CN115836753A - Atomizing core preparation method - Google Patents

Atomizing core preparation method Download PDF

Info

Publication number
CN115836753A
CN115836753A CN202111109385.1A CN202111109385A CN115836753A CN 115836753 A CN115836753 A CN 115836753A CN 202111109385 A CN202111109385 A CN 202111109385A CN 115836753 A CN115836753 A CN 115836753A
Authority
CN
China
Prior art keywords
layer
atomizing core
core
experimental example
heating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202111109385.1A
Other languages
Chinese (zh)
Inventor
邱伟华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changzhou Paiteng Electronic Technology Co Ltd
Original Assignee
Dongguan Vivante Intelligent Technology Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dongguan Vivante Intelligent Technology Co ltd filed Critical Dongguan Vivante Intelligent Technology Co ltd
Priority to CN202111109385.1A priority Critical patent/CN115836753A/en
Priority to PCT/CN2022/110238 priority patent/WO2023045583A1/en
Publication of CN115836753A publication Critical patent/CN115836753A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/46—Shape or structure of electric heating means
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/50—Control or monitoring
    • 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

Landscapes

  • Resistance Heating (AREA)

Abstract

The invention provides a preparation method of an atomizing core, which comprises the steps of firstly forming a conductive material on the outer surface of a porous ceramic substrate by a thin film deposition process to form the atomizing core with a heating layer on the surface; secondly, annealing and aging process is adopted to carry out annealing heat treatment on the heating layer of the atomizing core, so that crystal grains in the microstructure of the heating layer grow up, the heating layer is enabled to be more compact, and the micro defects of the heating layer are reduced; then, the atomized core after the annealing heat treatment is subjected to energization heating treatment to further age the microstructure of the heating layer. Like this, atomizing core can improve and improve the stability of layer resistance that generates heat after annealing thermal treatment and circular telegram ageing treatment, has strengthened the electrical stability on layer that generates heat, and then makes the layer that generates heat more even, prevents that atomizing core from appearing the phenomenon that local high temperature, can have good atomization effect to aerosol formation substrate.

