WO2021078248A1 - 一种发热体及其制备方法和用途 - Google Patents

一种发热体及其制备方法和用途 Download PDF

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Publication number
WO2021078248A1
WO2021078248A1 PCT/CN2020/123175 CN2020123175W WO2021078248A1 WO 2021078248 A1 WO2021078248 A1 WO 2021078248A1 CN 2020123175 W CN2020123175 W CN 2020123175W WO 2021078248 A1 WO2021078248 A1 WO 2021078248A1
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Prior art keywords
powder
heating element
phase
ball milling
preparation
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PCT/CN2020/123175
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English (en)
French (fr)
Inventor
刘华臣
李丹
陈义坤
刘磊
刘冰
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 EP20879559.1A priority Critical patent/EP3967166A4/en
Priority to KR1020217037058A priority patent/KR20220002961A/ko
Publication of WO2021078248A1 publication Critical patent/WO2021078248A1/zh

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    • 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
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/0688—Cermets, e.g. mixtures of metal and one or more of carbides, nitrides, oxides or borides
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B35/5607—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 refractory metal carbides
    • C04B35/5611—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 refractory metal carbides based on titanium carbides
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    • 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
    • C04B35/5607—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 refractory metal carbides
    • C04B35/5626—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 refractory metal carbides based on tungsten carbides
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/6261—Milling
    • C04B35/62615—High energy or reactive ball milling
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62645—Thermal treatment of powders or mixtures thereof other than sintering
    • C04B35/62655—Drying, e.g. freeze-drying, spray-drying, microwave or supercritical drying
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    • 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
    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/4515—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application application under vacuum or reduced pressure
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    • 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
    • C04B41/4505—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application
    • C04B41/4529—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements characterised by the method of application applied from the gas phase
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    • 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
    • C04B41/515—Other specific metals
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    • 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
    • C04B41/515—Other specific metals
    • C04B41/5155—Aluminium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
    • C22C29/067—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds comprising a particular metallic binder
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • 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
    • 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
    • H05B3/141—Conductive ceramics, e.g. metal oxides, metal carbides, barium titanate, ferrites, zirconia, vitrous compounds
    • 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
    • H05B3/16—Heating elements characterised by the composition or nature of the materials or by the arrangement of the conductor the conductor being mounted on an insulating base
    • 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
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
    • C04B2235/402—Aluminium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/40—Metallic constituents or additives not added as binding phase
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/604—Pressing at temperatures other than sintering temperatures
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    • C22C29/00—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
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    • C22C29/06—Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides based on carbides, but not containing other metal compounds
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    • H05B2203/013—Heaters using resistive films or coatings
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    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/017—Manufacturing methods or apparatus for heaters

Definitions

  • the invention relates to a heating element and a preparation method and application thereof, belonging to the technical field of composite materials and powder metallurgy.
  • the functional principle of low-temperature cigarettes is: through the heating element material under certain external field conditions, the temperature is rapidly raised to the target temperature (generally 300-400 °C (degrees Celsius)), and then the surrounding special tobacco leaves are roasted to produce the same as traditional cigarettes. Similar effects of smoking. Because low-temperature cigarettes have a lower smoking temperature, they are less toxic than traditional cigarettes, and can add special flavors or optimize taste according to different needs, and are extremely popular at home and abroad.
  • the heating method used in low-temperature cigarettes is usually resistance heating, and the heat source is generated by the way of current passing through the heating resistor.
  • the heating element in the related equipment is generally MCH ceramic (ceramic heating element).
  • the ceramic heating element usually prints the heating slurry on the ceramic blank according to a certain circuit, realizes the metallurgical bonding through the subsequent firing process, and then encapsulates the glaze to connect the electrodes.
  • the ceramic heating element can meet the product demand to a certain extent, its preparation process is complicated, the cost is high, and there are problems of uneven product quality. These shortcomings will seriously hinder the market application of low-temperature cigarettes. Therefore, there is an urgent need to develop new heating materials.
  • the performance requirements of the heating element for low-temperature cigarettes are mainly: 1) biocompatibility, non-toxic under low and high temperature conditions; 2) adjustable resistance; 3) able to withstand a certain degree of high temperature, good oxidation resistance and high temperature stability , And has a certain high temperature strength; 4) can withstand the corrosion of tobacco media, has good chemical stability; 5) good thermal conductivity; 6) good room temperature and high temperature mechanical properties; 7) more than tens of thousands of times the service life.
  • the existing single alloy or ceramic material can hardly meet the above requirements.
  • the purpose of the present invention is to provide a heating element and its preparation method and application, which can resist oxidation, has stable quality, good heating uniformity, simple and efficient preparation process, and good economy.
  • the present invention provides a heating element, including a substrate and a coating covering the outer surface of the substrate; wherein the substrate includes a hard phase and a continuous phase, and the hard phase It includes single-phase or multi-phase ceramics, and the continuous phase includes a single metal or alloy; and the coating is used to prevent the heating element from oxidizing.
  • the single metal is chromium or aluminum.
  • the alloy is an alloy containing chromium and/or aluminum.
  • the total mass fraction of chromium and/or aluminum in the alloy is 10%-50%.
  • the coating is a composite coating containing chromium and/or aluminum.
  • the composite coating is a composite nitride layer containing chromium and/or aluminum.
  • the total atomic fraction of chromium and/or aluminum in the composite nitride layer is 50%-100%.
  • the single-phase ceramic includes one of carbide ceramics, nitride ceramics, boride ceramics, and oxide ceramics.
  • the single-phase ceramics include single-phase solid solution ceramics formed by multiple substances of carbides, nitrides, borides, and oxides.
  • the multi-phase ceramic includes a plurality of single-phase ceramics.
  • the thickness of the coating is 0.5 to 1.5 microns.
  • the resistivity of the heating element is 0.001-0.05 ohm ⁇ cm.
  • the present invention also provides a method for preparing the above heating element, which includes the following steps: (1) Obtain single-phase or multi-phase ceramic powder, and single metal or alloy powder; (2) Combine the single-phase or The multiphase ceramic powder, the single metal or alloy powder and the additive powder are ball-milled to obtain a powder slurry; (3) drying the powder slurry to obtain a granulated powder; (4) making the powder The granulated powder is molded and then sintered to obtain the substrate; (5) surface coating the substrate to obtain the heating element.
  • the heating element is ground and polished on a grinder to improve the surface quality of the heating element.
  • the alloy powder when the alloy powder is obtained, a variety of simple metal powders including chromium and/or aluminum are added to the first ball milling tank according to a certain mass ratio, and argon gas is introduced after sealing. Mechanical alloying is carried out in the first ball mill; wherein, the ball-to-material ratio of the first ball mill is 15:1-25:1, the rotation speed is 300-500 revolutions per minute, and the ball milling time is 48-96 hours.
  • stearic acid is added to the first ball milling tank to continue ball milling, and the ball milling time is 0.5 to 4 hours.
