WO2017198233A1 - Matériau composite inorganique à coefficient de température positif, son procédé de fabrication et son application - Google Patents

Matériau composite inorganique à coefficient de température positif, son procédé de fabrication et son application Download PDF

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Publication number
WO2017198233A1
WO2017198233A1 PCT/CN2017/085396 CN2017085396W WO2017198233A1 WO 2017198233 A1 WO2017198233 A1 WO 2017198233A1 CN 2017085396 W CN2017085396 W CN 2017085396W WO 2017198233 A1 WO2017198233 A1 WO 2017198233A1
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ptc
inorganic composite
composite material
carbon
graphite
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PCT/CN2017/085396
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English (en)
Chinese (zh)
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张金柱
栾峰
张明
刘顶
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济南圣泉集团股份有限公司
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Publication of WO2017198233A1 publication Critical patent/WO2017198233A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5001—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with carbon or carbonisable materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
    • H01C7/021—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient formed as one or more layers or coatings
    • 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

Definitions

  • the invention relates to the field of composite material preparation with PTC properties, in particular to a PTC inorganic composite material and a preparation method and application thereof.
  • Carbon crystal heating plate is an emerging heating product. After nearly ten years of development, the technology is becoming more mature. Its characteristics are: 1. Subverting the heating tradition, saving energy and reducing emissions, adapting to the new requirements of the state and society; 2. No troubles with water seepage and water leakage, no troubles for collecting uniform heating costs. It is easy to install and use, that is, it is hot immediately; 3. It has the function of health care; the wavelength is 8-18 microns, and people in this environment for a long time are beneficial to the health of the body. 4. Relying on far-infrared heating and air convection, quiet, no noise, high sense of comfort; 5. Do not dry, release far infrared rays, do not take away the moisture in the air.
  • the solutions are as follows: (1) Develop a PTC material, that is, a material with a positive temperature coefficient. When a certain temperature is exceeded, the resistance value of the material increases with temperature. When the resistance is increased, the current and power are decreased, and the repetition can cause the temperature to fluctuate up and down around the target temperature without overheating. (2) Installing the thermostat, using the thermostat to monitor each board greatly increases the cost. On the other hand, in the case of a malfunction of the thermostat, local high heat may occur, and in a serious case, a fire may occur.
  • patent CN101407628A discloses a method for producing a water-soluble PTC functional conductive carbon paste, and a polymer-containing carbon containing oxide is disclosed in CN104371329A.
  • a method for preparing a slurry and a heating material having a PTC effect, a PTC carbon slurry constant temperature electric heating film is disclosed in the CN202652568U patent, and a PTC effect far infrared radiation heating cloth and a preparation method and use thereof are disclosed in the CN105415830A patent, but these
  • the PTC materials used in the technology are polymer materials or composites of carbon paste and silver paste, including polyethylene, polyurethane, stearic acid, monoglyceride, glycerin, ethylene glycol butyl ether acetate, isothiocyanate. Ester, silver paste, etc. Such materials are not stable.
  • PTC ceramic materials exist in the prior art, they are directly used as electronic devices after sintering.
  • CN104311004A discloses a PTC ceramic material and a method for improving the temperature stability of the PTC ceramic material below the Curie point.
  • CN102173786A discloses a novel PTC ceramic material composition comprising a ceramic phase and a glass phase, characterized in that the ceramic phase is a conventional PTC ceramic material and the glass phase is a PbO-BN material.
  • the content of the PbO-BN material is 1-10% by weight, and the content of the PTC ceramic material is 90-99% by weight.
  • This product uses PbO-BN glass phase to reduce the sintering temperature of PTC ceramic materials, and has high-performance PTC characteristics and a wide range of applications. It can be seen that inorganic ceramic PTC materials are used independently as electronic devices and both require high temperature sintering.
  • a first object of the present invention is to provide a PTC inorganic composite material by combining a nano ceramic material such as an inorganic material with a graphite-based carbon material coating agent, and using a carbon material to encapsulate the inorganic material itself, thereby realizing the carbon material.
  • Conductive, internal insulation effect the material can be applied to electric heating materials, for example, for carbon crystal heating plates, the performance is more stable, there will be no problems such as aging, flatulence, etc., which will bring subversive properties to the performance of the carbon crystal plate itself.
  • the ground lift greatly prolongs the service life and brings considerable economic benefits.
  • a second object of the present invention is to provide a method for preparing the above PTC inorganic composite material, which has the advantages of being able to completely retain the active ingredient of the raw material, and has the advantages of simple and easy operation, mild operating conditions, and no need for a high-temperature carbonization step.
  • a third object of the present invention is to provide the above-mentioned application of the PTC inorganic composite material, which can effectively solve the problem of overheating of the carbon crystal plate and increase of power runaway, and the carbon crystal plate has a frequency conversion function.
  • the increase in resistance causes the power to be appropriately attenuated to adjust to the appropriate power to control the temperature, thereby being more energy efficient than conventional carbon crystal plates.
  • the embodiment of the invention provides a PTC inorganic composite material, which is mainly prepared from the following raw materials: Percentage of mass, nano-ceramic material 75-95%, graphite-based carbon material coating agent 1-20%, dispersing agent 0.5-5%.
  • the present invention provides an inorganic composite material having PTC properties by combining a nano ceramic material with a graphite-based carbon material coating agent.