Description

Atomizing core preparation method
Technical Field
The invention belongs to the technical field of atomization, and particularly relates to a preparation method of an atomization core.
Background
In a film heating type atomizing wick used in an aerosol generating device, a heating film is generally attached to an atomizing surface of a porous ceramic, and an aerosol-forming substrate on the atomizing surface is heated by the heating film to atomize the aerosol-forming substrate to form aerosol. The current film heating type atomizing core has the problems of poor continuity and difficulty in adjusting and controlling the thickness, so that the resistance value stability of the film heating layer is poor easily, and the heating uniformity of the film heating type atomizing core is poor.
Disclosure of Invention
Based on the above problems in the prior art, an object of the embodiments of the present invention is to provide a method for preparing an atomizing core that improves and enhances the resistance stability of a heat generating layer.
In order to achieve the purpose, the invention adopts the technical scheme that: provided is a preparation method of an atomizing core, which comprises the following steps:
depositing a conductive material on at least part of the outer surface of the porous ceramic substrate by adopting a thin film deposition process so as to form a heating layer on the porous ceramic substrate and obtain an atomizing core with the heating layer on the surface;
and annealing and aging the atomization core by adopting an annealing and aging process.
Optionally, in the annealing heat treatment step, the temperature of the annealing heat treatment is 500 to 800 ℃, and the time of the annealing heat treatment is 5 to 60 minutes.
Optionally, in the annealing heat treatment step, the atomizing core annealing heat treatment process is performed in a protective gas atmosphere.
The atomization core preparation method further comprises a power-on aging treatment step, wherein the power-on aging treatment step comprises the following steps: and adopting a power-on aging process to supply power to the atomization core after annealing heat treatment, and heating the atomization core after annealing heat treatment after power-on so as to age the microstructure of the heating layer.
Optionally, in the step of the electrifying aging treatment, the electrifying power is 6-8W, and the electrifying time is 1-20 minutes.
Optionally, in the step of performing the electrification aging treatment, the electrification aging treatment process of the atomization core is performed in an atmospheric atmosphere.
Optionally, in the step of power-on aging treatment, a direct-current voltage-stabilizing power supply is used for supplying power to the atomizing core.
Optionally, the conductive material is a nichrome material, the nichrome material is deposited by the thin film deposition process to form a nichrome heating layer, and the deposition thickness of the nichrome heating layer is 1-5 μm.
Optionally, the mass ratio of Ni/(Ni + Cr) in the nichrome material is 0.2-0.9.
Optionally, the porosity of the porous ceramic substrate is 30% -80%, and the pore diameter of the porous ceramic substrate is 10-30 μm.
Compared with the prior art, one or more technical schemes in the embodiment of the invention have at least one of the following beneficial effects:
according to the preparation method of the atomization core, firstly, a conductive material is formed on the outer surface of a porous ceramic substrate through a thin film deposition process so as to form the atomization core with a heating layer on the surface; secondly, an annealing and aging process is adopted to carry out annealing heat treatment on the heating layer of the atomizing core, so that crystal grains in the microstructure of the heating layer grow up, the heating layer is enabled to be more compact, and the micro defects of the heating layer are reduced. Like this, atomizing core can improve and improve the stability of layer resistance that generates heat after annealing thermal treatment, has strengthened the electrical stability on layer that generates heat, and then makes the layer that generates heat more even, prevents that atomizing core from appearing the phenomenon of local high temperature, can form the substrate to aerosol and have good atomization effect.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings required to be used in the embodiments or the prior art description will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings may be obtained according to these drawings without inventive labor.
Fig. 1 is a schematic cross-sectional view of an atomizing core according to a first embodiment of the present invention;
FIG. 2 is another schematic cross-sectional view of an atomizing core provided in accordance with an embodiment of the present invention;
FIG. 3 is a schematic top view of an atomizing core according to a second embodiment of the present invention;
FIG. 4 is a schematic cross-sectional view of an atomizing core provided in the second embodiment of the present invention;
FIG. 5 is a schematic cross-sectional view of a porous substrate according to a second embodiment of the present invention;
FIG. 6 is a schematic sectional view of an atomizing core provided in the third embodiment of the present invention;
FIG. 7 is a schematic cross-sectional view of a porous substrate provided in example III of the present invention;
FIG. 8 is a schematic sectional view of an atomizing core provided in the fourth embodiment of the present invention;
FIG. 9 is a comparison graph of resistance values of the cycle tests of the atomizing cores prepared in examples 1 to 15 of the present invention;
FIG. 10 is a comparison graph of resistance values of the aerosol core cycle tests prepared in examples 2, 5, 8, 11 and 14 of the present invention;
FIG. 11 is a comparison graph of resistance values of the cycle tests of the atomizing cores prepared in examples 1 to 3 of the present invention;
FIG. 12 is a comparison graph of resistance values of the atomization cores prepared in example 2 and examples 4 to 6 of the present invention in a cycle test;
FIG. 13 is a comparison graph of resistance values of the atomization cores prepared in example 5 and examples 7-9 of the present invention by cycle testing;
FIG. 14 is a graph comparing resistance values of the atomization core prepared in example 8 and examples 10 to 12 of the present invention in a cycle test;
fig. 15 is a comparison graph of resistance values of the atomization cores prepared in example 11 and examples 13 to 15 of the present invention in a cycle test.
Wherein, in the figures, the respective reference numerals:
a porous ceramic substrate; 11-an atomizing surface; 11 a-a first region; 11 b-a second region; 11 c-a first surface; 11 d-a second surface; 11 e-a third surface; 11 f-a first transition surface; 11 g-a second transition surface; 12-a boss; 13-a first recess; 14-a second recess; 2-a transition layer;
3-heating layer; 31-a heat-generating portion; 32-a first connection; 321-a first side portion; 322-a first binding moiety; 33-a second connecting portion; 331-a second side; 332-a second junction;
4-a protective layer; 41-bare parts; 5-an electrode; 6-grooves.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
Referring to fig. 1 to 2, an atomizing core according to one embodiment of the present invention will now be described. The atomization core provided by the embodiment of the invention is used for the atomizer, and can generate heat under the electric drive of the power supply device of the aerosol generating device, and the aerosol forming substrate in the liquid storage cavity of the atomizer is heated and atomized to form smoke for a user to inhale so as to achieve the effect of simulating smoking.
Referring to fig. 2, an atomizing core according to an embodiment of the present invention includes a porous substrate 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 microporous structure with capillary adsorption inside, the porous substrate 1 can adsorb and store the aerosol-forming substrate through the microporous structure, and the adsorbed and stored aerosol-forming substrate can be continuously transported to the atomizing surface 11 through the microporous structure. The heat generating layer 3 is formed on at least a part of the atomizing surface 11. When the atomizing core is used, power is supplied to the atomizing core through a power supply device of the aerosol generating device, the heating layer 3 generates heat after being electrified, and the heat is transmitted to the aerosol forming substrate on the atomizing surface 11 to atomize the aerosol forming substrate to form smoke which can be sucked by a user.
In some embodiments, the porous substrate 1 may also be a porous material having liquid adsorption capacity, such as porous ceramic, porous metal, or the like. In some of these embodiments, the porous substrate 1 is a porous ceramic; further, in some more specific embodiments, the porosity of the porous substrate 1 is 30% to 80%, and the pore diameter of the porous substrate 1 is 10 to 30 μm.
In some embodiments, the heat generating layer 3 is a metal layer or an alloy layer with stable chemical properties and good electrical and thermal conductivity, and the heat generating layer 3 is a metal layer such as a copper layer, an iron layer, a nickel layer, a chromium layer, a gold layer, a silver layer, a platinum layer, a palladium layer, a molybdenum layer, or any one of a gold-silver alloy layer, a gold-platinum alloy layer, a gold-silver-platinum alloy layer, a silver-palladium alloy layer, a silver-platinum alloy layer, a palladium-copper alloy layer, a palladium-silver alloy layer, and a nickel-chromium alloy layer. In some embodiments, the heat generating layer 3 is a nichrome layer. The nichrome layer has good thermal performance, and the price of the nichrome layer is lower than that of precious metal layers such as gold layer, silver layer, platinum layer and palladium layer, or precious metal alloy layers such as 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 and palladium-silver alloy layer. In some more specific embodiments, the heat generating layer 3 is a nichrome layer having a mass ratio of Ni/(Ni + Cr) of 0.2 to 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, so that the purpose of adjusting the resistance value of the heating layer 3 can be achieved by adjusting and controlling the thickness of the heating layer 3. Meanwhile, in the development process, through a large number of experiments, the inventor finds that: when the thickness of the heating layer 3 is too thin, the heating layer 3 with a thin layer structure is loose and has poor continuity, the stability of the resistance value of the heating layer 3 is influenced, and the heating layer 3 is easily oxidized or carbonized at high temperature; the thicker the heating layer 3 is, the more the continuity and compactness of the heating layer 3 with a thin layer structure are increased, so that the oxidation resistance or carbonization resistance of the heating layer 3 is greatly enhanced, and the resistance stability of the heating layer 3 is enhanced. However, when the thickness of the heat generating layer 3 is too thick, on the one hand, the time required for forming the heat generating layer 3 is long, thereby greatly reducing the production efficiency; on the other hand, the larger the stress of the heat generating layer 3 is, the more the microstructure of the heat generating layer 3 is destroyed during the use of electrification, which affects the stability of the resistance value of the heat generating layer 3. And considering that the resistance of the heating layer 3 is too low, the safety hazard of short circuit overload of the heating layer 3 exists, and the resistance of the heating layer 3 is too high, the required heating power cannot be reached, so the common resistance of the heating layer 3 is 0.8-2 omega. Considering the influence of the thickness of the heat generating layer 3 on the stability of the resistance of the heat generating layer 3 and considering the positive correlation of the thickness of the heat generating layer 3 with the formation time period in combination with the usual resistance of the heat generating layer 3 of 0.8 to 2 Ω, the thickness of the heat generating layer 3 is set to 1 to 5 μm in combination with the above considerations. In some of these embodiments, generate heat layer 3 and be the nichrome layer, the thickness of nichrome layer sets up to 1 ~ 5 mu m to make the resistance stability who generates heat layer 3 improve, the resistance that generates heat layer 3 is in resistance range commonly used, and the formation time that generates heat layer 3 is moderate, and then makes the resistance stability of atomizing core improve, and the power that generates heat of atomizing core is great, and the atomizing effect of atomizing core is good, and the manufacturing cost of atomizing core is controllable.
In some of these embodiments, the thin film deposition process may be, but is not limited to, a magnetron sputtering process among thin film deposition processes. Because the heating area of the atomizing core is larger, the atomizing core generates heat more uniformly, the phenomenon of overhigh local temperature can not occur, and the improvement of the heated uniformity of the aerosol forming substrate is facilitated, thereby improving the atomizing effect. In some embodiments, the heating layer 3 is formed by deposition through a magnetron sputtering process, the heating layer 3 is a nichrome layer, and the power density of a target material of the magnetron sputtering process is 5-15W/cm 2 The sputtering pressure is 0.1-0.3 Pa, and the sputtering time is 30-90 min. In this way, a nichrome layer having a thickness of 1 to 5 μm is deposited on at least a part of the atomized surface 11 of the porous substrate 1 by the magnetron sputtering process, and the nichrome layer forms the heat generating layer 3.
In the process of forming the heat generating layer 3 by deposition through the thin film deposition process, the process of forming the heat generating layer 3 roughly includes: 1. island preliminary formation: the gaseous target material reaches the surface of the porous substrate 1, adheres and condenses to form a plurality of uniform and fine atomic groups capable of moving, and the original atomic groups are called 'islands'; 2. island number saturation: the island continuously receives new deposition atoms, and is combined with other small islands to grow gradually, and the number of the islands quickly reaches saturation; 3. and (3) island growing and nucleation: while the small 'islands' are combined continuously, new small 'islands' are formed on the surface of the vacated porous substrate 1; 4. merging, growing up and filling: the formation and combination of small 'islands' are continuously carried out, and the 'islands' with larger sizes continuously swallow the 'islands' with smaller sizes nearby; 5. filling pores and forming a film: the isolated small islands are connected with each other into pieces along with the combination, and finally only a plurality of isolated holes and channels are left and are continuously filled to form a film layer which is continuous in appearance and completely covered.