  • the total mass fraction of the chromium and/or aluminum elementary powder is 10%-50%.
  • the single-phase or multi-phase ceramic powder, the single metal or alloy powder, and the additive powder are added to the second ball milling tank, and absolute ethanol is added to the second ball milling tank.
  • the ball milling is performed in the second ball milling tank, wherein the ball-to-material ratio in the second ball milling tank is 5:1-10:1, the rotation speed is 120-350 revolutions per minute, and the ball milling time is 24-96 hours.
  • the mass fraction of each component in the material of the second ball milling tank is respectively: 42.00%-68.00% of the single-phase or multi-phase ceramic powder, and 12.00% of the single metal or alloy powder % ⁇ 30.00%, the additive powder is 16.5% ⁇ 46%.
  • the powder slurry is vacuum dried at a temperature of 75-90 degrees Celsius.
  • the compression pressure of the compression molding is 200-400 MPa, and the pressure-holding time is 0.5-2 minutes.
  • the molded blank is sintered under a vacuum degree greater than 1 ⁇ 10 ⁇ 1 Pa, the sintering temperature is 1220 to 1450 degrees Celsius, and the holding time is 15 to 60 minutes.
  • the substrate is surface-coated on a multi-target magnetron sputtering apparatus; wherein the target material of the multi-target magnetron sputtering apparatus is an alloy containing chromium and/or aluminum, and a vacuum
  • the temperature is greater than 3 ⁇ 10 -3 Pa
  • the target material is controlled by a DC cathode
  • the sputtering power is 80-120 watts
  • the sputtering time is 1 to 2 hours
  • the sputtering temperature is 280-320 degrees Celsius
  • the sputtering coating adopts argon.
  • Mixed gas of gas and nitrogen are examples of gases.
  • the total atomic fraction of chromium and/or aluminum in the target material is 50%-100%.
  • the additive powder includes tungsten carbide powder, molybdenum powder and graphite powder.
  • the present invention also proposes the use of the above heating element and the heating element prepared by the above method in a new type of tobacco product heater, especially the use of a low temperature smoke heater.
  • the heating element of the present invention includes a substrate and a coating for preventing oxidation of the substrate.
  • the hard phase of the substrate includes single-phase or multi-phase ceramics, and the continuous phase of the substrate includes A single metal or alloy has good oxidation resistance, stable quality, and good heating uniformity, which can meet the heating requirements of new tobacco products.
  • the hard phase of the present invention includes single-phase or multi-phase ceramics, which has high strength, good corrosion resistance, wear resistance and thermal stability.
  • the continuous phase of the present invention includes a single metal or alloy, and has good ductility and workability. 4.
  • the present invention is provided with a composite nitride layer, which can improve the oxidation resistance and stability of the coating. 5.
  • the continuous phase of the present invention is a single metal chromium or aluminum, or an alloy containing chromium and/or aluminum, and the coating is a composite coating containing chromium or aluminum, which can improve the bonding strength of the coating and the substrate.
  • the preparation method of the heating element of the present invention is simple, efficient, and economical. 7.
  • the invention can obtain an alloy of uniform quality through mechanical alloying, and improve the mechanical, physical and chemical properties of the alloy.
  • the present invention uses a multi-target magnetron sputtering apparatus for surface coating, which can improve the uniformity of the coating.
  • the additive powder of the present invention includes tungsten carbide powder, molybdenum powder and graphite powder, which can play the role of grain refinement, strengthening and toughening. 10.
  • the present invention has simple structure, convenient use and broad market prospects.
  • the heating element proposed by the present invention includes a base body and a coating covering the outer surface of the base body.
  • the matrix includes a hard phase and a continuous phase
  • the hard phase includes single-phase or multi-phase ceramics, which has high strength, good corrosion resistance, wear resistance and thermal stability.
  • the continuous phase includes a single metal or alloy with good ductility and workability.
  • the coating is used to prevent oxidation of the heating element.
  • the heating element of the invention has good oxidation resistance, stable product quality and good heating uniformity, and can meet the heating requirements of new tobacco products.
  • the single metal is chromium.
  • the single metal is aluminum.
  • the alloy is an alloy containing chromium and/or aluminum, which can improve thermal conductivity, wear resistance, corrosion resistance and oxidation resistance, so that the matrix has good mechanical, physical and chemical properties.
  • the total mass fraction of chromium and/or aluminum in the alloy is 10%-50%, which can further improve thermal conductivity, corrosion resistance and oxidation resistance.
  • the coating is a composite coating containing chromium and/or aluminum, which has good oxidation resistance and stability.
  • the continuous phase is a single metal chromium or aluminum, or an alloy containing chromium and/or aluminum, and the coating is a composite coating containing chromium and/or aluminum, the bonding strength of the coating and the substrate can be improved.
  • the composite coating is a composite nitride layer containing chromium and/or aluminum, which can improve oxidation resistance and stability.
  • the total atomic fraction of chromium and/or aluminum in the composite nitride layer is 50%-100%.
  • the single-phase ceramic includes one of carbide ceramics, nitride ceramics, boride ceramics, and oxide ceramics.
  • the single-phase ceramics include single-phase solid solution ceramics formed by multiple substances of carbides, nitrides, borides, and oxides.
  • the multi-phase ceramic includes a plurality of single-phase ceramics.
  • the thickness of the coating is 0.5 to 1.5 microns.
  • the resistivity of the heating element is 0.001-0.05 ohm ⁇ cm.
  • the preparation method of the heating element proposed in the present invention includes the following steps:
  • the substrate is surface-coated to obtain a heating element.
  • grinding and polishing the heating element on a grinder can improve the surface quality of the heating element.
  • the alloy powder when the alloy powder is obtained, a variety of simple metal powders including at least chromium or aluminum are added to the first ball milling tank according to a certain mass ratio, and argon gas is introduced after sealing, and then the first ball milling tank Mechanical alloying inside.
  • Mechanical alloying is a process in which high-energy grinders or ball mills can be used to achieve solid-state alloying. The process is simple, efficient, and economical. At the same time, mechanical alloying can make the quality of the alloy uniform and improve the mechanical, physical and chemical properties of the alloy.
  • the ball-to-material ratio of the first ball mill tank is 15:1-25:1
  • the rotating speed is 300-500 revolutions per minute
  • the ball milling time is 48-96 hours, which can improve the quality of ball milling.
  • stearic acid is added to the first ball milling tank to continue ball milling.
  • the milling time is 0.5 to 4 hours, which can refine the crystal grains and improve the fluidity of the crystal grains.
  • the dispersion is good.
  • the total mass fraction of the chromium and/or aluminum elemental powder is 10%-50%, which can further improve the thermal conductivity, corrosion resistance and oxidation resistance.
  • the single-phase or multi-phase ceramic powder, single metal or alloy powder, and additive powder are added to the second ball milling tank, and absolute ethanol is added and then ball milling is performed in the second ball milling tank.
