WO2020019120A1 - 一种陶瓷发热体及其制备方法和用途 - Google Patents

一种陶瓷发热体及其制备方法和用途 Download PDF

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Publication number
WO2020019120A1
WO2020019120A1 PCT/CN2018/096668 CN2018096668W WO2020019120A1 WO 2020019120 A1 WO2020019120 A1 WO 2020019120A1 CN 2018096668 W CN2018096668 W CN 2018096668W WO 2020019120 A1 WO2020019120 A1 WO 2020019120A1
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Prior art keywords
heating element
ceramic
paper
decal
ceramic heating
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PCT/CN2018/096668
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English (en)
French (fr)
Inventor
刘华臣
陈义坤
李丹
邓腾飞
胡腾斐
Original Assignee
湖北中烟工业有限责任公司
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Application filed by 湖北中烟工业有限责任公司 filed Critical 湖北中烟工业有限责任公司
Priority to US17/261,889 priority Critical patent/US20210410234A1/en
Priority to CA3117830A priority patent/CA3117830A1/en
Priority to PCT/CN2018/096668 priority patent/WO2020019120A1/zh
Priority to EP18927243.8A priority patent/EP3829265A4/en
Priority to JP2021503090A priority patent/JP7142146B2/ja
Priority to KR1020217002180A priority patent/KR102543746B1/ko
Priority to RU2021104230A priority patent/RU2758588C1/ru
Publication of WO2020019120A1 publication Critical patent/WO2020019120A1/zh
Priority to PH12021550138A priority patent/PH12021550138A1/en

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • C08L1/26—Cellulose ethers
    • C08L1/28—Alkyl ethers
    • 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
    • H05B3/42—Heating elements having the shape of rods or tubes non-flexible
    • H05B3/46—Heating elements having the shape of rods or tubes non-flexible heating conductor mounted on insulating base
    • 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
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/20—Devices using solid inhalable precursors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M3/00—Printing processes to produce particular kinds of printed work, e.g. patterns
    • B41M3/12—Transfer pictures or the like, e.g. decalcomanias
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
    • 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
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
    • C04B35/584—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on silicon nitride
    • 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
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • 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
    • C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
    • C04B41/5133—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal with a composition mainly composed of one or more of the refractory metals
    • 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
    • C04B41/88—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/05—Alcohols; Metal alcoholates
    • 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
    • H05B3/02—Details
    • 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
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible
    • H05B3/26—Heating elements having extended surface area substantially in a two-dimensional plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
    • 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
    • H05B3/42—Heating elements having the shape of rods or tubes non-flexible
    • H05B3/48—Heating elements having the shape of rods or tubes non-flexible heating conductor embedded in insulating material
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/46—Shape or structure of electric heating means
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/94—Products characterised by their shape
    • 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
    • H05B2203/013—Heaters using resistive films 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
    • 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 the field of heating devices, and more particularly, to a ceramic heating body, a preparation method and uses thereof.
  • Ceramic heating body is a kind of high-efficiency heater with uniform heat division and excellent thermal conductivity, which can ensure the uniform hot surface temperature, thereby eliminating the hot and cold points of the equipment.
  • the ceramic heating body also has a long life, good thermal insulation performance, Strong mechanical properties, corrosion resistance, magnetic field and other advantages.
  • PTC ceramic heating element is a thermistor. It is composed of PTC ceramic heating element and aluminum tube. It has the advantages of small thermal resistance and high heat exchange efficiency. It is an automatic constant temperature and power saving electric heater.
  • MCH ceramic heating elements use alumina ceramics as a new type of high-efficiency environmental protection and energy-saving ceramic heating elements. Compared with PTC ceramic heating elements, they can save 20-30% of electricity under the same heating effect.
  • MCH ceramic heating elements are mostly used as heating elements. Specifically, MCH ceramic heating elements are printed with a metal heating layer on a ceramic base layer by screen printing, that is, refractory metals such as molybdenum and tungsten. As an internal electrode of a heating circuit, a highly efficient and energy-saving cermet heating body obtained by co-firing in a reducing atmosphere of 1400 ° C to 1800 ° C through a series of special preparation processes, in which an aluminum oxide cast body is usually used as an insulating layer.
  • the prepared high-temperature metal thick film paste is printed and printed on one side of the body, and then the upper and lower alumina ceramic substrates are laminated and sliced, and the leads are welded after sintering in a hydrogen reduction furnace at high temperature to obtain MCH. heating stuff.
  • the internal electrode includes alumina ceramics on both sides and the alumina ceramic absorbs heat, the heating efficiency of the internal electrode is not high, and therefore the efficiency of the entire ceramic heating body is not high, and the ceramic heating body is caused by the external body. Thickened, difficult to pull in low temperature smoke.
  • the heating element produced by the electronic paste in the prior art has different batches, which results in a large deviation in the temperature coefficient of resistance, which results in The resistance control is extremely difficult, which results in a very high rate of defective products, and the error of the temperature coefficient of the product resistance is very large, and the circuit program cannot accurately control the temperature.