Referring to fig. 1 and 2 in combination, in some embodiments, the atomizing core further includes a transition layer 2 formed between the heat generating layer 3 and the porous substrate 1. In a specific embodiment, a transition layer 2 with the thickness of 0.1-1 μm is deposited on at least part of the atomization surface 11 of the porous substrate 1 through a thin film deposition process, and a heat-generating layer 3 is formed on one surface of the transition layer 2, which is far away from the porous substrate 1. Because the potential energy of the pits on the surface of the porous substrate 1 is the lowest, and the forming process of the transition layer 2 is the same as the forming process of the heating layer 3, the transition layer 2 reduces the roughness of the surface of the porous substrate 1, so that the heating layer 3 has good continuity, and the thickness of the heating layer 3 is convenient to adjust and control. And the transition layer 2 can also prevent sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field, so that the stability of the resistance of the heating layer 3 is enhanced. In addition, transition layer 2 can play and adjust the stress matching on layer 3 and porous basement 1 surface that generates heat, and the reinforcing generates heat the adhesive force between layer 3 and the porous basement 1 for layer 3 that generates heat firmly combines on porous basement 1, improves layer 3 working property's that generates heat stable reliability, prolongs atomizing core's life. In some of these embodiments, the thin film deposition process may be, but is not limited to, a magnetron sputtering process among thin film deposition processes.
In some embodiments, the transition layer 2 is deposited by a magnetron sputtering process with a target power density of 3-12W/cm 2 The sputtering pressure is 0.1-0.5 Pa, the sputtering time is 20-100 min, and the thickness of the transition layer 2 is 0.1-1 μm. When the thickness of the transition layer 2 is too thin, the transition layer 2 does not play the roles of reducing the roughness of the surface of the porous substrate 1 and preventing sodium and potassium ions of the porous substrate 1 from diffusing into the heat generating layer 3 under the action of an electric field(ii) a Along with the increase of the thickness of the transition layer 2, the transition layer 2 can gradually reduce the roughness of the surface of the porous substrate 1, gradually prevent sodium ions 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 stress matching of the heating layer 3 and the surface of the porous substrate 1; however, when the thickness of the transition layer 2 is too thick, the stress of the transition layer 2 is greatly increased, so that the microstructure of the transition layer 2 is damaged in the electrifying use process of the atomizing core, and sodium and potassium ions of the porous substrate 1 cannot be prevented by the transition layer 2 from diffusing into the heating layer 3 under the action of an electric field, thereby affecting the stability of the resistance value of the heating layer 3. Therefore, the thickness of the transition layer 2 is set to be 0.1-1 μm, so that the transition layer 2 reduces the roughness of the surface of the porous substrate 1, the transition layer 2 prevents sodium ions and potassium ions of the porous substrate 1 from diffusing into the heat generating layer 3 under the action of an electric field, and the transition layer 2 adjusts the stress matching between the heat generating layer 3 and the surface of the porous substrate 1. Preferably, the thickness of the transition layer 2 is set to be 0.3-0.8 μm, which is beneficial to preventing sodium and potassium ions of the porous substrate 1 from diffusing into the heat generating layer 3 under the action of an electric field while facilitating the reduction of the roughness of the surface of the porous substrate 1.
In some embodiments, the transition layer 2 and the porous substrate 1 have stress values close to each other, so that the transition layer 2 and the porous substrate 1 have better stress matching. In some embodiments, the porous substrate 1 is a porous ceramic, and the transition layer 2 is at least one of an aluminum nitride layer, a silicon nitride layer, a chromium carbide layer, or other ceramic layer.
Referring to fig. 1 and 2 in combination, in some embodiments, the atomizing core further includes a protective layer 4 formed on the heat generating layer 3. In a specific embodiment, a protective layer 4 with a thickness of 0.5 to 3 μm is deposited on the side of the heat generating layer 3 away from the porous substrate 1 by a thin film deposition process. 4 separation aerosol of protective layer forms substrate and outside air and gets into layer 3 that generates heat to avoid generating heat and take place oxidation or carbonization in 3 circular telegram use in the layer, the reinforcing generates heat the oxidation resistance and the anti-carbonization nature on layer 3, and the reinforcing generates heat the stability of 3 resistances on layer, improves the recycling life of atomizing core. In some of these embodiments, the thin film deposition process may be, but is not limited to, magnetron sputtering in a thin film deposition processAnd (5) processing. In some embodiments, the protective layer 4 is deposited by a magnetron sputtering process having a target power density of 3-12W/cm 2 The sputtering pressure is 0.1-0.5 Pa, and the sputtering time is 40-150 min. When the thickness of the protective layer 4 is too thin, the protective layer 4 does not play a role in blocking the aerosol-forming substrate and the external air from entering the heat-generating layer 3; with the increase of the thickness of the protective layer 4, the protective layer 4 can gradually block the aerosol-forming substrate and the outside air from entering the heating layer 3; however, when the thickness of protective layer 4 is too thick, protective layer 4 stress can appear increasing by a wide margin, causes protective layer 4 to suffer destruction in atomizing core circular telegram use microstructure, and protective layer 4 can't the separation aerosol forms matrix and outside air gets into layer 3 that generates heat for the oxidation resistance and the anti carbonization nature of layer 3 that generate heat weaken, influence the stability of layer 3 resistance that generates heat, shorten atomizing core's cycle life. In view of the above, the thickness of the protective layer 4 is set to 0.5 to 3 μm, so that the protective layer 4 blocks the aerosol-forming substrate and the outside air from entering the heat generating layer 3. It is preferable to set the thickness of the protective layer 4 to 0.8 to 1.5 μm to favorably block the aerosol-forming substrate and the outside air from entering the heat-generating layer 3.
In some of these embodiments, the protective layer 4 is chemically stable and structurally dense. In some embodiments, the protective layer 4 is at least 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.
Referring to fig. 2, in some embodiments, the heat generating layer 3 is provided with two exposed portions 41 which are not deposited to form the protective layer 4 and are arranged in pairs, and the exposed portions 41 are used for electrically connecting the power supply device and the heat generating layer 3.
The first embodiment of the invention further provides an atomizer which comprises the atomizing core provided by any one of the embodiments. The atomizer has all the technical characteristics of the atomizing core provided by any one of the above embodiments, so that the atomizer has the same technical effects as the atomizing core.
An embodiment of the present invention further provides an aerosol generating device, where the aerosol generating device includes the atomizing core provided in any one of the above embodiments or the atomizer provided in any one of the above embodiments. Since the aerosol generating device has all the technical characteristics of the atomizing core or the atomizer provided by any one of the above embodiments, the aerosol generating device has the same technical effects as the atomizing core.
The first embodiment of the present invention further provides a method for preparing the atomization core of the atomization core, where the method for preparing the atomization core in the first embodiment of the present invention includes the following steps:
step S1: depositing a transition layer: depositing and forming a transition layer 2 on at least part of the atomizing surface 11 of the porous substrate 1 by a thin film deposition process;
step S2: depositing a heating layer: depositing a heating layer 3 on one surface of the transition layer 2, which is far away from the porous substrate 1, through a thin film deposition process;
and step S3: depositing a protective layer: and depositing a protective layer 4 on one side of the heating layer 3, which is far away from the transition layer 2, by a thin film deposition process.
In the step S1 of depositing the transition layer, the transition layer 2 with a thickness of 0.1 to 1 μm is deposited on at least a part of the atomization 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 heating layer 3 has good continuity and the thickness of the heating layer 3 is convenient to adjust and control. And the transition layer 2 can also prevent sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field, so that the stability of the resistance of the heating layer 3 is enhanced. In addition, transition layer 2 can play and adjust the stress matching on layer 3 and porous basement 1 surface that generates heat, and the reinforcing generates heat the adhesive force between layer 3 and the porous basement 1 for layer 3 that generates heat firmly combines on porous basement 1, improves layer 3 working property's that generates heat stable reliability, prolongs atomizing core's life. Specifically, the thin film deposition process may be, but is not limited to, a magnetron sputtering process among the thin film deposition processes. When the transition layer 2 is formed by deposition through a magnetron sputtering process, the power density of the target material of the magnetron sputtering process is 3-12W/cm 2 The sputtering pressure is 0.1-0.5 Pa, the sputtering time is 20-100 min, and the thickness of the transition layer 2 is 0.1-1 μm. When the thickness of the transition layer 2 is too thin, the transition layer 2 does not function to reduce the roughness of the surface of the porous substrate 1 as described aboveAnd the function of preventing sodium and potassium ions of the porous substrate 1 from diffusing into the heating layer 3 under the action of an electric field; and when the thickness of transition layer 2 is too thick, the 2 stress of transition layer can appear increasing by a wide margin, causes transition layer 2 to suffer destruction in atomizing core circular telegram use microstructure, and the unable sodium of separation porous substrate 1 of transition layer 2, potassium ion diffusion under the electric field effect get into layer 3 that generates heat, influence the stability of layer 3 resistance value that generates heat. Therefore, the thickness of the transition layer 2 is set to be 0.1-1 μm, so that the transition layer 2 reduces the roughness of the surface of the porous substrate 1, the transition layer 2 prevents sodium ions and potassium ions of the porous substrate 1 from diffusing into the heat generating layer 3 under the action of an electric field, and the transition layer 2 adjusts the stress matching between the heat generating layer 3 and the surface of the porous substrate 1. Preferably, the thickness of the transition layer 2 is set to be 0.3-0.8 μm, which is beneficial to preventing sodium and potassium ions of the porous substrate 1 from diffusing into the heat generating layer 3 under the action of an electric field while facilitating the reduction of the roughness of the surface of the porous substrate 1. Specifically, the porous substrate 1 is porous ceramic, and the transition layer 2 is formed by depositing on at least a part of the atomization surface 11 of the porous ceramic through a thin film deposition process, wherein the transition layer 2 is at least any one of an aluminum nitride layer, a silicon nitride layer, a chromium carbide layer or other ceramic layers.
In the step S2 of depositing the heat-generating layer, the heat-generating layer 3 is deposited on the surface of the transition layer 2 away from the porous substrate 1 by a thin film deposition process. Specifically, the heat generating layer 3 is a nichrome layer, and the thickness of the nichrome layer is set to 1 to 5 μm. The nickel-chromium alloy layer has good thermal performance, and the price of the nickel-chromium alloy layer is cheaper than that of noble metal layers such as gold, silver, platinum and palladium layers or noble metal alloy layers such as gold, silver, platinum, gold-platinum, silver-palladium, silver-platinum, palladium-copper and palladium-silver alloy layers. In some more specific embodiments, the heat generating layer 3 is a nichrome layer with a mass ratio of Ni/(Ni + Cr) of 0.2 to 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, so that the purpose of adjusting the resistance value of the heating layer 3 can be achieved by adjusting and controlling the thickness of the heating layer 3. At the same time, in the process of research and developmentThrough a large number of experiments, the inventors found that: when the thickness of the heating layer 3 is too thin, the heating layer 3 with a thin layer structure is loose and has poor continuity, the stability of the resistance value of the heating layer 3 is influenced, and the heating layer 3 is easily oxidized or carbonized at high temperature; the thicker the heating layer 3 is, the more the continuity and compactness of the heating layer 3 with a thin layer structure are increased, so that the oxidation resistance or carbonization resistance of the heating layer 3 is greatly enhanced, and the resistance stability of the heating layer 3 is enhanced. However, when the thickness of the heat generating layer 3 is too thick, on the one hand, the time required for forming the heat generating layer 3 is long, thereby greatly reducing the production efficiency; on the other hand, the larger the stress of the heat generating layer 3 is, the more the microstructure of the heat generating layer 3 is destroyed during the use of the power supply, which affects the stability of the resistance value of the heat generating layer 3. And considering that the resistance of the heating layer 3 is too low, the safety hazard of short circuit overload of the heating layer 3 exists, and the resistance of the heating layer 3 is too high, the required heating power cannot be reached, so the common resistance of the heating layer 3 is 0.8-2 omega. Consider the influence of the thickness of layer 3 that generates heat to the stability of layer 3 resistance that generates heat, and consider the thickness of layer 3 that generates heat and the forward relevance of forming time duration, and the resistance that generates heat commonly used of layer 3 that combines is 0.8 ~ 2 omega, synthesize above-mentioned consideration, layer 3 that generates heat is nichrome layer, nichrome layer's thickness sets up 1 ~ 5 mu m, so that layer 3's that generates heat resistance stability improves, layer 3's that generates heat resistance is in resistance range commonly used, and layer 3's that generates heat formation time is moderate, and then make the resistance stability of atomizing core improve, atomizing core's the power that generates heat is great, atomizing core's atomization effect is good, atomizing core's manufacturing cost is controllable. Specifically, the thin film deposition process may be, but is not limited to, a magnetron sputtering process among the thin film deposition processes. When the heating layer 3 is formed by deposition through a magnetron sputtering process, the heating layer 3 is a nickel-chromium alloy layer, and the power density of the target material of the magnetron sputtering process is 5-15W/cm 2 The sputtering pressure is 0.1-0.3 Pa, and the sputtering time is 30-90 min. Thus, a nichrome layer with the thickness of 1-5 microns is deposited on at least part of the atomizing surface 11 of the porous substrate 1 through a magnetron sputtering process, and the nichrome layer is a heating layer 3.
