CN113826962A - Atomizing core, atomizer, aerosol generating device and atomizing core preparation method - Google Patents
Atomizing core, atomizer, aerosol generating device and atomizing core preparation method Download PDFInfo
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- CN113826962A CN113826962A CN202111109379.6A CN202111109379A CN113826962A CN 113826962 A CN113826962 A CN 113826962A CN 202111109379 A CN202111109379 A CN 202111109379A CN 113826962 A CN113826962 A CN 113826962A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000758 substrate Substances 0.000 claims abstract description 161
- 230000007704 transition Effects 0.000 claims abstract description 141
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910001120 nichrome Inorganic materials 0.000 claims abstract description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052737 gold Inorganic materials 0.000 claims abstract description 12
- 239000010931 gold Substances 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 12
- 239000004332 silver Substances 0.000 claims abstract description 12
- 229910052763 palladium Inorganic materials 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 8
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- 229910000623 nickel–chromium alloy Inorganic materials 0.000 claims description 19
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
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- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 10
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- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 229910001316 Ag alloy Inorganic materials 0.000 claims description 8
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- 238000004519 manufacturing process Methods 0.000 claims description 8
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- 229910001260 Pt alloy Inorganic materials 0.000 claims description 7
- IHWJXGQYRBHUIF-UHFFFAOYSA-N [Ag].[Pt] Chemical compound [Ag].[Pt] IHWJXGQYRBHUIF-UHFFFAOYSA-N 0.000 claims description 7
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- 239000010949 copper Substances 0.000 claims description 7
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- 238000005137 deposition process Methods 0.000 claims description 5
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- 239000011148 porous material Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 claims description 4
- UFGZSIPAQKLCGR-UHFFFAOYSA-N chromium carbide Chemical compound [Cr]#C[Cr]C#[Cr] UFGZSIPAQKLCGR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 4
- 229910003470 tongbaite Inorganic materials 0.000 claims description 4
- CXOWYMLTGOFURZ-UHFFFAOYSA-N azanylidynechromium Chemical compound [Cr]#N CXOWYMLTGOFURZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005304 joining Methods 0.000 claims 4
- 229910001414 potassium ion Inorganic materials 0.000 abstract description 20
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 12
- 239000011734 sodium Substances 0.000 abstract description 12
- 229910000510 noble metal Inorganic materials 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 6
- NPYPAHLBTDXSSS-UHFFFAOYSA-N Potassium ion Chemical compound [K+] NPYPAHLBTDXSSS-UHFFFAOYSA-N 0.000 abstract description 4
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- 238000012360 testing method Methods 0.000 description 104
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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
- 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
- A24F40/40—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
- A24F40/50—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 an atomizing core, an atomizer, an aerosol generating device and a preparation method of the atomizing core. Because the material that the layer that generates heat used is nichrome, its cost is far less than noble metal such as silver, palladium, gold, alright reduce the cost of atomizing core. And, the setting of transition layer not only can reduce the roughness on porous substrate surface for the layer that generates heat has good continuity, is convenient for adjust and control the thickness that generates heat the layer, and the transition layer can also obstruct the diffusion of porous substrate's sodium, potassium ion and get into the layer that generates heat under the electric field effect moreover, and the stability of the layer resistance that generates heat is strengthened.
Description
Technical Field
The invention belongs to the technical field of atomization, and particularly relates to an atomization core, an atomizer, an aerosol generating device and an atomization core preparation method.
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 an embodiment of the present invention is to provide an atomizing core, wherein a transition layer is first coated on at least a portion of an outer surface of a porous substrate, and a heating layer formed by processing a nickel-chromium alloy material is then coated on the transition layer, so that the heating layer has good continuity, the thickness of the heating layer is conveniently adjusted and controlled, the cost of the heating layer is reduced, and the resistance stability of the heating layer is enhanced.
In order to achieve the purpose, the invention adopts the technical scheme that: there is provided an atomizing core comprising:
a porous substrate, at least part of the outer surface of which is formed with an atomising surface for the heated atomisation of an aerosol-forming substrate, the porous substrate having within it a microporous structure for adsorbing and storing an aerosol-forming substrate, the aerosol-forming substrate adsorbed and stored by the porous substrate being transferable to the atomising surface via the microporous structure;
the transition layer is covered on at least part of the atomization surface;
the heating layer is used for heating and atomizing aerosol to form a matrix after being electrified, the heating layer is combined on one surface of the transition layer, which is far away from the porous substrate, and the heating layer is a nickel-chromium alloy layer; and
and the protective layer is arranged on one surface of the heating layer, which deviates from the transition layer.
Further, the atomizing core further comprises two electrodes for electrically connecting the heating layer and the power supply device, the electrodes are formed on the atomizing surface through a thick film deposition process, and the electrodes are at least 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.
Further, the protective layer 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.
Further, the thickness of the protective layer is 0.5-3 μm.
Further, the thickness of the heating layer is 1-5 μm.
Further, the transition layer is at least one of an aluminum nitride layer, a silicon nitride layer, a chromium nitride layer and a chromium carbide layer.
Further, the thickness of the transition layer is 0.1-1 μm.