  • the purpose of the present invention is to overcome the shortcomings in the prior art mentioned above, and provide a ceramic heating element that generates heat quickly, is easy to insert and withdraw in low-temperature smoke, and has different incredibly consistent and low temperature coefficients of resistance in different batches. To complete the present invention.
  • the present invention provides a ceramic heating element, wherein the ceramic heating element includes a ceramic rod substrate, and a surface of the ceramic rod substrate is provided with a resistance heating element, and the resistance heating element is An alloy containing tungsten, manganese, and at least one selected from ruthenium, tellurium, germanium, and vanadium.
  • a material of the ceramic rod substrate is at least one of alumina, silicon nitride, glass, aluminum nitride, and silicon carbide.
  • the resistance heating element is prepared by decal printing an electronic paste, the electronic paste contains tungsten, manganese, an additive, and an organic carrier, and the additive is selected from ruthenium, tellurium, At least one of germanium and vanadium.
  • one end of the ceramic rod base is tapered.
  • the size of the resistance heating element near the tapered end in the length direction of the ceramic rod base is larger than the other end.
  • the weight ratio of the tungsten and manganese is 7: 3-9.5: 0.5.
  • the content of the additive is 0.5 to 5% by weight based on the total weight of the tungsten and manganese.
  • the organic vehicle is a mixture of terpineol, ethyl cellulose, and absolute ethanol.
  • the content of the organic vehicle is 5-20% by weight.
  • the present invention also provides a method for preparing the ceramic heating element, wherein the method includes decal printing an electronic paste on a ceramic rod substrate.
  • the decal printing includes printing an electronic paste on a paper-based film to make decal paper.
  • the printing makes the application amount of the electronic paste on one end of the paper-based film greater than The amount applied at the other end.
  • the paper-based film is made of at least one of tissue paper, wood pulp paper, carbon fiber paper, synthetic fiber paper, natural fiber paper, and the like.
  • the decal printing further includes attaching the decal paper to a base of a ceramic rod treated with acid and alkali.
  • the decal printing further includes a ceramic rod with decal The substrate is fired at a temperature of 1200-1800 ° C for 1-4 hours.
  • the method further comprises performing dipping after the decal printing, and then firing at a temperature of 1000-1200 ° C.
  • the present invention also provides the use of the ceramic heating element according to the above-mentioned method and the ceramic heating element prepared according to the above-mentioned method in a new type of heater for tobacco products.
  • the ceramic heating element according to the above-mentioned method and the above-mentioned method are used.
  • the ceramic heating element according to the present invention and the ceramic heating element prepared according to the method of the present invention have the advantages of rapid heating and easy insertion and removal in low-temperature smoke.
  • the resistance temperature coefficient between different batches is unexpectedly consistent and low, making its resistance control abnormally easy, and the product defective rate is extremely low. . It has excellent performance with low temperature coefficient of resistance.
  • the electronic paste of the present invention is applied to a cermet heating element, it can obtain unexpectedly excellent performance with low temperature coefficient of resistance, which can ensure the calcination of each batch.
  • the product has the same temperature coefficient of resistance, and the resistance is subject to small temperature changes during use, which makes the circuit simple and the overall heating reliability high.
  • electronic paste is a basic material for the production of cermet heating elements, and is a paste formed by mixing and mixing solid powder and liquid solvent through three rolls.
  • electronic paste can be divided into dielectric paste, resistance paste and conductor paste; according to the type of substrate, electronic paste can be divided into ceramic substrate, polymer substrate, glass substrate, metal insulation substrate According to different sintering temperatures, electronic paste can be divided into high-temperature, medium-temperature and low-temperature drying electronic paste; according to different uses, electronic paste can be divided into general electronic paste and special electronic paste. According to the price of the conductive phase, electronic paste can also be divided into precious metal electronic paste and base metal electronic paste.
  • the temperature coefficient of resistance is a parameter closely related to the microstructure of a metal. It has a theoretical maximum without any defects. In other words, the size of the resistance temperature coefficient itself characterizes the performance of the metal process to a certain extent. In the research and development process of new technology processes or online monitoring, we can use the temperature coefficient of resistance to conduct early monitoring and rapid assessment of metal reliability.
  • the term "decal printing” refers to the use of ceramic pigments to print on a specific paper or plastic film surface according to a designed pattern through a printing process, and then the paper with the pattern is transferred to the surface of the substrate, and then subjected to high temperature sintering, The print is permanently attached to the surface of the substrate.
  • the present invention provides a ceramic heating element, wherein the ceramic heating element includes a ceramic rod substrate, and an electronic paste is printed on a surface decal of the ceramic rod substrate.
  • the ceramic heating element provided by the present invention is a rod-shaped ceramic heating element commonly used in new tobacco products, especially low-temperature smoke, and therefore generally includes a ceramic rod base to provide its basic shape, and There is no particular limitation on the material of the ceramic rod substrate, and it may be a ceramic substrate material commonly used in the art. In a preferred embodiment, a material of the ceramic rod substrate is at least one of alumina, silicon nitride, glass, aluminum nitride, and silicon carbide.
