas penetration reaction, and a magnetron for generating microwaves for resonance and heat generation of the heating element.
  • the heating device using the silicon carbide fiber heating element according to the present invention may be composed of an electric resistance type heating device including a power supply unit for stimulating the silicon carbide fiber heating element to generate heat (silicon carbide fiber heating element of a unit volume).
  • an electric resistance type heating device including a power supply unit for stimulating the silicon carbide fiber heating element to generate heat (silicon carbide fiber heating element of a unit volume).
  • heating by electric resistance method by adding power consumption of 17w, 35V, 0.49A, rapid heating to 1,000 ° C or more within 2 seconds, showing faster cooling behavior than the conventional heating element).
  • the silicon carbide fiber heating element rapidly generates heat within a short time of 2 to 5 seconds through wavelength absorption and resonance of the microwave generated from the magnetron, and due to the characteristics of the fiber, it is possible to minimize the loss of thermal energy, thereby achieving high efficiency characteristics. It can be secured.
  • the heating device which forms the core of the present invention is a silicon carbide fiber heating element
  • a heat conductor in contact with the silicon carbide fiber heating element A heat conductor in contact with the silicon carbide fiber heating element
  • It comprises a power supply for stimulating the silicon carbide fiber heating element to generate heat.
  • the heat conductor may be a metal panel, and the heating device may be a cooking utensil, a heating device, a dryer, or the like.
  • the power supply unit may include a magnetron for generating a microwave for the resonance and heat generation of the silicon carbide fiber heating element, the silicon carbide fiber heating element may take the form of electric resistance heating if necessary.
  • the power supply unit may include a magnetron for generating microwaves for resonance and heat generation of the silicon carbide fiber heating element.
  • the silicon carbide fiber heating element is preferably a silicon carbide fiber heating element manufactured through the sublimation gas penetration reaction described above.
  • FIG. 4 there is shown a conceptual diagram of a kind of hot air blower or boiler 100 showing a form in which the heat conductor is a conduit 111 through which a fluid flows.
  • the heat generating device 100 is provided with a silicon carbide fiber heating element 114 and a conduit 111 which is a heat conductor in contact with the casing 110.
  • Fluid flows through the conduit 111, and when the fluid is air supplied by a blower (not shown), the heat generating device is configured as a hot air blower, and the fluid is supplied by the circulation pump (not shown).
  • the heating device constitutes a boiler 100 that is a heating device.
  • the pipe 111 is preferably surrounded by a heat insulating material 112 to prevent heat loss, it is preferable to use a material having excellent thermal conductivity, such as copper.
  • the heat insulating material 112 is preferably a non-combustible material that can be used even at a high temperature (1300 °C or more) heating temperature.
  • the power supply unit for stimulating and heating the silicon carbide fiber heating element 114 generates a microwave, and a waveguide for guiding the microwaves generated from the magnetron 120 to the silicon carbide fiber heating element 114. 130).
  • a relay body 113 is further provided between the heat insulator 112 and the heating element 114 to be used as an additional waveguide member, and the microwave generated from the magnetron 120 is a waveguide 130 and a relay body ( It is guided to the silicon carbide fiber heating element 114 through 113, the relay body may utilize a ceramic material.
  • the casing 120 preferably employs a material (eg, SUS) for preventing microwaves from being released to the outside and protecting internal components from external shocks.
  • a material eg, SUS
  • the microwave generated from the magnetron is transferred to the silicon carbide fiber heating element through the heat insulating material and the relay (ceramic) inside the casing via the waveguide, and the silicon carbide fiber is finally delivered to the wavelength of the microwave.
  • the silicon carbide fibers generated by resonance and heat generation can heat the heating water passing through the adjacent pipe line by the heat rapidly increasing between 1 to 5 seconds.
  • FIG. 4 describes that the silicon carbide fiber heating element is disposed only in the lower part of the conduit, the silicon carbide fiber heating element may be configured to surround the conduit.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Resistance Heating (AREA)