  • the mixing effect is good. , Can improve the quality of ball milling; wherein, the ball-to-material ratio in the second ball milling tank is 5:1-10:1, the rotating speed is 120-350 revolutions per minute, and the milling time is 24-96 hours, which can improve the quality of ball milling.
  • the mass fractions of the components in the material of the second ball mill are respectively: single-phase or multiphase ceramic powder 42.00%-68.00%, single metal or alloy powder 12.00%-30.00%, adding Material powder 16.5% ⁇ 46%.
  • the powder slurry is vacuum dried at a temperature of 75-90 degrees Celsius, which can increase the drying speed and has a good drying effect.
  • the compression pressure of the compression molding is 200-400 MPa, and the pressure-holding time is 0.5-2 minutes.
  • the molded blank is sintered under a vacuum degree greater than 1 ⁇ 10 -1 Pa, the sintering temperature is 1220 to 1450 degrees Celsius, and the holding time is 15 to 60 minutes, which can improve the compactness of the matrix. , which improves the comprehensive mechanical properties of the matrix.
  • the surface coating is performed on the multi-target magnetron sputtering apparatus, which can improve the uniformity of the coating; wherein, the target material of the multi-target magnetron sputtering apparatus contains Alloy of chromium and/or aluminum, the vacuum degree is greater than 3 ⁇ 10 -3 Pa, the target material is controlled by DC cathode, the sputtering power is 80-120 watts, the sputtering time is 1 to 2 hours, and the sputtering temperature is 280-320 In degrees Celsius, the sputtering coating adopts a mixed gas of argon and nitrogen, which can prevent oxidation and improve the oxidation resistance of the coating.
  • the purity of the mixed gas is not less than 99.999%, which can further improve the oxidation resistance of the coating.
  • the gas flow ratio of argon to nitrogen is 1:1, which has good stability.
  • the total atomic fraction of chromium and/or aluminum in the target material is 50%-100%.
  • the coating is a composite coating containing chromium and/or aluminum, which has good oxidation resistance and stability, and can improve the bonding strength of the coating.
  • the composite coating is a composite nitride layer containing chromium and/or aluminum, which can improve oxidation resistance and stability.
  • the total atomic fraction of chromium and/or aluminum in the composite nitride layer is 50%-100% of the metal element, which can further improve the oxidation resistance and stability of the coating.
  • the additive powder includes tungsten carbide powder, molybdenum powder and graphite powder, which can play a role in strengthening, toughening, and grain refinement.
  • the preparation method of the heating element of the invention is simple and efficient, has good economic efficiency, the prepared heating element has good oxidation resistance, the product quality is more stable, and the heating is more uniform.
  • the present invention provides the use of the above-mentioned heating element according to the present invention and the heating element prepared according to the above-mentioned method of the present invention in the preparation of a new type of heating element for tobacco products.
  • the heating element is used to heat low-temperature cigarettes.
  • the preparation method of the heating element includes the following steps:
  • Ni (nickel) and Cr (chromium) are added to the first high-energy ball milling tank at a mass fraction of 1:1, and Ar (argon) gas is injected into the first high-energy ball milling tank for mechanical alloying.
  • Ar argon
  • the first high-energy ball milling tank The ball-to-material ratio is 15:1, the rotating speed is 300rpm (revolutions per minute), and the milling time is 48h (hours).
  • SA stearic acid
  • the granulated powder is compression-molded, the compression pressure is 400 MPa (megapascals), the pressure holding time is 1 min (minutes), and the molded blank is in a vacuum greater than 1 ⁇ 10 -1 Pa (Pa). Sintering is carried out at a temperature of 1420 degrees Celsius, and the holding time is 60 minutes.
  • the surface is coated on a multi-target magnetron sputtering apparatus.
  • the target material is a CrAl (chromium aluminum) alloy, and the atomic ratio of Al (aluminum) and Cr (chromium) is 1:1;
  • the vacuum degree is 2.5 ⁇ 10 -3 Pa, the sputtering power is 80 watts, the sputtering time is 1.5 hours, and the sputtering temperature is 280 degrees Celsius;
  • the sputtering coating adopts a mixed gas of argon and N 2 (nitrogen) , Its purity is less than 99.999%, and the gas flow ratio of argon and nitrogen is 1:1.
  • the test results show that as shown in Table 1, it can meet the electrical and structural characteristics of the heating element in the heater for low-temperature cigarettes.
  • coated sample is ground and polished on a grinder.
  • the mass fraction of titanium carbonitride solid solution powder is 42%
  • the mass fraction of nickel-chromium alloy powder is 30%
  • the mass fraction of tungsten carbide powder is 13%
  • the mass fraction of molybdenum powder is 14%
  • the mass fraction of graphite powder is The score is 1%.
  • the preparation method of the heating element includes the following steps:
  • Ni (nickel) and Al (aluminum) are added to the first high-energy ball mill tank according to the mass fraction of 1:2, and argon gas is passed into the tank for mechanical alloying.
  • the ball-to-material ratio of the first high-energy ball mill tank is The speed is 20:1, the speed is 350 revolutions per minute, and the ball milling time is 64 hours.
  • take out NiAl (nickel aluminum) alloy powder are added to the first high-energy ball mill tank according to the mass fraction of 1:2, and argon gas is passed into the tank for mechanical alloying.
  • the ball-to-material ratio of the first high-energy ball mill tank is The speed is 20:1, the speed is 350 revolutions per minute, and the ball milling time is 64 hours.
  • add 2% mass fraction of stearic acid to the first high-energy ball milling tank and continue ball milling for 2 hours.
  • the granulated powder is compression-molded, the compression pressure is 300 MPa, the holding time is 1 minute, and the molded blank is sintered at a vacuum degree higher than 1 ⁇ 10 -1 Pa.
  • the sintering temperature is 1250 degrees Celsius, and the holding time is 45 minutes.
  • the surface is coated on a multi-target magnetron sputtering apparatus.
  • the target material is TiAl (titanium aluminum) alloy, and the atomic ratio of aluminum to Ti (titanium) is 5:1 ,
  • the vacuum degree is 3 ⁇ 10 -3 Pa, the sputtering power is 110 watts, the sputtering time is 2 hours, the sputtering temperature is 300 degrees Celsius; the sputtering coating adopts a mixed gas of argon and nitrogen, and its purity is 99.999% ,
  • the gas flow ratio of argon and nitrogen is 1:1.
  • coated sample is ground and polished on a grinder.
  • the mass fraction of solid solution powder formed by titanium carbide and boron carbide is 45%
  • the mass fraction of nickel-aluminum alloy powder is 27%
  • the mass fraction of tungsten carbide powder is 12%
  • the mass fraction of molybdenum powder is 15%
  • the mass fraction of graphite is 1%.
  • the preparation method of the heating element includes the following steps:
  • the first high-energy ball milling tank has a ball-to-battery ratio of 25:1.