  • tungsten is the main heating element, but the high temperature coefficient of resistance of tungsten results in a high temperature coefficient of resistance of the entire electronic paste, and it is difficult to obtain a heating element with a consistent and reliable temperature coefficient of resistance.
  • each batch of the produced product has an enormous and consistent resistance temperature coefficient, and can greatly reduce the resistance temperature of the electronic paste. Coefficient, thereby achieving the beneficial effect of a low temperature coefficient of resistance of the ceramic heating element.
  • the electronic paste contains tungsten, manganese, an additive, and an organic vehicle, and the additive is selected from at least one of ruthenium, tellurium, germanium, and vanadium. More preferably, the content of the additive may be 0.5 to 5% by weight (for example, 1.5% by weight, 2% by weight, or 2.5% by weight).
  • the type and content of the organic vehicle in the electronic paste of the present invention are not particularly limited, and may be the types and content of the organic vehicle commonly used in the art.
  • the organic vehicle may be a mixture of terpineol, ethyl cellulose and absolute ethanol, such as 90-95% by weight (eg, 94% by weight) terpineol, 3-5
  • the weight (for example, 5% by weight) of ethyl cellulose and 1-3% by weight (for example, 1% by weight) of absolute ethanol, preferably, based on the total weight of the tungsten and manganese, the content of the organic vehicle may be 5- 20% by weight.
  • one end of the ceramic rod base body in order to better insert and insert the ceramic heating element in the low-temperature smoke, one end of the ceramic rod base body can be made into a sharp shape, and according to the ordinary insertion manner of the ceramic heating element in the low-temperature smoke, the sharp-shaped end As the insertion end, it is closer to the cigarette support structure, and the other end is closer to the power supply.
  • the other end of the electronic paste can be made less. So that the temperature at the other end is lower. Therefore, in a preferred embodiment, one end of the ceramic rod substrate may be tapered.
  • the concentration of the electronic slurry near the tapered end in the length direction of the ceramic rod substrate may be higher than that of the other end of the ceramic rod substrate. Electronic paste concentration.
  • the present invention also provides a method for preparing the ceramic heating element, wherein the method includes printing an electronic paste on a ceramic rod substrate.
  • the preparation method of the present invention uses an applique printing method to attach the electronic paste to the ceramic rod substrate, which can not only effectively reduce the ceramic
  • the thickness of the heating element, and the printed circuit (ie the electronic paste) can be directly exposed on the surface of the ceramic heating element, so the heating efficiency is greatly improved.
  • the electronic paste at one end can also be made. Less to make the end work cooler.
  • the pattern design is performed on a plane, different printed circuit patterns can be easily designed according to needs, so that the ceramic heating body produced also has a desired appearance.
  • the decal printing may include printing (for example, missing printing, coating, etc.) an electronic paste on a paper-based film to make decal paper.
  • the printing makes the electronic paste on The concentration of the paper-based film at one end may be greater than the concentration at the other end.
  • the composition of the paper-based film there is no particular limitation on the composition of the paper-based film, and it can be made of raw materials commonly used in the art.
  • the paper-based film is made of at least one of tissue paper, wood pulp paper, carbon fiber paper, synthetic fiber paper, natural fiber paper, and the like.
  • the decal paper after the decal paper of the electronic paste of the present invention is prepared, the decal paper can be transferred to the ceramic rod substrate, and the subsequent processing can be performed to completely adhere the electronic paste to the surface of the ceramic rod substrate.
  • the decal printing further includes attaching the decal paper to a base of a ceramic rod treated with acid and alkali.
  • the decal printing further includes a base of a ceramic rod with decal applied ( Preferably, it is fired under a mixed gas of H 2 and N 2 ) at a temperature of 1200-1800 ° C. for 1-4 h.
  • the decal printing before the firing step further comprises drying the ceramic rod base with the decal paper at 100-150 ° C, and then debinding at 300-600 ° C.
  • a glaze layer may be further provided on the surface of the ceramic heating element. Therefore, in a preferred embodiment, the method further comprises dipping the glaze after the decal printing, and then firing at a temperature of 1000-1200 ° C. After firing, the ceramic heating element can also be provided with a lead. Therefore, the method of the present invention may further include surface-treating the ceramic heating element at a solder joint, and using a wire bonding tool to fix the lead with the solder joint and solder into the kiln. The furnace is wire-bonded at about 700 ° C to make a finished product.
  • the preparation method of the ceramic heating element of the present invention includes: (1) designing the diameter and length of the ceramic rod base body according to the product requirements, the electronic paste, printing weight, and production requirements that meet the requirements (2) In a clean room, use a precision screen printer to leak the prepared electronic paste through the circuit part of the screen printing plate onto the surface of the paper base coated with water-soluble glue.
