WO2023045583A1 - 雾化芯制备方法 - Google Patents
雾化芯制备方法 Download PDFInfo
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- WO2023045583A1 WO2023045583A1 PCT/CN2022/110238 CN2022110238W WO2023045583A1 WO 2023045583 A1 WO2023045583 A1 WO 2023045583A1 CN 2022110238 W CN2022110238 W CN 2022110238W WO 2023045583 A1 WO2023045583 A1 WO 2023045583A1
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
- A24F40/46—Shape or structure of electric heating means
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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
- A24F40/50—Control or monitoring
-
- 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
Definitions
- the invention belongs to the technical field of atomization, and in particular relates to a method for preparing an atomization core.
- the thin-film heating atomizing core used in the aerosol generating device usually attaches a heating film to the atomizing surface of porous ceramics, and heats the aerosol-forming substrate on the atomizing surface through the heating film, so that the aerosol forms a matrix mist turned into smoke.
- the current thin-film heating atomizing core has the problems of poor continuity and difficult adjustment and control of thickness, which easily leads to poor resistance resistance stability of the thin-film heating layer, which in turn leads to poor heating uniformity of the thin-film heating atomizing core.
- the purpose of the embodiments of the present invention is to provide a method for preparing an atomizing core that improves and enhances the stability of the resistance value of the heating layer.
- the technical solution adopted by the present invention is to provide a method for preparing an atomizing core, which includes the following steps:
- An annealing and aging process is adopted to perform annealing heat treatment on the atomization core.
- the temperature of the annealing heat treatment is 500-800° C.
- the time of the annealing heat treatment is 5-60 minutes.
- the annealing heat treatment process of the atomization core is carried out in a protective gas atmosphere.
- the preparation method of the atomizing core further includes the step of energizing and aging treatment.
- the step of energizing and aging treatment includes: adopting the energizing and aging process, supplying power to the atomizing core after the annealing heat treatment, and electrifying the atomizing core after the annealing heat treatment. After heating, the microstructure of the heating layer is subjected to aging treatment.
- the energizing power is 6-8W
- the energizing time is 1-20 minutes.
- the energization aging treatment process of the atomizing core is carried out in an atmospheric atmosphere.
- a DC stabilized voltage power supply is used to supply power to the atomizing core.
- the conductive material is a nickel-chromium alloy material
- the nickel-chromium alloy material is deposited through the thin film deposition process to form a nickel-chromium alloy heating layer, and the deposition thickness of the nickel-chromium alloy heating layer is 1-5 ⁇ m.
- the mass ratio of Ni/(Ni+Cr) in the nickel-chromium alloy material is 0.2-0.9.
- the porosity of the porous ceramic substrate is 30%-80%, and the pore diameter of the porous ceramic substrate is 10-30 ⁇ m.
- a conductive material is formed on the outer surface of the porous ceramic substrate through a thin film deposition process to form an atomizing core with a heating layer on the surface;
- the heating layer of the chemical core is annealed to make the crystal grains in the microstructure of the heating layer grow up, make the heating layer more compact, and reduce the microscopic defects of the heating layer.
- the atomizing core can improve and increase the stability of the resistance of the heating layer, enhance the electrical stability of the heating layer, and then make the heating layer more uniform, and prevent the local temperature of the atomizing core from being too high , can have a good atomization effect on aerosol-forming substrates.
- Fig. 1 is a schematic cross-sectional structure diagram of an atomizing core provided by Embodiment 1 of the present invention
- Fig. 2 is another schematic cross-sectional structure diagram of the atomizing core provided by Embodiment 1 of the present invention.
- Fig. 3 is a schematic top view structure diagram of the atomization core provided by Embodiment 2 of the present invention.
- Fig. 4 is a schematic cross-sectional structure diagram of the atomization core provided by Embodiment 2 of the present invention.
- Fig. 5 is a schematic cross-sectional structure diagram of a porous substrate provided by Embodiment 2 of the present invention.
- Fig. 6 is a schematic cross-sectional structure diagram of the atomization core provided by the third embodiment of the present invention.
- Fig. 7 is a schematic cross-sectional structure diagram of a porous substrate provided by Embodiment 3 of the present invention.
- Fig. 8 is a schematic cross-sectional structure diagram of the atomization core provided by Embodiment 4 of the present invention.
- Fig. 9 is a comparison chart of the resistance values of the atomizing cores prepared in Example 1 to Example 15 of the present invention in a cycle test;
- Fig. 10 is a comparison chart of the resistance values of atomizing cores prepared in Example 2, Example 5, Example 8, Example 11 and Example 14 of the present invention in cycle tests;
- Fig. 11 is a comparison chart of resistance values of atomizing cores prepared in Examples 1 to 3 of the present invention in cycle tests;
- Fig. 12 is a comparison chart of the resistance values of the atomizing cores prepared in Example 2 and Example 4 to Example 6 of the present invention in a cycle test;
- Fig. 13 is a comparison chart of the resistance values of the atomizing cores prepared in Example 5 and Example 7 to Example 9 of the present invention in a cycle test;
- Fig. 14 is a comparison chart of the resistance values of the atomizing cores prepared in Example 8 and Example 10 to Example 12 of the present invention in a cycle test;
- Fig. 15 is a comparison chart of the resistance values of the atomizing cores prepared in Example 11 and Example 13 to Example 15 of the present invention in a cycle test.
- Porous ceramic substrate 11-atomization surface; 11a-first region; 11b-second region; 11c-first surface; 11d-second surface; 11e-third surface; 11f-first transition surface; 11g-second Two transition surfaces; 12-protrusion; 13-first depression; 14-second depression; 2-transition layer;
- 3-heating layer 31-heating part; 32-first connecting part; 321-first side part; 322-first joint part; 33-second connecting part; 331-second side part; 332-second joint department;
- the atomizing core provided by Embodiment 1 of the present invention is used in an atomizer, which can generate heat under the electric drive of the power supply device of the aerosol generating device, and heat and atomize the aerosol-forming substrate in the liquid storage chamber of the atomizer to form The smoke is for the user to inhale to achieve the effect of simulating smoking.
- the atomizing core provided by Embodiment 1 of the present invention includes a porous base 1 and a heat generating layer 3 . At least part of the outer surface of the porous substrate 1 is formed with an atomizing surface 11 .
- the porous substrate 1 has a capillary adsorption microporous structure inside, the porous substrate 1 can absorb and store aerosols through the microporous structure to form a matrix, and the adsorbed and stored aerosol-formed matrix can be continuously transported to the atomizing surface 11 through the microporous structure .
- the heat generating layer 3 is formed on at least part of the atomizing surface 11 .
- the heating layer 3 When the atomizing core is in use, power is supplied to the atomizing core through the power supply device of the aerosol generating device, the heating layer 3 generates heat after being energized, and the heat is transmitted to the aerosol forming matrix on the atomizing surface 11, so that the aerosol forming matrix Atomization forms smoke that can be inhaled by the user.
- the porous substrate 1 can also be a porous material capable of absorbing liquid, such as porous ceramics and porous metal.
- the porous substrate 1 is porous ceramics; further, in some of the more specific embodiments, the porosity of the porous substrate 1 is 30%-80%, and the pore diameter of the porous substrate 1 is 10-30 ⁇ m.
- the heating layer 3 is a metal layer or an alloy layer with stable chemical properties and good electrical and thermal conductivity, and the heating layer 3 is a copper layer, an iron layer, a nickel layer, a chromium layer, a gold layer, a silver layer, or a platinum layer. , palladium layer, molybdenum layer and other metal layers and gold-silver alloy layer, gold-platinum alloy layer, gold-silver-platinum alloy layer, silver-palladium alloy layer, silver-platinum alloy layer, palladium-copper alloy layer, palladium-silver alloy layer, nickel-chromium alloy layer at least any of the .