  • the ball milling time is 320 revolutions per minute and the ball milling time is 72 hours.
  • the granulated powder is compression-molded, the compression pressure is 300 MPa, and the holding time is 2 minutes, and the molded blank is sintered under a vacuum degree greater than 1 ⁇ 10 -1 Pa.
  • the sintering temperature is 1450 degrees Celsius, and the holding time is 60 minutes.
  • the target material is a nickel-chromium alloy, in which the atomic ratio of chromium to nickel is 3:1, and the vacuum degree is 2.5 ⁇ 10 -3 Pa, sputtering power of 80 watts, sputtering time of 1 hour, sputtering temperature of 320 degrees Celsius; sputtering coating using a mixed gas of argon and nitrogen, the purity of which is less than 99.999%, argon and nitrogen
  • the airflow ratio is 1:1.
  • coated sample is ground and polished on a grinder.
  • the mass fraction of titanium carbide solid solution powder is 68%
  • the mass fraction of nickel-chromium alloy powder is 12%
  • the mass fraction of tungsten carbide powder is 13%
  • the mass fraction of molybdenum powder is 6%
  • the mass fraction of graphite powder is 1%.
  • the preparation method of the heating element includes the following steps:
  • the elemental powders of iron, chromium and nickel are added to the first high-energy ball mill tank at a mass fraction of 1:4:1, and the argon gas is introduced into the first high-energy ball mill for mechanical alloying.
  • the ball-to-material ratio of the first high energy ball mill is 20 :1.
  • Rotation speed is 350 revolutions per minute, ball milling time is 96 hours.
  • add 2% stearic acid to the ball mill tank and continue ball milling for 4 hours.
  • the surface is coated on a multi-target magnetron sputtering apparatus.
  • the target is a chromium aluminum alloy, and the atomic ratio of aluminum to chromium is 1:1, and the vacuum degree is 2.5 ⁇ 10 -3 Pa, sputtering power of 120 watts, sputtering time of 1 hour, sputtering temperature of 320 degrees Celsius, sputtering coating using a mixed gas of argon and nitrogen, the purity of which is 99.999%, argon and nitrogen
  • the airflow ratio is 1:1.
  • coated sample is ground and polished on a grinder.
  • the mass fraction of titanium carbide and alumina solid solution powder is 51%
  • the mass fraction of nickel-chromium alloy powder is 20%
  • the mass fraction of tungsten carbide powder is 14%
  • the mass fraction of molybdenum powder is 14%
  • the mass fraction of graphite powder is The mass fraction is 1%.
  • the preparation method of the heating element includes the following steps:
  • the first high-energy ball mill tank has a ball-to-battery ratio of 15:1, and the rotation speed
  • the ball milling time is 300 revolutions per minute, and the ball milling time is 48 hours.
  • the granulated powder is compression-molded, the compression pressure is 400 MPa, and the holding time is 1 minute, and the molded blank is sintered under a vacuum degree greater than 1 ⁇ 10 -1 Pa.
  • the sintering temperature is 1410 degrees Celsius, and the holding time is 60 minutes.
