WO2023029466A1 - Matériau de chauffage électromagnétique à température de curie contrôlable pour une cigarette à basse température et procédé de préparation pour celui-ci - Google Patents

Matériau de chauffage électromagnétique à température de curie contrôlable pour une cigarette à basse température et procédé de préparation pour celui-ci Download PDF

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Publication number
WO2023029466A1
WO2023029466A1 PCT/CN2022/084152 CN2022084152W WO2023029466A1 WO 2023029466 A1 WO2023029466 A1 WO 2023029466A1 CN 2022084152 W CN2022084152 W CN 2022084152W WO 2023029466 A1 WO2023029466 A1 WO 2023029466A1
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WIPO (PCT)
Prior art keywords
electromagnetic heating
temperature
heating material
low
powder
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PCT/CN2022/084152
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English (en)
Chinese (zh)
Inventor
刘华臣
黄婷
谭健
吴聪
唐良颖
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湖北中烟工业有限责任公司
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Publication of WO2023029466A1 publication Critical patent/WO2023029466A1/fr

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Classifications

    • 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
    • A24F40/70—Manufacture
    • 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
    • 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
    • A24F40/50—Control or monitoring
    • A24F40/57—Temperature control
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/241—Chemical after-treatment on the surface
    • B22F2003/242—Coating