In the protective layer deposition step S3, a protective layer 4 with a thickness of 0.5-3 μm and a stable chemical property and a compact structure is deposited on a surface of the heating layer 3 away from the porous substrate 1 by a thin film deposition process. Protective layer 4 separation aerosol forms matrix and outside air and gets into layer 3 that generates heat to avoid generating heat 3 circular telegram in-process in taking place oxidation or carbonization, the reinforcing generates heat the oxidation resistance and the anti-carbonization nature of layer 3, and the reinforcing generates heat the stability of layer 3 resistance, improves the cycle life of atomizing core. In some of these embodiments, the thin film deposition process may be, but is not limited to, a magnetron sputtering process among thin film deposition processes. In some embodiments, the protective layer 4 is deposited by a magnetron sputtering process, wherein the target power density of the magnetron sputtering process is 3-12W/cm 2, the sputtering pressure is 0.1-0.5 Pa, and the sputtering time is 40-150 min. When the thickness of the protective layer 4 is too thin, the protective layer 4 does not play a role in blocking the aerosol-forming substrate and the external air from entering the heating layer 3; with the increase of the thickness of the protective layer 4, the protective layer 4 can gradually block the aerosol-forming substrate and the outside air from entering the heating layer 3; however, when the thickness of protective layer 4 is too thick, protective layer 4 stress can appear increasing by a wide margin, causes protective layer 4 to suffer destruction in atomizing core circular telegram use microstructure, and protective layer 4 can't the separation aerosol forms matrix and outside air gets into layer 3 that generates heat for the oxidation resistance and the anti carbonization nature of layer 3 that generate heat weaken, influence the stability of layer 3 resistance that generates heat, shorten atomizing core's cycle life. In view of the above, the thickness of the protective layer 4 is set to 0.5 to 3 μm, so that the protective layer 4 blocks the aerosol-forming substrate and the outside air from entering the heat generating layer 3. The protective layer 4 is preferably set to a thickness of 0.8 to 1.5 μm, which can well block the aerosol-forming substrate and the outside air from entering the heat-generating layer 3. Specifically, the protective layer 4 is at least 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.
It can be understood that, the above atomizing core preparation method mainly includes depositing a conductive material on at least a part of the outer surface of the porous ceramic substrate by using a thin film deposition process to form a heat-generating layer on the porous ceramic substrate, so as to obtain the atomizing core with the heat-generating layer on the surface. In some embodiments, when the transition layer 2 and/or the protective layer 4 are not included, the corresponding film layer forming steps S1, S3 may be omitted accordingly.
In other embodiments, the method for preparing the atomizing core of the atomizing core further comprises the following annealing and aging treatment:
and step S4: and annealing and aging to perform annealing heat treatment on the atomizing core.
In some embodiments, the method for preparing the atomization core of the atomization core further comprises the following steps of electrifying and aging:
step S5: and a power-on aging process is adopted to supply power to the atomization core after annealing heat treatment, and the atomization core after annealing heat treatment generates heat after being powered on so as to perform aging treatment on the microstructure of the heating layer 3.
In the step S4, annealing and aging processes are used to perform annealing heat treatment on the atomizing core with the heating layer 3. The purpose of annealing heat treatment is to eliminate the micro defects of the heating layer 3, promote the growth of crystal grains in the microstructure of the heating layer 3, make the heating layer 3 more compact, thereby improve the stability of the resistance value of the atomizing core in the recycling process, further make the atomizing core generate heat stably with uniform heating and good atomizing effect. In combination with the above-described process of forming the heat generating layer 3, from the viewpoint of thermodynamic conditions, in a certain volume of the heat generating layer 3, the coarser the crystal grains in the heat generating layer 3, the smaller the total grain boundary surface area, and the lower the total surface energy. Since the coarsening of the crystal grains can reduce the surface energy, the heating layer 3 is in a more stable state with lower free energy, and to realize the trend of changing towards the stable direction with lower free energy, the atoms of the conductive material need to have stronger diffusion capability to complete the migration movement of the crystal grain boundary when the crystal grains grow up, and the high-temperature annealing heat treatment makes the condition. Consequently, to have the annealing heat treatment that carries out of the atomizing core that generates heat layer 3, can make the grain growth in the microstructure on layer 3 that generates heat for layer 3 that generates heat is more compact, improves the stability of layer 3 resistance in the circular telegram use, thereby improves the stability of atomizing core resistance in the circular telegram use.
In some embodiments, the temperature of the annealing heat treatment on the heat-generating layer 3 of the atomizing core is 500-800 ℃, and the time of the annealing heat treatment is 5-60 min. In the step S4, the annealing heat treatment process of the atomized core is performed in a protective gas atmosphere. Specifically, the atomization core is placed in a tube furnace for annealing heat treatment, and protective gas is continuously filled into the tube furnace in the atomization core annealing heat treatment process to prevent the heating layer 3 from being oxidized in the atomization core annealing heat treatment process. The shielding gas may be, but is not limited to, nitrogen.
It is understood that the transition layer 2 and the protective layer 4 have the same tendency to change during the annealing heat treatment as the heat generating layer 3. Specifically, from the viewpoint of thermodynamic conditions, in a certain volume of the transition layer 2 or the protective layer 4, the coarser the grains in the transition layer 2 or the protective layer 4, the smaller the total grain boundary surface area, and the lower the total surface energy. The coarsening of the crystal grains can reduce the surface energy, so that the transition layer 2 or the protective layer 4 is in a stable state with lower free energy, and the transition layer 2 or the protective layer 4 needs to have stronger diffusion capability of conductive material atoms to complete the migration movement of crystal grain boundaries when the crystal grains grow up in order to realize the change trend towards the stable state with lower free energy, and the high-temperature annealing heat treatment meets the condition. Therefore, annealing heat treatment is carried out on the transition layer 2 or the protective layer 4 of the atomizing core, so that crystal grains in the microstructure of the transition layer 2 or the protective layer 4 can be promoted to grow, the transition layer 2 or the protective layer 4 is more compact, and the stability of the resistance value of the atomizing core in the recycling process is improved.
In the step S5, the atomized core after the annealing heat treatment is subjected to an energization aging treatment: the atomization core after annealing heat treatment is powered on, the atomization core after annealing heat treatment is powered on to generate heat, and the microstructure of the heating layer 3 is aged to enhance the electrical stability of the heating layer 3. In some specific embodiments, in the atmosphere, a direct-current voltage-stabilizing power supply is adopted to supply power to the heating layer 3 of the atomizing core, the power is 6-8W, and the power-on time is 1-20 min. The aim of carrying out electrifying aging treatment on the atomizing core is to improve the stability of the resistor in the electrifying use process of the atomizing core.
Compared with the prior art, the atomization core preparation method in the first embodiment of the invention adopts the annealing and aging process to carry out annealing heat treatment on the heating layer 3 of the atomization core, so that grains in the microstructure of the heating layer 3 grow up, the heating layer 3 is more compact, and the micro defects of the heating layer 3 are reduced; then, the atomized core after the annealing heat treatment is subjected to energization heat generation treatment to further age the microstructure of the heat generation layer 3. Like this, atomizing core can improve and improve the stability that generates heat layer 3 resistance after annealing thermal treatment and circular telegram ageing treatment, has strengthened the electrical stability that generates heat layer 3, and then makes layer 3 that generates heat more even, prevents that atomizing core from appearing the phenomenon that local temperature is too high, can form the substrate to the aerosol and have good atomization effect.
It should be noted that in the first embodiment of the present invention, the atomization core having the heat generation layer 3 is subjected to annealing heat treatment, and then the atomization core subjected to annealing heat treatment is subjected to electrical aging treatment. The above processing order cannot be changed, which is to simulate the real using atmosphere of the atomizing core, since the electrical aging treatment is generally performed in the atmosphere, and the annealing heat treatment is generally performed in the protective gas atmosphere, if the electrical aging treatment is performed on the atomizing core first, the stability of the protective layer 4 is poor, and the heat generating layer 3 is oxidized or carbonized in the atmosphere, which affects the service life of the heat generating layer 3. Therefore, annealing heat treatment is carried out to the atomizing core that has layer 3 that generates heat under the protective gas atmosphere earlier, make the crystalline grain alligatoring of layer 3 inner structure that generates heat in order to reduce surface energy, thereby make transition layer 2 on the atomizing core, layer 3 and protective layer 4 that generate heat are in more stable, the lower state of free energy, and then make transition layer 2, layer 3 and protective layer 4 generate heat are more compact, reduce transition layer 2, the microcosmic defect of layer 3 and protective layer 4 generates heat, improve transition layer 2, the stability of layer 3 and protective layer 4 generate heat. On one hand, after annealing heat treatment, the stable and compact transition layer 2 can prevent sodium and potassium ions of the porous ceramic substrate 1 from diffusing into the heating layer 3 under the action of an electric field, so that the resistance stability of the heating layer 3 is further improved; on the other hand, after annealing heat treatment, the stable and compact heating layer 3 can enhance the resistance stability of the heating layer 3; on the other hand, after annealing heat treatment, the stable and compact protective layer 4 can isolate the heating layer 3 from the aerosol-forming substrate and oxygen in the air, and improve the oxidation resistance and the carbonization resistance of the heating layer 3, thereby improving the resistance stability of the heating layer 3. Then, the atomization core with the heating layer 3 is subjected to electrifying aging treatment under the atmosphere: and the microstructure of the transition layer 2, the heating layer 3 and the protective layer 4 is subjected to aging treatment, so that the resistance stability of the heating layer 3 is further improved.
Example two
The atomizing core of the second embodiment differs from the atomizing core of the first embodiment in that:
the atomizing core further comprises two electrodes 5 for electrically connecting the heat generating layer 3 with a power supply device. Referring to fig. 4 and 5, in one embodiment, the electrode 5 is formed on the atomization surface 11 of the porous substrate 1 by a thick film deposition process, and the thickness of the electrode 5 is 20-60 μm. On the one hand, make electrode 5 combine firmly on porous substrate 1, prevent that electrode 5 from taking place to drop under the impact of high temperature high speed aerosol formation matrix fluid, on the other hand, make electrode 5 enough intensity support it and bear the butt action force that comes from the metal bullet needle when being connected with the metal bullet needle electricity, on the other hand, make electrode 5 have sufficient area of contact and be connected with the metal bullet needle electricity, then can conveniently realize the electricity through metal bullet needle and power supply unit and be connected, and then be convenient for generate heat layer 3 and realize the electricity through electrode 5 and power supply unit and be connected.