- the heating layer 3 is a nickel-chromium alloy layer.
- the nickel-chromium alloy layer has good thermal performance, and the price of the nickel-chromium alloy layer is higher than that of precious metal layers such as gold layer, silver layer, platinum layer, palladium layer, or gold-silver alloy layer, gold-platinum alloy layer, gold-silver-platinum alloy layer, and silver-palladium alloy layer. , silver-platinum alloy layer, palladium-copper alloy layer, palladium-silver alloy layer and other precious metal alloy layers are cheap.
- the heating layer 3 is a nickel-chromium alloy layer, and the mass ratio of Ni/(Ni+Cr) is 0.2-0.9. According to the resistance calculation formula, the thickness of the heating layer 3 determines the resistance value of the heating layer 3.
- the thickness of the heating layer 3 is adjusted and controlled to achieve the purpose of adjusting the resistance value of the heating layer 3 .
- the inventor found that: when the thickness of the heating layer 3 is too thin, the heating layer 3 of the thin layer structure is relatively loose and the continuity is not good, which affects the stability of the resistance value of the heating layer 3 , the heat generating layer 3 is relatively easy to be oxidized or carbonized at high temperature; the thicker the heat generating layer 3 is, the continuity and compactness of the heat generating layer 3 of the thin layer structure will also increase accordingly, so that the resistance to oxidation or carbonization of the heat generating layer 3 The ability is greatly enhanced, thereby enhancing the stability of the resistance of the heating layer 3.
- the formation time of the heat generating layer 3 is longer, thereby greatly reducing the production efficiency;
- the microstructure is destroyed, affecting the stability of the resistance value of the heating layer 3 .
- the resistance of the heating layer 3 is too low, there is a potential safety hazard of short circuit overload of the heating layer 3, and the resistance of the heating layer 3 is too high, there is a problem that the required heating power cannot be reached, so the common resistance of the heating layer 3 is 0.8 ⁇ 2 ⁇ .
- the heat generation is set to be 1 ⁇ 5 ⁇ m.
- the heating layer 3 is a nickel-chromium alloy layer, and the thickness of the nickel-chromium alloy layer is set to 1-5 ⁇ m, so that the resistance stability of the heating layer 3 is improved, and the resistance of the heating layer 3 is within the common resistance range , and the formation time of the heating layer 3 is moderate, thereby improving the resistance stability of the atomizing core, the heating power of the atomizing core is relatively large, the atomizing effect of the atomizing core is good, and the manufacturing cost of the atomizing core is controllable.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process. Because the heating area of the atomizing core is larger and the heating is more uniform, there will be no local overheating phenomenon, which is beneficial to improve the uniformity of heating of the aerosol-forming substrate, thereby improving the atomization effect.
- the heating layer 3 is formed by depositing the magnetron sputtering process, the heating layer 3 is a nickel-chromium alloy layer, the target power density of the magnetron sputtering process is 5-15W/cm 2 , and the sputtering pressure is 0.1-0.3Pa, and the sputtering time is 30-90min.
- a nickel-chromium alloy layer with a thickness of 1-5 ⁇ m is deposited on at least part of the atomized surface 11 of the porous substrate 1 by magnetron sputtering, and the nickel-chromium alloy layer forms the heating layer 3 .
- the formation process of the heating layer 3 generally includes: 1. Initial formation of the island: the gaseous target material reaches the surface of the porous substrate 1, adheres and condenses to form some uniform and fine The moving atomic group, the in-situ group is called "island”; 2. The number of islands is saturated: the “island” continuously accepts new deposited atoms, and gradually grows up by merging with other small “islands", and the number of islands quickly reaches saturation; 3. Island growth and nucleation: while small “islands” merge continuously, new small “islands” will be formed on the surface of the vacated porous substrate 1; 4.
- Merge and grow filling the formation of small "islands” The merger continues, and the larger “islands” continue to annex the smaller “islands” nearby; 5. Filling the pores to form a film: the isolated small “islands” are connected to each other as the merger progresses, and finally only some Isolated holes and channels, these holes and channels are continuously filled to form a film with continuous morphology and complete coverage.
- the atomization core further includes a transition layer 2 formed between the heat generating layer 3 and the porous substrate 1 .
- a transition layer 2 with a thickness of 0.1-1 ⁇ m is deposited on at least part of the atomized surface 11 of the porous substrate 1 by a thin film deposition process, and a heat generating layer 3 is formed on the side of the transition layer 2 away from the porous substrate 1 .
- the process of forming the transition layer 2 is the same as that of the above-mentioned heat generating layer 3, so the transition layer 2 reduces the roughness of the surface of the porous substrate 1, so that the heat generating layer 3 has a good continuity. It is convenient to adjust and control the thickness of the heating layer 3 . Moreover, the transition layer 2 can also prevent sodium and potassium ions from the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field, thereby enhancing the stability of the resistance of the heating layer 3 .
- the transition layer 2 can adjust the stress matching between the heating layer 3 and the surface of the porous substrate 1, enhance the adhesion between the heating layer 3 and the porous substrate 1, make the heating layer 3 firmly bonded to the porous substrate 1, and improve the heat generation.
- the stable and reliable working performance of layer 3 prolongs the service life of the atomizing core.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process.
- the transition layer 2 is deposited and formed by the magnetron sputtering process, the target power density of the magnetron sputtering process is 3-12W/cm 2 , the sputtering pressure is 0.1-0.5Pa, and the sputtering time is 20-100 min, and the thickness of the transition layer 2 is 0.1-1 ⁇ m.
- the transition layer 2 When the thickness of the transition layer 2 is too thin, the transition layer 2 cannot achieve the above-mentioned effect of reducing the roughness of the porous substrate 1 surface and blocking the sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field; As the thickness of the layer 2 increases, the transition layer 2 can gradually reduce the roughness of the surface of the porous substrate 1, gradually prevent the sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field, and gradually adjust the heating layer 3 and the surface of the porous substrate 1.
- the stress of the transition layer 2 will increase significantly, causing the microstructure of the transition layer 2 to be destroyed during the electrification of the atomizing core, and the transition layer 2 cannot block the porous substrate
- the sodium and potassium ions in 1 diffuse into the heating layer 3 under the action of the electric field, which affects the stability of the resistance value of the heating layer 3 .
- the thickness of the transition layer 2 is set to 0.1-1 ⁇ m, so that the transition layer 2 reduces the roughness of the surface of the porous substrate 1, so that the transition layer 2 prevents the sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field,
- the transition layer 2 adjusts the stress matching between the heating layer 3 and the surface of the porous substrate 1 .
- the thickness of the transition layer 2 is set to 0.3-0.8 ⁇ m, which facilitates reducing the surface roughness of the porous substrate 1 and at the same time helps to block the diffusion of sodium and potassium ions in the porous substrate 1 into the heating layer 3 under the action of an electric field.
- the stress values of the transition layer 2 and the porous substrate 1 are close to each other, so that the stresses of the transition layer 2 and the porous substrate 1 are well matched.
- the porous substrate 1 is porous ceramics, and the transition layer 2 is at least any one of aluminum nitride layer, silicon nitride layer, chromium nitride layer, chromium carbide layer or other ceramic layers.
- the atomizing core further includes a protective layer 4 formed on the heat generating layer 3 .
- the protection layer 4 with a thickness of 0.5-3 ⁇ m is deposited and formed on the side of the heating layer 3 facing away from the porous substrate 1 through a thin film deposition process.
- the protective layer 4 blocks the formation of the aerosol matrix and the outside air from entering the heating layer 3, so as to avoid oxidation or carbonization of the heating layer 3 during energization and use, enhance the oxidation resistance and carbonization resistance of the heating layer 3, and enhance the stability of the resistance of the heating layer 3 performance, improve the cycle life of the atomizing core.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process.
