WO2023029466A1 - Curie temperature controllable electromagnetic heating material for low-temperature cigarette and preparation method therefor - Google Patents

Curie temperature controllable electromagnetic heating material for low-temperature cigarette and preparation method therefor 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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Prior art keywords
electromagnetic heating
temperature
heating material
low
powder
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PCT/CN2022/084152
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French (fr)
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/en

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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
    • A24F40/70—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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Abstract

Disclosed in the present invention are a Curie temperature controllable electromagnetic heating material for a low-temperature cigarette and a preparation method therefor. The Curie temperature controllable electromagnetic heating material comprises an electromagnetic heating material matrix and an anti-oxidant ceramic coating coated on the surface of the electromagnetic heating material matrix, wherein the electromagnetic heating material matrix is a ferromagnetic material that is a solid solution composed of a ferromagnetic alloy matrix and a paramagnetic material. The preparation method is as follows: S1. cleaning; S2. ball milling; S3. adhesive addition; S4. granulation; S5. compression molding; S6. degreasing; S7. sintering; S8. coating; and S9. grinding and polishing. By using a solid solution of a paramagnetic material and a ferromagnetic alloy substrate as a heating material, the present invention can implement efficient heating of a low-temperature cigarette, shortens an atomization time, optimizes anti-oxidant performance, and improves use experience; moreover, the Curie temperature of the heating material can be effectively adjusted according to product requirements, thereby facilitating the improvement of heating temperature controllability; in addition, the material also features low production cost and a simple production process.

Description

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Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and preparation method thereof 技术领域technical field
本发明涉及卷烟用电磁加热材料技术领域，具体涉及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。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.
背景技术Background technique
目前，市场上低温卷烟的发热方式主要有电阻加热、电磁感应加热等。电阻加热的发热体主要有PTC加热片与MCH陶瓷等。其中以MCH陶瓷更为常见，也称金属化陶瓷，其原理主要是将金属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，通电后产生焦耳热。由于烟丝受热主要是通过热传导的方式，因此很大程度上取决于发热体的形状、位置以及接触条件等，发热效率较低且均匀性差。At present, 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. Among them, 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.
技术问题technical problem
电磁感应加热是将合金材料置于感应线圈中，当线圈中存在一定频率的交流电时，由于磁滞损耗和涡流引起的焦耳热效应，合金中会产生大量的热量。目前电磁感应在低温烟草产品中已经有了一定的应用，其加热材料多为常见的铁合金。但是其发热体向周围烟草的传热形式主要为热传导，其传热效率极大程度地受到烟草分布及接触形式的限制，往往使得产品出现加热不均匀、不充分的现象，存在着加热效率低、温度控制较差以及抗氧化差等缺点，严重影响消费者的使用感受，阻碍低温卷烟的市场化应用。Electromagnetic induction heating is to place the alloy material in the induction coil. When there is 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. At present, electromagnetic induction has been applied in low-temperature tobacco products, and its heating materials are mostly common iron alloys. However, 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.
中国专利【CN202010194214.2】公开了一种柔性发热元件，其顺序包括基层(A)，发热层(B)和保护层(C)。该发明还公开了所述柔性发热元件及用于加热不燃烧卷烟的用途。该发明的柔性发热元件制备方法简单，用于加热不燃烧卷烟可避免其与烟草的直接接触，通过保护层可以增加其使用寿命。然而该发明只是提高发热元件的使用寿命和升温速率，其发热元件的发热均匀性仍较低，而且发热元件的温度提升较快，无法对其进行有效控制。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. However, 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.
技术解决方案technical solution
为解决上述问题，本发明提供了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，通过将顺磁性材料与铁磁性合金基体固溶作为加热材料，可以实现对低温卷烟高效加热的目的，同时还能缩短雾化时间，优化抗氧化性能，提升消费者的使用感受，而且加热材料的居里温度可以根据产品的需求进行有效调整，有利于提高加热温度的可控性。In order to solve the above problems, the present invention provides a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and a preparation method thereof. By solid-solving the paramagnetic material and the ferromagnetic alloy matrix as the heating material, high-efficiency heating of low-temperature cigarettes can be realized. 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 the needs of the product, which is conducive to improving the controllability of the heating temperature.