Definitions

  • the invention relates to the technical field of electromagnetic heating materials for cigarettes, in particular to an electromagnetic heating material with controllable Curie temperature for low-temperature cigarettes and a preparation method thereof.
  • the heating methods of low-temperature cigarettes on the market mainly include resistance heating and electromagnetic induction heating.
  • the heating element of resistance heating mainly includes PTC heating sheet and MCH ceramics.
  • MCH ceramics are more common, also known as metallized ceramics.
  • the principle is to print the metal heating paste on the ceramic blank according to a certain circuit, and realize the metallurgical combination through the subsequent firing process, and then perform the glaze encapsulation. Connect the electrodes and generate Joule heat when electrified. Since shredded tobacco is heated mainly through heat conduction, it largely depends on the shape, position and contact conditions of the heating element, and the heating efficiency is low and the uniformity is poor.
  • Electromagnetic induction heating is to place the alloy material in the induction coil.
  • a certain frequency of alternating current in the coil due to the Joule heating effect caused by hysteresis loss and eddy current, a large amount of heat will be generated in the alloy.
  • electromagnetic induction has been applied in low-temperature tobacco products, and its heating materials are mostly common iron alloys.
  • the heat transfer form of the heating element to the surrounding tobacco is mainly heat conduction, and its heat transfer efficiency is greatly limited by the distribution and contact form of the tobacco, which often makes the product appear uneven and insufficient heating, and there is a low heating efficiency. Disadvantages such as poor temperature control and poor anti-oxidation seriously affect the experience of consumers and hinder the market application of low-temperature cigarettes.
  • Chinese patent [CN202010194214.2] discloses a flexible heating element, which sequentially includes a base layer (A), a heating layer (B) and a protective layer (C).
  • the invention also discloses the flexible heating element and its application for heating non-burning cigarettes.
  • the preparation method of the flexible heating element of the invention is simple, it can avoid direct contact with tobacco when used in heat-not-burn cigarettes, and its service life can be increased through the protective layer.
  • this invention only improves the service life and temperature rise rate of the heating element, and the heating uniformity of the heating element is still low, and the temperature of the heating element increases rapidly, so it cannot be effectively controlled.
  • the present invention provides a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and a preparation method thereof.
  • a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and a preparation method thereof.
  • the present invention provides a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, including an electromagnetic heating material substrate and an anti-oxidation ceramic coating coated on the surface of the electromagnetic heating material substrate.
  • the electromagnetic heating material matrix is a ferromagnetic material
  • the ferromagnetic material is a solid solution composed of a ferromagnetic alloy matrix and a paramagnetic material.
  • the mass ratio of the ferromagnetic alloy matrix to the paramagnetic material is (75-100):(0-25).
  • the ferromagnetic alloy matrix includes at least one of iron base, nickel base, and cobalt base
  • the paramagnetic material includes at least one of Mo, Ti, V, and Ta paramagnetic materials.
  • the anti-oxidation ceramic coating includes at least one of alumina ceramic coating, zirconia ceramic coating, and nickel oxide ceramic coating, and the thickness of the anti-oxidation ceramic coating is 1-50 ⁇ m.
  • the present invention provides a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling;
  • step S4 granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieved;
  • step S5 compression molding, the powder obtained by granulating the above step S4 is subjected to compression molding;
  • step S8 coating, coating the oxide powder on the surface of the sintered body obtained in the above step S7 by any one of thermal spraying, vapor deposition, and supersonic cold spraying;
  • the ball-to-material ratio used for ball milling is 10:1-30:1, the rotation speed is 200-500 rpm, the ball milling medium is high-purity Ar, and the ball milling time is 24-96 hours.
  • the molding agent is a polyvinyl alcohol solution with a concentration of 1%-10%, and the mass ratio of the polyvinyl alcohol to the mixed powder is (0.03-0.08):1.
  • the compression molding pressure in the step S5 is 200-400 MPa, and the holding time is 30-120s.
  • the vacuum degree of the vacuum furnace in the step S6 is 0.30-1.00Pa
  • the degreasing temperature is 150-600°C
  • the holding time is 6-30h.
  • the vacuum degree of sintering in the step S7 is 0.3 ⁇ 10-1-1 ⁇ 10-1 Pa
  • the sintering temperature is 1250-1400° C.
  • the holding time is 15-60 minutes.
  • the Curie temperature also known as the magnetic transition point, refers to the temperature at which the spontaneous magnetization in a magnetic material drops to zero, and is the critical point at which a ferromagnetic or ferrimagnetic substance transforms into a paramagnetic substance.
  • the temperature is lower than the Curie point temperature, the substance becomes ferromagnetic, and the magnetic field associated with the material is difficult to change at this time.
  • the temperature is higher than the Curie point temperature, the substance becomes a paramagnet, and the magnetic field of the magnet is easily changed with the change of the surrounding magnetic field.