- the protective layer 4 is formed by depositing the magnetron sputtering process, the target power density of the magnetron sputtering process is 3-12W/cm 2 , the sputtering pressure is 0.1-0.5Pa, and the sputtering time is 40-150 minutes.
- the protective layer 4 cannot play the role of blocking the aerosol-forming matrix and the outside air from entering the heating layer 3; as the thickness of the protective layer 4 increases, the protective layer 4 can gradually block the aerosol-forming matrix And the outside air enters the heating layer 3; however, when the thickness of the protective layer 4 is too thick, the stress of the protective layer 4 will increase significantly, causing the microstructure of the protective layer 4 to be destroyed during the electrification of the atomizing core, and the protective layer 4 The aerosol-forming matrix and outside air cannot be blocked from entering the heating layer 3, which weakens the oxidation resistance and carbonization resistance of the heating layer 3, affects the stability of the resistance of the heating layer 3, and shortens the cycle life of the atomizing core.
- the thickness of the protective layer 4 is set to 0.5-3 ⁇ m, so that the protective layer 4 blocks the aerosol-forming matrix and external air from entering the heating layer 3 .
- the thickness of the protective layer 4 is set at 0.8-1.5 ⁇ m, which can well block the aerosol-forming substrate and external air from entering the heat-generating layer 3 .
- the protective layer 4 is chemically stable and has a compact structure.
- the protection layer 4 is at least any one of an aluminum oxide layer, a silicon oxide layer, an aluminum nitride layer, a silicon nitride layer, a titanium oxide layer, and a titanium nitride layer.
- the heating layer 3 is provided with two exposed parts 41 that are not deposited to form a protective layer 4.
- the exposed parts 41 are used to realize the electrical connection between the power supply device and the heating layer 3. connect.
- Embodiment 1 of the present invention also provides an atomizer, and the atomizer includes the atomizing core provided in any one of the above embodiments. Since the atomizer has all the technical features of the atomizing core provided by any of the above embodiments, it has the same technical effect as the atomizing core.
- Embodiment 1 of the present invention also provides an aerosol generating device, which includes the atomizing core provided in any of the above embodiments or the atomizer provided in any of the above embodiments. Since the aerosol generating device has all the technical features of the atomizing core or atomizer provided by any of the above embodiments, it has the same technical effect as the atomizing core.
- Embodiment 1 of the present invention also provides a method for preparing the above-mentioned atomizing core.
- the method for preparing the atomizing core in Embodiment 1 of the present invention includes the following steps:
- Step S1 depositing a transition layer: depositing a transition layer 2 on at least part of the atomized surface 11 of the porous substrate 1 through a thin film deposition process;
- Step S2 Depositing the heat generating layer: depositing the heat generating layer 3 on the side of the transition layer 2 facing away from the porous substrate 1 through a thin film deposition process;
- Step S3 depositing a protective layer: a protective layer 4 is deposited on the side of the heat generating layer 3 facing away from the transition layer 2 through a thin film deposition process.
- a transition layer 2 with a thickness of 0.1-1 ⁇ m is deposited on at least part of the atomized surface 11 of the porous substrate 1 by a thin film deposition process, and the stress value of the transition layer 2 is close to that of the porous substrate 1 .
- the transition layer 2 reduces the roughness of the surface of the porous substrate 1 , so that the heat generating layer 3 has good continuity, and it is convenient to adjust and control the thickness of the heat generating layer 3 .
- the transition layer 2 can also prevent sodium and potassium ions from the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field, thereby enhancing the stability of the resistance of the heating layer 3 .
- the transition layer 2 can adjust the stress matching between the heating layer 3 and the surface of the porous substrate 1, enhance the adhesion between the heating layer 3 and the porous substrate 1, make the heating layer 3 firmly bonded to the porous substrate 1, and improve the heat generation.
- the stable and reliable working performance of layer 3 prolongs the service life of the atomizing core.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process.
- the target power density of the magnetron sputtering process is 3-12W/cm 2
- the sputtering pressure is 0.1-0.5Pa
- the sputtering time is 20-100min.
- the thickness of layer 2 is 0.1-1 ⁇ m.
- the transition layer 2 When the thickness of the transition layer 2 is too thin, the transition layer 2 cannot play the above-mentioned effect of reducing the roughness of the porous substrate 1 surface and blocking the sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field; If the thickness of the layer 2 is too thick, the stress of the transition layer 2 will increase significantly, causing the microstructure of the transition layer 2 to be destroyed during the electrification and use of the atomizing core, and the transition layer 2 cannot block the sodium and potassium ions of the porous substrate 1 in the electric field. Diffusion into the heating layer 3 under action affects the stability of the resistance value of the heating layer 3 .
- the thickness of the transition layer 2 is set to 0.1-1 ⁇ m, so that the transition layer 2 reduces the roughness of the surface of the porous substrate 1, so that the transition layer 2 prevents the sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field,
- the transition layer 2 adjusts the stress matching between the heating layer 3 and the surface of the porous substrate 1 .
- the thickness of the transition layer 2 is set to 0.3-0.8 ⁇ m, which facilitates reducing the surface roughness of the porous substrate 1 and at the same time helps to block the diffusion of sodium and potassium ions in the porous substrate 1 into the heating layer 3 under the action of an electric field.
- the porous substrate 1 is a porous ceramic, and a transition layer 2 is deposited on at least part of the atomized surface 11 of the porous ceramic by a thin film deposition process.
- the transition layer 2 is an aluminum nitride layer, a silicon nitride layer, a chromium nitride layer, At least any one of a chromium carbide layer or other ceramic layers.
- the heat generating layer 3 is deposited on the side of the transition layer 2 facing away from the porous substrate 1 by a thin film deposition process.
- the heating layer 3 is a nickel-chromium alloy layer, and the thickness of the nickel-chromium alloy layer is set to 1-5 ⁇ m.
- the nickel-chromium alloy layer has good thermal performance, and the price of the nickel-chromium alloy layer is higher than that of precious metal layers such as gold layer, silver layer, platinum layer, palladium layer, or gold-silver alloy layer, gold-platinum alloy layer, gold-silver-platinum alloy layer, and silver-palladium alloy layer.
- the heating layer 3 is a nickel-chromium alloy layer, and the mass ratio of Ni/(Ni+Cr) is 0.2-0.9. According to the resistance calculation formula, the thickness of the heating layer 3 determines the resistance value of the heating layer 3. The thinner the heating layer 3 is, the larger the resistance value is, and the thicker the heating layer 3 is, the smaller the resistance value is. The thickness of the heating layer 3 is adjusted and controlled to achieve the purpose of adjusting the resistance value of the heating layer 3 .
- the inventor found that: when the thickness of the heating layer 3 is too thin, the heating layer 3 of the thin layer structure is relatively loose and the continuity is not good, which affects the stability of the resistance value of the heating layer 3 , the heat generating layer 3 is relatively easy to be oxidized or carbonized at high temperature; the thicker the heat generating layer 3 is, the continuity and compactness of the heat generating layer 3 of the thin layer structure will also increase accordingly, so that the resistance to oxidation or carbonization of the heat generating layer 3 The ability is greatly enhanced, thereby enhancing the stability of the resistance of the heating layer 3.
- the formation time of the heat generating layer 3 is longer, thereby greatly reducing the production efficiency;
- the microstructure is destroyed, affecting the stability of the resistance value of the heating layer 3 .
- the resistance of the heating layer 3 is too low, there is a potential safety hazard of short circuit overload of the heating layer 3, and the resistance of the heating layer 3 is too high, there is a problem that the required heating power cannot be reached, so the common resistance of the heating layer 3 is 0.8 ⁇ 2 ⁇ .
