CN114657405B - Electromagnetic heating material for low-temperature cigarettes and preparation method thereof - Google Patents

Electromagnetic heating material for low-temperature cigarettes and preparation method thereof Download PDF

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Publication number
CN114657405B
CN114657405B CN202210299921.7A CN202210299921A CN114657405B CN 114657405 B CN114657405 B CN 114657405B CN 202210299921 A CN202210299921 A CN 202210299921A CN 114657405 B CN114657405 B CN 114657405B
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electromagnetic heating
temperature
low
phase material
heating material
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CN114657405A (en
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刘华臣
谭健
唐良颖
黄婷
吴聪
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China Tobacco Hubei Industrial LLC
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China Tobacco Hubei Industrial LLC
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/04Making non-ferrous alloys by powder metallurgy
    • C22C1/05Mixtures of metal powder with non-metallic powder
    • C22C1/051Making hard metals based on borides, carbides, nitrides, oxides or silicides; Preparation of the powder mixture used as the starting material therefor
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24FSMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/46Shape or structure of electric heating means
    • A24F40/465Shape or structure of electric heating means specially adapted for induction heating
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/005Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides comprising a particular metallic binder
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys 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
    • C22C29/065Alloys 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 based on SiC
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/02Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on carbides or carbonitrides
    • C22C29/06Alloys 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
    • C22C29/067Alloys 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
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C29/00Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides
    • C22C29/12Alloys based on carbides, oxides, nitrides, borides, or silicides, e.g. cermets, or other metal compounds, e.g. oxynitrides, sulfides based on oxides

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)

Abstract

The invention provides an electromagnetic heating material for low-temperature cigarettes and a preparation method thereof, wherein the preparation raw materials of the electromagnetic heating material comprise magnetic metal phase materials and ceramic phase materials; the mass ratio of the magnetic metal phase material to the ceramic phase material is (1:1) - (1:10). The beneficial effects are that: 1) The electromagnetic heating material has higher magnetic permeability and heating efficiency; 2) The resistivity of the electromagnetic heating material has better identifiability, which is beneficial to realizing the temperature control of the system through the TCR and obtaining higher temperature control precision.