  • the paper base is made of at least one of cotton paper, wood pulp paper, carbon fiber paper, synthetic fiber paper, natural fiber paper, etc .; (3) decal paper printed with heating circuit is pasted on Alkali-treated ceramic rod substrate; (4) Dry ceramic rods with decal paper at 100-150 ° C, and then perform debinding at 300-600 ° C; (5) After debinding, the whole is in H 2 and N 2 firing under mixed gas and at a temperature of 1200-1800 °C for 1-4 hours; (6) hang the fired ceramic heating rod with a layer of transparent thin glaze by dipping, and then push it into the reducing atmosphere furnace , High-temperature firing at a temperature of 1000-1200 ° C; (7) The ceramic heating body after firing is at a solder joint After the surface treatment, using a wire bonding system with the leads and pads, the solder is fixed into the kiln for wire bonding at about 700 deg.] C conditions to finished products.
  • the present invention also provides the use of the ceramic heating element according to the above-mentioned method and the ceramic heating element prepared according to the above-mentioned method in a new type of heater for tobacco products, especially the use in a low-temperature smoke heater.
  • a mixture of 94% by weight terpineol, 5% by weight ethylcellulose, and 1% by weight absolute ethanol was used as an organic vehicle, which was magnetically weighed by weighing terpineol, ethylcellulose, and absolute ethanol in proportion.
  • the stirrer is prepared by mixing uniformly at a water bath temperature of 90 ° C. Weigh 90 parts by weight of tungsten powder and 10 parts by weight of manganese powder and mix well. The mixed powder is mixed with 10 parts by weight of an organic carrier and put into a planetary ball mill for ball milling.
  • absolute ethanol is used as the ball milling medium, and the mixture and the ball milling medium are used.
  • the weight ratio was 1.5: 1, the ball milling speed was 500 r / min, and the time was 1.5 h, so as to obtain an electronic slurry composition C1. In the same manner, 5 batches of the electronic slurry composition C1 were obtained.
  • the electronic slurry compositions C2-C8 were prepared in the same manner as described above, and each batch of each electronic slurry was prepared in 5 batches. Then, all batches of the electronic slurry composition were passed through, for example, Conventional techniques in the art, such as screen printing, print it on a ceramic substrate to form a heating element.
