WO2017146391A1 - Composition de chauffage au carbone et procédé de fabrication d'élément de chauffage au carbone utilisant celle-ci - Google Patents

Composition de chauffage au carbone et procédé de fabrication d'élément de chauffage au carbone utilisant celle-ci Download PDF

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WO2017146391A1
WO2017146391A1 PCT/KR2017/001141 KR2017001141W WO2017146391A1 WO 2017146391 A1 WO2017146391 A1 WO 2017146391A1 KR 2017001141 W KR2017001141 W KR 2017001141W WO 2017146391 A1 WO2017146391 A1 WO 2017146391A1
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carbon
weight
heating
exothermic composition
composition
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Korean (ko)
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김민규
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    • 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
    • H05B3/10—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
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017—Manufacturing methods or apparatus for heaters

Definitions

  • the present invention relates to a carbon heating composition and a method for producing a carbon heating element using the same, and more particularly, a carbon heating composition for producing a carbon heating element by vapor-depositing a heating composition containing carbon on various insulators in a thin film and a carbon heating element using the same It relates to a manufacturing method of.
  • Conventional heating elements were used by winding a metal wire such as a nichrome wire or a Kanthal wire in coil form with an electric wire.
  • This heating element had a number of problems, the most characteristic is the low conversion efficiency of converting the electrical resistance into thermal energy, the consumption of electricity is high, air pollution and the like.
  • the carbon heating element uses a carbon material as a heating means, and the carbon material has conductivity and electrostatic resistance, can evenly distribute currents throughout the heating element, and is environmentally safe, inexpensive, and relatively easy to handle. have.
  • the carbon heating element was manufactured by a method of forming a heating layer on the surface of a substrate using a composition composed of a carbon material, ie, a graphite, carbon black, carbon nanotube, etc., as a dispersant and a synthetic resin binder.
  • the carbon material is precipitated to the lower portion of the heat generating layer, so that the overall electrical conductivity is nonuniform.
  • the carbon material when used as a conductive material only carbon material, there was also a disadvantage of poor conductivity.
  • such a carbon heating element has a disadvantage in that it is difficult to manufacture a thin film due to low resistance value and durability.
  • Prior literatures related to the present invention include Korean Patent Publication No. 10-1994-0014694, Korean Patent Registration No. 10-1573142, and the like.
  • an object of the present invention is to provide a carbon exothermic composition having excellent conductivity by forming a carbon exothermic composition from graphite, stannic chloride, antimony chloride, bismuth chloride, molybdenum, germanium, aluminum and the like.
  • vapor deposition of the carbon exothermic composition on a variety of insulators in a thin film provides not only excellent conductivity and durability, but also a carbon exothermic body having a uniform resistance value and a constant exothermic temperature.
  • Carbon exothermic composition of the present invention for achieving the above object graphite, ditin (SnCl 4 ), antimony trichloride (SbCl 3 ), bismuth chloride (BiCl 3 ), molybdenum (Mo), aluminum (Al), It is characterized by including germanium (Ge), acetic acid (acetic acid) and a surfactant.
  • the graphite 25 to 35% by weight chloride of tin (SnCl 4) 15 ⁇ 25 wt%, antimony trichloride (SbCl 3) 2 ⁇ 4 wt% of chloride, bismuth (BiCl 3) 0.5 ⁇ 1.5 wt%, molybdenum (Mo) 0.5 to 1.5% by weight, aluminum (Al) 1 to 3% by weight, germanium (Ge) 2 to 4% by weight, acetic acid (acetic acid) 7 to 13% by weight and 25 to 35% by weight do.
  • the method for producing a carbon heating element comprises the steps of (a) mixing graphite, surfactant and acetic acid, (b) dissolving stannic chloride in ethanol, and (c) step (a) Mixing the mixture with the solution of step (b), (d) adding antimony trichloride, bismuth chloride, molybdenum, aluminum and germanium to the mixture of step (c), stirring and mixing, (e) A) preparing a carbon exothermic composition by aging the mixture of step (d) for 20-30 hours, and (f) evaporating the carbon exothermic composition prepared in step (e) by gas phase evaporation. And depositing electrodes on the surface of the substrate, and (g) forming electrodes at both ends of the deposition layer of step (f).
  • step (f) after placing the substrate in the main furnace in the electric furnace, placing the carbon exothermic composition on the evaporation zone in the electric furnace, the carbon exothermic composition in the vapor state is vaporized while evaporating the carbon exothermic composition. It is characterized in that to deposit on.
  • the carbon heating composition and the carbon heating element according to the present invention have a high conductivity and excellent heat generation capacity and energy efficiency to suppress power waste and have excellent durability.
  • the resistance of the heating layer is uniform, the heating temperature is constant, and not only radiates far-infrared rays, which are beneficial to the human body, the manufacturing process is simple, economical and does not cause environmental pollution, and thus may be usefully applied as a heating element in various fields.
  • FIG. 1 is a view showing a manufacturing procedure of the carbon heating element according to the present invention.
  • the present invention is to solve the shortcomings of the conventional carbon heating element, and for the high conductivity, it is characterized by using not only graphite as the conductive material, but also other non-metal conductive material and metal.
  • the carbon exothermic composition according to the present invention is graphite, tin dichloride (SnCl 4 ), antimony trichloride (SbCl 3 ), bismuth chloride (BiCl 3 ), molybdenum (Mo), aluminum (Al), acetic acid ( acetic acid) and surfactants.
  • the carbon exothermic composition configured as described above is formed in consideration of the electrical resistance characteristics of the unit area, the emissivity of far-infrared rays, chemical stability, etc., and has a high conductivity, and can form a carbon exothermic layer as a thin film, and also has durability Has excellent properties.