Description

Electromagnetic heating material for low-temperature cigarettes and preparation method thereof
Technical Field
The invention belongs to the technical field of electromagnetic heating materials, and particularly relates to an electromagnetic heating material for low-temperature cigarettes and a preparation method thereof.
Background
At present, the heating mode in low-temperature cigarette products mainly comprises resistance heating and electromagnetic heating, wherein the resistance heating mainly comprises the steps of printing metal heating slurry on a ceramic blank to form a circuit, and generating Joule heat under the energizing condition after firing. The tobacco shreds are heated mainly by heat conduction, so that the heat efficiency is low. Electromagnetic induction heating is to generate eddy current in the metal body by using high-frequency alternating current, so that the Joule heating effect is caused, and the heat conversion efficiency is high. At present, most of heating materials used in electromagnetic induction low-temperature tobacco products are metal, and although the heating materials can generate heat effectively under certain conditions, the temperature control accuracy of the heating materials is still insufficient.
The TCR temperature control is to establish the corresponding relation between the resistance of the heating element and the temperature of the heating element, and judge the temperature of the heating element at different times by identifying the resistance value of the heating element, so the temperature control is more accurate. However, most of the conventional heating elements are iron-based metals, and the resistivity of the conventional heating elements is extremely low, so that the resistance of the conventional heating elements cannot be effectively identified and distinguished by the system, and therefore the temperature cannot be controlled through the TCR.
Disclosure of Invention
In view of the above, the invention aims to provide an electromagnetic heating material for low-temperature cigarettes and a preparation method thereof, wherein the electromagnetic heating material has higher resistivity.
The invention provides an electromagnetic heating material for low-temperature cigarettes, which is prepared from the following raw materials of magnetic metal phase materials and ceramic phase materials;
the mass ratio of the magnetic metal phase material to the ceramic phase material is (1:1) - (1:10).
In the magnetic field generated by the induction coil, the metal ceramic generates heat to heat the tobacco, so that the high magnetic permeability can effectively improve the heating efficiency and shorten the atomization time. The controllable resistivity is beneficial to realizing the accurate control of the heating temperature.
In the present invention, the magnetic metal phase material includes a ferromagnetic material and/or an alloy material containing a ferromagnetic material; the initial magnetic conductivity of the magnetic metal phase material is 1.0 Hm/m-10 Hm/m, and the saturation magnetic induction intensity is 0.1-1.5T. The magnetic metal phase material is selected from magnetic metals such as Fe, co, ni and the like and alloys of the magnetic metals with other metals; in specific embodiments, the magnetic metal phase material is selected from one or more of Fe50Ni50 (mass ratio) alloy, pure Fe, fe50Co50 alloy (mass ratio), 430 stainless steel, and pure Co.
In the invention, the ceramic phase material is formed by compounding one or more of insulating or high-resistivity ceramics; the ceramic phase material is preferably selected from one or more of zirconia, alumina and silicon carbide. The resistivity of the ceramic phase material is 1×10 8 ~1×10 25 μΩ·cm。
In the invention, the mass ratio of the magnetic metal phase material to the ceramic phase material is (1:1) - (1:10); in a specific embodiment, the mass ratio of the magnetic metal phase material to the ceramic phase material is 1:1, a step of; or 1:10; or 1:5; or 1:2; or 1:3.
In the invention, the resistivity of the electromagnetic heating material for low-temperature cigarettes is 500-10000 mu omega cm, and the electromagnetic heating material has high resistance identification. The resistance temperature coefficient of the electromagnetic heating material for the low-temperature cigarettes is 500-3000, and TCR temperature control can be realized. The bending strength of the electromagnetic heating material for the low-temperature cigarettes is 200-1000 MPa, and the strength of the electromagnetic heating material can meet the use requirement.
The invention provides a preparation method of the electromagnetic heating material for the low-temperature cigarettes, which comprises the following steps:
mixing the cleaned magnetic metal phase material and ceramic phase material, ball milling and drying to obtain mixed powder;
homogenizing the mixed powder and the forming agent, granulating, compression molding, degreasing and sintering to obtain the electromagnetic heating material for the low-temperature cigarettes.
The method provided by the invention has the advantages of simple process and low cost.
The invention preferably carries out acid washing and ultrasonic cleaning on the magnetic metal phase material to remove oxide films and pollutants on the surface. The invention adopts high-purity ethanol as the ball grinding agent; the mass ratio of the ball materials is preferably 5:1-20:1; in a specific embodiment, the ball-to-material ratio is 20:1; or 5:1. The rotation speed of the ball milling is 100-600 rpm, and the time of the ball milling is 2-48 h.
The powder slurry prepared by ball milling is dried in vacuum, and the temperature of the vacuum drying is 60-100 ℃; in specific embodiments, the vacuum drying temperature is 60 ℃, or 100 ℃, or 90 ℃, or 80 ℃.