  • the Curie temperature of the heating material is determined by the chemical composition and crystal structure of the substance.
  • the paramagnetic material is solid-dissolved with the ferromagnetic alloy matrix.
  • the outer electron part is transferred to the ferromagnetic element, and the spin is reversely filled to weaken the magnetic exchange effect.
  • the paramagnetic substance dissolves into it, the lattice of the ferromagnetic substance increases, and the distance between the magnetic elements increases, which also weakens the magnetic exchange effect, thereby changing the permeability and Curie of the ferromagnetic substance. temperature. Therefore, the solid solution of the paramagnetic material into the ferromagnetic alloy matrix can realize the change of the microstructure, and realize the adjustability of the magnetic permeability and the Curie temperature point.
  • the ferromagnetic base material In the magnetic field generated by the induction coil, the ferromagnetic base material generates heat to heat the tobacco.
  • the higher magnetic permeability can effectively improve the heating efficiency and shorten the atomization time.
  • the controllable Curie temperature is conducive to the precise control of the heating temperature. .
  • a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and a preparation method thereof provided by the present invention can achieve the purpose of efficiently heating low-temperature cigarettes by solid-solving the paramagnetic material and the ferromagnetic alloy matrix as the heating material, At the same time, it can shorten the atomization time, optimize the anti-oxidation performance, and improve the user experience of consumers. Moreover, the Curie temperature of the heating material can be effectively adjusted according to product requirements, which is conducive to improving the controllability of the heating temperature.
  • a Curie temperature-controllable electromagnetic heating material for low-temperature cigarettes provided by the present invention and its preparation method, the electromagnetic heating material has adjustable magnetic permeability, wide application range, and the electromagnetic heating material saturates the magnetic induction at 0°C Not less than 0.2T, and the Curie temperature is 100-1000°C.
  • a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes provided by the present invention and its preparation method. Since the electromagnetic heating substrate is mostly a metal material, its oxidation resistance is poor, so a protective coating needs to be added.
  • the present invention provides Among the electromagnetic heating materials, the anti-oxidation ceramic coating coated on the surface of the electromagnetic heating material substrate has strong oxidation resistance and is an insulator, which will not affect the effect of the substrate under magnetic field conditions. The cost is low and the coating preparation process is simple. , strong adhesion.
  • Fig. 1 is a flowchart of a method for preparing an electromagnetic heating material with controllable Curie temperature for low-temperature cigarettes in an embodiment of the present invention.
  • a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling, the ball-to-material ratio used is 10:1, the rotating speed is 200rpm, the ball milling medium is high-purity Ar, and the ball milling time is 24h;
  • the molding agent is polyvinyl alcohol solution (PVA), the concentration is 1%, and the mass ratio of polyvinyl alcohol to the mixed powder is 0.03:1, to improve the strength and formability of powder compacts;
  • step S4 granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieving, the particle size of the obtained powder is 0.5mm;
  • compression molding the powder obtained in the above step S4 granulation is subjected to compression molding, the compression pressure is 200MPa, and the holding time is 30s;
  • the aluminum oxide powder is coated on the surface of the sintered body obtained in the above step S7 by thermal spraying, and the coating thickness is 50 ⁇ m;
  • a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling, the ball-to-material ratio used is 30:1, the rotating speed is 500rpm, the ball milling medium is high-purity Ar, and the ball milling time is 96h;
  • the molding agent is polyvinyl alcohol solution (PVA), the concentration is 10%, and the mass ratio of polyvinyl alcohol to the mixed powder is 0.08:1;
  • step S4 granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieving, the particle size of the obtained powder is 2mm;
  • compression molding the powder obtained in the above step S4 granulation is subjected to compression molding, the compression pressure is 400MPa, and the holding time is 120s;
  • the zirconia powder is evenly coated on the surface of the sintered body obtained in the above step S7 by a physical vapor deposition process, and the coating thickness is 40 ⁇ m;
  • a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling, the ball-to-material ratio used is 20:1, the rotating speed is 300rpm, the ball milling medium is high-purity Ar, and the ball milling time is 48h;
  • the molding agent is polyvinyl alcohol solution (PVA), the concentration is 8%, and the mass ratio of polyvinyl alcohol to the mixed powder is 0.06:1;
  • step S4 granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieving, the particle size of the obtained powder is 1.6mm;
  • compression molding the powder obtained by the granulation in the above step S4 is subjected to compression molding, the compression pressure is 300MPa, and the holding time is 60s;
  • the aluminum oxide powder is evenly coated on the surface of the sintered body obtained in the above step S7 by a supersonic spraying process, and the coating thickness is 30 ⁇ m;