本发明提供的技术方案如下：一方面，本发明提供了一种低温卷烟用居里温度可控电磁加热材料，包括电磁加热材料基体以及涂覆在所述电磁加热材料基体表面的抗氧化陶瓷涂层，所述电磁加热材料基体为铁磁性材料，所述铁磁性材料为铁磁性合金基体与顺磁性材料组成的固溶体。 The technical solution provided by the present invention is as follows: On the one hand, 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, and the ferromagnetic material is a solid solution composed of a ferromagnetic alloy matrix and a paramagnetic material.
进一步的，所述铁磁性合金基体与顺磁性材料的质量比为（75-100）：（0-25）。Further, the mass ratio of the ferromagnetic alloy matrix to the paramagnetic material is (75-100):(0-25).
进一步的，所述铁磁性合金基体包括铁基、镍基、钴基中的至少一种，所述顺磁性材料包括Mo、Ti、V、Ta顺磁性材料中的至少一种。Further, the ferromagnetic alloy matrix includes at least one of iron base, nickel base, and cobalt base, and the paramagnetic material includes at least one of Mo, Ti, V, and Ta paramagnetic materials.
进一步的，所述抗氧化陶瓷涂层包括氧化铝陶瓷涂层、氧化锆陶瓷涂层、氧化镍陶瓷涂层中的至少一种，所述抗氧化陶瓷涂层的厚度为1-50μm。Further, 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 μm.
另一方面，本发明提供了一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：In another aspect, the present invention provides a method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将铁磁性合金基体粉末和顺磁性材料粉末进行酸洗和超声波清洗；S1, cleaning, pickling and ultrasonic cleaning the ferromagnetic alloy matrix powder and paramagnetic material powder;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨；S2, ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理；S3, mixing with glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛；S4, granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieved;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型；S5, compression molding, the powder obtained by granulating the above step S4 is subjected to compression molding;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained by molding the above step S5;
S7、烧结，将上述步骤S6脱脂得到的坯料在真空下进行烧结；S7, sintering, sintering the blank obtained by degreasing the above step S6 under vacuum;
S8、涂层，将氧化物粉末采用热喷涂、气相沉积、超音速冷喷涂中的任意一种方式涂覆在上述步骤S7得到的烧结体表面；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;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
进一步的，所述步骤S2中，球磨采用的球料比为10:1-30:1，转速为200-500rpm，球磨介质为高纯Ar，球磨时间为24-96h。Further, in the step S2, 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.
进一步的，所述步骤S3中成型剂为聚乙烯醇溶液，其浓度为1%-10%，所述聚乙烯醇与所述混合粉末的质量比为（0.03-0.08）：1。Further, in the step S3, 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.
进一步的，所述步骤S5中模压成型的压力为200-400MPa，保压时间为30-120s。Further, the compression molding pressure in the step S5 is 200-400 MPa, and the holding time is 30-120s.
进一步的，所述步骤S6中真空炉的真空度为0.30-1.00Pa，脱脂温度150-600℃，保温时间6-30h。Further, the vacuum degree of the vacuum furnace in the step S6 is 0.30-1.00Pa, the degreasing temperature is 150-600°C, and the holding time is 6-30h.
进一步的，所述步骤S7中烧结的真空度为0.3×10-1-1×10-1Pa，烧结温度为1250-1400℃，保温时间为15-60min。Further, 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., and the holding time is 15-60 minutes.
居里温度又叫磁性转变点，是指磁性材料中自发磁化强度降到零时的温度，是铁磁性或亚铁磁性物质转变成顺磁性物质的临界点。温度低于居里点温度时该物质成为铁磁体，此时和材料有关的磁场很难改变。温度高于居里点温度时，该物质成为顺磁体，磁体的磁场很容易随周围磁场的改变而改变。而加热材料的居里温度由物质的化学成分和晶体结构决定。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. When 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. When 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.