- the heat generation Layer 3 is a nickel-chromium alloy layer, and the thickness of the nickel-chromium alloy layer is set to 1-5 ⁇ m, so that the resistance stability of the heating layer 3 is improved, the resistance of the heating layer 3 is within the common resistance range, and the formation time of the heating layer 3 is moderate , so that the resistance stability of the atomizing core is improved, the heating power of the atomizing core is larger, the atomizing effect of the atomizing core is good, and the manufacturing cost of the atomizing core is controllable.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process.
- the heating layer 3 is deposited by magnetron sputtering process
- the heating layer 3 is a nickel-chromium alloy layer
- the target power density of the magnetron sputtering process is 5-15W/cm 2
- the sputtering pressure is 0.1-0.3Pa.
- the injection time is 30-90 minutes.
- a nickel-chromium alloy layer with a thickness of 1-5 ⁇ m is deposited and formed on at least part of the atomized surface 11 of the porous substrate 1 through a magnetron sputtering process, and the nickel-chromium alloy layer is the heating layer 3 .
- a chemically stable and dense protective layer 4 with a thickness of 0.5-3 ⁇ m is deposited on the side of the heating layer 3 facing away from the porous substrate 1 by a thin film deposition process.
- the protective layer 4 blocks the formation of the aerosol matrix and the outside air from entering the heating layer 3, so as to avoid oxidation or carbonization of the heating layer 3 during energization and use, enhance the oxidation resistance and carbonization resistance of the heating layer 3, and enhance the stability of the resistance of the heating layer 3 performance, improve the cycle life of the atomizing core.
- the thin film deposition process may be, but not limited to, a magnetron sputtering process in the thin film deposition process.
- the protective layer 4 is formed by depositing the magnetron sputtering process, the target power density of the magnetron sputtering process is 3-12W/cm2, the sputtering pressure is 0.1-0.5Pa, and the sputtering time is 40 ⁇ 150min.
- the protective layer 4 cannot play the role of blocking the aerosol-forming matrix and the outside air from entering the heating layer 3; as the thickness of the protective layer 4 increases, the protective layer 4 can gradually block the aerosol-forming matrix And the outside air enters the heating layer 3; however, when the thickness of the protective layer 4 is too thick, the stress of the protective layer 4 will increase significantly, causing the microstructure of the protective layer 4 to be destroyed during the electrification of the atomizing core, and the protective layer 4 The aerosol-forming matrix and outside air cannot be blocked from entering the heating layer 3, which weakens the oxidation resistance and carbonization resistance of the heating layer 3, affects the stability of the resistance of the heating layer 3, and shortens the cycle life of the atomizing core.
- the thickness of the protective layer 4 is set to 0.5-3 ⁇ m, so that the protective layer 4 blocks the aerosol-forming matrix and external air from entering the heating layer 3 .
- the thickness of the protective layer 4 is set at 0.8-1.5 ⁇ m, which can well block the aerosol-forming substrate and external air from entering the heat-generating layer 3 .
- the protection layer 4 is at least any one of an aluminum oxide layer, a silicon oxide layer, an aluminum nitride layer, a silicon nitride layer, a titanium oxide layer, and a titanium nitride layer.
- the above method for preparing the atomizing core mainly includes depositing a conductive material on at least part of the outer surface of the porous ceramic substrate by using a thin film deposition process, so as to form a heating layer on the porous ceramic substrate, and obtain a heating layer on the surface. atomizing core.
- the transition layer 2 and/or the protective layer 4 are not included, the corresponding film layer forming steps S1 and S3 can be correspondingly omitted.
- the atomization core preparation method of the above-mentioned atomization core also includes the following annealing and aging treatment:
- Step S4 using the annealing and aging process to perform annealing heat treatment on the atomizing core.
- the atomization core preparation method of the above-mentioned atomization core also includes the following electrification aging treatment step:
- Step S5 adopting the energization aging process, supplying power to the atomizing core after the annealing heat treatment, and then heating the atomizing core after the annealing heat treatment, so as to perform aging treatment on the microstructure of the heating layer 3 .
- the annealing heat treatment is performed on the atomization core with the heating layer 3 by adopting an annealing aging process.
- the purpose of the annealing heat treatment is to eliminate the microscopic defects of the heat-generating layer 3, promote the grain growth in the micro-structure of the heat-generating layer 3, and make the heat-generating layer 3 more compact, thereby improving the stability of the resistance value of the atomizing core in the process of recycling, and then The heating power of the atomizing core is stable, the heating is uniform, and the atomization effect is good.
- the heat generating layer 3 is in a relatively stable state with low free energy. To achieve a change trend towards a stable state with low free energy, it is necessary for the conductive material atoms to have a strong Diffusion ability to complete the grain boundary migration movement when the grain grows, and the high temperature annealing heat treatment makes it have this condition.
- the annealing heat treatment of the atomizing core with the heat generating layer 3 can promote the growth of the crystal grains in the microstructure of the heat generating layer 3, making the heat generating layer 3 more dense, and improving the resistance of the heat generating layer 3 during energization and use. Stability, so as to improve the stability of the resistance of the atomizing core during energization and use.
- the annealing heat treatment temperature of the heat generating layer 3 of the atomizing core is 500-800° C., and the annealing heat treatment time is 5-60 minutes.
- the annealing heat treatment process of the atomizing core is carried out in a protective gas atmosphere.
- the atomizing core is placed in a tube furnace for annealing heat treatment.
- the tube furnace is continuously filled with protective gas to prevent the heat generation layer 3 from forming during the annealing heat treatment process of the atomizing core. oxidation.
- the shielding gas can be, but is not limited to, nitrogen.
- transition layer 2 and protective layer 4 have the same change trend as that of the heat generating layer 3 during the annealing heat treatment.
- the coarser the grains in the transition layer 2 or protective layer 4 the smaller the total grain boundary surface area and the lower the total surface energy . Since grain coarsening can reduce the surface energy, the transition layer 2 or protective layer 4 is in a relatively stable state with low free energy.
- conductive material atoms are required It has a strong diffusion ability to complete the migration movement of the grain boundary when the grain grows, and the high temperature annealing heat treatment makes it have this condition.
- annealing the transition layer 2 or protective layer 4 of the atomization core can promote the grain growth in the microstructure of the transition layer 2 or protective layer 4, making the transition layer 2 or protective layer 4 denser, thereby improving The stability of the resistance value of the atomizing core during the cycle use.
- the atomization core after the annealing heat treatment is subjected to energization and aging treatment: the atomization core after the annealing heat treatment is powered, the atomization core after the annealing heat treatment is energized and then generates heat, and the microstructure of the heating layer 3 is subjected to aging treatment.
- aging treatment to enhance the electrical stability of the heat generating layer 3 .
- the heating layer 3 of the atomizing core is powered by a DC stabilized power supply, the power is 6-8W, and the power-on time is 1-20min.
- the purpose of carrying out the electrification aging treatment on the atomizing core is to improve the resistance stability of the atomizing core during electrification and use.
- the preparation method of the atomizing core in the first embodiment of the present invention adopts the annealing and aging process to perform annealing heat treatment on the heating layer 3 of the atomizing core, so that the crystal grains in the microstructure of the heating layer 3 grow, Make the heating layer 3 denser and reduce the microscopic defects of the heating layer 3 ; then, conduct energization and heating treatment on the atomizing core after the annealing heat treatment, so as to perform further aging treatment on the microstructure of the heating layer 3 .
- the atomizing core can improve and increase the resistance stability of the heating layer 3, enhance the electrical stability of the heating layer 3, and then make the heating layer 3 generate more uniform heat, preventing the atomizing core from The phenomenon that the local temperature is too high can have a good atomization effect on the aerosol-forming substrate.
- the annealing heat treatment is first performed on the atomizing core with the heat generating layer 3 , and then the energized aging treatment is performed on the annealing heat-treated atomizing core.
- the order of the above-mentioned processing cannot be changed. This is to simulate the real use atmosphere of the atomizing core. Because the electrification aging treatment is generally carried out in the atmosphere, and the annealing heat treatment is usually carried out in the protective gas atmosphere.