  • the target material is a titanium aluminum alloy, where the atomic ratio of aluminum to titanium is 2:1, and the vacuum degree is 2.5 ⁇ 10 -3 Pa, sputtering power of 80 watts, sputtering time of 2 hours, sputtering temperature of 320 degrees Celsius, sputtering coating using a mixed gas of argon and nitrogen, its purity is 99.999%, argon and nitrogen
  • the airflow ratio is 1:1.
  • coated sample is ground and polished on a grinder.
  • the mass fraction of tungsten carbide solid solution powder is 52%
  • the mass fraction of nickel aluminum alloy powder is 30%
  • the mass fraction of tungsten carbide powder is 8%
  • the mass fraction of molybdenum powder is 9%
  • the mass fraction of graphite powder is 1%.

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Abstract

一种发热体及其制备方法和用途，发热体包括基体和包覆在基体外表面的涂层；基体包括硬质相和连续相，硬质相包括单相或多相陶瓷，连续相包括单一金属或合金；涂层用于防止发热体氧化。发热体的制备方法包括以下步骤：(1)获取单相或多相陶瓷粉，以及单一金属或合金粉；(2)将单相或多相陶瓷粉、单一金属或合金粉以及添加物粉进行球磨，获取粉末浆料；(3)烘干粉末浆料，获取造粒后的粉料；(4)将造粒后的粉料模压成型后进行烧结，获取基体；(5)将基体进行表面涂层，获取发热体。以及发热体在新型烟草制品用加热器中的用途。该发热体抗氧化性好，质量稳定，发热均匀性好，且制备工艺简洁高效，经济性好。

Description

一种发热体及其制备方法和用途 技术领域
本发明涉及一种发热体及其制备方法和用途，属于复合材料和粉末冶金技术领域。
背景技术
低温卷烟的功能性原理为：通过发热体材料在一定的外场条件下，迅速升温到目标温度(一般为300～400℃(摄氏度))，随后对周围的特制烟叶进行烘烤从而产生与传统香烟相似的吸烟效果。由于低温卷烟的发烟温度较低，因此毒性较传统香烟小，且能够根据不同需求添加特制香味或优化口感，在国内外受到极大的欢迎。目前低温卷烟所采用的发热方式通常为电阻式发热，通过电流通过发热电阻的方式产生热源，相关设备中发热体一般为MCH陶瓷(陶瓷发热体)。该陶瓷发热体通常是将发热浆料按照一定的电路印制在陶瓷坯料上，通过后续的烧成工艺实现冶金结合，再进行釉料封装后连接电极。然而，虽然该陶瓷发热体能够一定程度的满足产品需求，但其制备工艺复杂、成本高，同时存在着产品质量不均匀问题，这些不足会严重阻碍低温卷烟的市场化应用。因此，急需开发新型发热材料。低温卷烟用发热体的性能需求主要为：1)生物相容性，在低温、高温条件下无毒；2)电阻可调；3)能够承受一定程度的高温，抗氧化性、高温稳定性好，且具有一定的高温强度；4)能够承受烟草介质腐蚀，具有较好的化学稳定性；5)导热性好；6)良好的室温和高温力学性能；7)数万次以上的使用寿命。现有的单一合金或陶瓷材料很难满足上述要求。
发明内容
针对上述问题，本发明的目的是提供一种发热体及其制备方法和用途，其能够抗氧化，质量稳定，发热均匀性好，且制备工艺简洁高效，经济性好。
为实现上述目的，一方面，本发明提出了一种发热体，包括基体和包覆在所述基体外表面的涂层；其中，所述基体包括硬质相和连续相，所述硬质相包 括单相或多相陶瓷，所述连续相包括单一金属或合金；所述涂层用于防止所述发热体氧化。
在一个具体实施例中，所述单一金属为铬或铝。
在一个具体实施例中，所述合金为含铬和/或铝的合金。
在一个具体实施例中，所述合金中铬和/或铝的总质量分数为10％～50％。
在一个具体实施例中，所述涂层为含铬和/或铝的复合涂层。
在一个具体实施例中，所述复合涂层为含铬和/或铝的复合氮化物层。
在一个具体实施例中，所述复合氮化物层中铬和/或铝占金属元素的总原子分数为50％～100％。
在一个具体实施例中，所述单相陶瓷包括碳化物陶瓷、氮化物陶瓷、硼化物陶瓷以及氧化物陶瓷中的一种。
在一个具体实施例中，所述单相陶瓷包括碳化物、氮化物、硼化物以及氧化物中的多种物质形成的单相固溶体陶瓷。
在一个具体实施例中，所述多相陶瓷包括多种单相陶瓷。
在一个具体实施例中，所述涂层的厚度为0.5～1.5微米。
在一个具体实施例中，所述发热体的电阻率为0.001～0.05欧姆·厘米。
另一方面，本发明还提出了一种制备上述发热体的方法，包括以下步骤：(1)获取单相或多相陶瓷粉，以及单一金属或合金粉；(2)将所述单相或多相陶瓷粉、所述单一金属或合金粉以及添加物粉进行球磨，获取粉末浆料；(3)烘干所述粉末浆料，获取造粒后的粉料；(4)将所述造粒后的粉料模压成型后进行烧结，获取所述基体；(5)将所述基体进行表面涂层，获取所述发热体。
在一个具体实施例中，将所述发热体在研磨机上进行研磨抛光，用于提高所述发热体的表面质量。
在一个具体实施例中，获取所述合金粉时，将包括铬和/或铝的多种金属单质粉末按照一定质量配比加入第一球磨罐中，密封后通入氩气，然后在所述第一球磨罐内进行机械合金化；其中，所述第一球磨罐的球料比为15:1～25:1，转速为300～500转每分钟，球磨时间为48～96小时。
在一个具体实施例中，所述机械合金化完成后，向所述第一球磨罐中添加硬脂酸继续球磨，球磨时间为0.5～4小时。
在一个具体实施例中，所述铬和/或铝单质粉末的总质量分数为10％～50％。
在一个具体实施例中，将所述单相或多相陶瓷粉、所述单一金属或合金粉以及所述添加物粉加入第二球磨罐中，添加无水乙醇后在所述第二球磨罐中进行球磨，其中，所述第二球磨罐中球料比为5:1～10:1，转速为120～350转每分钟，球磨时间为24～96小时。
在一个具体实施例中，所述第二球磨罐的物料中各组分所占的质量分数分别为：所述单相或多相陶瓷粉42.00％～68.00％，所述单一金属或合金粉12.00％～30.00％，所述添加物粉16.5％～46％。
在一个具体实施例中，所述粉末浆料进行真空烘干，温度为75～90摄氏度。
在一个具体实施例中，所述模压成型的压制压力为200～400兆帕，保压时间为0.5～2分钟。