In some of the embodiments, 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. In some embodiments, the electrode 5 is formed by screen printing a metal paste on the porous substrate 1, drying, and sintering. The metal paste is made of 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.
Referring to fig. 3 and 4, in some embodiments, the electrodes 5 are disposed in pairs and spaced apart in the first region 11a on the atomization surface 11, the heat generating layer 3 covers at least the second region 11b on the atomization surface 11, the second region 11b is a region of the atomization surface 11 outside the first region 11a, such that the first region 11a and the second region 11b are continuous on the atomization surface 11, the heat generating layer 3 includes a heat generating portion 31 of the second region 11b formed on the atomization surface 11 of the porous substrate 1, a first connecting portion 32 formed on at least a portion of the surface of one of the electrodes 5, and a second connecting portion 33 formed on at least a portion of the surface of the other electrode 5, and the first connecting portion 32 and the second connecting portion 33 are respectively connected to the heat generating portion 31. The contact form through face and face will generate heat layer 3 and corresponding electrode 5 electrical property and link to each other, avoid electrode 5 and generate heat layer 3 bad contact to improve the stable reliability to the layer 3 power supply that generates heat.
Referring to fig. 3 and 4, in some embodiments, the electrodes 5 are arranged in pairs and at intervals on the first region 11a of the atomization surface 11, the transition layer 2 is formed on the second region 11b of the atomization surface 11, and the heat generating layer 3 is disposed on a surface of the transition layer 2 facing away from the porous substrate 1. It will be understood that, in this embodiment, the second region 11b is also a region of the atomization surface 11 other than the first region 11a, so that the first region 11a and the second region 11b are continuous regions on the atomization surface 11. The heat generating layer 3 comprises a heat generating part 31 formed on one surface of the transition layer 2, which is far away from the porous substrate 1, a first connecting part 32 formed on at least part of the surface of one electrode 5, and a second connecting part 33 formed on at least part of the surface of the other electrode 5, wherein the first connecting part 32 and the second connecting part 33 are respectively connected with the heat generating part 31. The contact form through face and face will generate heat layer 3 and corresponding electrode 5 electrical property and link to each other, avoid electrode 5 and generate heat layer 3 bad contact to improve the stable reliability to the layer 3 power supply that generates heat.
Referring to fig. 4 and 5, in some embodiments, the thickness of the electrode 5 is greater than the sum of the thicknesses of the transition layer 2, the heating portion 31 and the protective layer 4, a groove 6 may be formed between the two electrodes 5, the transition layer 2, the heating portion 31 and the protective layer 4 are sequentially stacked from bottom to top in the groove 6 from the inner bottom surface of the groove 6, and the transition layer 2, the heating portion 31 and the protective layer 4 are accommodated and positioned in the groove 6 between the two electrodes 5, which is beneficial to enhancing the stability of the transition layer 2, the heating portion 31 and the protective layer 4 combined on the porous substrate 1.
Referring to fig. 4, in one embodiment, the heat generating layer 3 is also at least partially formed on the electrode 5.
Referring to fig. 4, in some embodiments, the first connection portion 32 includes a first side portion 321 extending from the heat generating portion 31 to a side of one of the electrodes 5 and bent along a thickness direction of the electrode 5, the second connection portion 33 includes a second side portion 331 extending from the heat generating portion 31 to a side of the other electrode 5 and bent along the thickness direction of the electrode 5, and the first side portion 321 and the second side portion 331 are respectively combined with corresponding side surfaces of the corresponding electrodes 5. Accessible first lateral part 321 and second lateral part 331 combine with corresponding side of corresponding electrode 5 respectively, and the contact form through face and face will generate heat layer 3 and corresponding electrode 5 electrical property and link to each other, avoids electrode 5 and the layer 3 that generates heat contact failure to improve the reliability and stability to the layer 3 power supply that generates heat.
Referring to fig. 4, in some more specific embodiments, the first connection portion 32 further includes a first combination portion 322 formed on a side of one of the electrodes 5 facing away from the porous substrate 1, the second connection portion 33 further includes a second combination portion 332 formed on a side of the other electrode 5 facing away from the porous substrate 1, a corresponding side of the first combination portion 322 is connected to a corresponding side of the first side portion 321, and a corresponding side of the second combination portion 332 is connected to a corresponding side of the second side portion 331. On one hand, the contact area between the electrode 5 and the heating layer 3 is increased, which is beneficial to improving the stability of the electrode 5 supplying power to the heating layer 3; on the other hand, the contact area between the electrode 5 and the heating layer 3 is increased, so that the contact resistance between the heating layer 3 and the electrode 5 is reduced, and the heating area is favorably concentrated on the heating part 31; on the other hand, the adhesion of the heat generating layer 3 can be enhanced, so that the heat generating layer 3 is more firmly combined on the porous substrate 1 and the electrode 5. Specifically, the atomizing surface 11 in the above embodiment is a plane.
It is understood that the heat generating portion 31, the first connecting portion 32 and the second connecting portion 33 are formed at a time when the heat generating layer 3 is formed, and in a case where the first connecting portion 32 does not include the first bonding portion 322 and the second connecting portion 33 does not include the second bonding portion 332, it is only necessary to mask a surface of the electrode 5 facing 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 on a surface of the electrode 5 facing away from the porous substrate 1.
The second embodiment of the invention also provides an atomizer which comprises the atomizing core provided by any one of the embodiments. The atomizer has all the technical characteristics of the atomizing core provided by any one of the above embodiments, so that the atomizer has the same technical effects as the atomizing core.
An embodiment of the present invention further provides an aerosol generating device, where the aerosol generating device includes the atomizing core provided in any one of the embodiments or the atomizer provided in any one of the embodiments. Since the aerosol generating device has all the technical characteristics of the atomizing core or the atomizer provided by any one of the above embodiments, the aerosol generating device has the same technical effects as the atomizing core.
The second embodiment of the present invention further provides a method for preparing the atomizing core of the atomizing core, and the method for preparing the atomizing core in the second embodiment of the present invention is different from the method for preparing the atomizing core in the first embodiment in that:
the preparation method of the atomization core also comprises the following steps:
step S0: electrode manufacturing: and (3) screen printing the metal slurry on the porous substrate 1 by adopting a screen printing mode, and drying and sintering to form the electrode 5. It will be appreciated that in other embodiments, the electrode 5 may be formed in other ways.
In some embodiments, the porous substrate 1 screen-printed with the electrode 5 is placed in a vacuum chamber, evacuated to 0.003Pa, and ion-cleaned for 2-10 min using a koffman-type ion source before the step of depositing the transition layer.
EXAMPLE III
The atomizing core in example three differs from the atomizing core in example two in that: the atomizing surface 11 is not a plane. Specifically, referring to fig. 6 and 7, a first concave portion 13 and a second concave portion 14 are respectively formed on a surface of the porous substrate 1 in a concave manner, the first concave portion 13 and the second concave portion 14 are arranged at intervals, so that a portion between the first concave portion 13 and the second concave portion 14 forms a convex portion 12, the atomization surface 11 includes a first surface 11c of the convex portion 12 facing away from the porous substrate 1, a second surface 11d of the first concave portion 13 facing away from the porous substrate 1, a third surface 11e of the second concave portion 14 facing away from the porous substrate 1, a first transition surface 11f connecting the first surface 11c and the second surface 11d, and a second transition surface 11g connecting the first surface 11c and the third surface 11 e. One of the electrodes 5 is formed in the first recess 13 by deposition, the other electrode 5 is formed in the second recess 14 by deposition, the heat generating portion 31 is formed on the first surface 11c of the convex portion 12 by deposition, and the upper end surfaces of the two electrodes 5 are higher than the upper end surface of the heat generating portion 31.
Example four
The atomizing core in example four differs from the atomizing core in example three in that: the upper end surfaces of the two electrodes 5 are flush with the lower end surface of the heating layer 3, and the heating layer 3 is a continuous sheet-shaped structural layer formed on the porous substrate 1 and the electrodes 5. Specifically, referring to fig. 8, the heat generating layer 3 includes a heat generating portion 31 formed in the second region 11b on the atomizing surface 11 of the porous substrate 1, a first connecting portion 32 formed on at least a portion of the surface of one of the electrodes 5, and a second connecting portion 33 formed on at least a portion of the surface of the other electrode 5, wherein the first connecting portion 32 and the second connecting portion 33 are respectively connected to the heat generating portion 31. The first connection portion 32 includes a first bonding portion 322 formed on a face of one of the electrodes 5 facing away from the porous substrate 1, and the second connection portion 33 includes a second bonding portion 332 formed on a face of the other electrode 5 facing away from the porous substrate 1. The corresponding side of the first combining portion 322 is connected to the corresponding side of the heat generating portion 31, and the corresponding side of the second combining portion 332 is connected to the corresponding side of the heat generating portion 31. That is, the first connection portion 32 may not include the first side portion 321, the second connection portion 33 may not include the second side portion 331, the first bonding portion 322 of the first connection portion 32 connects one of the electrodes 5 and the heat generating portion 31, respectively, and the second bonding portion 332 of the second connection portion 33 connects the other electrode 5 and the heat generating portion 31, respectively. On one hand, the contact area between the electrode 5 and the heating layer 3 is increased, which is beneficial to improving the stability of the electrode 5 supplying power to the heating layer 3; on the other hand, the contact area between the electrode 5 and the heating layer 3 is increased, so that the contact resistance between the heating layer 3 and the electrode 5 is reduced, and the heating area is favorably concentrated on the heating part 31; on the other hand, the adhesion of the heat generating layer 3 can be enhanced, so that the heat generating layer 3 is more firmly combined on the porous substrate 1 and the electrode 5. Specifically, the atomizing surface 11 in the above embodiment is a plane.
Examples of the experiments
In order that the details of the above-described implementation and operation of the present invention may be clearly understood by those skilled in the art and that the improved performance of the method for producing atomizing cores according to the present invention will be apparent, the following description will be given by way of specific experimental examples illustrating the specific implementation of the method for producing atomizing cores according to the present invention.
Experimental example 1
1) And screen printing silver palladium metal slurry on the porous substrate 1 by adopting a screen printing process, and drying and sintering to form the electrode 5. Wherein the drying temperature of the electrode 5 is 80 ℃, the drying time of the electrode 5 is 20min, and the sintering condition is that the temperature is kept at 910 ℃ for 20min;
2) Placing the porous substrate 1 with the silver-palladium metal electrode 5 printed on the screen mesh into a magnetron sputtering vacuum chamber, vacuumizing to 0.003Pa, and carrying out ion cleaning on the substrate for 5min by adopting a Kaufman type ion source with the ion source power of 200W;
3) And directly depositing a heating layer 3 on the outer surface of the porous substrate 1 subjected to ion cleaning by adopting a magnetron sputtering process. Wherein the mass ratio of Ni/(Ni + Cr) in the used nickel-chromium alloy target is 80%, and the sputtering power density of the nickel-chromium alloy target is 10W/cm 2 The sputtering pressure is 0.3Pa, and the sputtering time is 30min.
The thickness of the heat generating layer 3 deposited on the porous substrate 1 in experimental example 1 was measured by using a step profiler, and the thickness of the heat generating layer 3 was measured to be 1 μm. The atomization core prepared in the experimental example 1 is marked as S-1, and the atomization core S-1, a battery and a smoke cartridge are assembled into an electronic cigarette to be subjected to a simulated smoking test on an electronic cigarette smoking machine. And after the test is finished, taking the atomizing core S-1 out to measure the change of the resistance value. It is apparent from fig. 9 that the resistance of the atomizing core S-1 changes very significantly in the initial period of the test and the subsequent resistance changes significantly in a reduced range in the previous 3000 cycles. Reasons for the apparent change of the atomized core S-1 resistance value at the initial stage of the cycle test are as follows: on one hand, under the high temperature condition, sodium ions and potassium ions in the porous substrate 1 permeate into the heating layer 3 under the action of an electric field, so that the microstructure of the heating layer 3 is changed; on the other hand, the heat generating layer 3 is carbonized or oxidized with oxygen in the aerosol-forming substrate or air under high temperature conditions.