- annealing heat treatment is first performed on the atomizing core with the heating layer 3 under the protective gas atmosphere, so that the grains of the internal structure of the heating layer 3 are coarsened to reduce the surface energy, so that the transition layer 2 and the heating layer on the atomizing core
- the layer 3 and the protective layer 4 are in a relatively stable state with low free energy, thereby making the transition layer 2, the heating layer 3 and the protective layer 4 denser, reducing the microscopic defects of the transition layer 2, the heating layer 3 and the protective layer 4, Improve the stability of transition layer 2, heat generating layer 3 and protective layer 4.
- the stable and dense transition layer 2 can prevent the sodium and potassium ions of the porous ceramic substrate 1 from diffusing into the heating layer 3 under the action of an electric field, further improving the resistance stability of the heating layer 3;
- the stable and dense heating layer 3 can enhance the resistance stability of the heating layer 3;
- the stable and dense protective layer 4 can make the heating layer 3 and the aerosol form a matrix and air Oxygen isolation in the heat-generating layer 3 improves the anti-oxidation performance and anti-carbonization performance of the heat-generating layer 3, thereby improving the resistance stability of the heat-generating layer 3.
- the atomizing core also includes two electrodes 5 for electrically connecting the heating layer 3 with the power supply device. Please refer to FIG. 4 and FIG. 5 together.
- the electrode 5 is formed on the atomizing surface 11 of the porous substrate 1 through a thick film deposition process, and the thickness of the electrode 5 is 20-60 ⁇ m.
- the electrode 5 is firmly combined on the porous substrate 1 to prevent the electrode 5 from falling off under the impact of the high-temperature and high-speed aerosol-forming matrix fluid; It bears the pressing force from the metal spring pins.
- the electrode 5 has enough contact area to be electrically connected with the metal spring pins, so that the electrical connection can be easily realized with the power supply device through the metal spring pins, thereby facilitating the heating of the heating layer. 3 and achieve electrical connection with the power supply device through the electrode 5.
- the electrode 5 is at least any one of a gold layer, a silver layer, a platinum layer, a palladium layer, an aluminum layer, a copper layer, a gold-silver alloy layer, a silver-platinum alloy layer, and a silver-palladium alloy layer.
- the metal paste is screen-printed on the porous substrate 1 by a screen-printing process, and the electrodes 5 are formed after drying and sintering.
- the metal paste is at least any one of gold, silver, platinum, palladium, aluminum, copper, gold-silver alloy, silver-platinum alloy, and silver-palladium alloy to form the electrode 5 on the porous substrate 1 .
- the electrodes 5 are arranged in pairs and spaced apart on the first region 11a on the atomizing surface 11, and the heat generating layer 3 is at least covered on the second region 11a on the atomizing surface 11.
- the second area 11b is the area outside the first area 11a on the atomizing surface 11, so that the first area 11a and the second area 11b are continuous areas on the atomizing surface 11, and the heat generating layer 3 includes The heating part 31 of the second region 11b on the atomizing surface 11 of the porous substrate 1, the first connecting part 32 formed on at least part of the surface of one of the electrodes 5, and the second connecting part 33 formed on at least part of the surface of the other electrode 5 , the first connecting portion 32 and the second connecting portion 33 are respectively connected to the heat generating portion 31 .
- the heating layer 3 is electrically connected to the corresponding electrode 5 through surface-to-surface contact to avoid poor contact between the electrode 5 and the heating layer 3 , thereby improving the stability and reliability of power supply to the heating layer 3 .
- the electrodes 5 are arranged in pairs and spaced apart on the first region 11a on the atomizing surface 11, and the transition layer 2 is formed on the second region 11b on the atomizing surface 11. , the heat generating layer 3 is covered on the side of the transition layer 2 facing away from the porous substrate 1 .
- the second area 11b is also an area on the atomizing surface 11 outside the first area 11a, so that the first area 11a and the second area 11b are continuous areas on the atomizing surface 11 .
- the heat generation layer 3 includes a heat generation portion 31 formed on the side of the transition layer 2 away from the porous substrate 1, a first connection portion 32 formed on at least part of the surface of one of the electrodes 5, and a second connection portion 32 formed on at least part of the surface of the other electrode 5.
- the part 33, the first connecting part 32, and the second connecting part 33 are respectively connected to the heating part 31.
- the heating layer 3 is electrically connected to the corresponding electrode 5 through surface-to-surface contact to avoid poor contact between the electrode 5 and the heating layer 3 , thereby improving the stability and reliability of power supply to the heating layer 3 .
- the thickness of the electrode 5 is greater than the sum of the thicknesses of the transition layer 2, the heat generating part 31 and the protective layer 4, and a groove 6 can be formed between the two electrodes 5.
- the transition layer 2, the heating part 31 and the protective layer 4 are sequentially stacked from bottom to top from the inner bottom surface of the groove 6, and the transition layer 2, the heating part 31 and the protective layer 4 are accommodated and positioned on the two electrodes.
- the groove 6 between 5 it is beneficial to enhance the stability of the transition layer 2, the heating part 31 and the protective layer 4 on the porous substrate 1.
- the heat generating layer 3 is at least partially formed on the electrode 5 .
- the first connecting portion 32 includes a first side portion 321 extending from the side of the heating portion 31 close to one of the electrodes 5 and bent along the thickness direction of the electrode 5
- the second connecting portion 33 includes a second side portion 331 extending from the side of the heating portion 31 close to the other electrode 5 and extending along the thickness direction of the electrode 5 .
- the first side portion 321 and the second side portion 331 are respectively combined with on the corresponding side of the corresponding electrode 5 .
- the first side part 321 and the second side part 331 can be respectively combined with the corresponding side of the corresponding electrode 5, and the heating layer 3 can be electrically connected with the corresponding electrode 5 through the surface-to-surface contact form, so as to avoid the occurrence of the electrode 5 and the heating layer 3. Poor contact, thereby improving the stability and reliability of power supply to the heating layer 3 .
- the first connection part 32 also includes a first connection part 322 formed on the side of one of the electrodes 5 away from the porous substrate 1
- the second connection part 33 also includes a In the second bonding portion 332 on the side of the other electrode 5 away from the porous substrate 1, the corresponding side of the first bonding portion 322 is connected to the corresponding side of the first side portion 321, and the corresponding side of the second bonding portion 332 is connected to the corresponding side of the second bonding portion 332. Corresponding sides of the second side portion 331 are connected.
- the contact area between the electrode 5 and the heating layer 3 is increased, which is conducive to improving the stability of the power supply from the electrode 5 to the heating layer 3; on the other hand, the contact area between the electrode 5 and the heating layer 3 is increased, thereby reducing heat generation.
- the contact resistance between the layer 3 and the electrode 5 is beneficial to concentrate the heating area on the heating part 31; on the other hand, it can enhance the adhesion of the heating layer 3, so that the heating layer 3 is more firmly combined with the porous substrate 1 and the electrode 5.
- the atomizing surface 11 in the above embodiment is a plane.
- the heat generation part 31, the first connection part 32 and the second connection part 33 are formed at one time when the heat generation layer 3 is formed, and the first connection part 32 does not include the first joint part 322, and the second connection part 33 does not include In the case of the second joint portion 332, it is only necessary to perform masking treatment on the side of the electrode 5 away from the porous substrate 1 when the heat generating layer 3 is formed by a thin film deposition process, so that the heat generating layer 3 cannot be deposited and formed on the electrode 5 away from the porous substrate 1. side.
- Embodiment 2 of the present invention also provides an atomizer, and the atomizer includes the atomizing core provided in any one of the above embodiments. Since the atomizer has all the technical features of the atomizing core provided by any of the above embodiments, it has the same technical effect as the atomizing core.
- Embodiment 2 of the present invention also provides an aerosol generating device.