在一个具体实施例中，将所述模压成型后的坯料在大于1×10 -1帕真空度下进行烧结，烧结温度为1220～1450摄氏度，保温时间为15～60分钟。
在一个具体实施例中，将所述基体在多靶磁控溅射仪上进行表面涂层；其中，所述多靶磁控溅射仪的靶材为含铬和/或铝的合金，真空度大于3×10 -3帕，所述靶材采用直流阴极控制，溅射功率为80～120瓦，溅射时间为1～2小时，溅射温度为280～320摄氏度，溅射镀膜采用氩气与氮气的混合气体。
在一个具体实施例中，所述靶材中铬和/或铝占金属元素的总原子分数为50％～100％。
在一个具体实施例中，所述添加物粉包括碳化钨粉、钼粉以及石墨粉。
再一方面，本发明还提出了上述发热体和通过上述方法制备的发热体在新型烟草制品用发热器中的用途，特别是低温烟用发热器中的用途。
本发明由于采取以上技术方案，其具有以下优点：1、本发明的发热体包括基体和用于防止基体氧化的涂层，基体的硬质相包括单相或多相陶瓷，基体的连续相包括单一金属或合金，抗氧化性好，质量稳定，且发热均匀性好，能够 满足新型烟草制品的加热要求。2、本发明的硬质相包括单相或多相陶瓷，强度高，耐腐蚀性、耐磨性和热稳定性好。3、本发明的连续相包括单一金属或合金，延展性好，可加工性好。4、本发明设置了复合氮化物层，能够提高涂层的抗氧化性和稳定性。5、本发明的连续相为单一金属铬或铝，或为含铬和/或铝的合金，且涂层为含铬或铝的复合涂层，能够提高涂层与基体的结合强度。6、本发明的发热体的制备方法简洁高效，经济性好。7、本发明通过机械合金化能够获取质量均匀的合金，提高合金的机械性能、物理性能和化学性能。8、本发明通过多靶磁控溅射仪进行表面涂层，能够提高涂层的均匀性。9、本发明的添加物粉包括碳化钨粉、钼粉和石墨粉，能够起到细化晶粒、增强以及增韧的作用。10、本发明的结构简单，使用方便，市场前景广阔。
本发明的其它特征和优点将在随后的说明书中阐述，并且部分的从说明书中变得显而易见，或者通过实施本发明而了解。本发明的目的和其他优点可通过在说明书和权利要求书中所特别指出的结构来实现和获得。
具体实施方式
以下将结合实施例来详细说明本发明的实施方式，借此对本发明如何应用技术手段来解决技术问题，并达成技术效果的实现过程能充分理解并据以实施。需要说明的是，只要不构成冲突，本发明中的各个实施例以及各实施例中的各个特征可以相互结合，所形成的技术方案均在本发明的保护范围之内。
一方面，本发明提出的发热体，包括基体和包覆在基体外表面的涂层。其中，基体包括硬质相和连续相，硬质相包括单相或多相陶瓷，强度高，耐腐蚀性、耐磨性以及热稳定性好。连续相包括单一金属或合金，延展性好，可加工性好。涂层用于防止发热体氧化。本发明的发热体抗氧化性好，产品质量稳定，发热均匀性好，能够满足新型烟草制品的加热要求。
在一个优选的实施例中，单一金属为铬。
在另一个优选的实施例中，单一金属为铝。
在一个具体的实施例中，合金为含铬和/或铝的合金，能够提高导热性、耐磨性、抗腐蚀性以及抗氧化性，使得基体具有良好的机械性能、物理性能和化学性能。
在一个具体的实施例中，合金中铬和/或铝的总质量分数为10％～50％，能够进一步提高导热性、抗腐蚀性以及抗氧化性。
在一个具体的实施例中，涂层为含铬和/或铝的复合涂层，抗氧化性和稳定性好。同时，由于连续相为单一金属铬或铝，或为含铬和/或铝的合金，涂层为含铬和/或铝的复合涂层，因此能够提高涂层与基体的结合强度。
在一个优选的实施例中，复合涂层为含铬和/或铝的复合氮化物层，能够提高抗氧化性和稳定性。
在一个具体实施例中，复合氮化物层中铬和/或铝占金属元素的总原子分数为50％～100％。
在一个具体的实施例中，单相陶瓷包括碳化物陶瓷、氮化物陶瓷、硼化物陶瓷以及氧化物陶瓷中的一种。
在一个具体的实施例中，单相陶瓷包括碳化物、氮化物、硼化物以及氧化物中的多种物质形成的单相固溶体陶瓷。
在一个具体的实施例中，多相陶瓷包括多种单相陶瓷。
在一个具体的实施例中，涂层的厚度为0.5～1.5微米。
在一个具体的实施例中，发热体的电阻率为0.001～0.05欧姆·厘米。
另一方面，在上述发热体的基础上，本发明提出的发热体的制备方法，包括以下步骤：
(1)获取单相或多相陶瓷粉，以及单一金属或合金粉；
(2)将单相或多相陶瓷粉、单一金属或合金粉以及添加物粉进行球磨，获取粉末浆料；
(3)烘干粉末浆料，获取造粒后的粉料；
(4)将造粒后的粉料模压成型后进行烧结，获取基体；
(5)将基体进行表面涂层，获取发热体。
在一个具体的实施例中，将发热体在研磨机上进行研磨抛光，能够提高发热体的表面质量。
在一个具体的实施例中，获取合金粉时，将至少包括铬或铝的多种金属单质粉末按照一定质量配比加入第一球磨罐中，密封后通入氩气，然后在第一球磨罐内进行机械合金化。机械合金化是能够采用高能研磨机或球磨机实现固态合金化的过程，工艺简洁高效，经济性好。同时机械合金化能够使得合金质量均匀，提高合金的机械性能、物理性能和化学性能。其中，第一球磨罐的球料比为15:1～25:1，转速为300～500转每分钟，球磨时间为48～96小时，能够提高球磨质量。
在一个具体的实施例中，机械合金化完成后，向第一球磨罐中添加硬脂酸继续球磨，球磨时间为0.5～4小时，能够细化晶粒，改善晶粒流动性，粉体颗粒的分散性好。
在一个具体的实施例中，铬和/或铝单质粉末的总质量分数为10％～50％，能够进一步提高导热性、抗腐蚀性以及抗氧化性。
在一个具体的实施例中，将单相或多相陶瓷粉、单一金属或合金粉以及添加物粉加入第二球磨罐中，添加无水乙醇后在第二球磨罐中进行球磨，混合效果好，能够提高球磨质量；其中，第二球磨罐中球料比为5:1～10:1，转速120～350转每分钟，球磨时间为24～96小时，能够提高球磨质量。
在一个具体的实施例中，第二球磨机的物料中各组分所占的质量分数分别为：单相或多相陶瓷粉42.00％～68.00％，单一金属或合金粉12.00％～30.00％，添加物粉16.5％～46％。
在一个具体的实施例中，粉末浆料进行真空烘干，温度为75～90摄氏度，能够提高烘干速度，烘干效果好。
在一个具体的实施例中，模压成型的压制压力为200～400兆帕，保压时间为0.5～2分钟。
在一个具体的实施例中，将模压成型后的坯料在大于1×10 -1帕真空度下进行烧结，烧结温度为1220～1450摄氏度，保温时间为15～60分钟，能够提高基体的致密性，使得基体的综合力学性能得到提高。
在一个具体的实施例中，将基体清洗、干燥后在多靶磁控溅射仪上进行表面涂层，能够提高涂层的均匀性；其中，多靶磁控溅射仪的靶材为含铬和/或铝 的合金，真空度大于3×10 -3帕，靶材采用直流阴极控制，溅射功率为80～120瓦，溅射时间为1～2小时，溅射温度为280～320摄氏度，溅射镀膜采用氩气与氮气的混合气体，能够防止发生氧化作用，提高涂层的抗氧化性能。
在一个具体的实施例中，混合气体的纯度均不低于99.999％，能够进一步提高涂层的抗氧化性能。
在一个具体的实施例中，氩气与氮气的气流比为1:1，稳定性好。
在一个优选的实施例中，靶材中铬和/或铝占金属元素的总原子分数为50％～100％。
在一个具体的实施例中，涂层为含铬和/或铝的复合涂层，抗氧化性和稳定性好，同时能够提高涂层的结合强度。