  • the graphite is a basic component of the carbon exothermic composition according to the present invention.
  • the graphite is an excellent conductive material, environmentally safe, and inexpensive material. Therefore, when the graphite is used as a base component of the carbon heating composition, excellent conductivity, price competitiveness, and the like can be secured.
  • the method of the ball milling is sufficient using a method known in the art to which the technology belongs, the particle size is preferably 2 ⁇ 3000nm.
  • the graphite may be included in 25 to 35% by weight based on 100% by weight of the carbon heating composition excluding the solvent, if the content is less than 25% by weight is poor conductivity, if the content exceeds 35% by weight is dispersed Because there are disadvantages.
  • the tin tin chloride (SnCl 4 ) which is one of the non-metal conductive materials, is also a basic component of the composition of the present invention, which provides excellent conductivity to the heat generating layer so that the heat generating element can generate heat at a high temperature.
  • the tin tin chloride may be included in 15 to 25% by weight based on 100% by weight of the total carbon heating composition excluding the solvent, if the content is less than 15% by weight, the conductivity is poor, if the content exceeds 25% by weight of the heating layer This is because the stability of the.
  • the antimony trichloride (SbCl 3 ) is also a component that provides excellent conductivity to the exothermic layer, it may be included in 2 to 4% by weight based on 100% by weight of the total carbon exothermic composition excluding the solvent. This is because if the content is less than 2% by weight or more than 4% by weight, the heat generating layer is uneven and resistance becomes uneven.
  • the bismuth chloride (BiCl 3 ) also provides conductivity in the heat generating layer, and also improves durability and thermal stability of the heat generating layer.
  • the bismuth chloride may be included as 0.5 to 1.5% by weight based on 100% by weight of the total carbon exothermic composition excluding the solvent, the content is less than 0.5% by weight, the effect is less than 1.5% by weight rather exothermic This is because the durability of the layer is lowered.
  • the molybdenum (Mo), aluminum (Al) and germanium (Ge) is a metal component for imparting conductivity, and the molybdenum, aluminum, germanium forms a crystal together with graphite and other nonmetallic conductive materials to form a heating layer, that is, a thin film. Form.
  • the germanium radiates a large amount of far-infrared radiation when exothermic, and when applied to an electric heater, an agricultural warmer, or a dryer, may have a beneficial effect on the human body and agricultural products.
  • the molybdenum, aluminum, germanium may be included as molybdenum 0.5 to 1.5% by weight, aluminum 1 to 3% by weight, germanium 2 to 4% by weight, based on 100% by weight of the total carbon heating composition excluding the solvent, each of If the content is less than the reference value, the effect of improving the conductivity is inferior, and if each content exceeds the reference value, there is a disadvantage in that the overall manufacturing cost increases.
  • the acetic acid stabilizes the composition, makes the exothermic layer form a thin film, and improves its durability.
  • the acetic acid may be included in the range of 7 to 13% by weight based on 100% by weight of the total carbon exothermic composition, excluding the solvent, if the content is too small, the above-mentioned effect is insignificant, and when the excess is excessive, it will adversely affect the conductivity Because it's crazy.
  • the surfactant is to improve the dispersibility of the graphite, it is possible to use a variety of nonionic, cationic, anionic surfactants known in the art. Silicone glycol copolymers can be used as an example of the surfactant.
  • Such a surfactant may be included in 25 to 35% by weight based on 100% by weight of the total carbon exothermic composition excluding the solvent.
  • the carbon exothermic composition according to the present invention containing the above components may further include a solvent, preferably using ethanol as a solvent.
  • the solvent may include about 0.8 to about 1.2 weight ratios of the above composition, that is, the carbon exothermic composition except the solvent, but is not necessarily limited thereto. This is because the solvent is a component that is volatilized during the production of the heating element, and thus does not affect the physical properties such as overall conductivity and durability.
  • the carbon exothermic composition configured as described above includes a carbon material as a conductive material as well as a non-metal conductive material such as antimony trichloride and bismuth chloride, and a metal material such as molybdenum, aluminum, germanium, and the like. Compared to the example using only the non-metallic conductive material alone except for a significantly superior conductivity, as well as excellent durability.
  • the carbon heating element of the present invention is a thin film heating layer is formed on the surface of the substrate, the heating layer is formed by depositing the carbon heating composition described above.
  • the substrate may be made of glass, quartz, of course, materials other than the above, and the shape may also be various shapes such as a plate and a ring, and the type and shape of the substrate are not limited.
  • the manufactured carbon heating element may be applied to various devices such as heating, hot water supply, drying, food cooking, etc. requiring high temperature or heat, and the type of the heating element is not limited.
  • Such a method for producing a carbon heating element comprises the steps of: (a) mixing graphite, surfactant and acetic acid, (b) dissolving ditin chloride in ethanol, and (c) step (a) Mixing the mixture of (b) and the solution of step (b), (d) adding antimony trichloride, bismuth chloride, molybdenum, aluminum and germanium to the mixture of step (c), stirring and mixing, ( e) aging the mixture of step (d) for 20 to 30 hours to prepare a carbon exothermic composition, and (f) evaporating the carbon exothermic composition prepared through step (e) by gas phase evaporation. And depositing a heating layer on the surface of the substrate, and (g) forming electrodes at both ends of the heating layer.
  • graphite, surfactant, and acetic acid are measured to suit each content ratio, and then, they are added to a blender and mixed for about 15 to 25 minutes. At this time, the graphite is used that is pulverized into nanoparticles of 2 ⁇ 3000nm size by a ball mill.