将顺磁性材料与铁磁性合金基体固溶，根据铁磁性理论，顺磁性的物质固溶进去之后，外层电子部分转移到铁磁性元素里面，自旋反向填充，减弱磁交换作用。另一方面，顺磁的物质固溶进去之后使得铁磁性物质的晶格增大，磁性元素间的距离增加了，这样也会减弱磁交换作用，从而改变铁磁性物质的磁导率和居里温度。因此，顺磁性材料向铁磁性合金基体中的固溶能够实现微观组织的改变，实现磁导率和居里温度点的可调性。The paramagnetic material is solid-dissolved with the ferromagnetic alloy matrix. According to the theory of ferromagnetism, after the paramagnetic material is solid-dissolved, the outer electron part is transferred to the ferromagnetic element, and the spin is reversely filled to weaken the magnetic exchange effect. On the other hand, after 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.
在感应线圈所产生的磁场中，铁磁性基体材料产生热量加热烟草，较高的磁导率能够有效提升加热效率，缩短雾化时间，同时可控的居里温度有利于实现加热温度的精准控制。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. At the same time, the controllable Curie temperature is conducive to the precise control of the heating temperature. .
有益效果Beneficial effect
本发明的有益效果在于：The beneficial effects of the present invention are:
1.本发明提供的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，通过将顺磁性材料与铁磁性合金基体固溶作为加热材料，可以实现对低温卷烟高效加热的目的，同时还能缩短雾化时间，优化抗氧化性能，提升消费者的使用感受，而且加热材料的居里温度可以根据产品需求进行有效调整，有利于提高加热温度的可控性。1. 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.
2.本发明提供的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，该电磁加热材料具有可调控的磁导率，适用范围广，电磁加热材料在0℃时饱和磁感应强度不低于0.2T，居里温度为100-1000℃。2. 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.
3.本发明提供的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，由于电磁加热基体多为金属材料，其抗氧化能力差，因此需添加保护性涂层，本发明提供的电磁加热材料中，涂覆在电磁加热材料基体表面的抗氧化陶瓷涂层的抗氧化能力强，且为绝缘体，不会影响基体磁场条件下的作用效果，成本较低，涂层制备工艺简单，附着力强。3. 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.
附图说明Description of drawings
图1是本发明实施例中一种低温卷烟用居里温度可控电磁加热材料的制备方法的流程图。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.
本发明的实施方式Embodiments of the present invention
为了更清楚地说明本发明实施例和现有技术中的技术方案，下面将对照附图说明本发明的具体实施方式。In order to more clearly illustrate the embodiments of the present invention and the technical solutions in the prior art, the specific implementation manners of the present invention will be described below with reference to the accompanying drawings.
显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图，并获得其他的实施方式，本发明并不限制于该实施例。Obviously, the accompanying drawings in the following description are only some embodiments of the present invention, and those skilled in the art can obtain other accompanying drawings based on these drawings and obtain For other embodiments, the present invention is not limited to this example.
本发明具体实施例如下：Specific examples of the present invention are as follows:
实施例1Example 1
一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将Fe粉、Ni粉和顺磁性材料Mo粉进行酸洗和超声波清洗，以去除表面氧化膜及污染物，其中Fe粉、Ni粉、Mo粉的质量比为3：12：5；S1, cleaning, carry out pickling and ultrasonic cleaning with Fe powder, Ni powder and paramagnetic material Mo powder, to remove surface oxide film and pollutant, wherein the mass ratio of Fe powder, Ni powder, Mo powder is 3:12:5;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨，采用的球料比为10：1，转速为200rpm，球磨介质为高纯Ar，球磨时间24h；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;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理，成型剂为聚乙烯醇溶液（PVA），浓度为1%，聚乙烯醇与混合粉末的质量比为0.03：1，以提高粉末压坯强度与成型性能；S3, mixing glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent, 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;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛，所得粉末颗粒尺寸为0.5mm；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;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型，压制压力为200MPa，保压时间为30s；S5, 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;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂，真空度为1.00Pa，脱脂温度150℃，保温时间6h；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained in the above step S5, the vacuum degree is 1.00Pa, the degreasing temperature is 150°C, and the holding time is 6h;
S7、烧结，将上述步骤S6脱脂后的坯料在1×10-1Pa真空度下进行烧结，烧结温度为1250℃，保温时间为15min；S7, sintering, sintering the billet degreased in the above step S6 under a vacuum degree of 1×10-1Pa, the sintering temperature is 1250° C., and the holding time is 15 minutes;