- the aerosol generating device includes the atomizing core provided in any of the above embodiments or the atomizer provided in any of the above embodiments. Since the aerosol generating device has all the technical features of the atomizing core or atomizer provided by any of the above embodiments, it has the same technical effect as the atomizing core.
- Embodiment 2 of the present invention also provides a method for preparing the above-mentioned atomizing core.
- the difference between the method for preparing the atomizing core in Embodiment 2 of the present invention and the method for preparing the atomizing core in Embodiment 1 is that:
- the atomization core preparation method of the above atomization core also includes:
- Step S0 Electrode fabrication: screen printing metal paste on the porous substrate 1 by screen printing, drying and sintering to form the electrode 5 . It can be understood that in other implementation manners, the electrode 5 can also be formed in other ways.
- the porous substrate 1 screen-printed with the electrode 5 is placed in a vacuum chamber, and the vacuum is evacuated to 0.003Pa, and the porous substrate 1 is subjected to a Kaufmann-type ion source pair. Ion cleaning 2 ⁇ 10min.
- the difference between the atomizing core in the third embodiment and the atomizing core in the second embodiment is that the atomizing surface 11 is not a plane.
- a first concave portion 13 and a second concave portion 14 are respectively concavely formed on one surface of the porous matrix 1, and the first concave portion 13 and the second concave portion 14 are arranged at intervals to The part between the first depression 13 and the second depression 14 forms a raised portion 12, the atomizing surface 11 includes a first surface 11c where the raised portion 12 is away from the porous matrix 1, and the first depression 13 is away from the porous base 1
- the second surface 11d of the second concave portion 14 is away from the third surface 11e of the porous matrix 1, the first transition surface 11f connecting the first surface 11c and the second surface 11d, and the first transition surface 11f connecting the first surface 11c and the third surface 11e
- the second transition surface 11g is provided.
- One of the electrodes 5 is deposited and formed in the first recessed portion 13, the other electrode 5 is deposited and formed in the second recessed portion 14, the heating portion 31 is deposited and formed on the first surface 11c of the raised portion 12, and the two electrodes 5
- the upper end surface is higher than the upper end surface of the heat generating part 31 .
- the heating layer 3 includes a heating portion 31 formed in the second region 11 b on the atomizing surface 11 of the porous substrate 1 , and a first connecting portion 32 formed on at least part of the surface of one of the electrodes 5 , The second connecting portion 33 formed on at least part of the surface of the other electrode 5 , the first connecting portion 32 and the second connecting portion 33 are respectively connected to the heating portion 31 .
- the first connection part 32 includes a first joint part 322 formed on the side of one electrode 5 away from the porous substrate 1, and the second connection part 33 includes a second joint part formed on the side of the other electrode 5 away from the porous substrate 1 332.
- Corresponding sides of the first combining portion 322 are connected to corresponding sides of the heating portion 31
- corresponding sides of the second combining portion 332 are connected to corresponding sides of the heating portion 31 .
- the first connecting portion 32 may not include the first side portion 321, the second connecting portion 33 may not include the second side portion 331, and the first connecting portion 322 of the first connecting portion 32 is respectively connected to one of the electrodes 5 and The heating part 31 and the second connecting part 332 of the second connection part 33 are respectively connected to the other electrode 5 and the heating part 31 .
- the contact area between the electrode 5 and the heating layer 3 is increased, which is conducive to improving the stability of the power supply from the electrode 5 to the heating layer 3; on the other hand, the contact area between the electrode 5 and the heating layer 3 is increased, thereby reducing heat generation.
- the contact resistance between the layer 3 and the electrode 5 is conducive to concentrating the heating area on the heating part 31; on the other hand, it can enhance the adhesion of the heating layer 3, so that the heating layer 3 is more firmly combined with the porous substrate 1 and the electrode 5.
- the atomizing surface 11 in the above embodiment is a plane.
- the silver-palladium metal paste is screen-printed on the porous substrate 1 by a screen-printing process, and the electrode 5 is formed after drying and sintering.
- the drying temperature of the electrode 5 is 80°C
- the drying time of the electrode 5 is 20 minutes
- the sintering condition is to keep the temperature environment at 910°C for 20 minutes;
- porous substrate 1 screen-printed with silver-palladium metal electrodes 5 into a magnetron sputtering vacuum chamber, evacuate to 0.003Pa, and use a Kaufmann-type ion source to perform ion cleaning on the substrate for 5 minutes.
- the power of the ion source is 200W;
- a magnetron sputtering process is used to directly deposit the heating layer 3 on the outer surface of the ion-cleaned porous substrate 1 .
- the mass ratio of Ni/(Ni+Cr) in the nickel-chromium alloy target used is 80%
- the sputtering power density of the nickel-chromium alloy target is 10W/cm 2
- the sputtering pressure is 0.3Pa
- the thickness of the heat-generating layer 3 deposited on the porous substrate 1 in Experimental Example 1 was tested by using a procedural instrument, and the thickness of the heat-generating layer 3 was measured to be 1 ⁇ m.
- the atomizing core prepared in Experimental Example 1 is marked as S-1, and the atomizing core S-1 is assembled with a battery and a pod to form an electronic cigarette, and a simulated smoking test is performed on an electronic cigarette smoking machine. After the test, the atomizing core S-1 was taken out to measure the change of its resistance value. It can be clearly seen from Figure 9 that in the first 3000 cycles, the resistance value of the atomizing core S-1 changed significantly at the beginning of the test, and the range of subsequent resistance value changes decreased significantly.
- the difference between Experimental Example 2 and Experimental Example 1 is that the time for magnetron sputtering of the heating layer 3 is different.
- the sputtering time in Experimental Example 2 is 60 minutes to increase the thickness of the heating layer 3 deposited on the porous substrate 1 .
- the thickness of the heating layer 3 in Experimental Example 2 was measured to be 3 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 2 was marked as S-2.
- the electronic cigarette was assembled into a simulated smoking test on the electronic cigarette smoking machine, and the resistance value change of the atomizing core was measured after the test.
- the difference between Experimental Example 3 and Experimental Example 1 is: the time of magnetron sputtering heating layer 3 is different, and the sputtering time in Experimental Example 3 is 90min, to increase the thickness of deposition heating layer 3 on porous substrate 1.
- the thickness of the heat generating layer 3 in Experimental Example 3 was measured to be 5 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 3 was marked as S-3.
- the electronic cigarette was assembled into a simulated smoking test on the electronic cigarette smoking machine, and the resistance value change of the atomizing core was measured after the test.
- the difference between this experimental example and experimental example 2 is: before depositing the heating layer 3, the silver-palladium metal electrode 5 screen-printed on the porous substrate 1 is covered by a mask, and then at least part of the outer surface of the porous substrate 1 An aluminum nitride transition layer 2 is deposited to prevent aluminum nitride from being deposited on the silver-palladium metal electrode 5 . Specifically, aluminum nitride is deposited on the porous substrate 1 using a magnetron sputtering process.
- the reaction gas is nitrogen
- argon is the working gas
- the nitrogen/argon gas flow ratio is 1.2
- the sputtering pressure is 0.35Pa
- the metal aluminum target sputtering power density is 8W/cm 2
- the sputtering time is 20min.
- the thickness of the aluminum nitride transition layer 2 in Experimental Example 4 was measured to be 0.1 ⁇ m by using a step meter. After the aluminum nitride transition layer 2 is deposited, the heat generating layer 3 is continuously deposited on the side of the aluminum nitride transition layer 2 facing away from the porous substrate 1 using the same process steps as in Experimental Example 1.
- the thickness of the heating layer 3 in Experimental Example 4 was measured to be 3 ⁇ m by using the same instrument and testing method as in Experimental Example 1.
- the atomizing core prepared in Experimental Example 4 is marked as S-4, and the cycle reliability test of the atomizing core S-4 is carried out by the same method as in Experimental Example 1, and its resistance value is measured.