在一个优选的实施例中，复合涂层为含铬和/或铝的复合氮化物层，能够提高抗氧化性和稳定性。
在一个具体的实施例中，复合氮化物层中铬和/或铝占金属元素的总原子分数为50％～100％，能够进一步提高涂层的抗氧化性和稳定性。
在一个具体的实施例中，添加物粉包括碳化钨粉、钼粉和石墨粉，能够起到增强、增韧以及细化晶粒的作用。
本发明发热体的制备方法简捷高效，经济性好，制备的发热体抗氧化性好，产品质量更加稳定，发热更加均匀。
再一方面，本发明提供了根据本发明的上述发热体和根据本发明的上述方法制得的发热体在制备新型烟草制品用发热器中的用途。
在一个具体的实施例中，发热体用于加热低温卷烟。
下面列举多个具体的实施例
实施例1
在本实施例中，发热体的制备方法包括以下步骤：
(1)将Ni(镍)、Cr(铬)单质粉末按照质量分数1:1加入第一高能球磨罐中，通入Ar(氩)气后进行机械合金化，其中，第一高能球磨罐的球料比为 15:1，转速300rpm(转每分钟)，球磨时间48h(小时)，完成后向第一高能球磨罐中添加质量分数2％SA(硬脂酸)继续球磨0.5小时，完成后取出NiCr(镍铬)合金粉末。
(2)将Ti(C，N)(碳氮化钛)固溶体粉、镍铬合金粉、WC(碳化钨)粉、Mo(钼)粉以及C(石墨)粉加入第二高能球磨罐中，添加无水乙醇后进行球磨，其中，第二高能球磨罐的球料比为5:1，转速为120转每分钟，球磨时间为24小时。
(3)将制备的粉末浆料进行真空烘干，温度为80℃(摄氏度)，获取造粒后的粉料。
(4)将造粒后的粉料进行模压成型，压制压力为400MPa(兆帕)，保压时间为1min(分钟)，并将模压成型的坯料在大于1×10 -1Pa(帕)真空度下进行烧结，烧结温度为1420摄氏度，保温时间为60分钟。
(5)将上述烧结后的样品清洗、干燥后在多靶磁控溅射仪上进行表面涂层，靶材为CrAl(铬铝)合金，其中Al(铝)、Cr(铬)原子比为1:1；真空度为2.5×10 -3帕，溅射功率为80瓦，溅射时间为1.5小时，溅射温度为280摄氏度；溅射镀膜采用氩气与N 2(氮气)的混合气体，其纯度为于99.999％，氩气和氮气的气流比为1:1。经测试得到的结果表明如表1所示，能够满足低温卷烟用加热器中发热体的电学和结构特性的要求。
进一步地，将涂层后的样品在研磨机上进行研磨抛光。
进一步地，碳氮化钛固溶体粉的质量分数为42％，镍铬合金粉的质量分数为30％，碳化钨粉的质量分数为13％，钼粉的质量分数为14％，石墨粉的质量分数为1％。
实施例2
在本实施例中，发热体的制备方法包括以下步骤：
(1)将Ni(镍)、Al(铝)单质粉末按照质量分数1:2加入第一高能球磨罐中，通入氩气后进行机械合金化，其中，第一高能球磨罐的球料比为20:1，转速为350转每分钟，球磨时间64小时，完成后向第一高能球磨罐中添加质量分数2％硬脂酸继续球磨2小时，完成后取出NiAl(镍铝)合金粉末。
(2)将碳化钛及碳化硼粉、镍铝合金粉、碳化钨粉、钼粉以及石墨粉加入第二高能球磨罐中，添加无水乙醇后进行球磨，其中，第二高能球磨罐的球料比为7:1，转速为220转每分钟，球磨时间为36小时。
(3)将制备的粉末浆料进行真空烘干，温度为75摄氏度，获取造粒后的粉料。
(4)将造粒后的粉料进行模压成型，压制压力为300兆帕，保压时间为1分钟，并将模压成型后的坯料在高于1×10 -1帕真空度下进行烧结，烧结温度为1250摄氏度，保温时间为45分钟。
(5)将上述烧结后的样品清洗、干燥后在多靶磁控溅射仪上进行表面涂层，靶材为TiAl(钛铝)合金，其中铝、Ti(钛)原子比为5:1，真空度为3×10 -3帕，溅射功率为110瓦，溅射时间为2小时，溅射温度为300摄氏度；溅射镀膜采用氩气与氮气的混合气体，其纯度为于99.999％，氩气和氮气的气流比为1:1。经测试得到的结果表明如表1所示，能够满足低温卷烟用加热器中发热体的电学和结构特性的要求。
进一步地，将涂层后的样品在研磨机上进行研磨抛光。
进一步地，碳化钛和碳化硼形成的固溶体粉的质量分数为45％，镍铝合金粉的质量分数为27％，碳化钨粉的质量分数为12％，钼粉的质量分数为15％，石墨粉的质量分数为1％。
实施例3
在本实施例中，发热体的制备方法包括以下步骤：
(1)将镍、铬单质粉末按照质量分数3:1加入第一高能球磨罐中，通入氩气后进行机械合金化，其中，第一高能球磨罐的球料比为25:1，转速为320转每分钟，球磨时间72小时，完成后向球磨罐中添加质量分数2％硬脂酸继续球磨2小时，完成后取出镍铬合金粉末。
(2)将碳化钛粉、镍铬合金粉、碳化钨粉、钼粉以及石墨粉加入第二高能球磨罐中，添加无水乙醇后进行球磨，其中，第二高能球磨罐的球料比为7:1，转速为350转每分钟，球磨时间为48小时。
(3)将制备的粉末浆料进行真空烘干，温度为90摄氏度，获取造粒后的粉料。
(4)将造粒后的粉料进行模压成型，压制压力为300兆帕，保压时间为2分钟，并将模压成型后的胚料在大于1×10 -1帕真空度下进行烧结，烧结温度为1450摄氏度，保温时间为60分钟。
(5)将上述烧结后的样品清洗、干燥后在多靶磁控溅射仪上进行表面涂层，靶材为镍铬合金，其中铬、镍原子比为3:1，真空度为2.5×10 -3帕，溅射功率为80瓦，溅射时间为1小时，溅射温度为320摄氏度；溅射镀膜采用氩气与氮气的混合气体，其纯度为于99.999％，氩气和氮气的气流比为1:1。经测试得到的结果表明如表1所示，能够满足低温卷烟用加热器中发热体的电学和结构特性的要求。
进一步地，将涂层后的样品在研磨机上进行研磨抛光。
进一步地，碳化钛固溶体粉的质量分数为68％，镍铬合金粉的质量分数为12％，碳化钨粉的质量分数为13％，钼粉的质量分数为6％，石墨粉的质量分数为1％。
实施例4
在本实施例中，发热体的制备方法包括以下步骤：
(1)将铁、铬以及镍单质粉末按照质量分数1:4:1加入第一高能球磨罐中，通入氩气后进行机械合金化，其中，第一高能球磨罐的球料比为20:1，转速为350转每分钟，球磨时间96小时，完成后向球磨罐中添加质量分数2％硬脂酸继续球磨4小时，完成后取出FeCrNi(铁铬镍)合金粉末。
(2)将TiC(碳化钛)及Al 2O 3(氧化铝)粉、铁铬镍合金粉、碳化钨粉、钼粉以及石墨粉加入第二高能球磨罐中，添加无水乙醇后进行球磨，其中，第二高能球磨罐的球料比为5:1，转速为230转每分钟，球磨时间为24小时。
(3)将制备的粉末浆料进行真空烘干，温度为80摄氏度，获取造粒后的粉料。
(4)将造粒后的粉料进行模压成型，压制压力为300兆帕，保压时间为1 分钟，并将模压成型后的胚料在高于1×10 -1帕真空度下进行烧结，烧结温度为1350摄氏度，保温时间为60分钟。
(5)将上述烧结后的样品清洗、干燥后在多靶磁控溅射仪上进行表面涂层，靶材为铬铝合金，其中铝、铬原子比为1:1，真空度为2.5×10 -3帕，溅射功率为120瓦，溅射时间为1小时，溅射温度为320摄氏度，溅射镀膜采用氩气与氮气的混合气体，其纯度为于99.999％，氩气和氮气的气流比为1:1。经测试得到的结果表明如表1所示，能够满足低温卷烟用加热器中发热体的电学和结构特性的要求。
进一步地，将涂层后的样品在研磨机上进行研磨抛光。