S8、涂层，将氧化铝粉末采用热喷涂方式涂覆在上述步骤S7得到的烧结体表面，涂覆厚度为50μm；S8, coating, 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 μm;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
实施例2Example 2
一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将Fe粉和顺磁性材料Ti粉进行酸洗以及超声波清洗，以去除表面氧化膜及污染物，其中Fe粉、Ti粉的质量比为9：1；S1, cleaning, carry out pickling and ultrasonic cleaning with Fe powder and paramagnetic material Ti powder, to remove surface oxide film and pollutant, wherein the mass ratio of Fe powder, Ti powder is 9:1;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨，采用的球料比为30：1，转速为500rpm，球磨介质为高纯Ar，球磨时间96h；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;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理，成型剂为聚乙烯醇溶液（PVA），浓度为10%，聚乙烯醇与混合粉末的质量比为0.08：1；S3, mixing glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent, 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;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛，所得粉末颗粒尺寸为2mm；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;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型，压制压力为400MPa，保压时间为120s；S5, 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;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂，真空度为0.8Pa，脱脂温度600℃，保温时间30h；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained in the above step S5, the vacuum degree is 0.8Pa, the degreasing temperature is 600°C, and the holding time is 30h;
S7、烧结，将上述步骤S6脱脂后的坯料在0.8×10-1Pa真空度下进行烧结，烧结温度为1400℃，保温时间为60min；S7, sintering, sintering the billet degreased in the above step S6 at a vacuum degree of 0.8×10-1Pa, the sintering temperature is 1400°C, and the holding time is 60min;
S8、涂层，将氧化锆粉末采用物理气相沉积工艺均匀涂覆在上述步骤S7得到的烧结体表面，涂覆厚度为40μm；S8, coating, 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 μm;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
实施例3Example 3
一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将Fe粉、Co粉和顺磁性材料V粉进行酸洗以及超声波清洗，以去除表面氧化膜及污染物，其中Fe粉、Co粉和V粉的质量比为16：4：5；S1, cleaning, pickling Fe powder, Co powder and V powder of paramagnetic material and ultrasonic cleaning to remove surface oxide film and pollutants, wherein the mass ratio of Fe powder, Co powder and V powder is 16:4:5;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨，采用的球料比为20：1，转速为300rpm，球磨介质为高纯Ar，球磨时间48h；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;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理，成型剂为聚乙烯醇溶液（PVA），浓度为8%，聚乙烯醇与混合粉末的质量比为0.06：1；S3, mixing with glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent, 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;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛，所得粉末颗粒尺寸为1.6mm；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;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型，压制压力为300MPa，保压时间为60s；S5, 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;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂，真空度为1.0Pa，脱脂温度400℃，保温时间20h；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained in the above step S5, the vacuum degree is 1.0Pa, the degreasing temperature is 400°C, and the holding time is 20h;
S7、烧结，将上述步骤S6脱脂后的坯料在0.9×10-1Pa真空度下进行烧结，烧结温度为1350℃，保温时间为45min；S7, sintering, sintering the billet degreased in the above step S6 at a vacuum degree of 0.9×10-1Pa, the sintering temperature is 1350°C, and the holding time is 45min;
S8、涂层，将氧化铝粉末采用超音速喷涂工艺均匀涂覆在上述步骤S7得到的烧结体表面，涂覆厚度为30μm；S8, coating, 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 μm;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
实施例4Example 4
一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将Ni粉、Co粉和顺磁性材料Ta粉进行酸洗以及超声波清洗，以去除表面氧化膜及污染物，其中Ni粉、Co粉和Ta粉的质量比为19：19：2；S1, cleaning, pickling Ni powder, Co powder and paramagnetic material Ta powder and ultrasonic cleaning to remove surface oxide film and pollutants, wherein the mass ratio of Ni powder, Co powder and Ta powder is 19:19:2;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨，采用的球料比为20：1，转速为350rpm，球磨介质为高纯Ar，球磨时间40h；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;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理，成型剂为聚乙烯醇溶液（PVA），浓度为7%，聚乙烯醇与混合粉末的质量比为0.03：1；S3, mixing glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent, 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;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛，所得粉末颗粒尺寸为1.0mm；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;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型，压制压力为300MPa，保压时间为45s；S5, 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;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂，真空度为0.6Pa，脱脂温度450℃，保温时间22h；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained in the above step S5, the vacuum degree is 0.6Pa, the degreasing temperature is 450°C, and the holding time is 22h;