- the difference between Experimental Example 5 and Experimental Example 4 lies in that the time for magnetron sputtering the transition layer of aluminum nitride 2 is different, and the sputtering time is 50 minutes.
- the thickness of the aluminum nitride transition layer 2 in Experimental Example 5 was measured to be 0.5 ⁇ m by using a step meter, and the atomization core prepared in Experimental Example 5 was marked as S-5.
- the cycle reliability test was carried out on the atomizing core S-5, and its resistance value was measured.
- the difference between Experimental Example 6 and Experimental Example 4 lies in that the time for magnetron sputtering the aluminum nitride transition layer 2 is different, and the sputtering time is 100 min.
- the thickness of the aluminum nitride transition layer 2 in Experimental Example 6 was measured to be 1 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 6 was marked as S-6.
- the cycle reliability test was carried out on the atomizing core S-6, and its resistance value was measured.
- Experimental Example 7 The difference between Experimental Example 7 and Experimental Example 5 is that an aluminum oxide protective layer is deposited on the heating layer 3, that is, after the heating layer 3 is deposited in Experimental Example 5, the magnetron sputtering process is used to continue to place the heating layer 3 away from the porous substrate 1 A protective layer of aluminum oxide is deposited on one side. Before magnetron sputtering the aluminum oxide protective layer, a mask is used to shield the silver-palladium metal electrode 5 screen-printed on the porous substrate 1 to prevent aluminum oxide from being deposited on the silver-palladium metal electrode 5 . Specifically, a magnetron sputtering process is used to deposit the aluminum oxide protective layer.
- the reactive gas of magnetron sputtering is oxygen, argon is the working gas, the gas flow ratio of oxygen/argon is 1.5, the sputtering pressure is 0.4Pa, and the metal aluminum
- the sputtering power density of the target is 9W/cm 2 , and the sputtering time is 40min.
- the thickness of the aluminum oxide protective layer in Experimental Example 7 was measured to be 0.5 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 7 was marked as S-7. Using the same method as in Experimental Example 1, the cycle reliability test was carried out on the atomizing core S-7, and its resistance value was measured.
- Experimental Example 8 The difference between Experimental Example 8 and Experimental Example 7 is that the time for magnetron sputtering the aluminum oxide protective layer is different, and the sputtering time is 90 minutes.
- the thickness of the aluminum oxide protective layer in Experimental Example 8 was measured to be 1.5 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 8 was marked as S-8. Using the same method as in Experimental Example 1, the cycle reliability test was carried out on the atomizing core S-8, and its resistance value was measured.
- Experimental Example 9 The difference between Experimental Example 9 and Experimental Example 7 is that the time for magnetron sputtering of the aluminum oxide protective layer is different, and the sputtering time is 150 minutes.
- the thickness of the aluminum oxide protective layer in Experimental Example 9 was measured to be 3 ⁇ m by using a step meter, and the atomizing core prepared in Experimental Example 9 was marked as S-9. Using the same method as in Experimental Example 1, the cycle reliability test was carried out on the atomizing core S-9, and its resistance value was measured.
- Experimental Example 10 The difference between Experimental Example 10 and Experimental Example 8 is that: the atomizing core prepared in Experimental Example 8 was placed in a tube furnace for annealing heat treatment.
- the protective gas in the tube furnace is nitrogen
- the annealing temperature is 500° C.
- the annealing time is 10 min.
- the annealed atomizing core in Experimental Example 10 is marked as S-10, and the cycle reliability test of atomizing core S-10 is carried out by the same method as Experimental Example 1, and its resistance value is measured.
- Experimental Example 11 The difference between Experimental Example 11 and Experimental Example 10 is that the annealing temperature is different, and the annealing temperature is 700°C.
- the annealed atomizing core in Experimental Example 11 is marked as S-11, and the cycle reliability test of atomizing core S-11 is carried out by the same method as Experimental Example 1, and its resistance value is measured.
- Experimental Example 12 The difference between Experimental Example 12 and Experimental Example 10 is that the annealing temperature is different, and the annealing temperature is 800°C.
- the annealed atomizing core in Experimental Example 12 is marked as S-12, and the cycle reliability test of atomizing core S-12 is carried out by the same method as Experimental Example 1, and its resistance value is measured.
- Experimental Example 13 The difference between Experimental Example 13 and Experimental Example 11 is that: the atomizing core prepared in Experimental Example 11 is subjected to energization, heating and aging treatment.
- the power supply used in the energization and heating aging treatment is a DC stabilized power supply with a power of 5W. After energizing for 2s, stop for 5s, then continue to energize for 2s and stop for 5s, a total of 100 cycles are performed.
- the atomizing core after energizing, heating and aging treatment in Experimental Example 13 is marked as S-13, and the cycle reliability test of atomizing core S-13 is carried out by the same method as Experimental Example 1, and its resistance value is measured.
- Experimental Example 14 The difference between Experimental Example 14 and Experimental Example 13 is that the energized power is 7W.
- the atomizing core after energized heating and aging treatment in Experimental Example 14 is marked as S-14, and the cycle reliability test of atomizing core S-14 is carried out by the same method as in Experimental Example 1, and its resistance value is measured.
- Experimental Example 15 The difference between Experimental Example 15 and Experimental Example 13 is that the energized power is 9W.
- the atomizing core after electrification heating aging treatment in Experimental Example 15 is marked as S-15, and the cycle reliability test of atomizing core S-15 is carried out by the same method as Experimental Example 1, and its resistance value is measured.
- Table 1 The data table of the resistance value of the atomizing core cycle test in Experimental Example 1 to Experimental Example 15
- the change resistance value of the total cycle in Table 1 refers to the difference between the resistance value of the test sample after the 3000th cycle test and the initial resistance value of the test sample
- the change resistance value of the total cycle in Table 1 refers to The ratio of the above-mentioned change resistance value of the test sample to the initial resistance value of the test sample. It can be understood that the smaller the change resistance value of the total cycle and/or the smaller the change resistivity of the total cycle, it can be judged that the change of the resistance value after the cycle test is reduced, and the resistance stability of the test sample in the cycle test is higher.
- the cycle test data of atomizing core S-1 to atomizing core S-15 in Table 1 are the data obtained through the test of one test sample. Except atomizing core S-1 to atomizing core S-3, the initial resistance values are different because they have heat-generating layers 3 with different thicknesses.
- the comparative example of controlling a single variation will select test samples with similar initial resistance values from multiple test samples in the same batch, for example: atomizing core S-4 to atomizing core S-6 is controlled as a single change in the thickness of the transition layer 2, and the test samples with relatively similar initial resistance values are selected from the multiple test samples of the atomizing core S-2 with the heating layer 3 thickness of 3 ⁇ m in the same batch.
- the atomizing core S-1 in Experimental Example 1 has a thickness of heating layer 3 of 1 ⁇ m, and its initial resistance value is 1.56 ⁇
- the atomizing core in Experimental Example 2 S-2 the thickness of the heating layer 3 is 3 ⁇ m, and its initial resistance value is 1.25 ⁇
- the atomizing core S-3 in Experimental Example 3 the thickness of the heating layer 3 is 5 ⁇ m, and its initial resistance value is 1.07 ⁇
- the corresponding initial resistance value will also be different accordingly: the thicker the heating layer 3 is, the lower the initial resistance value is. In this way, the initial resistance value of the atomizing core can be adjusted by changing the thickness of the heating layer 3 .
- the atomizing core S-1 in Experimental Example 1 has a heat generating layer 3 with a thickness of 1 ⁇ m, a changing resistance value of 1.21 ⁇ in a cycle test, and a changing resistivity of 77.6%.
- the thickness of the heat-generating layer 3 is 3 ⁇ m
- the changing resistance value of the cycle test is 0.67 ⁇
- the changing resistivity is 53.6%
- the atomizing core S-2 in Experimental Example 3 is 3.