After the mixed powder is obtained, the mixed powder and the forming agent are mixed and homogenized, namely the glue mixing treatment is carried out; the forming agent is polyvinyl alcohol solution; the mass concentration of the polyvinyl alcohol solution is 1-10%; the polyvinyl alcohol solution accounts for 1-10% of the mass of the mixed powder; in specific embodiments, the polyvinyl alcohol solution comprises 5%, or 8%, or 10%, or 1% of the mass of the mixed powder.
The invention granulates the mixture after glue mixing in a granulator, and then sieves the mixture, and the size of the obtained powder particles is 0.2-2 mm. In specific embodiments, the powder particles are 1.5mm, 1mm, 2mm, or 0.2mm in size.
The invention carries out compression molding on the granulated powder; the pressure of the compression molding is 200-400 MPa, and the pressure maintaining time is 60-120 s; in specific embodiments, the pressure of the compression molding is 200MPa, or 400MPa, or 300MPa; the dwell time was 60s, or 120s.
Degreasing the molded blank after compression molding in a vacuum furnace; the degreasing temperature is 200-600 ℃ and the degreasing time is 2-10 h; the vacuum degree of degreasing is not lower than 1Pa; in specific embodiments, the degreasing temperature is 200 ℃, or 600 ℃, or 500 ℃, or 600 ℃; the time is 2h, or 10h, or 8h, or 6h,
Sintering the degreased blank; the sintering temperature is 1250-1400 ℃, the sintering time is 15-120 min, and the sintering vacuum degree is not less than 1X 10 -3 Pa. In specific embodiments, the sintering temperature is 1250 ℃, or 1400 ℃, or 1380 ℃, or 1390 ℃; sintering time is 15min, or 120min, or 80min, or 60min; the degree of vacuum of sintering is not less than 1X 10 -3 Pa。
According to the invention, through scientific proportioning and tissue optimization of the ceramic phase material and the magnetic metal phase material with high magnetic conductivity, the composite material with high magnetic conductivity, higher resistivity and TCR value is obtained, so that the temperature can be judged by identifying the resistance value of the material while heating, and further the accurate control of the temperature is realized.
Detailed Description
In order to further illustrate the present invention, the electromagnetic heating material for low-temperature cigarettes and the preparation method thereof provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
(1) Cleaning: pickling and ultrasonic cleaning are carried out on Fe50Ni50 powder so as to remove surface oxide films and pollutants;
(2) Ball milling: and (3) placing the washed Fe50Ni50 powder and zirconia powder into a ball milling tank for ball milling and mixing, wherein the mass ratio is 1:1, and then adding high-purity ethanol for ball milling and mixing. The ball-material ratio is 5:1, the rotating speed is 100rpm, and the ball milling time is 2 hours;
(3) And (3) drying: vacuum drying is carried out on the prepared powder slurry, and the temperature is 60 ℃;
(4) And (3) doping: mixing and homogenizing the dried mixed powder with a forming agent, wherein the forming agent is polyvinyl alcohol solution (PVA) with the concentration of 1%, and the proportion of the forming agent is 1% of the mass of the mixed powder;
(5) Granulating: mixing and granulating the mixture after the glue doping in a granulator, and sieving to obtain powder with the particle size of 0.2mm;
(6) And (3) compression molding: carrying out compression molding on the granulated powder, wherein the compression pressure is 200MPa, and the pressure maintaining time is 60s;
(7) Degreasing: vacuum degreasing the formed blank in a vacuum furnace, wherein the vacuum degree is not lower than 1.00Pa, the degreasing temperature is 200 ℃, and the heat preservation time is 2 hours;
(8) Sintering: for the blank after degreasing, the blank is not less than 1 multiplied by 10 -3 Sintering is carried out under Pa vacuum degree, the sintering temperature is 1250 ℃, and the heat preservation time is 15min.
The properties of the prepared electromagnetic heating material are shown in table 1.
Example 2:
(1) Cleaning: washing pure Fe with acid and ultrasonic cleaning to remove surface oxide film and pollutant;
(2) Ball milling: and (3) placing the cleaned iron powder and the cleaned alumina powder into a ball milling tank for ball milling and mixing, wherein the mass ratio of the iron powder to the alumina powder is 1:10, and then adding high-purity ethanol for ball milling and mixing. The ball-material ratio is 20:1, the rotating speed is 600rpm, and the ball milling time is 48 hours;
(3) And (3) drying: vacuum drying is carried out on the prepared powder slurry, and the temperature is 100 ℃;
(4) And (3) doping: mixing and homogenizing the dried mixed powder with a forming agent, wherein the forming agent is polyvinyl alcohol solution (PVA) with the concentration of 10 percent and the proportion of the forming agent is 10 percent of the mass of the mixed powder;
(5) Granulating: mixing and granulating the mixture after the glue doping in a granulator, and sieving to obtain powder with the particle size of 2mm;
(6) And (3) compression molding: carrying out compression molding on the granulated powder, wherein the compression pressure is 400MPa, and the pressure maintaining time is 120s;
(7) Degreasing: vacuum degreasing the formed blank in a vacuum furnace, wherein the vacuum degree is not lower than 1.00Pa, the degreasing temperature is 600 ℃, and the heat preservation time is 10 hours;
(8) Sintering: for the blank after degreasing, the blank is not less than 1 multiplied by 10 -3 Sintering is carried out under Pa vacuum degree, the sintering temperature is 1400 ℃, and the heat preservation time is 120min.
The properties of the prepared electromagnetic heating material are shown in table 1.
Example 3:
(1) Cleaning: washing pure Fe50Co50 with acid and ultrasonic cleaning to remove surface oxide film and pollutant;
(2) Ball milling: and (3) placing the cleaned Fe50Co50 powder and the aluminum oxide powder into a ball milling tank for ball milling and mixing, wherein the mass ratio of the powder to the aluminum oxide powder is 1:5, and then adding high-purity ethanol for ball milling and mixing. The ball-material ratio is 20:1, the rotating speed is 400rpm, and the ball milling time is 48 hours;