S7、烧结，将上述步骤S6脱脂后的坯料在0.8×10-1Pa真空度下进行烧结，烧结温度为1300℃，保温时间为60min；S7, sintering, sintering the billet degreased in the above step S6 under a vacuum degree of 0.8×10-1Pa, the sintering temperature is 1300°C, and the holding time is 60min;
S8、涂层，将氧化铝粉末采用超音速喷涂工艺均匀涂覆在上述步骤S7得到的烧结体表面，涂覆厚度为20μm；S8, coating, 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 μm;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
实施例5Example 5
一种低温卷烟用居里温度可控电磁加热材料的制备方法，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, comprising the following steps:
S1、清洗，将Fe粉和Ni粉进行酸洗以及超声波清洗，以去除表面氧化膜及污染物，其中Fe粉和Ni粉的质量比为2：1；S1, cleaning, carry out pickling and ultrasonic cleaning with Fe powder and Ni powder, to remove surface oxide film and pollutant, wherein the mass ratio of Fe powder and Ni powder is 2:1;
S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨，采用的球料比为20：1，转速为350rpm，球磨介质为高纯Ar，球磨时间40h；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;
S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理，成型剂为聚乙烯醇溶液（PVA），浓度为5%，聚乙烯醇与混合粉末的质量比为0.05：1；S3, mixing glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent, 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;
S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛，所得粉末颗粒尺寸为1.0mm；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;
S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型，压制压力为300MPa，保压时间为60s；S5, 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;
S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂，真空度为0.6Pa，脱脂温度600℃，保温时间24h；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained in the above step S5, the vacuum degree is 0.6Pa, the degreasing temperature is 600°C, and the holding time is 24h;
S7、烧结，将上述步骤S6脱脂后的坯料在0.3×10-1Pa真空度下进行烧结，烧结温度为1350℃，保温时间为60min；S7, sintering, sintering the billet degreased in the above step S6 under a vacuum degree of 0.3×10-1Pa, the sintering temperature is 1350°C, and the holding time is 60min;
S8、涂层，将氧化锆粉末采用超音速喷涂工艺均匀涂覆在上述步骤S7得到的烧结体表面，涂覆厚度为1μm；S8, coating, 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 μm;
S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
将实施例1-5制备的电磁加热材料进行性能测试，结果如表1所示。The electromagnetic heating materials prepared in Examples 1-5 were tested for performance, and the results are shown in Table 1.
表1-实施例1-5制备的电磁加热材料性能测试数据Table 1-Electromagnetic heating material performance test data prepared in embodiment 1-5
Figure dest_path_image002
Figure dest_path_image002
由表1的结果可知，实施例5的相对磁导率最大，但是其居里温度较低。实施例4的相对磁导率适中，其居里温度最高。这是由于实施例5中没有加入顺磁性材料，而实施例4加入顺磁性材料后，顺磁性的物质固溶进去之后，外层电子部分转移到铁磁性元素里面，自旋反向填充，减弱磁交换作用。另一方面，顺磁的物质固溶进去之后使得铁磁性物质的晶格增大，磁性元素间的距离增加了，这样也会减弱磁交换作用，从而降低铁磁性物质的磁导率，提升其居里温度。而实施例1中居里温度最低，说明顺磁性物质的加入需要控制合理的比例。因此，顺磁性材料向铁磁性合金基体中的固溶能够实现微观组织的改变，实现磁导率和居里温度点的可调性。进而实现对低温卷烟的高效加热的目的，还可以缩短雾化时间，优化抗氧化性能，提升使用感受。而且通过铁磁性合金与顺磁性元素的科学配比及组织优化，实现材料的居里温度在100-1000℃可控，有利于提高电磁加热低温卷烟系统中温控响应的灵敏性，并在此基础上优化低温卷烟的发烟效率。From the results in Table 1, it can be seen that 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. On the other hand, after 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. However, 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. In order to achieve the purpose of high-efficiency heating of low-temperature cigarettes, it can also shorten the atomization time, optimize the anti-oxidation performance, and improve the user experience. Moreover, through the scientific ratio of ferromagnetic alloys and paramagnetic elements and structure optimization, 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.