- the thickness of the heating layer 3 is 5 ⁇ m
- the change resistance value of the cycle test is 0.54 ⁇
- the change resistance rate is 50.5%.
- the thicker the heat generation layer 3 is, the greater the thickness of the heat generation layer 3 is, the greater the thickness of the heat generation layer 3 after the cycle test.
- the resistance change is reduced. This is because the heating layer 3 is formed on the porous substrate 1 by thin film deposition. If the surface roughness of the porous substrate 1 is relatively large and the heating layer 3 is relatively thin, the heating layer 3 is discontinuous and loosely distributed.
- the heat generating layer 3 is easily oxidized or carbonized, which affects the stability of its resistance value.
- the thicker the heating layer 3 is, the distribution of the heating layer 3 is continuous and dense, which improves the oxidation resistance or carbonization resistance, so that the resistance value is more stable.
- the aluminum nitride transition layer 2 of the atomizing core S-6 in Experimental Example 6 has a thickness of 1 ⁇ m, and the change resistance value of the cycle test is 0.47 ⁇ , and the change resistivity is 37.9%, and the stability of the resistance value decreases instead. This is because the aluminum nitride transition layer 2 can block sodium and potassium ions in the porous substrate 1 from penetrating into the heating layer 3 under an electric field.
- the aluminum nitride transition layer 2 is within a certain thickness range, and the thicker the thickness, the better the barrier effect.
- the stress of the aluminum nitride transition layer will increase significantly, causing the microstructure of the heating layer 3 to be destroyed during the cycle test, resulting in the resistance value of the atomizing core cycle test Stability decreased instead.
- the resistance value change of atomizing core S-7, atomizing core S-8 and atomizing core S-9 in Experimental Example 7 to Experimental Example 9 is obviously smaller than that of Experimental Example 5
- the atomizing core S-5 in the middle is due to the setting of the aluminum oxide protective layer, which isolates the heating layer 3 from the aerosol forming matrix and the oxygen in the air, so as to avoid the influence of the heating layer 3 being carbonized and oxidized by high temperature during long-term use.
- the stability of the resistance value improves the resistance stability of the heating layer 3 of the atomizing core, and increases the cycle life of the atomizing core.
- the aluminum oxide protective layer of atomizing core S-9 in Experimental Example 9 has a thickness of 3 ⁇ m, and its resistance value in the cycle test is 0.29 ⁇ , and the change resistivity is 22.7%.
- the stability of the resistance value in the cycle test decreases instead. This is because the aluminum oxide protective layer is within a certain thickness range, and the thicker the aluminum oxide protective layer is, the higher the density is, which can better isolate the heating layer 3 from the aerosol-forming matrix and oxygen in the air.
- the stress of the alumina protective layer will increase significantly, resulting in the destruction of the microstructure of the alumina protective layer during the cycle test, resulting in the stability of the resistance value of the atomizing core cycle test Instead, it declined.
- the change of the resistance value of atomizing core S-10, atomizing core S-11 and atomizing core S-12 in Experimental Example 10 to Experimental Example 12 is obviously smaller than that of Experimental Example 8 In the atomizing core S-8, this is because the annealing heat treatment can reduce the microscopic defects of the transition layer 2, the heating layer 3 and the protective layer 4, so that the crystal grains in the microstructure of the heating layer 3 grow up, and the heating layer 3 is made more Dense, so as to improve the stability of the heating layer 3 cycle test resistance of the atomizing core.
- the annealing temperature was increased to 700°C.
- the changing resistance value of the cycle test was 0.13 ⁇ , and the changing resistivity was 9.7%.
- the atomizing core in Experimental Example 11 The resistance stability of the S-11 cycle test is significantly improved.
- the annealing temperature was further increased to 800°C in Experimental Example 12
- the changing resistance value of the atomizing core S-12 in Experimental Example 12 was 0.21 ⁇ , and the changing resistivity was 15.4%.
- the resistance stability of the atomizing core S-12 cycle test decreases instead, because too high temperature will destroy the microstructure of the transition layer 2, heating layer 3 or protective layer 4, and affect the stability of the resistance of the heating layer 3 cycle test.
- the power of the energization heating aging treatment is too low, the heating value of the heating layer 3 is small, the microstructure of the heating layer 3 is improved slightly, and thus the stability of the resistance of the heating layer 3 is improved slightly.
- the power of the energized heating aging treatment is 7W
- the change resistance value of the cycle test is 0.07 ⁇
- the change resistivity is 4.8%, which can significantly improve the heating layer of the atomizing core. 3 Stability of cycle resistance.
- the power of the heating and aging treatment was increased to 9W, and the changing resistance value of the cycle test was 0.41 ⁇ , and the changing resistivity was 27.7%.
- the heating layer of the atomizing core was 3 On the contrary, the stability of the cycle resistance decreased. This is because the power of the energization heating aging treatment is too high, the greater the heating value of the heating layer 3, the excessive heating value will destroy the microstructure of the heating layer 3, thereby reducing the stability of the heating layer 3 resistance.
Landscapes
- Resistance Heating (AREA)
Abstract
Description
Claims (10)
- 一种雾化芯制备方法,其特征在于,包括如下步骤:采用薄膜沉积工艺将导电材料沉积在多孔陶瓷基底的至少部分外表面上,以在所述多孔陶瓷基底上形成发热层,获得表面具有发热层的雾化芯;采用退火老化工艺,对所述雾化芯进行退火热处理。
- 如权利要求1所述的雾化芯制备方法,其特征在于,所述退火热处理步骤中,所述退火热处理的温度为500~800℃,所述退火热处理的时间为5~60分钟。
- 如权利要求1所述的雾化芯制备方法,其特征在于,所述退火热处理步骤中,所述雾化芯退火热处理过程,在保护气体氛围中进行。
- 如权利要求1所述的雾化芯制备方法,其特征在于,所述雾化芯制备方法还包括通电老化处理步骤,所述通电老化处理步骤包括:采用通电老化工艺,对退火热处理后的所述雾化芯进行供电,退火热处理后的所述雾化芯通电后发热,以对所述发热层的微观结构进行老化处理。
- 如权利要求4所述的雾化芯制备方法,其特征在于,所述通电老化处理步骤中,通电功率为6~8W,通电时间为1~20分钟。
- 如权利要求4所述的雾化芯制备方法,其特征在于,所述通电老化处理步骤中,所述雾化芯的通电老化处理过程,在大气氛围下进行。
- 如权利要求4所述的雾化芯制备方法,其特征在于,所述通电老化处理步骤中,采用直流稳压电源对所述雾化芯进行供电。
- 如权利要求1至7任一项所述的雾化芯制备方法,其特征在于,所述导电材料为镍铬合金材料,所述镍铬合金材料通过所述薄膜沉积工艺沉积形成镍铬合金发热层,所述镍铬合金发热层的沉积厚度为1~5μm。
- 如权利要求8所述的雾化芯制备方法,其特征在于,所述镍铬合金材料中Ni/(Ni+Cr)的质量比为0.2~0.9。
- 如权利要求1至7任一项所述的雾化芯制备方法,其特征在于,所述多孔陶瓷基底的孔隙率为30%~80%,所述多孔陶瓷基底的孔径为10~30μm。
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| US20230050630A1 (en) * | 2021-08-13 | 2023-02-16 | Shenzhen Smoore Technology Limited | Atomization component, atomizer, and electronic atomization device |
| CN117383962A (zh) * | 2023-10-31 | 2024-01-12 | 深圳市吉迩科技有限公司 | 一种陶瓷雾化芯热处理方法及其应用 |
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| CN119054954A (zh) * | 2023-05-31 | 2024-12-03 | 思摩尔国际控股有限公司 | 一种发热薄膜、雾化芯及雾化装置 |
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