  • the resistance values of the heating elements obtained from each batch of the electronic paste composition C1-C8 at 25 ° C, 83 ° C, 150 ° C, and 230 ° C were measured, and then the resistance values of each batch were subjected to a least square method and a linear simulation. Then, the temperature coefficient of resistance is obtained.
  • the average resistance temperature coefficient (average TCR) of the 5 batches was calculated based on the resistance temperature coefficients TCR1, TCR2, TCR3, TCR4, and TCR5 of the 5 batches, and each Batch resistance temperature coefficient deviation rate TCR (TCRn-average TCR) / average TCR (n is 1, 2, 3, 4 or 5), and further calculate the average deviation rate of the resistance temperature coefficient of 5 batches (5
  • the average resistance temperature coefficient deviation rate of the batches) is shown in Table 2.
  • the electronic paste composition (C5-C8) of the present invention can prepare an excellent heating element, so that the average deviation of the temperature coefficient of resistance between a plurality of batches is significantly lower than that of other
  • the average deviation of the temperature coefficient of resistance of the heating element prepared from the electronic paste composition (C1-C4) shows excellent performance with a uniform and low temperature coefficient of resistance.

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Abstract

一种陶瓷发热体及其制备方法，陶瓷发热体包括陶瓷棒基体，并且陶瓷棒基体的表面贴花印刷有电子浆料；制备方法包括将电子浆料贴花印刷在陶瓷棒基体上。此外，还提供了该陶瓷发热体在烟草制品用发热器中的用途。

Description

一种陶瓷发热体及其制备方法和用途 技术领域
本发明涉及发热装置领域，更具体地，涉及一种陶瓷发热体及其制备方法和用途。
背景技术
陶瓷加热体是一种高效热分部均匀且热导性极佳的加热器，可以确保热面温度均匀，从而消除设备的热点及冷点，此外陶瓷加热体还具有长寿命、保温性能好、机械性能强、耐腐蚀、抗磁场等优点。目前，陶瓷加热体主要分两种，分别是PTC陶瓷发热体和MCH陶瓷发热体。这两种产品所使用的材质是完全不同的，只是成品类似于陶瓷，所以统称为“陶瓷发热体”。PTC陶瓷发热体是热敏电阻，采用PTC陶瓷发热元件与铝管组成，有热阻小、换热效率高的优点，是一种自动恒温、省电的电加热器。MCH陶瓷发热体使用氧化铝陶瓷是一种新型高效环保节能陶瓷发热元件，相比PTC陶瓷发热体，具有相同加热效果情况下节约20～30％电能。
在目前的低温烟领域中大多采用MCH陶瓷发热体作为发热元件，具体地，MCH陶瓷发热体是用丝网印刷法将金属发热层印刷于陶瓷基层上，即以钼钨等耐高温难熔金属作为发热电路的内电极，通过一系列特殊的制备工艺在1400℃至1800℃的还原气氛下共烧得到的一种高效节能的金属陶瓷发热体，其中通常采用氧化铝流延坯体作为绝缘层和基体，将制备好的高温金属厚膜浆料布线印刷在坯体的一面上，然后将上下氧化铝陶瓷基层叠压、切片，在氢气还原炉中经高温烧结后焊接引线，从而制得MCH发热体。但是由于内电极包括在两侧的氧化铝陶瓷中间且氧化铝陶瓷吸热，导致内电极的发热效率不高，并因此整个陶瓷发热体的效率不高，而且由于外加坯体，导致陶瓷发热体变粗，在低温烟中不易抽插。虽然现在技术中存在各式各样的用于制备发热元件的电子浆料产品，然而，现有技术中的电子浆料制得的发热元件存在批次不同导致电阻温度系数偏差极大，从而导致电阻控制难度极高，导致生产产品次品率极高，产 品电阻温度系数误差很大，电路程序无法精确控温。此外，对于现有的电子浆料产品而言，很难在保证电阻温度系数误差满意的同时达到低电阻温度系数。