  • the addition of the PTC inorganic composite material of the invention to the carbon slurry can effectively solve the problem of overheating of the carbon crystal plate and an increase in power runaway.
  • the PTC material allows the carbon crystal plate to have a frequency conversion function. When the temperature gradually reaches the set temperature, the increase in resistance causes the power to be appropriately weakened to adjust to a suitable power to control the temperature, thereby greatly saving energy compared to the conventional carbon crystal plate.
  • Nano-ceramic materials Compared with other materials with PTC properties, this inorganic type of material can effectively prevent the failure of PTC materials caused by decomposition, gas release and aging.
  • the graphite-based carbon material coating agent is coated on the outer surface of the ceramic material, the outer surface has good electrical conductivity, the inner surface has good insulation, and when used as an electric heating material, the far-infrared radiation effect can be improved, and mixed with other carbon materials. Improve the dispersion effect.
  • the graphite-based carbon material coating agent is a nano-sheet carbon material, and the nano-sheet carbon material has a thickness of 100 nm or less, preferably 50 nm or less, more preferably 30 nm or less, including nano-scale graphite, graphene oxide, and graphene. One or several mixtures, preferably graphene.
  • graphene itself has high electrical and thermal conductivity, and has the advantages of light weight, good flexibility, large-area use, and low oxidation resistance. It has far-infrared radiation performance more prominent than other carbon materials.
  • the heating element has the characteristics of high somatosensory temperature and good thermal comfort, so it has the characteristics of excellent electrothermal material.
  • the sheet structure of graphene is also more favorable for completing the coating of the nano ceramic inorganic material particles, and further improving the dispersibility of the inorganic material and the carbon material.
  • the structure of graphene itself includes a single-layer graphene structure and a multi-layer graphene structure, and may be a six-membered ring-shaped honeycomb layer structure of 1-10 layers of carbon, and may also be a single layer, a double layer or a 3-10 layer.
  • any combination of any one or more of the structures it is the graphene having such a lamellar structure that is composite coated with the nanoceramic inorganic material, so that the performance of the ceramic inorganic material is more excellent, and when used in subsequent use Longer life, and the use of graphene to increase the far-infrared ability in subsequent applications, so that heating comfort is further improved, and heating efficiency is improved to indirectly save energy.
  • the invention fully utilizes the advantages of the nano ceramic material and the graphite carbon material coating agent respectively, and the PTC inorganic composite material prepared by using the specific raw material of the invention improves the compatibility of the powder and the carbon slurry on the one hand, It helps to disperse the powder; on the other hand, it makes the surface of such insulator particles have certain conductivity.
  • the inventor has also optimized the optimal addition amount of each raw material through a large number of practices.
  • the amount of nano ceramic material is generally 75-95% (in terms of mass percentage), and may be 80-91%, more preferably 85.
  • the main components include one or more of metal oxides, non-metal oxides, and metal borides, including Ti, Si, Ba, Sn, Cu, Fe, Ag, B, One or several of the O and C elements, of course, if the conditions permit, the nano ceramic material can be prepared by itself.
  • the state of the nano ceramic material is powdery, because the powder shape is favorable for the subsequent uniform formation of the graphene composite.
  • the substance preferably has a particle size of between 0.1 and 10 ⁇ m, and may also be 1 ⁇ m, 2 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or the like.
  • the nano ceramic material used in the present invention is different from the ordinary ceramic material, and the powder is ultra-fineized by nano-crystallization, so that the surface electronic structure and crystal structure of the ceramic material are changed, and a bulk material is produced.
  • the amount of the graphite-based carbon material coating agent is 1-20% (in terms of mass percentage), and may be 5-16%, more preferably 13%, or 2%, 3%, 4%, 6%. 7%, 8%, 9%, etc., the mass ratio of the nano-ceramic material to the graphite-based carbon material coating agent is controlled to be optimal between (5-9):1, and the compounding ratio is obtained under such a ratio.
  • PTC inorganic composite materials have superior performance in all aspects.
  • a dispersing agent is added to the raw material to stabilize the dispersed medium, improve the surface properties of the powder, and adjust the powder.
  • the kinetic action enables the graphite-based carbon material coating agent to effectively coat the inorganic material, and the conventional addition amount is 0.5-5% (in terms of mass percentage), and may also be 1-4%, more preferably 2%.
  • the addition amount may also be 0.7%, 0.9%, 1.2%, 1.4%, 2%, 3%, 4.5%, etc.
  • the amount of the dispersant added as an additive should not be too large (generally not more than 5%), so The range of quantities also needs to be strictly controlled.
  • the type of dispersing agent includes one or more of polyvinyl alcohol, polyethylene glycol, and polypropylene glycol.
  • the preferred choice of polyvinyl alcohol, the dispersing agent of the alcohol can substantially meet the dispersion requirement in the solution of the present invention, and does not need to be used.
  • Other dispersants such as silanes, these types of dispersants are not environmentally friendly, so they are not recommended.
  • the present invention also provides a preferred preparation method of the above composite material, which specifically includes the following steps:
  • Ethanol acts as a solvent to dissolve and disperse, and is not the main raw material.
  • the formula of Ming is not reflected, and there is no certain requirement for the addition amount.
  • the subsequent heat treatment is performed to remove the volatile components in the composite material, and the heat treatment is performed.
  • the temperature is controlled below 200 ° C, the better heat treatment temperature is controlled between 80-150 ° C, and the heat treatment time is 40-80 min, mainly to achieve the evaporation of the added solvent and dispersant.
  • the method of mixing uniformity includes one of ultrasonic, ball milling and agitation.