  • ethanol and tin dichloride are also measured to meet the respective content ratios, and then the tin tin chloride is added to ethanol and dissolved therein.
  • step (c) mixing the mixture of step (a) and the solution of step (b).
  • step (a) is added to the solution of step (b) and mixed.
  • the mixing is simply enough to add the mixture of step (a) to the solution of step (b), and does not need to be stirred separately.
  • step (d) adding antimony trichloride, bismuth chloride, molybdenum, aluminum and germanium to the mixture of step (c), followed by stirring and mixing.
  • step (c) antimony trichloride, bismuth chloride, molybdenum, aluminum and germanium are measured according to the content ratio, and then this is added to the mixture of step (c). And it is stirred for about 90 to 150 minutes using a stirrer. At this time, the temperature of the stirrer is to be 45 ⁇ 55 °C degree so that the stirring and mixing is sufficiently made.
  • the reason for separating and mixing each component in the steps (a), (b), (c), and (d) in the present invention is for ease of mixing of each component, as well as for chemical stabilization of the mixture.
  • step (e) aging the mixture of step (d) for 20-30 hours to prepare a carbon exothermic composition.
  • the preparation of the carbon exothermic composition is completed.
  • the above-mentioned natural aging is sufficient if the composition is left at about room temperature (15 to 30 ° C).
  • step (f) evaporating the carbon exothermic composition prepared in step (e) by gas phase evaporation and depositing it on the surface of the substrate.
  • the carbon exothermic composition prepared in step (e) is deposited on the surface of the substrate by vapor deposition to form a exothermic layer.
  • the vapor deposition method it is preferable to use a nano-vapor deposition method different from the conventional physical vapor deposition (PVD) or chemical vapor deposition (CVD), through the nano-vapor deposition method
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • the above-described nano-vapor deposition method is to deposit in an electric furnace including a main zone and an evaporation zone, and first, the substrate is fixed on the top of the main zone. And the fixed base material is preheated for 20 to 40 minutes about 500-1000 degreeC. This preheating is for the safe deposition of the heating layer, it is possible to improve the durability and resistance of the heating element.
  • the carbon exothermic composition is all evaporated by placing the carbon exothermic composition prepared before the evaporation zone in the electric furnace.
  • the temperature of the evaporation zone is about 200 ⁇ 300 °C.
  • the solvent is volatilized and only the remaining components are vaporized, in which the molecules are uniformly deposited on the surface of the substrate.
  • the thickness of the deposition layer that is, the heating layer can be controlled by the amount of the carbon heating composition to be placed on the evaporation bar, since the molecules are deposited in a vaporized state, it is possible to form a thin film, forming a uniform resistance will be. Therefore, the thickness of the heat generating layer is adjusted according to the desired amount of heat generated.
  • the substrate is not a plate-shaped it can be natural to form a uniform heating layer through the rotation of the substrate.
  • the substrate on which deposition is completed is subjected to post-heating for about 5 to 15 minutes at about 350 to 450 ° C., and gradually cooled at room temperature.
  • step (g) forming electrodes at both ends of the deposition layer of step (f).
  • an electrode for applying a voltage to both ends of the deposition layer, that is, the heating layer is formed.
  • the electrodes may be formed in at least one pair in the longitudinal or transverse direction of the heating layer.
  • the material for forming the electrode is not limited, but silver powder having excellent conductivity is used. Specifically, the electrode solution prepared by mixing silver powder with rosin at a ratio of 1: 0.5 to 1 by volume is smeared on both ends of the heat generating layer.
  • an electrode may be formed using a known electrode material and method.
  • the heating element of the present invention is excellent in the electrical resistance characteristics for the unit area, it is possible to generate a high temperature, has a uniform resistance value and excellent durability. In addition, it not only radiates far infrared rays, it is excellent in energy conversion efficiency can reduce power, there is an advantage that the manufacturing process can be lowered because the manufacturing process is simple, unlike the prior art.
  • the carbon heating element according to the present invention the heating (bedding) such as heating mats or pads, residential heating, such as floor heating in apartments or general houses, industrial heating in the office or workplace, printing drying and It can be applied to various industrial heating devices such as coating dryness, agricultural facilities such as vinyl houses and barns, agricultural product drying systems, and freezing prevention devices for melting snow on roads and parking lots.
  • a heat generating composition having a composition as shown in Table 1.
  • a heat generating layer was formed on one side of the ceramic plate of 200mm ⁇ 200mm ⁇ 10mm size using the prepared heating composition.
  • the formation of the heat generating layer is fixed to the main of the electric furnace, preheated at 800 ° C. for 30 minutes, and 20 g of each heat generating composition is placed on the evaporation table (temperature of about 230 ° C.) of the electric furnace (mainly about 700 ° C.). And all evaporated.
  • the temperature of the electric furnace was about 400 ° C., followed by 10 minutes of heating, and the post-heating ceramic plate was gradually cooled at room temperature.
  • the electrode After coating the electrode at both ends of the deposited layer, and dried at 25 °C for about 2 hours, it was put in an electrode forming furnace and heated for 2 hours at 200 °C, and further heated at 800 °C 1 hour It was aged to room temperature in the electrode forming furnace.
  • the electrode was an electrode solution in which silver powder and rosin were mixed in a 1: 1 volume ratio.
  • Example 2 It carried out similarly to Example 1, but did not use graphite, molybdenum, aluminum, and germanium.
  • Example 2 The same procedure as in Example 1 was carried out, but no ditin, antimony trichloride, or bismuth chloride was used.