发明内容
本发明的目的在于克服上述提及的现有技术中的缺陷，提供一种发热快、在低温烟中易于抽插、不同批次均具有难以置信的一致且低的电阻温度系数的陶瓷发热体，从而完成本发明。
本专利的发明人经过大量试验非常惊奇地发现，某些组分的电子浆料制得的各批次产品具有难以置信的、一致的电阻温度系数，并且该电阻温度系数令人满意地低，从而获得本发明。
为了实现上述目的，一方面，本发明提供了一种陶瓷发热体，其中，所述陶瓷发热体包括陶瓷棒基体，并且所述陶瓷棒基体的表面设置有电阻发热元件，所述电阻发热元件是包含钨、锰和选自钌、碲、锗和钒中的至少一种的合金。
在本发明的一个优选实施方式中，所述陶瓷棒基体的材料为氧化铝、氮化硅、玻璃、氮化铝和碳化硅中的至少一种。
在本发明的一个优选实施方式中，所述电阻发热元件是通过贴花印刷电子浆料制备的，所述电子浆料包含钨、锰、添加剂和有机载体，并且所述添加剂选自钌、碲、锗和钒中的至少一种。
在本发明的一个优选实施方式中，所述陶瓷棒基体的一端为锥形，优选地，所述陶瓷棒基体的长度方向上的靠近锥形一端的电阻发热元件的尺寸大于另一端。
在本发明的一个优选实施方式中，所述钨和锰的重量比为7:3-9.5:0.5。在本发明的一个优选实施方式中，其中，基于所述钨和锰的总重量，所述添加剂的含量为0.5-5重量％。在本发明的一个优选实施方式中，所述有机载体为松油醇、乙基纤维素和无水乙醇的混合物，优选地，基于所述钨和锰的总重量，所述有机载体的含量为5-20重量％。
另一方面，本发明还提供了一种制备上述陶瓷发热体的方法，其中，所述 方法包括将电子浆料贴花印刷在陶瓷棒基体上。
在本发明的一个优选实施方式中，所述贴花印刷包括将电子浆料印刷在纸基薄膜上以制成贴花纸，优选地，所述印刷使得电子浆料在纸基薄膜一端的施加量大于另一端的施加量。
在本发明的一个优选实施方式中，所述纸基薄膜由绵纸、木浆纸、炭纤维纸、合成纤维纸、天然纤维纸等中的至少一种制成。
在本发明的一个优选实施方式中，所述贴花印刷还包括将所述贴花纸贴在经酸碱处理的陶瓷棒基体上，优选地，所述贴花印刷还包括将贴有贴花纸的陶瓷棒基体在1200-1800℃的温度下烧制1-4h。
在本发明的一个优选实施方式中，所述方法还包括在所述贴花印刷之后进行浸釉，然后在1000-1200℃的温度下烧制。
再一方面，本发明还提供了根据上述的陶瓷发热体和根据上述的方法制备的陶瓷发热体在新型烟草制品用发热器中的用途，优选地，根据上述的陶瓷发热体和根据上述的方法制备的陶瓷发热体在新型烟草制品用发热器特别是低温烟用发热器中的用途。
综上所述，根据本发明的陶瓷发热体和根据本发明的上述方法制备的陶瓷发热体具有发热快、在低温烟中易于抽插的优点。此外，使用本发明的电子浆料贴花印刷的陶瓷发热体，不同批次之间的电阻温度系数令人意外地一致且低，使得其电阻控制变得异常地容易，生产产品次品率极低。具有低电阻温度系数的优异性能，在将其本发明的电子浆料应用于金属陶瓷发热体时，能够获得出人意料地一致且低的电阻温度系数的优异性能，可以确保各批次烧成后的产品电阻温度系数一致，在使用过程中电阻受温度变化小，使得电路简单，整体发热可靠性能高。
具体实施方式
以下对本发明的具体实施方式进行详细说明。应当理解的是，此处所描述的具体实施方式仅用于说明和解释本发明，并不用于限制本发明。
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。
如本文所述，术语“电子浆料”是制造金属陶瓷发热体的基础材料，是一种由将固体粉末和液体溶剂经过三辊轧制混合均匀而形成的膏状物，其中，根据用途的不同，电子浆料可以分为介质浆料、电阻浆料和导体浆料；根据基片种类的不同，电子浆料又可以分为陶瓷基片、聚合物基片、玻璃基片、金属绝缘基片电子浆料等；根据烧结温度的不同，电子浆料又可以分为高温、中温和低温烘干电子浆料；根据用途的不同，电子浆料又可以分为通用电子浆料和专用电子浆料；根据导电相的价格不同，电子浆料也可以分为贵金属电子浆料和贱金属电子浆料。
如本文所用，术语“电阻温度系数”(temperature coefficient of resistance，简称TCR)表示电阻当温度改变1度时，电阻值的相对变化(即电阻值变化相对于该电阻的变化率)，计算公式为TCR＝(R T2-R T1)/[(T 2-T 1)×R T1]，单位为ppm/℃，其中T 1表示第一温度，T 2表示第二温度，R T1表示第一温度下的电阻值，R T2表示第二温度下的电阻值。电阻温度系数是一个与金属的微观结构密切相关的一个参数，在没有任何缺陷的情况下，它具有理论上的最大值。也就是说，电阻温度系数本身的大小在一定程度上表征了金属工艺的性能。在新技术工艺的研发过程或在线监测中，我们可以利用电阻温度系数对金属的可靠性进行早期监测与快速评估。
如本文所用，术语“贴花印刷”是指采用陶瓷颜料通过印刷工艺按照设计好的纹样印刷到特定纸张或塑料膜表面，然后将带有图案的纸张移贴到基体表面，然后再进行高温烧结，印花就永久性的粘附在基体表面。
一方面，本发明提供了一种陶瓷发热体，其中，所述陶瓷发热体包括陶瓷棒基体，并且所述陶瓷棒基体的表面贴花印刷有电子浆料。
根据本发明待解决的现有技术中的缺陷，本发明提供的陶瓷发热体是通常用于新型烟草制品特别是低温烟的棒状陶瓷发热体，因此通常包括陶瓷棒基体 以提供其基本形状，而对陶瓷棒基体的材料没有特别限制，可以为本领域中常见的陶瓷基体材料。在一个优选的实施方式中，所述陶瓷棒基体的材料为氧化铝、氮化硅、玻璃、氮化铝和碳化硅中的至少一种。