上面描述的内容可以单独地或者以各种方式组合起来实施，而这些变型方式都在本发明的保护范围之内。The content described above can be implemented alone or combined in various ways, and these variants are all within the protection scope of the present invention.
需要说明的是，在本文中，诸如第一和第二等之类的关系术语仅仅用来将一个实体或者操作与另一个实体或操作区分开来，而不一定要求或者暗示这些实体或操作之间存在任何这种实际的关系或者顺序。而且，术语“包括”、“包含”或者其任何其他变体意在涵盖非排他性的包含，从而使得包含一系列要素的过程、方法、物品或者设备不仅包括那些要素，而且还包括没有明确列出的其他要素，或者是还包括为这种过程、方法、物品或者设备所固有的要素。在没有更多限制的情况下，由语句“包括一个…”限定的要素，并不排除在包括要素的过程、方法、物品或者设备中还存在另外的相同要素。It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply that there is a relationship between these entities or operations. There is no such actual relationship or order between them. Furthermore, the term "comprises", "comprises" or any other variation thereof is intended to cover a non-exclusive inclusion such that a process, method, article, or apparatus comprising a set of elements includes not only those elements, but also includes elements not expressly listed. other elements of or also include elements inherent in such a process, method, article, or device. Without further limitations, an element defined by the phrase "comprising a" does not preclude the presence of additional identical elements in the process, method, article or apparatus that includes the element.
以上内容是结合具体的优选实施方式对本发明所做的进一步详细说明，不能认定本发明的具体实施例只局限于这些说明。对于本发明所属技术领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干简单推演或替换，都应当视为属于本发明的保护范围。The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be assumed that the specific embodiments of the present invention are limited to these descriptions. For those of ordinary skill in the technical field of the present invention, without departing from the concept of the present invention, some simple deduction or replacement can be made, which should be regarded as belonging to the protection scope of the present invention.

Claims (10)

  1. 一种低温卷烟用居里温度可控电磁加热材料，其特征在于，包括电磁加热材料基体以及涂覆在所述电磁加热材料基体表面的抗氧化陶瓷涂层，所述电磁加热材料基体为铁磁性材料，所述铁磁性材料为铁磁性合金基体与顺磁性材料组成的固溶体。A Curie temperature controllable electromagnetic heating material for low-temperature cigarettes, characterized in that it includes an electromagnetic heating material substrate and an anti-oxidation ceramic coating coated on the surface of the electromagnetic heating material substrate, and the electromagnetic heating material substrate is ferromagnetic The ferromagnetic material is a solid solution composed of a ferromagnetic alloy matrix and a paramagnetic material.
  2. 根据权利要求1所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述铁磁性合金基体与顺磁性材料的质量比为（75-100）：（0-25）。The Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 1, wherein the mass ratio of the ferromagnetic alloy matrix to the paramagnetic material is (75-100): (0-25) .
  3. 根据权利要求1所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述铁磁性合金基体包括铁基、镍基、钴基中的至少一种，所述顺磁性材料包括Mo、Ti、V、Ta顺磁性材料中的至少一种。The Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 1, wherein the ferromagnetic alloy matrix includes at least one of iron-based, nickel-based, and cobalt-based, and the paramagnetic The material includes at least one of Mo, Ti, V, Ta paramagnetic materials.
  4. 根据权利要求1所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述抗氧化陶瓷涂层包括氧化铝陶瓷涂层、氧化锆陶瓷涂层、氧化镍陶瓷涂层中的至少一种，所述抗氧化陶瓷涂层的厚度为1-50μm。The Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 1, wherein the anti-oxidation ceramic coating comprises alumina ceramic coating, zirconia ceramic coating, nickel oxide ceramic coating At least one of them, the thickness of the anti-oxidation ceramic coating is 1-50 μm.