Experimental example 2
Experimental example 2 differs from experimental example 1 in that: the time for magnetron sputtering the heat-generating layer 3 is different, and the sputtering time in the experimental example 2 is 60min, so as to increase the thickness of the heat-generating layer 3 deposited on the porous substrate 1. The thickness of the heat generating layer 3 in experimental example 2 was measured to be 3 μm using a step meter, and the atomizing core prepared in experimental example 2 was marked as S-2. The electronic cigarette is assembled to be a simulated smoking test on an electronic cigarette smoking machine in the same way as in the experimental example 1, and the resistance value change of the atomizing core is measured after the test is finished.
Experimental example 3
Experimental example 3 differs from experimental example 1 in that: the time for magnetron sputtering the heat generating layer 3 is different, and the sputtering time in the experimental example 3 is 90min, so as to increase the thickness of the heat generating layer 3 deposited on the porous substrate 1. The thickness of the heat generating layer 3 in experimental example 3 was measured to be 5 μm using a step meter, and the atomizing core prepared in experimental example 3 was marked as S-3. The electronic cigarette is assembled to be a simulated smoking test on an electronic cigarette smoking machine in the same way as in the experimental example 1, and the resistance value change of the atomizing core is measured after the test is finished.
Experimental example 4
This experimental example differs from experimental example 2 in that: before the heat generating layer 3 is deposited, a mask is adopted to shield the silver palladium metal electrode 5 which is printed on the porous substrate 1 by screen printing, and then the aluminum nitride transition layer 2 is deposited on at least part of the outer surface of the porous substrate 1 to prevent the 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. Wherein the reaction gas is nitrogen, the argon gas is working gas, the gas flow ratio of nitrogen gas/argon gas is 1.2, the sputtering pressure is 0.35Pa, and the sputtering power density of the metallic aluminum target material 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 μm using a step meter. After the deposition of the aluminum nitride transition layer 2, the same process steps as in experimental example 1 were carried out in the presence of nitrogenAnd a heating layer 3 is deposited on one side of the aluminum oxide transition layer 2, which is far away from the porous substrate 1. Meanwhile, the thickness of the heat generating layer 3 in Experimental example 4 was measured to be 3 μm using the same instrument and test method as those in Experimental example 1. And, the atomizing core prepared in experimental example 4 was marked as S-4, and the atomizing core S-4 was subjected to a cycle reliability test and its resistance value was measured in the same manner as in experimental example 1.
Experimental example 5
Experimental example 5 differs from experimental example 4 in that: the time for magnetron sputtering the aluminum nitride transition layer 2 is different, and the sputtering time is 50min. The thickness of the aluminum nitride transition layer 2 in experimental example 5 was measured to be 0.5 μm using a step meter, and the atomizing core prepared in experimental example 5 was marked as S-5. The atomizing core S-5 was subjected to a cycle reliability test in the same manner as in experimental example 1, and its resistance value was measured.
Experimental example 6
Experimental example 6 differs from Experimental example 4 in that: the time for magnetron sputtering the aluminum nitride transition layer 2 is different, and the sputtering time is 100min. The thickness of the aluminum nitride transition layer 2 in experimental example 6 was measured to be 1 μm using a step meter, and the atomizing core prepared in experimental example 6 was marked as S-6. The atomized core S-6 was subjected to a cycle reliability test in the same manner as in experimental example 1, and its resistance value was measured.
Experimental example 7
Experimental example 7 is different from Experimental example 5 in that: an alumina protective layer is deposited on the heating layer 3, namely after the heating layer 3 is deposited in the experimental example 5, the alumina protective layer is continuously deposited on the side, away from the porous substrate 1, of the heating layer 3 by adopting a magnetron sputtering process. Before the aluminum oxide protective layer is subjected to magnetron sputtering, the silver palladium metal electrode 5 which is screen-printed on the porous substrate 1 is shielded by adopting a mask, so that aluminum oxide is prevented from being deposited on the silver palladium metal electrode 5. Specifically, the aluminum oxide protective layer is deposited by adopting a magnetron sputtering process, the reaction gas of magnetron sputtering is oxygen, argon is working gas, the gas flow ratio of oxygen/argon is 1.5, the sputtering pressure is 0.4Pa, and the sputtering power density of the metal aluminum target is 9W/cm 2 The sputtering time is 40min. The thickness of the alumina protective layer in Experimental example 7 was measured to be 0.5 μm using a step meter, and the atomizing core prepared in Experimental example 7 was markedIs S-7. The atomized core S-7 was subjected to a cycle reliability test in the same manner as in experimental example 1, and its resistance value was measured.
Experimental example 8
Experimental example 8 is different from Experimental example 7 in that: the time for magnetron sputtering the alumina protective layer is different, and the sputtering time is 90min. The alumina protective layer in experimental example 8 was measured to have a thickness of 1.5 μm using a step meter, and the atomizing core prepared in experimental example 8 was marked as S-8. The atomized core S-8 was subjected to a cycle reliability test in the same manner as in experimental example 1, and its resistance value was measured.
Experimental example 9
Experimental example 9 is different from Experimental example 7 in that: the time for magnetron sputtering the alumina protective layer is different, and the sputtering time is 150min. The alumina protective layer in experimental example 9 was measured to have a thickness of 3 μm using a step meter, and the atomizing core prepared in experimental example 9 was marked as S-9. The atomized core S-9 was subjected to a cycle reliability test in the same manner as in experimental example 1, and its resistance value was measured.
Experimental example 10
Experimental example 10 is different from Experimental example 8 in that: the atomizing core prepared in experimental example 8 was placed in a tube furnace for annealing heat treatment. Wherein the protective gas in the tube furnace is nitrogen, the annealing temperature is 500 ℃, and the annealing time is 10min. The atomized core after annealing treatment in experimental example 10 was marked as S-10, and the atomized core S-10 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Experimental example 11
Experimental example 11 is different from Experimental example 10 in that: the annealing temperatures were varied and were 700 ℃. The atomized core after annealing treatment in experimental example 11 was marked as S-11, and the atomized core S-11 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Experimental example 12
Experimental example 12 is different from Experimental example 10 in that: the annealing temperature is different, and the annealing temperature is 800 ℃. The atomized core after annealing treatment in experimental example 12 was labeled as S-12, and the atomized core S-12 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Experimental example 13
Experimental example 13 is different from Experimental example 11 in that: the atomizing core prepared in experimental example 11 was subjected to an energization heat-generating aging treatment. The power supply used for the electrifying, heating and aging treatment is a direct-current stabilized power supply, the electrifying power is 5W, the power supply is stopped for 5s after being electrified for 2s, then the power supply is continuously electrified for 2s and stopped for 5s, and 100 cycles are carried out in total. The atomizing core after the energization heating aging treatment in experimental example 13 was designated as S-13, and the atomizing core S-13 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Experimental example 14
Experimental example 14 is different from Experimental example 13 in that: the energization power was 7W. The atomizing core after the energization heating aging treatment in experimental example 14 was labeled as S-14, and the atomizing core S-14 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Experimental example 15
Experimental example 15 is different from Experimental example 13 in that: the energization power was 9W. The atomizing core after the energization heating aging treatment in experimental example 15 was marked as S-15, and the cycle reliability test of the atomizing core S-15 was performed by the same method as in experimental example 1, and the resistance value thereof was measured.
Testing the relevant performance of the atomizing core:
the atomizing cores of the above experimental examples 1 to 15 were subjected to a cycle reliability test, and the resistance values thereof were measured. The test results are shown in table 1 below.
Table 1 table of resistance values of atomized core cycle test in experimental examples 1 to 15
Figure BDA0003273711750000211
Figure BDA0003273711750000221
It should be noted that the resistance to change of the total cycle in table 1 is a difference between the resistance of the test sample after the 3000 th cycle test and the initial resistance of the test sample, and the resistivity to change of the total cycle in table 1 is a ratio of the resistance to change of the test sample to the initial resistance of the test sample. It is 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 resistance value change after the cycle test is reduced and the resistance stability of the test sample in the cycle test is higher.
It should be noted that the cycle test data of the atomizing core S-1 to the atomizing core S-15 in table 1 are data obtained by testing one test sample. The atomization cores S-1 to S-3 have different initial resistance values because the heat generation layers 3 having different thicknesses are provided. In the rest atomizing cores, before the cycle test, the comparison example for controlling the single variation selects a test sample with a closer initial resistance value from a plurality of test samples in the same batch, such as: the atomization cores S-4 and S-6 are controlled to be single variable quantities with different thicknesses of the transition layer 2, and test samples with approximate initial resistance values are selected from a plurality of test samples of the atomization cores S-2 with the thicknesses of 3 mu m of the heating layer 3 in the same batch.
As can be seen from fig. 9 and 11 and table 1, the resistance of the atomizing core S-1 in experimental example 1 changes very obviously in the previous 3000 cycles, and the resistance change value reaches 1.21 Ω and the resistivity change reaches 77.6% in the cycle test. The reason why the resistance value of the atomizing core S-1 in experimental example 1 significantly changed in the cycle test was: on one hand, under the high temperature condition, the sodium ions and the potassium ions in the porous substrate 1 permeate into the heating layer 3 under the action of the electric field, so that the microstructure of the heating layer 3 is changed, and the sodium ions and the potassium ions in the porous substrate 1 permeate into the heating layer 3 under the action of the electric field; on the other hand, the heat generating layer 3 is carbonized or oxidized with oxygen in the aerosol-forming substrate or air under high temperature conditions.
As can be seen from fig. 9, 11 and table 1, the thickness of the heat generating layer 3 of the atomizing core S-1 in experimental example 1 is 1 μm and the initial resistance value thereof is 1.56 Ω, the thickness of the heat generating layer 3 of the atomizing core S-2 in experimental example 2 is 3 μm and the initial resistance value thereof is 1.25 Ω, and the thickness of the heat generating layer 3 of the atomizing core S-3 in experimental example 3 is 5 μm and the initial resistance value thereof is 1.07 Ω, since the thicknesses of the heat generating layers 3 in experimental examples 1 to 3 are respectively different, the corresponding initial resistance values are also different: the larger the thickness of the heat generating layer 3, the lower the initial resistance value thereof. Thus, the initial resistance value of the atomizing core can be adjusted by changing the thickness of the heat generating layer 3.
As can be seen from fig. 11 and table 1, in the atomizing core S-1 of experimental example 1, the thickness of the heat generating layer 3 is 1 μm, the resistance to change in the cycle test is 1.21 Ω, and the resistivity to change is 77.6%, in the atomizing core S-2 of experimental example 2, the thickness of the heat generating layer 3 is 3 μm, the resistance to change in the cycle test is 0.67 Ω, and the resistivity to change is 53.6%, and in the atomizing core S-3 of experimental example 3, the thickness of the heat generating layer 3 is 5 μm, the resistance to change in the cycle test is 0.54 Ω, and the resistivity to change is 50.5%, because the thickness of the heat generating layer 3 having different thicknesses is larger, the resistance change after the cycle test is reduced. The reason is that the heating layer 3 is formed on the porous substrate 1 by a thin film deposition method, 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 discontinuously and loosely distributed, and the heating layer 3 is easily oxidized or carbonized in the using process, so that the stability of the resistance value is influenced. The thicker the heating layer 3 is, the more the heating layer 3 is distributed in a continuous and compact manner, so that the oxidation resistance or carbonization resistance is improved, and the more stable the resistance value is.