  • the operating conditions of the ball mill are: the ball milling time is controlled at 2-3 h, the rotation speed is controlled at 400-500 rpm, and the stirring operation condition is: the stirring time is controlled at 30. -40min, the speed is controlled at 700-800rpm, the operating conditions of the ultrasonic are: the ultrasonic power is controlled at 700-900W, and the ultrasonic time is controlled at 60-70min.
  • These three operation modes can be freely selected according to actual operating conditions, as long as they can be realized.
  • the method of mixing the raw materials uniformly can be used.
  • the PTC inorganic composite material of the invention has a good application in the carbon crystal heating plate, and the specific method is to uniformly mix the PTC inorganic composite material and the carbon slurry, and more preferably, the PTC inorganic composite material is added in the amount described above. 2 to 5 wt% of the mass of the carbon paste, in such a manner, a carbon slurry having enhanced PTC properties and far-infrared properties can be obtained.
  • the amount of addition of the PTC inorganic composite material is limited, and is not unlimitedly added.
  • the control is 2-5 wt% of the mass of the carbon paste, and may also be 3 wt% and 4 wt%.
  • the performance of the carbon crystal heating plate is optimal, and the service life is also the longest, if the taste is increased.
  • the addition of PTC inorganic composite material will not continue to enhance the performance of the carbon slurry, but will also have the opposite effect, so the addition amount is best controlled.
  • the present invention develops a novel PTC inorganic composite material, which is obtained by compounding an inorganic material such as a nano ceramic material with a graphite-based carbon material coating agent, and encapsulating the inorganic material itself by using a carbon material.
  • the material can be electrically conductive and has internal insulation effect.
  • the material can be applied to electric heating materials, for example, for carbon crystal heating plates, the performance is more stable, and there is no aging, flatulence, etc. The problem is to subvert the performance of the carbon crystal plate itself, greatly extending the service life, and at the same time bringing considerable economic benefits;
  • the preparation method of the PTC inorganic composite material of the present invention has the advantages of being able to completely retain the active ingredient of the raw material, and has the advantages of simple and easy operation, mild operating conditions, high temperature carbonization step, and the like, and can realize graphene and nano ceramics.
  • the two materials of the material are well compounded and have good performance when applied in the subsequent addition of carbon slurry;
  • the PTC inorganic composite material of the invention is added to the carbon slurry, which can effectively solve the problem of overheating of the carbon crystal plate and an increase in power runaway.
  • the PTC material allows the carbon crystal plate to have a frequency conversion function.
  • the increase in resistance causes the power to be appropriately weakened to adjust to a suitable power to control the temperature, thereby greatly saving energy compared to the conventional carbon crystal plate.
  • Example 1 is a graph showing changes in temperature of a carbon slurry having PTC properties prepared according to Example 3 of the present invention as a function of time.
  • the molar ratio of each element Ti is 5-15%, Si is 20-50%, Fe is 1-5%, B 5-10%, O 50-70%;
  • the obtained product is heat-treated to remove the polyvinyl alcohol, the heat treatment temperature is 200 ° C, the temperature is kept for 30 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 2 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • the molar ratio of each element Ba is 10-20%, Ti is 5-30%, Si is 5-10%, Ag is 5-10 %, O is 50-75%;
  • the obtained product is heat-treated to remove the polyethylene glycol, the heat treatment temperature is 150 ° C, the temperature is kept for 40 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 5 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • the molar ratio of each element Ti is 10-30%, Fe is 5-10%, Si is 10-20%, Cu 5-10%, Sn is 1-5%, O is 50-70%;
  • the obtained product is heat-treated to remove the polyethylene glycol, the heat treatment temperature is 150 ° C, the temperature is maintained for 80 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 4 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • the molar ratio of each element Ti is 10-30%, Fe is 5-10%, Si is 10-20%, Cu 5-10%, Sn is 1-5%, O is 50-70%;
  • the obtained product is heat-treated to remove the polyethylene glycol, the heat treatment temperature is 80 ° C, the heat preservation is 60 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 3 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • the molar ratio of each element Ti is 10-30%, Fe is 5-10%, Si is 10-20%, Cu 5-10%, Sn is 1-5%, O is 50-70%;
  • the obtained product is heat-treated to remove the polyethylene glycol, the heat treatment temperature is 150 ° C, the heat preservation is 60 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 3 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • the molar ratio of each element Ti is 10-30%, Fe is 5-10%, Si is 10-20%, Cu 5-10%, Sn is 1-5%, O is 50-70%;
  • the obtained product is heat-treated to remove the polyethylene glycol, the heat treatment temperature is 150 ° C, the heat is kept for 60 min, and the whole process is vacuum N 2 protection;
  • the heat-treated product is sieved and uniformly compounded with the carbon slurry, and the addition ratio is 3 wt%, that is, a carbon slurry having PTC properties and enhanced far-infrared properties is obtained.
  • a water-soluble PTC functional conductive carbon paste prepared by the method of Example 1 of the CN101407628A patent.
  • the carbon paste prepared in Example 3 and Comparative Example 1 was subjected to temperature change with time.
  • the specific results can be seen in the accompanying drawings of FIG. 1.
  • the carbon paste resistance of the organic material PTC material added in Comparative Example 1 is The response of the temperature has a certain delay, and the resistance is gradually increased to lower the temperature after the residence time is longer in the high temperature phase.
  • the inorganic PTC material of Embodiment 3 of the present invention reaches the temperature warning point, the resistance increases immediately and the temperature is quickly lowered, and the subsequent process is stable overall, precisely because of the present invention.
  • the material has sufficient smoothness in temperature, which greatly extends the life of the material itself in subsequent use.