(3) And (3) drying: vacuum drying is carried out on the prepared powder slurry, and the temperature is 90 ℃;
(4) And (3) doping: mixing and homogenizing the dried mixed powder with a forming agent, wherein the forming agent is polyvinyl alcohol solution (PVA), the concentration is 8%, and the ratio of the forming agent to the polyvinyl alcohol solution is 10% of the mass of the mixed powder;
(5) Granulating: mixing and granulating the mixture after the glue doping in a granulator, and sieving to obtain powder with the particle size of 1mm;
(6) And (3) compression molding: carrying out compression molding on the granulated powder, wherein the compression pressure is 300MPa, and the pressure maintaining time is 120s;
(7) Degreasing: vacuum degreasing the formed blank in a vacuum furnace, wherein the vacuum degree is not lower than 1.00Pa, the degreasing temperature is 500 ℃, and the heat preservation time is 8 hours;
(8) Sintering: for the blank after degreasing, the blank is not less than 1 multiplied by 10 -3 Sintering is carried out under Pa vacuum degree, the sintering temperature is 1380 ℃, and the heat preservation time is 80min.
The properties of the prepared electromagnetic heating material are shown in table 1.
Example 4:
(1) Cleaning: pickling and ultrasonic cleaning are carried out on the 430 stainless steel powder so as to remove surface oxide films and pollutants;
(2) Ball milling: and (3) placing the cleaned 430 stainless steel powder and alumina powder into a ball milling tank for ball milling and mixing, wherein the mass ratio is 1:2, and then adding high-purity ethanol for ball milling and mixing. The ball-material ratio is 20:1, the rotating speed is 600rpm, and the ball milling time is 48 hours;
(3) And (3) drying: vacuum drying is carried out on the prepared powder slurry, and the temperature is 80 ℃;
(4) And (3) doping: mixing and homogenizing the dried mixed powder with a forming agent, wherein the forming agent is polyvinyl alcohol solution (PVA) with the concentration of 5%, and the proportion is 8% of the mass of the mixed powder;
(5) Granulating: mixing and granulating the mixture after the glue doping in a granulator, and sieving to obtain powder with the particle size of 1mm;
(6) And (3) compression molding: carrying out compression molding on the granulated powder, wherein the compression pressure is 300MPa, and the pressure maintaining time is 120s;
(7) Degreasing: vacuum degreasing the formed blank in a vacuum furnace, wherein the vacuum degree is not lower than 1.00Pa, the degreasing temperature is 600 ℃, and the heat preservation time is 6 hours;
(8) Sintering: for the blank after degreasing, the blank is not less than 1 multiplied by 10 -3 Sintering is carried out under Pa vacuum degree, the sintering temperature is 1400 ℃, and the heat preservation time is 60min.
The properties of the prepared electromagnetic heating material are shown in table 1.
Example 5:
(1) Cleaning: washing pure Co with acid and ultrasonic cleaning to remove surface oxide film and pollutant;
(2) Ball milling: and (3) placing the cleaned Co powder and silicon carbide powder into a ball milling tank for ball milling and mixing, wherein the mass ratio of the Co powder to the silicon carbide powder is 1:3, and then adding high-purity ethanol for ball milling and mixing. The ball-material ratio is 20:1, the rotating speed is 450rpm, and the ball milling time is 48 hours;
(3) And (3) drying: vacuum drying is carried out on the prepared powder slurry, and the temperature is 80 ℃;
(4) And (3) doping: mixing and homogenizing the dried mixed powder with a forming agent, wherein the forming agent is polyvinyl alcohol solution (PVA) with the concentration of 5%, and the proportion is 5% of the mass of the mixed powder;
(5) Granulating: mixing and granulating the mixture after the glue doping in a granulator, and sieving to obtain powder with the particle size of 1.5mm;
(6) And (3) compression molding: carrying out compression molding on the granulated powder, wherein the compression pressure is 400MPa, and the pressure maintaining time is 120s;
(7) Degreasing: vacuum degreasing the formed blank in a vacuum furnace, wherein the vacuum degree is not lower than 1.00Pa, the degreasing temperature is 600 ℃, and the heat preservation time is 10 hours;
(8) Sintering: for the blank after degreasing, the blank is not less than 1 multiplied by 10 -3 Sintering is carried out under Pa vacuum degree, the sintering temperature is 1390 ℃, and the heat preservation time is 60min.
The properties of the prepared electromagnetic heating material are shown in table 1.
The resistivity of the electromagnetic heating material is tested by adopting a four-probe resistance tester; calculating the temperature coefficient of the material resistance by fitting the T-R value; the magnetic permeability is tested by an MPMS magnetic measurement system; flexural strength was tested by a three-point flexural strength tester.
TABLE 1 results of Performance test of electromagnetic electrothermal materials prepared in examples 1 to 5
As can be seen from the above examples, the electromagnetic heating material for low-temperature cigarettes provided by the invention comprises magnetic metal phase material and ceramic phase material; the mass ratio of the magnetic metal phase material to the ceramic phase material is (1:1) - (1:10). The beneficial effects are that: 1) The electromagnetic heating material has higher magnetic permeability and heating efficiency; 2) The resistivity of the developed electromagnetic heating material has better identifiability, and is favorable for realizing temperature control of a system through TCR (temperature control coefficient) and obtaining higher temperature control precision. The experimental results show that: the resistivity of the electromagnetic heating material is 522-8934 mu omega cm, and the bending strength is 256-892 MPa; the relative magnetic permeability is 800-3000.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (6)