  5. 如权利要求1-4任一项所述的一种低温卷烟用居里温度可控电磁加热材料的制备方法，其特征在于，包括如下步骤：A method for preparing a Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to any one of claims 1-4, characterized in that it comprises the following steps:
    S1、清洗，将铁磁性合金基体粉末和顺磁性材料粉末进行酸洗和超声波清洗；S1, cleaning, pickling and ultrasonic cleaning the ferromagnetic alloy matrix powder and paramagnetic material powder;
    S2、球磨，将上述步骤S1清洗后的粉末放入球磨罐中进行球磨；S2, ball milling, put the powder cleaned in the above step S1 into a ball milling tank for ball milling;
    S3、掺胶，将上述步骤S2球磨后的混合粉末与成型剂进行混合并均匀化处理；S3, mixing with glue, mixing and homogenizing the mixed powder after ball milling in the above step S2 with the molding agent;
    S4、造粒，将上述步骤S3掺胶后得到的混合物在造粒机中进行混合造粒，过筛；S4, granulation, mixing and granulating the mixture obtained after the above step S3 is mixed with glue in a granulator, and sieved;
    S5、模压成形，将上述步骤S4造粒得到的粉料进行模压成型；S5, compression molding, the powder obtained by granulating the above step S4 is subjected to compression molding;
    S6、脱脂，将上述步骤S5模压得到的成型坯在真空炉中进行真空脱脂；S6, degreasing, carry out vacuum degreasing in the vacuum furnace with the molded blank obtained by molding the above step S5;
    S7、烧结，将上述步骤S6脱脂得到的坯料在真空下进行烧结；S7, sintering, sintering the blank obtained by degreasing the above step S6 under vacuum;
    S8、涂层，将氧化物粉末采用热喷涂、气相沉积、超音速冷喷涂中的任意一种方式涂覆在上述步骤S7得到的烧结体表面；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;
    S9、研磨抛光，将上述步骤S8涂层后的样品在研磨机上研磨抛光得到电磁加热材料。S9. Grinding and polishing, grinding and polishing the sample coated in the above step S8 on a grinder to obtain an electromagnetic heating material.
  6. 根据权利要求5所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述步骤S2中，球磨采用的球料比为10：1-30：1，转速为200-500rpm，球磨介质为高纯Ar，球磨时间为24-96h。The Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 5, characterized in that, in the step S2, the ball-to-material ratio used in the ball mill is 10:1-30:1, and the rotation speed is 200- 500rpm, the ball milling medium is high-purity Ar, and the ball milling time is 24-96h.
  7. 根据权利要求5所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述步骤S3中成型剂为聚乙烯醇溶液，其浓度为1%-10%，所述聚乙烯醇与所述混合粉末的质量比为（0.03-0.08）：1。A Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 5, characterized in that, in the step S3, the forming agent is a polyvinyl alcohol solution, the concentration of which is 1%-10%, and the polyvinyl alcohol solution is 1%-10%. The mass ratio of vinyl alcohol to the mixed powder is (0.03-0.08):1.
  8. 根据权利要求5所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述步骤S5中模压成型的压力为200-400MPa，保压时间为30-120s。The electromagnetic heating material with controllable Curie temperature for low-temperature cigarettes according to claim 5, characterized in that, in the step S5, the molding pressure is 200-400 MPa, and the holding time is 30-120s.
  9. 根据权利要求5所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述步骤S6中真空炉的真空度为0.30-1.00Pa，脱脂温度150-600℃，保温时间6-30h。A Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 5, characterized in that the vacuum degree of the vacuum furnace in the step S6 is 0.30-1.00Pa, the degreasing temperature is 150-600°C, and the holding time is 6-30h.
  10. 根据权利要求5所述的一种低温卷烟用居里温度可控电磁加热材料，其特征在于，所述步骤S7中烧结的真空度为0.3×10 -1-1×10 -1Pa，烧结温度为1250-1400℃，保温时间为15-60min。 The Curie temperature controllable electromagnetic heating material for low-temperature cigarettes according to claim 5, characterized in that the vacuum degree of sintering in the step S7 is 0.3×10 -1 -1×10 -1 Pa, and the sintering temperature is The temperature is 1250-1400℃, and the holding time is 15-60min.
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CN106011581A (en) * 2016-05-18 2016-10-12 华中科技大学 Vanadium-containing non-magnetic Ti(C, N)-based metal ceramic and preparation method thereof
CN210184528U (en) * 2019-02-27 2020-03-27 广东达昊科技有限公司 Cigarette/electronic cigarette heating device
CN113712285A (en) * 2021-09-06 2021-11-30 湖北中烟工业有限责任公司 Curie temperature controllable electromagnetic heating material for low-temperature cigarettes and preparation method thereof

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