进一步地，碳化钛及氧化铝固溶体粉的质量分数为51％，镍铬合金粉的质量分数为20％，碳化钨粉的质量分数为14％，钼粉的质量分数为14％，石墨粉的质量分数为1％。
实施例5
在本实施例中，发热体的制备方法包括以下步骤：
(1)将镍、铝单质粉末按照质量分数1:4加入第一高能球磨罐中，通入氩气后进行机械合金化，其中，第一高能球磨罐的球料比为15:1，转速为300转每分钟，球磨时间48小时，完成后向第一高能球磨罐中添加质量分数2％硬脂酸继续球磨2小时，完成后取出镍铝合金粉末。
(2)将碳化硅粉、镍铝合金粉、碳化钨粉、钼粉以及石墨粉加入第二高能球磨罐中，添加无水乙醇后进行球磨添加无水乙醇后进行球磨，其中，第二高能球磨罐的球料比为7:1，转速320转每分钟，球磨时间为24小时。
(3)将制备的粉末浆料进行真空烘干，温度为80摄氏度，获取造粒后的粉料。
(4)将造粒后的粉料进行模压成型，压制压力为400兆帕，保压时间为1分钟，并将模压成型后的胚料在大于1×10 -1帕真空度下进行烧结，烧结温度为1410摄氏度，保温时间为60分钟。
(5)将上述烧结后的样品清洗、干燥后在多靶磁控溅射仪上进行表面涂层， 靶材为钛铝合金，其中铝、钛原子比为2:1，真空度为2.5×10 -3帕，溅射功率为80瓦，溅射时间为2小时，溅射温度为320摄氏度，溅射镀膜采用氩气与氮气的混合气体，其纯度为于99.999％，氩气和氮气的气流比为1:1。经测试得到的结果表明如表1所示，能够满足低温卷烟用加热器中发热体的电学和结构特性的要求。
进一步地，将涂层后的样品在研磨机上进行研磨抛光。
进一步地，碳化钨固溶体粉的质量分数为52％，镍铝合金粉的质量分数为30％，碳化钨粉的质量分数为8％，钼粉的质量分数为9％，石墨粉的质量分数为1％。
表1各实施例中发热体材料的性能
Figure PCTCN2020123175-appb-000001
虽然本发明所公开的实施方式如上，但所述的内容只是为了便于理解本发明而采用的实施方式，并非用以限定本发明。任何本发明所属技术领域内的技术人员，在不脱离本发明所公开的精神和范围的前提下，可以在实施的形式上及细节上作任何的修改与变化，但本发明的专利保护范围，仍须以所附的权利要求书所界定的范围为准。

Claims (26)

  1. 一种发热体，其特征在于，包括基体和包覆在所述基体外表面的涂层；其中，所述基体包括硬质相和连续相，所述硬质相包括单相或多相陶瓷，所述连续相包括单一金属或合金；所述涂层用于防止所述发热体氧化。
  2. 根据权利要求1所述的发热体，其特征在于，所述单一金属为铬或铝。
  3. 根据权利要求1所述的发热体，其特征在于，所述合金为含铬和/或铝的合金。
  4. 根据权利要求3所述的发热体，其特征在于，所述合金中铬和/或铝的总质量分数为10％～50％。
  5. 根据权利要求1所述的发热体，其特征在于，所述涂层为含铬和/或铝的复合涂层。
  6. 根据权利要求5所述的发热体，其特征在于，所述复合涂层为含铬和/或铝的复合氮化物层。
  7. 根据权利要求6所述的发热体，其特征在于，所述复合氮化物层中铬和/或铝占金属元素的总原子分数为50％～100％。
  8. 根据权利要求1所述的发热体，其特征在于，所述单相陶瓷包括碳化物陶瓷、氮化物陶瓷、硼化物陶瓷以及氧化物陶瓷中的一种。
  9. 根据权利要求1所述的发热体，其特征在于，所述单相陶瓷包括碳化物、氮化物、硼化物以及氧化物中的多种物质形成的单相固溶体陶瓷。
  10. 根据权利要求1所述的发热体，其特征在于，所述多相陶瓷包括多种单相陶瓷。
  11. 根据权利要求1所述的发热体，其特征在于，所述涂层的厚度为0.5～1.5微米。
  12. 根据权利要求1所述的发热体，其特征在于，所述发热体的电阻率为0.001～0.05欧姆·厘米。
  13. 一种制备根据权利要求1～12中任一项所述的发热体的方法，其特征在于，包括以下步骤：
    (1)获取单相或多相陶瓷粉，以及单一金属或合金粉；
    (2)将所述单相或多相陶瓷粉、所述单一金属或合金粉以及添加物粉进行 球磨，获取粉末浆料；
    (3)烘干所述粉末浆料，获取造粒后的粉料；
    (4)将所述造粒后的粉料模压成型后进行烧结，获取所述基体；
    (5)将所述基体进行表面涂层，获取所述发热体。
  14. 根据权利要求13所述的制备方法，其特征在于，将所述发热体在研磨机上进行研磨抛光，用于提高所述发热体的表面质量。
  15. 根据权利要求13所述的制备方法，其特征在于，获取所述合金粉时，将包括铬和/或铝的多种金属单质粉末按照一定质量配比加入第一球磨罐中，密封后通入氩气，然后在所述第一球磨罐内进行机械合金化；
    其中，所述第一球磨罐的球料比为15:1～25:1，转速为300～500转每分钟，球磨时间为48～96小时。
  16. 根据权利要求15所述的制备方法，其特征在于，所述机械合金化完成后，向所述第一球磨罐中添加硬脂酸继续球磨，球磨时间为0.5～4小时。
  17. 根据权利要求15所述的制备方法，其特征在于，所述铬和/或铝单质粉末的总质量分数为10％～50％。
  18. 根据权利要求13所述的制备方法，其特征在于，将所述单相或多相陶瓷粉、所述单一金属或合金粉以及所述添加物粉加入第二球磨罐中，添加无水乙醇后在所述第二球磨罐中进行球磨；
    其中，所述第二球磨罐中球料比为5:1～10:1，转速为120～350转每分钟，球磨时间为24～96小时。
  19. 根据权利要求18所述的制备方法，其特征在于，所述第二球磨罐的物料中各组分所占的质量分数分别为：所述单相或多相陶瓷粉42.00％～68.00％，所述单一金属或合金粉12.00％～30.00％，所述添加物粉16.5％～46％。
  20. 根据权利要求13所述的制备方法，其特征在于，所述粉末浆料进行真空烘干，温度为75～90摄氏度。
  21. 根据权利要求13所述的制备方法，其特征在于，所述模压成型的压制压力为200～400兆帕，保压时间为0.5～2分钟。
  22. 根据权利要求13所述的制备方法，其特征在于，将所述模压成型后的坯料在大于1×10 -1帕真空度下进行烧结，烧结温度为1220～1450摄氏度，保温时间为15～60分钟。
  23. 根据权利要求13所述的制备方法，其特征在于，将所述基体在多靶磁控溅射仪上进行表面涂层；
    其中，所述多靶磁控溅射仪的靶材为含铬和/或铝的合金，真空度大于3×10 -3帕，所述靶材采用直流阴极控制，溅射功率为80～120瓦，溅射时间为1～2小时，溅射温度为280～320摄氏度，溅射镀膜采用氩气与氮气的混合气体。
  24. 根据权利要求23所述的制备方法，其特征在于，所述靶材中铬和/或铝占金属元素的总原子分数为50％～100％。
  25. 根据权利要求13所述的制备方法，其特征在于，所述添加物粉包括碳化钨粉、钼粉以及石墨粉。
  26. 根据权利要求1～12中任一项所述的发热体和根据权利要求13～25中任一项所述的方法制备的发热体在新型烟草制品用加热器中的用途。
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