1. An electromagnetic heating material for low-temperature cigarettes is characterized in that the preparation raw materials comprise a magnetic metal phase material and a ceramic phase material;
the mass ratio of the magnetic metal phase material to the ceramic phase material is (1:1) - (1:10);
the magnetic metal phase material is selected from Fe50Ni50 alloy or Fe50Co50 alloy; the initial magnetic permeability of the magnetic metal phase material is 1.0 Hm/m-10 Hm/m, and the saturation magnetic induction intensity is 0.1-1.5T;
the ceramic phase material is selected from one or more of zirconia, alumina and silicon carbide; the resistivity of the ceramic phase material is 1×10 8 ~1×10 25 μΩ▪cm;
The bending strength of the electromagnetic heating material for the low-temperature cigarettes is 200-1000 MPa.
2. The electromagnetic heating material for low-temperature cigarettes according to claim 1, wherein the electrical resistivity of the electromagnetic heating material for low-temperature cigarettes is 500-10000 μΩ cm.
3. The electromagnetic heating material for low-temperature cigarettes according to claim 1, wherein the electromagnetic heating material for low-temperature cigarettes has a temperature coefficient of resistance of 500-3000.
4. A method for preparing the electromagnetic heating material for low-temperature cigarettes according to any one of claims 1-3, comprising the following steps:
mixing the cleaned metal phase material and ceramic phase material, ball milling and drying to obtain mixed powder;
homogenizing the mixed powder and the forming agent, granulating, compression molding, degreasing and sintering to obtain the electromagnetic heating material for the low-temperature cigarettes.
5. The method according to claim 4, wherein the forming agent is a polyvinyl alcohol solution;
the mass concentration of the polyvinyl alcohol solution is 1-10%;
the mass ratio of the forming agent to the mixed powder is 1-10:100.
6. The preparation method according to claim 4, wherein the degreasing temperature is 200-600 ℃ and the degreasing time is 2-10 h;
the sintering temperature is 1250-1400 ℃, the sintering time is 15-120 min, and the sintering vacuum degree is not less than 1X 10 -3 Pa。
CN202210299921.7A 2022-03-25 2022-03-25 Electromagnetic heating material for low-temperature cigarettes and preparation method thereof Active CN114657405B (en)

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CN112375951A (en) * 2019-09-10 2021-02-19 湖北中烟工业有限责任公司 Metal ceramic heating material and preparation method thereof

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CN101063187A (en) * 2007-05-23 2007-10-31 济南钢铁股份有限公司 Preparation method of ceramic-metal composite material
CN112375951A (en) * 2019-09-10 2021-02-19 湖北中烟工业有限责任公司 Metal ceramic heating material and preparation method thereof

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