钨系浆料中，钨为主要发热元素，但钨的电阻温度系数很高，导致整个电子浆料的电阻温度系数很高，并且难于获得电阻温度系数一致可靠的发热元件。然而，经过本发明人的研究发现，选择适宜的钨系浆料的组成，制得的各批次产品具有难以置信的、一致的电阻温度系数，并且可以有利地大幅降低电子浆料的电阻温度系数，从而实现陶瓷发热体电阻温度系数低的有益效果。因此，在一个优选的实施方式中，所述电子浆料包含钨、锰、添加剂和有机载体，并且所述添加剂选自钌、碲、锗和钒中的至少一种。更优选地，所述添加剂的含量可以为0.5-5重量％(例如1.5重量％、2重量％或2.5重量％)。
此外，对本发明的电子浆料中有机载体的种类和含量没有特别限制，可以为本领域中常见的有机载体种类和含量。在本发明的一个优选实施方式中，所述有机载体可以为松油醇、乙基纤维素和无水乙醇的混合物，例如90-95重量％(例如94重量％)松油醇、3-5重量(例如5重量％)乙基纤维素和1-3重量％(例如1重量％)无水乙醇，优选地，基于所述钨和锰的总重量，所述有机载体的含量可以为5-20重量％。
根据本发明，为了使陶瓷发热体在低温烟中更好地进行抽插，可以将陶瓷棒基体的一端制成尖锐形状，并且根据陶瓷发热体在低温烟中的通常插入方式，尖锐形状的一端将作为插入端，更靠近烟支结构，而另一端更靠近电源，为了使陶瓷发热体在有效燃烧烟支的情况下尽可能地保护电源，可以将使该另一端的电子浆料更少，以使该另一端的温度更低。因此，在一个优选的实施方式中，所述陶瓷棒基体的一端可以为锥形，优选地，所述陶瓷棒基体的长度方向上的靠近锥形一端的电子浆料浓度可以高于另一端的电子浆料浓度。
另一方面，本发明还提供了一种制备上述陶瓷发热体的方法，其中，所述方法包括将电子浆料贴花印刷在陶瓷棒基体上。
对于本发明的陶瓷发热体的制备方法中的陶瓷棒基体和电子浆料，所述陶瓷棒基体的材料和形状以及所述电子浆料的组成等的优选实施方式可以与先前所述的一样，因此在此不再赘述。
根据本发明，为了使陶瓷发热体具有发热快、在低温烟中易于抽插的优点，本发明的制备方法采用贴花印刷的方式将电子浆料附着在陶瓷棒基体上，这样不仅可以有效降低陶瓷发热体的厚度，而且可以使印刷电路(即电子浆料)直接外露在陶瓷发热体表面，因此大大提高了发热效率，出于与之前相同的保护电源的考虑，同样可以使得一端的电子浆料更少，以使该端的工作温度更低。此外，在采用贴花印刷的过程中，由于是在平面上进行图案设计，因此容易地可以根据需要设计出不同的印刷电路图案，使得制成的陶瓷发热体还具备期望的外观。在一个优选的实施方式中，所述贴花印刷可以包括将电子浆料印刷(例如漏印、涂布等)在纸基薄膜上以制成贴花纸，优选地，所述印刷使得电子浆料在纸基薄膜一端的浓度可以大于另一端的浓度。
根据本发明，对纸基薄膜的组成没有特别限制，可以由本领域中常见的原料制成。在一个优选的实施方式中，所述纸基薄膜由绵纸、木浆纸、炭纤维纸、合成纤维纸、天然纤维纸等中的至少一种制成。
根据本发明，在制得本发明的电子浆料的贴花纸后，可以将该贴花纸再转移到陶瓷棒基体上，并且可以经过后续的加工以将电子浆料完全粘附在陶瓷棒基体表面。在一个优选的实施方式中，所述贴花印刷还包括将所述贴花纸贴在经酸碱处理的陶瓷棒基体上，优选地，所述贴花印刷还包括将贴有贴花纸的陶瓷棒基体(优选地在H 2和N 2的混合气体下)在1200-1800℃的温度下烧制1-4h。在一个更优选的实施方式中，所述贴花印刷在烧制步骤之前还包括将贴有贴花纸的陶瓷棒基体在100-150℃下干燥，再在300-600℃的条件下进行排胶。
根据本发明，为了起到绝缘、提高强度、保护加热器的作用，可以还在陶瓷发热体表面设置釉层。因此，在一个优选的实施方式中，所述方法还包括在所述贴花印刷之后进行浸釉，然后在1000-1200℃的温度下烧制。在烧制好后，还可以对陶瓷发热体设置引线，因此本发明的方法还可以包括将陶瓷发热体在焊点处进行表面处理，利用焊线制具将引线与焊点、焊料固定进入窑炉在700℃左右的条件下进行引线焊接，从而制成成品。
本发明的上述各个优选实施方式可以单独使用或者与其它优选实施方式组合使用。在一个特别优选的实施方式中，本发明的陶瓷发热体的制备方法包括：(1)根据产品要求，设计陶瓷棒基体的直径、长度，符合要求的电子浆料、印 刷印重以及生产所需的模具、制具；(2)在无尘室中，利用精密丝印机，将制备好的电子浆料通过丝网印版的电路部分漏印到涂覆有水溶性胶的纸基表面，制成贴花纸，所述纸基由绵纸、木浆纸、炭纤维纸、合成纤维纸、天然纤维纸等中的至少一种制成；(3)将印刷有发热电路的贴花纸贴在经酸碱处理的陶瓷棒基体上；(4)将贴有贴花纸的陶瓷棒在100-150℃干燥，再在300-600℃条件下进行排胶；(5)排胶后整体在H 2和N 2混合气体下以及1200-1800℃的温度下烧制1-4小时；(6)将烧制后的陶瓷加热棒通过浸釉的方式挂上一层透明薄釉，再推入还原气氛炉中，在1000-1200℃的温度下进行高温烧制；(7)烧制好后的陶瓷发热体在焊点处进行表面处理后，利用焊线制具将引线与焊点、焊料固定进入窑炉在700℃左右的条件下进行引线焊接，从而制成成品。
再一方面，本发明还提供了根据上述的陶瓷发热体和根据上述的方法制备的陶瓷发热体在新型烟草制品用发热器中的用途，特别是在低温烟用发热器中的用途。
实施例