As can be seen by combining the test data in fig. 9, fig. 12 and table 1, taking the atomizing core S-2 in experimental example 2 as a comparative example, the resistance change value of the cycle test is 0.67 Ω, the resistivity change is 53.6%, the resistance change value of the atomizing core S-4 in experimental example 4 is 0.53 Ω, the resistivity change is 42.7%, the resistance change value of the atomizing core S-5 in experimental example 5 is 0.4 Ω, the resistivity change is 32.5%, and the resistance change value of the atomizing core S-6 in experimental example 6 is 0.47 Ω, the resistivity change is 37.9%, and the resistance change of the atomizing core in the previous 3000 cycles is smaller than that of the atomizing core S-2 in experimental example 2, which illustrates the arrangement of the aluminum nitride transition layer 2 and improves the resistance stability of the heat generating layer 3 of the atomizing core. The reason is that the aluminum nitride transition layer 2 can reduce the roughness of the surface of the porous substrate 1 and improve the continuity of the heating layer 3, and meanwhile, the aluminum nitride transition layer 2 can also prevent sodium and potassium ions in the porous substrate 1 from permeating into the heating layer 3, so that the aim of improving and improving the resistance stability of the heating layer 3 of the atomizing core is fulfilled.
As can be seen by combining fig. 12 and table 1, taking the atomizing core S-2 in experimental example 2 as a comparative example, the resistance change value in the cycle test is 0.67 Ω and the resistivity change is 53.6%, and in the atomizing cores S-4, S-5 and S-6 in experimental examples 4 to 6, the aluminum nitride transition layer 2 of the atomizing core S-4 in experimental example 4 has a thickness of 0.1 μm, the resistance change value in the cycle test is 0.53 Ω and the resistivity change is 42.7%, and the resistance value stability is improved; the thickness of the aluminum nitride transition layer 2 of the atomizing core S-5 in experimental example 5 was 0.5 μm, the resistance change value in the cycle test was 0.4 Ω, the resistivity change was 32.5%, and the resistance value stability was further improved. The aluminum nitride transition layer 2 of the atomizing core S-6 in experimental example 6 had a thickness of 1 μm, and the resistance value was 0.47 Ω in the cycle test and 37.9% in the cycle test, but the resistance value stability was rather lowered. The aluminum nitride transition layer 2 can prevent sodium and potassium ions in the porous substrate 1 from permeating into the heating layer 3 under an electric field, and the aluminum nitride transition layer 2 has a thickness within a certain range, and the thicker the aluminum nitride transition layer 2 is, the better the blocking effect is. However, as the thickness of the aluminum nitride transition layer 2 is increased to 1 μm, the stress of the aluminum nitride transition layer is greatly increased, so that the microstructure of the heating layer 3 is damaged in the cycle test process, and the stability of the resistance value of the atomization core cycle test is reduced.
As can be seen by combining the test data in fig. 9, fig. 13 and table 1, with the atomizing core S-5 in experimental example 5 as a comparative example, the resistance change value of the cycle test was 0.4 Ω and the resistivity change was 32.5%, the atomizing core S-7 in experimental example 7, after 3000 cycle tests, the resistance change value of the cycle test was 0.34 Ω and the resistivity change was 27%, the atomizing core S-8 in experimental example 8, after 3000 cycle tests, the resistance change value of the cycle test was 0.24 Ω and the resistivity change was 18.9%, the atomizing core S-9 in experimental example 9, after 3000 cycle tests, the resistance change value of the cycle test was 0.29 Ω and the resistivity change was 22.7%, the resistance change of the atomizing core S-7, the atomizing core S-8 and the atomizing core S-9 in experimental examples 7 to 9 was significantly smaller than that of the atomizing core S-5 in experimental example 5, because the aluminum oxide protective layer was provided, the heat generating layer 3 was formed with the substrate and the oxygen in the atomizing core S-9, and the stability of the aerosol used in the heat generating layer was improved, and the stability of the aerosol was improved.
As can be seen from fig. 13 and table 1, in the case where the atomizing core S-5 in experimental example 5 is a comparative example, the resistance change value in the cycle test is 0.4 Ω and the resistivity change is 32.5%, and in the atomizing cores S-7, the atomizing cores S-8 and the atomizing cores S-9 in experimental examples 7 to 9, the thickness of the alumina protective layer of the atomizing core S-7 in experimental example 7 is 0.5 μm, the resistance change value in the cycle test is 0.34 Ω and the resistivity change is 27%, the resistance value stability in the cycle test is improved, and the thickness of the alumina protective layer of the atomizing core S-8 in experimental example 8 is 1.5 μm, the resistance change value in the cycle test is 0.24 Ω and the resistivity change is 18.9%, and the resistance value stability in the cycle test is further improved. The atomized core S-9 of experimental example 9 had an alumina protective layer thickness of 3 μm, a resistance change value of 0.29 Ω in the cycle test, and a resistivity change value of 22.7%, and the resistance value stability in the cycle test was rather lowered. This is because the thicker the alumina protective layer is, the more dense the alumina protective layer is, the better the heat generating layer 3 can be isolated from the aerosol-forming substrate and oxygen in the air within a certain thickness range. However, as the thickness of the aluminum oxide protective layer is increased to 3 μm, the stress of the aluminum oxide protective layer is greatly increased, so that the microstructure of the aluminum oxide protective layer is damaged in the cycle test process, and the stability of the resistance value of the atomization core in the cycle test is reduced.
As can be seen by combining the test data in fig. 9, fig. 14 and table 1, taking the atomizing core S-8 in experimental example 8 as a comparative example, the resistance change value of the cycle test is 0.24 Ω, and the resistivity change is 18.9%, the atomizing core S-10 in experimental example 10, after 3000 cycle tests, the resistance change value of the cycle test is 0.18 Ω, and the resistivity change is 13.5%, the atomizing core S-11 in experimental example 11, after 3000 cycle tests, the resistance change value of the cycle test is 0.13 Ω, and the resistivity change is 9.7%, the atomizing core S-12 in experimental example 12, after 3000 cycle tests, the resistance change value of the cycle test is 0.21 Ω, and the resistivity change is 15.4%, the resistance change of the atomizing core S-10, the atomizing core S-11 and the atomizing core S-12 in experimental example 10 to experimental example 12 is significantly smaller than that of the atomizing core S-8 in experimental example 8, because the annealing heat-generating layer 3 reduces the defects in the transition layer 2, the heat-generating layer 3, and the heat-generating layer 3 increases the stability of the atomizing heat-generating layer.
As can be seen by referring to fig. 14 and the test data in table 1, taking the atomizing core S-8 in experimental example 8 as a comparative example, the resistance value of the atomization core S-8 in the cycle test was 0.24 Ω, and the resistivity of the atomization core S-9 and the atomization core S-11 and the atomization core S-12 in experimental examples 10 to 12, and the resistance value of the atomization core S-10 in experimental example 10 in the cycle test was 0.18 Ω and the resistivity of the atomization core S-10 in experimental example 10 was 13.5%, the resistance value stability of the cycle test of the atomization core S-10 in experimental example 10 was not significantly improved as compared to the resistance value stability of the cycle test of the atomization core S-8 in experimental example 8 which was not annealed and heat-treated, because the temperature of 500 ℃ was too low, and the energy required for grain growth in the microstructure of the heat generating layer 3 was not achieved. In the experimental example 11, the annealing temperature was increased to 700 ℃, the atomizing core S-11 in the experimental example 11 had a resistance change value of 0.13 Ω and a resistivity change of 9.7% in a cycle test, and the resistance stability in the cycle test of the atomizing core S-11 in the experimental example 11 was significantly improved. However, as the annealing temperature is further increased to 800 ℃ in experimental example 12, the atomizing core S-12 in experimental example 12 has a resistance value of 0.21 Ω in cycle test and a resistivity value of 15.4%, and the atomizing core S-12 in experimental example 12 has a resistance stability in cycle test, which is rather low because an excessively high temperature may destroy the microstructure of the transition layer 2, the heat generating layer 3, or the protective layer 4, and affect the stability of the heat generating layer 3 in cycle test.
As can be seen from the test data in fig. 9, fig. 15 and table 1, taking the atomizing core S-11 in experimental example 11 as a comparative example, the resistance change value in the cycle test is 0.13 Ω, and the resistivity change is 9.7%, the atomizing core S-13 in experimental example 13, after 3000 cycles, the resistance change value in the cycle test is 0.1 Ω, and the resistivity change is 6.8%, and the atomizing core S-14 in experimental example 14, after 3000 cycles, the resistance change value in the cycle test is 0.07 Ω, and the resistivity change is 4.8%, and the resistance change of the atomizing core S-13 and the atomizing core S-14 in experimental examples 13 to 14 is significantly smaller than that of the atomizing core S-11 in experimental example 11, which is that the resistance change of the heat generating layer 3 is improved by the energization heat generating aging treatment, and the purpose of improving and enhancing the stability of the resistance in the cycle test of the high heat generating layer 3 is achieved.
As can be seen from the test data in fig. 10, fig. 15 and table 1, the atomizing core S-11 in experimental example 11 was used as a comparative example, the resistance value in cycle test was 0.13 Ω, and the resistivity in cycle test was 9.7%, the atomizing core S-13 in experimental example 13 had a power of 5W for the energization heating aging treatment, the resistance value in cycle test was 0.1 Ω, and the resistivity in cycle test was 6.8%, and the resistance value stability in cycle test of the atomizing core S-13 in experimental example 13 was not significantly improved as compared with the resistance value stability in cycle test of the atomizing core S-11 in experimental example 11 which was not subjected to annealing heat treatment. The reason is that the power of the electrifying heating aging treatment is too low, the heating amount of the heating layer 3 is smaller, the microstructure improvement of the heating layer 3 is smaller, and therefore the stability improvement range of the resistance of the heating layer 3 is small. In the atomizing core S-14 in experimental example 14, the power of the energization heating aging treatment was 7W, the resistance change value in the cycle test was 0.07 Ω, and the resistivity change was 4.8%, which can significantly improve the stability of the cycle resistance of the heating layer 3 of the atomizing core. In the atomizing core S-15 of experimental example 15, the power of the energization heating aging treatment was increased to 9W, the resistance change value in the cycle test was 0.41 Ω, and the resistivity change was 27.7%, but the stability of the cycle resistance of the heat generating layer 3 of the atomizing core was rather lowered. This is because the power of the energization heating aging treatment is too high, and the larger the heat generation amount of the heat generation layer 3 is, the larger the heat generation amount is, the microstructure of the heat generation layer 3 is destroyed by the too large heat generation amount, thereby reducing the stability of the resistance of the heat generation layer 3.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The preparation method of the atomization core is characterized by comprising the following steps:
depositing a conductive material on at least part of the outer surface of the porous ceramic substrate by adopting a thin film deposition process so as to form a heating layer on the porous ceramic substrate and obtain an atomizing core with the heating layer on the surface;
and annealing and aging the atomization core by adopting an annealing and aging process.
2. The method for preparing an atomizing core according to claim 1, characterized in that, in the annealing heat treatment step, the temperature of the annealing heat treatment is 500 to 800 ℃, and the time of the annealing heat treatment is 5 to 60 minutes.
3. The atomization core preparation method according to claim 1, wherein in the annealing heat treatment step, the atomization core annealing heat treatment process is performed in a protective gas atmosphere.
4. The atomization core preparation method of claim 1 further comprising a power-on aging treatment step comprising: and adopting a power-on aging process to supply power to the atomization core after annealing heat treatment, and heating the atomization core after annealing heat treatment after power-on so as to age the microstructure of the heating layer.
5. The atomization core preparation method according to claim 4, wherein in the electrification aging treatment step, the electrification power is 6 to 8W, and the electrification time is 1 to 20 minutes.
6. The method for producing an atomizing core according to claim 4, wherein in the electrification aging treatment step, the electrification aging treatment process of the atomizing core is performed in an atmospheric atmosphere.
7. The method for preparing an atomizing core according to claim 4, wherein in the step of electrifying and aging, the atomizing core is powered by a direct-current voltage-stabilizing power supply.
8. The method for preparing the atomizing core according to any one of claims 1 to 7, characterized in that the conductive material is a nichrome material, the nichrome material is deposited by the thin film deposition process to form a nichrome heating layer, and the deposition thickness of the nichrome heating layer is 1-5 μm.
9. The method of preparing an atomizing core according to claim 8, wherein the mass ratio of Ni/(Ni + Cr) in the nichrome material is 0.2 to 0.9.
10. The atomizing core preparation method according to any one of claims 1 to 7, wherein the porosity of the porous ceramic substrate is 30 to 80%, and the pore diameter of the porous ceramic substrate is 10 to 30 μm.
CN202111109385.1A 2021-09-22 2021-09-22 Atomizing core preparation method Pending CN115836753A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202111109385.1A CN115836753A (en) 2021-09-22 2021-09-22 Atomizing core preparation method
PCT/CN2022/110238 WO2023045583A1 (en) 2021-09-22 2022-08-04 Atomizing core preparation method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202111109385.1A CN115836753A (en) 2021-09-22 2021-09-22 Atomizing core preparation method