Abstract

La présente invention concerne un procédé permettant de produire directement une fibre de carbure de silicium et une fibre de carbure de silicium dopée par un métal en convertissant la fibre de carbure dans la fibre de carbure de silicium et la fibre de carbure de silicium dopée par un métal par le biais d'une réaction d'infiltration de gaz à haute température plus simple qu'un procédé de production classique. Plus particulièrement, la présente invention concerne un procédé de production d'une fibre de carbure de silicium et d'une fibre de carbure de silicium dopée par un métal par le biais d'une étape de sublimation à haute température et d'une étape consistant à disposer des éléments métalliques supplémentaires, une fibre de carbure de silicium produite par ce procédé, et une application d'un élément chauffant à fibre de carbure de silicium et d'un dispositif de chauffage l'utilisant, etc. Selon la présente invention, le procédé de production est simple, et il est possible de produire de façon continue une fibre de carbure de silicium cristallin qui possède une faible teneur en oxygène et d'excellentes propriétés physiques. En particulier, il est possible de produire une fibre de carbure de silicium dopée par un métal présentant une résistance améliorée à l'oxydation, une résistance thermique, etc.
PCT/KR2016/002609 2015-06-25 2016-03-16 Procédé de production d'une fibre de carbure de silicium, fibre de carbure de silicium et élément chauffant à fibre de carbure de silicium produit à l'aide de celle-ci, et dispositif de chauffage l'utilisant Ceased WO2016208846A1 (fr)

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
KR10-2015-0090437 2015-06-25
KR1020150090437A KR101684600B1 (ko) 2015-06-25 2015-06-25 탄화규소 섬유의 제조방법 및 이에 의한 탄화규소 섬유
KR1020150150501A KR101732573B1 (ko) 2015-10-28 2015-10-28 섬유상 세라믹 발열체 및 그 제조방법
KR10-2015-0150501 2015-10-28
KR1020160006913A KR101734472B1 (ko) 2016-01-20 2016-01-20 마이크로웨이브를 이용한 탄화규소 섬유 발열체 및 이를 이용한 발열장치
KR10-2016-0006913 2016-01-20

Publications (1)

Publication Number Publication Date
WO2016208846A1 true WO2016208846A1 (fr) 2016-12-29

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PCT/KR2016/002609 Ceased WO2016208846A1 (fr) 2015-06-25 2016-03-16 Procédé de production d'une fibre de carbure de silicium, fibre de carbure de silicium et élément chauffant à fibre de carbure de silicium produit à l'aide de celle-ci, et dispositif de chauffage l'utilisant

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WO (1) WO2016208846A1 (fr)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000129413A (ja) * 1998-08-21 2000-05-09 Osaka Gas Co Ltd 炭素繊維含有金属材料およびその製造方法
JP2002266170A (ja) * 2000-12-20 2002-09-18 Showa Denko Kk 分岐状気相法炭素繊維、透明導電性組成物及びその用途
KR20090093203A (ko) * 2008-02-28 2009-09-02 충남대학교산학협력단 금속 촉매가 균일하게 증착된 수소저장매체용 탄소나노섬유및 그 제조방법
JP2009298610A (ja) * 2008-06-11 2009-12-24 Shin-Etsu Chemical Co Ltd 炭化ケイ素チューブの製造方法
KR20140095137A (ko) * 2013-01-23 2014-08-01 주식회사 비엠에스이앤씨 마이크로파를 이용한 배수구 동결 방지 장치 및 동결 방지 방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000129413A (ja) * 1998-08-21 2000-05-09 Osaka Gas Co Ltd 炭素繊維含有金属材料およびその製造方法
JP2002266170A (ja) * 2000-12-20 2002-09-18 Showa Denko Kk 分岐状気相法炭素繊維、透明導電性組成物及びその用途
KR20090093203A (ko) * 2008-02-28 2009-09-02 충남대학교산학협력단 금속 촉매가 균일하게 증착된 수소저장매체용 탄소나노섬유및 그 제조방법
JP2009298610A (ja) * 2008-06-11 2009-12-24 Shin-Etsu Chemical Co Ltd 炭化ケイ素チューブの製造方法
KR20140095137A (ko) * 2013-01-23 2014-08-01 주식회사 비엠에스이앤씨 마이크로파를 이용한 배수구 동결 방지 장치 및 동결 방지 방법

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