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  • Resistance Heating (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)

Abstract

La composition de chauffage au carbone et l'élément de chauffage au carbone selon la présente invention présentent des avantages selon lesquels la conductivité est élevée, de sorte qu'une quantité de chauffage par surface unitaire et le rendement énergétique soient excellents, ce qui évite de gaspiller de l'énergie, et la durabilité est excellente. De plus, une couche de chauffage a une valeur de résistance uniforme de sorte que la température de chauffage soit constante, des rayons infrarouges lointains bénéfiques pour le corps humain soient émis, et un procédé de fabrication soit simple et économique, et n'entraîne pas de contamination environnementale. Ainsi, la présente invention peut être appliquée utilement à divers domaines en tant qu'élément chauffant.
PCT/KR2017/001141 2016-02-26 2017-02-02 Composition de chauffage au carbone et procédé de fabrication d'élément de chauffage au carbone utilisant celle-ci Ceased WO2017146391A1 (fr)

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KR1020160023137A KR101637526B1 (ko) 2016-02-26 2016-02-26 탄소 발열 조성물 및 이를 이용한 탄소 발열체의 제조방법
KR10-2016-0023137 2016-02-26

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KR102279537B1 (ko) * 2020-09-28 2021-07-21 주식회사 그린머테리얼솔루션 투명박막발열체용 조성물
JP7162164B1 (ja) * 2021-05-07 2022-10-28 福建晶▲しい▼新材料科技有限公司 半導体電熱膜の前駆体溶液、半導体電熱膜構造、及び電熱構造の製造方法

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