  • a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling, the ball-to-material ratio used is 20:1, the rotating speed is 350rpm, the ball milling medium is high-purity Ar, and the ball milling time is 40h;
  • the molding agent is polyvinyl alcohol solution (PVA), the concentration is 7%, and the mass ratio of polyvinyl alcohol to the mixed powder is 0.03:1;
  • step S4 granulation, mixing and granulating the mixture obtained in the above step S3 after mixing with glue in a granulator, and sieving, the particle size of the obtained powder is 1.0mm;
  • compression molding the powder obtained in the above step S4 granulation is subjected to compression molding, the compression pressure is 300MPa, and the holding time is 45s;
  • the aluminum oxide powder is evenly coated on the surface of the sintered body obtained in the above step S7 by a supersonic spraying process, and the coating thickness is 20 ⁇ m;
  • a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes comprising the following steps:
  • step S2 ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling, the ball-to-material ratio used is 20:1, the rotating speed is 350rpm, the ball milling medium is high-purity Ar, and the ball milling time is 40h;
  • the molding agent is polyvinyl alcohol solution (PVA), the concentration is 5%, and the mass ratio of polyvinyl alcohol to the mixed powder is 0.05:1;
  • step S4 granulation, mixing and granulating the mixture obtained in the above step S3 after mixing with glue in a granulator, and sieving, the particle size of the obtained powder is 1.0 mm;
  • compression molding the powder obtained by the granulation in the above step S4 is subjected to compression molding, the compression pressure is 300MPa, and the holding time is 60s;
  • the zirconia powder is evenly coated on the surface of the sintered body obtained in the above step S7 by a supersonic spraying process, and the coating thickness is 1 ⁇ m;
  • Example 5 the relative magnetic permeability of Example 5 is the largest, but its Curie temperature is lower.
  • the relative permeability of Example 4 is moderate, and its Curie temperature is the highest. This is because no paramagnetic material is added in Example 5, but after the paramagnetic material is added in Example 4, after the paramagnetic material is solid-dissolved, the outer electrons are partially transferred to the ferromagnetic element, and the spin is reversely filled and weakened. magnetic exchange.
  • the paramagnetic substance dissolves into it, the lattice of the ferromagnetic substance increases, and the distance between the magnetic elements increases, which also weakens the magnetic exchange effect, thereby reducing the permeability of the ferromagnetic substance and increasing its Curie temperature.
  • the Curie temperature in Example 1 is the lowest, indicating that the addition of paramagnetic substances needs to be controlled in a reasonable ratio. Therefore, the solid solution of the paramagnetic material into the ferromagnetic alloy matrix can realize the change of the microstructure, and realize the adjustability of the magnetic permeability and the Curie temperature point.
  • the Curie temperature of the material can be controlled at 100-1000°C, which is conducive to improving the sensitivity of temperature control response in the electromagnetic heating low-temperature cigarette system, and here On the basis of optimizing the smoking efficiency of low-temperature cigarettes.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un matériau de chauffage électromagnétique à température de Curie contrôlable pour une cigarette à basse température et un procédé de préparation pour celui-ci. Le matériau de chauffage électromagnétique à température de Curie contrôlable comprend une matrice de matériau de chauffage électromagnétique et un revêtement de céramique antioxydant revêtu sur la surface de la matrice de matériau de chauffage électromagnétique, la matrice de matériau de chauffage électromagnétique étant un matériau ferromagnétique qui est une solution solide composée d'une matrice d'alliage ferromagnétique et d'un matériau paramagnétique. Le procédé de préparation est comme suit : S1. nettoyage ; S2. broyage à boulets ; S3. ajout d'adhésif ; S4. granulation ; S5. moulage par compression ; S6. dégraissage ; S7. frittage ; S8. revêtement ; et S9. meulage et polissage. En utilisant une solution solide d'un matériau paramagnétique et d'un substrat d'alliage ferromagnétique comme matériau de chauffage, la présente invention peut mettre en œuvre un chauffage efficace d'une cigarette à basse température, raccourcit un temps d'atomisation, optimise une performance antioxydante et améliore l'expérience d'utilisation ; de plus, la température de Curie du matériau de chauffage peut être efficacement ajustée en fonction d'exigences de produit, facilitant ainsi l'amélioration de la contrôlabilité de la température de chauffage ; en outre, le matériau présente également un faible coût de production et un procédé de production simple.
PCT/CN2022/084152 2021-09-06 2022-03-30 Matériau de chauffage électromagnétique à température de curie contrôlable pour une cigarette à basse température et procédé de préparation pour celui-ci WO2023029466A1 (fr)

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CN202111037128.1A CN113712285A (zh) 2021-09-06 2021-09-06 一种低温卷烟用居里温度可控电磁加热材料及其制备方法
CN202111037128.1 2021-09-06

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CN113712285A (zh) * 2021-09-06 2021-11-30 湖北中烟工业有限责任公司 一种低温卷烟用居里温度可控电磁加热材料及其制备方法

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CN106011581A (zh) * 2016-05-18 2016-10-12 华中科技大学 一种含钒无磁Ti(C,N)基金属陶瓷及其制备方法
CN210184528U (zh) * 2019-02-27 2020-03-27 广东达昊科技有限公司 一种香烟/电子烟加热装置
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