Abstract

L'invention concerne un matériau composite inorganique à coefficient de température positif fabriqué à l'aide des matières premières primaires suivantes, en pourcentage en poids : de 75 à 95 % d'une nanocéramique, de 1 à 20 % d'un agent de revêtement à base de carbone de graphite, et de 0,5 à 5 % d'un agent dispersant. Le procédé de fabrication consiste à mélanger de manière uniforme la nanocéramique et l'agent de revêtement à base de carbone de graphite, puis à ajouter l'agent dispersant et une quantité appropriée d'éthanol pour obtenir une solution homogénéisée, et à effectuer un traitement thermique avec une protection par les gaz inertes et à une température maximale de 200 °C. Le procédé combine la nanocéramique avec l'agent de revêtement à base de carbone de graphite. Un matériau carboné est utilisé pour revêtir une particule inorganique, ce qui permet d'obtenir une conductivité électrique au moyen du matériau carboné et une isolation électrique fournie par un matériau intérieur. Le matériau composite peut être appliqué dans un matériau électrochauffant, tel qu'un panneau chauffant à cristal de carbone.
PCT/CN2017/085396 2016-05-20 2017-05-22 Matériau composite inorganique à coefficient de température positif, son procédé de fabrication et son application WO2017198233A1 (fr)

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CN106467412B (zh) * 2016-05-20 2020-02-04 济南圣泉集团股份有限公司 一种ptc无机复合材料及其制备方法、应用
CN107374941A (zh) * 2017-05-23 2017-11-24 于长江 用于灸的量子、灸材及其应用
CN108383521A (zh) * 2018-05-16 2018-08-10 奥普家居股份有限公司 一种BaTiO3陶瓷片的制备方法
CN110611964B (zh) * 2018-06-14 2022-05-24 浙江汉纳新材料科技有限公司 具有ptc效应的加热膜材料及其制备方法
CN111099917B (zh) * 2018-10-29 2022-01-04 中国石油化工股份有限公司 一种微波中产生电弧的多孔复合材料及制备方法
CN115475743B (zh) * 2022-10-28 2023-05-23 江苏萃隆精密铜管股份有限公司 一种冷凝器的冷凝管制造加工工艺

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