使用94重量％松油醇、5重量％乙基纤维素和1重量％无水乙醇的混合物作为有机载体，其通过将松油醇、乙基纤维素和无水乙醇按比例称量后通过磁力搅拌器在水浴温度为90℃下混合均匀来制备。称取90重量份钨粉、10重量份锰粉并混合均匀，将混合粉末与10重量份有机载体混合后放入行星球磨机中进行球磨，其中，使用无水乙醇作为球磨介质，混合物与球磨介质的重量比为1.5:1，球磨速度为500r/min，时间为1.5h，从而制得电子浆料组合物C1。采用同样的方式获得5个批次的电子浆料组合物C1。
按照表1所示的含量，按照上述相同的方式制备电子浆料组合物C2-C8，每种电子浆料各制备5个批次，然后，将全部批次的电子浆料组合物均通过诸如丝网印刷等本领域中常规的技术将其印刷在陶瓷基体上，形成发热元件。测量由电子浆料组合物C1-C8的各批次获得的发热元件在25℃、83℃、150℃和230℃下的电阻值，然后将各批次的电阻值通过最小二乘法和线性拟合，得到电阻温度系数。对于电子浆料组合物C1-C8中的每一种，根据5个批次电阻温度系数 TCR1、TCR2、TCR3、TCR4和TCR5，计算5个批次平均电阻温度系数(平均TCR)，以及每个批次的电阻温度系数偏差率TCR(TCRn-平均TCR)/平均TCR(n为1、2、3、4或5)，并进一步计算5个批次的电阻温度系数的平均偏差率(5个批次的电阻温度系数偏差率的平均值)，如表2所示。
表1
    钨 锰 铁 钼 钌 锗 钒 碲
C1 钨锰 90 10 - - - - - -
C2 钨锰铁 90 10 2 - - - - -
C3 钨锰钼 90 10 - 2 - - - -
C4 钨钌 98 - - - 2 - - -
C5 钨锰钌 90 10 - - 1 - - -
C6 钨锰锗 90 10 - - - 0.5 - -
C7 钨锰钒 90 10 - - - - 5 -
C8 钨锰碲 90 10 - - - - - 2
表2
    TCR1 TCR2 TCR3 TCR4 TCR5 平均TCR 平均偏差率
C1 钨锰 3742 3528 3854 3928 3468 3704 4.45％
C2 钨锰铁 3516 3324 3418 3589 3615 3492 2.78％
C3 钨锰钼 2995 3258 3196 3298 3028 3155 3.64％
C4 钨钌 3395 3216 3329 3428 3365 3347 1.77％
C5 钨锰钌 3275 3329 3314 3228 3295 3288 0.89％
C6 钨锰锗 3108 3182 3189 3203 3199 3176 0.70％
C7 钨锰钒 2988 3077 2923 3081 3029 3020 1.70％
C8 钨锰碲 3419 3499 3386 3420 3398 3424 0.87％
由上述实施例可知，通过本发明的电子浆料组合物(C5-C8)，可以制备优异性的发热元件，使得多个批次之间的电阻温度系数的平均偏差显著地低于其他的其他电子浆料组合物(C1-C4)制备的发热元件的电阻温度系数的平均偏差，显示出均一且低的电阻温度系数的优异性能。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不违背本发明的思想，其同样应当视为本发明所公开的内容。

Claims (15)

  1. 一种陶瓷发热体，其中，所述陶瓷发热体包括陶瓷棒基体，并且所述陶瓷棒基体的表面设置有电阻发热元件，所述电阻发热元件是包含钨、锰和选自钌、碲、锗和钒中的至少一种的合金。
  2. 根据权利要求1所述的陶瓷发热体，其中，所述陶瓷棒基体的材料为氧化铝、氮化硅、玻璃、氮化铝和碳化硅中的至少一种。
  3. 根据权利要求1所述的陶瓷发热体，其中，所述电阻发热元件是通过贴花印刷电子浆料制备的，所述电子浆料包含钨、锰、添加剂和有机载体，并且所述添加剂选自钌、碲、锗和钒中的至少一种。
  4. 根据权利要求1所述的陶瓷发热体，其中，所述陶瓷棒基体的一端为锥形，优选地，所述陶瓷棒基体的长度方向上的靠近锥形一端的电阻发热元件的尺寸大于另一端。
  5. 根据权利要求3或4所述的陶瓷发热体，其中，所述钨和锰的重量比为7:3-9.5:0.5。
  6. 根据权利要求3至5任一项所述的陶瓷发热体，其中，基于所述钨和锰的总重量，所述添加剂的含量为0.5-5重量％。
  7. 根据权利要求3至6任一项所述的陶瓷发热体，其中，所述有机载体为松油醇、乙基纤维素和无水乙醇的混合物，优选地，基于所述钨和锰的总重量，所述有机载体的含量为5-20重量％。
  8. 一种制备权利要求1至7中任一项所述陶瓷发热体的方法，其中，所述方法包括将电子浆料贴花印刷在陶瓷棒基体上。
  9. 根据权利要求8所述的方法，其中，所述贴花印刷包括将电子浆料印刷在纸基薄膜上以制成贴花纸，
  10. 根据权利要求9所述的方法，其中，所述印刷使得电子浆料在纸基薄膜一端的施用量大于另一端的施用量。
  11. 根据权利要求9或者权利要求10所述的方法，其中，所述纸基薄膜由 绵纸、木浆纸、炭纤维纸、合成纤维纸、天然纤维纸等中的至少一种制成。
  12. 根据权利要求9或者权利要求10所述的方法，其中，所述贴花印刷还包括将所述贴花纸贴在经酸碱处理的陶瓷棒基体上，优选地，所述贴花印刷还包括将贴有贴花纸的陶瓷棒基体在1200-1800℃的温度下烧制1-4h。
  13. 根据权利要求8所述的方法，其还包括在所述贴花印刷之后进行浸釉，然后在1000-1200℃的温度下烧制。
  14. 根据权利要求1至7中任一项所述的陶瓷发热体和根据权利要求8至13中任一项所述的方法制备的陶瓷发热体在新型烟草制品用发热器中的用途。
  15. 根据权利要求14所述的用途，其中所述新型烟草制品为低温烟。
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