Publications (1)

Publication Number Publication Date
CN115836753A true CN115836753A (en) 2023-03-24

Family

ID=85574417

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202111109385.1A Pending CN115836753A (en) 2021-09-22 2021-09-22 Atomizing core preparation method

Country Status (2)

Country Link
CN (1) CN115836753A (en)
WO (1) WO2023045583A1 (en)

Family Cites Families (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008101253A (en) * 2006-10-20 2008-05-01 Ntn Corp Film deposition system
KR100899846B1 (en) * 2007-04-19 2009-05-27 한국기계연구원 A lead-free piezoceramic film and fabrication method thereof
CN205390303U (en) * 2015-12-16 2016-07-27 深圳市欧比斯科技有限公司 Electron cigarette and atomizer and atomizing core thereof
CN106579564B (en) * 2016-12-23 2020-03-31 湘潭大学 Porous heating film and preparation method thereof
CN109527660A (en) * 2019-01-18 2019-03-29 胡雪涛 A kind of electronic cigarette film heating sheets
CN112385898A (en) * 2019-08-13 2021-02-23 彭晓峰 Novel atomizing core

Also Published As

Publication number Publication date
WO2023045583A1 (en) 2023-03-30

Similar Documents

Publication Publication Date Title
CN113826962A (en) Atomizing core, atomizer, aerosol generating device and atomizing core preparation method
CN216059229U (en) Atomizing core, atomizer and aerosol generating device
CN104886775B (en) Electrically heated smoking system for receiving an aerosol-forming substrate
EP3850967A1 (en) Electronic cigarette, atomization assembly, and atomization component for same
EP4023090A1 (en) Electronic baking cigarette utensil and heat generating device thereof
JP2851291B2 (en) Method of manufacturing PTC temperature sensor and PTC temperature sensor element for PTC temperature sensor
US20220295602A1 (en) Flexible heating element, fabrication method therefor, flexible heating assembly thereof, and aerosol generator
CN216059228U (en) Atomizing core, atomizer and aerosol generating device
JP2014501433A (en) Reduced ceramic heating element
WO2023045598A1 (en) Atomizing core, atomizer, aerosol generating device, and atomizing core preparation method
US20230337742A1 (en) Atomizing core, atomizer, aerosol generating device and method for manufacturing atomizing core
US4065370A (en) Method of ion plating a thin metallic strip for flashlamp starting
CN115836753A (en) Atomizing core preparation method
JP4532047B2 (en) Heater circuit, in particular a heater circuit for a sensor, and a method of manufacturing the heater circuit
JP2007066671A (en) Chip type fuse element and its manufacturing method
JPS634321B2 (en)
CN218790577U (en) Heating element and aerosol generating device
CN219422198U (en) Atomizing core, atomizer and aerosol generating device
US20230337743A1 (en) Electronic vaporization device, vaporizer, vaporization core, and preparation method therefor
CN220211949U (en) Atomizing core, atomizer and aerosol generating device
CN217547272U (en) Heating element and electronic atomization device
CN211960905U (en) Embedded heating cigarette heating element
CN219069484U (en) Composite heating film atomization core and atomization device
US20230413908A1 (en) Heating element, vaporizer, and electronic vaporization device
JP2001235442A (en) Gas sensor

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
TA01 Transfer of patent application right
TA01 Transfer of patent application right

Effective date of registration: 20230517

Address after: Room 2207, Building 3, No. 1590 Longjin Road, Xinbei District, Changzhou City, Jiangsu Province, 213000

Applicant after: CHANGZHOU PATENT ELECTRONIC TECHNOLOGY Co.,Ltd.

Address before: Room 401, workshop 6, modern enterprise accelerator, No.24, Gongye East Road, Songshanhu high tech Industrial Development Zone, Dongguan City, Guangdong Province, 523000

Applicant before: Dongguan Vivante Intelligent Technology Co.,Ltd.