Further, the electrodes are arranged in pairs and at intervals in a first area on the atomization surface, the transition layer covers a second area on the atomization surface, the second area is an area on the atomization surface outside the first area, so that the first area and the second area are continuous areas on the atomization surface, and the thickness of the electrodes is larger than the sum of the thickness of the heating layer and the thickness of the transition layer.
Furthermore, a groove is formed between the two electrodes, the transition layer, the heating part of the heating layer and the protective layer are sequentially stacked from bottom to top from the inner bottom surface of the groove, and the thickness of the electrodes is greater than the sum of the thicknesses of the transition layer, the heating part and the protective layer.
Further, the heat generating layer includes a heat generating portion formed in the second region, a first connecting portion formed on at least a partial surface of one of the electrodes, and a second connecting portion formed on at least a partial surface of the other of the electrodes, and the first connecting portion and the second connecting portion are respectively connected to the heat generating portion.
Further, the first connecting portion includes a first connecting portion formed on a surface of one of the electrodes facing away from the porous substrate, the second connecting portion includes a second connecting portion formed on a surface of the other of the electrodes facing away from the porous substrate, a corresponding side of the first connecting portion is connected to a corresponding side of the heat generating portion, and a corresponding side of the second connecting portion is connected to a corresponding side of the heat generating portion.
Further, the thickness of the electrode is 20-60 mu m.
Based on the above problems in the prior art, it is a second object of the embodiments of the present invention to provide an atomizer having an atomizing core provided in any of the above aspects.
In order to achieve the purpose, the invention adopts the technical scheme that: an atomizer is provided, which comprises the atomizing core provided by any scheme above.
Based on the above problems in the prior art, it is a further object of the embodiments of the present invention to provide an aerosol generating device having an atomizing core or an atomizer provided in any of the above aspects.
In order to achieve the purpose, the invention adopts the technical scheme that: there is provided an aerosol generating device comprising the atomizing wick or the atomizer provided in any of the above aspects.
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 atomizing core, the atomizer and the aerosol generating device in the embodiment of the invention, the atomizing core is provided with the transition layer on the atomizing surface, and then the heating layer formed by processing the nickel-chromium alloy material is arranged on the transition layer, so that the transition layer is arranged between the heating layer and the porous substrate at intervals. Because the material that the layer that generates heat used is nichrome, its cost is far less than noble metal such as silver, palladium, gold, alright reduce the cost of atomizing core. And, the setting of transition layer not only can reduce the roughness on porous substrate surface for the layer that generates heat has good continuity, is convenient for adjust and control the thickness that generates heat the layer, and the transition layer can also obstruct the diffusion of porous substrate's sodium, potassium ion and get into the layer that generates heat under the electric field effect moreover, and the stability of the layer resistance that generates heat is strengthened. In addition, the transition layer can play and adjust the nichrome layer that generates heat and the stress matching on porous substrate surface, strengthens the nichrome and generates heat the adhesive force between layer and the porous substrate, improves the reliable and stable nature of layer working property that generates heat, prolongs atomizing core's life.
Based on the above problems in the prior art, it is a fourth object of the embodiments of the present invention to provide a method for preparing an atomizing core.
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 transition layer: depositing a transition layer on at least part of the atomization surface of the porous substrate by a thin film deposition process;
depositing a heating layer: depositing a heating layer on one surface of the transition layer, which is far away from the porous substrate, by a thin film deposition process, wherein the heating layer is a nickel-chromium alloy layer;
depositing a protective layer: and depositing to form a protective layer on one surface of the heating layer, which is far away from the transition layer, by a thin film deposition process.
Optionally, in the nichrome material of the heating layer, the mass ratio of Ni/(Ni + Cr) is 0.2-0.9.
Optionally, the porosity of the porous substrate is 30% -80%, and the pore diameter of the porous 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 atomizing core, the transition layer is formed on the atomizing surface in a film deposition mode, the heating layer is formed on the surface, away from the porous ceramic matrix, of the transition layer through a film deposition process, the protective layer is formed on the heating layer through a film deposition process, and the heating layer is a metal layer formed by processing a nickel-chromium alloy material. Because the material that the layer that generates heat used is nichrome, its cost is far less than noble metal such as silver, palladium, gold, alright reduce the cost of atomizing core. And, the setting of transition layer not only can reduce the roughness on porous substrate surface for the layer that generates heat has good continuity, is convenient for adjust and control the thickness that generates heat the layer, and the transition layer can also obstruct the diffusion of porous substrate's sodium, potassium ion and get into the layer that generates heat under the electric field effect moreover, and the stability of the layer resistance that generates heat is strengthened. Simultaneously, the transition layer can play the stress matching of adjusting nichrome alloy layer and porous substrate surface that generates heat, strengthens the adhesion force between nichrome alloy layer and the porous substrate that generates heat, and the protective layer prevents effectively that nichrome alloy layer that generates heat from taking place carbonization or oxidation, improves the reliability and stability of layer working property that generates heat, prolongs atomizing core's life. In addition, the atomizing core processed by the atomizing core preparation method in the embodiment of the invention has larger heating area and more uniform heating, and the phenomenon of overhigh local temperature can not occur.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions 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 it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
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 comparison graph of resistance values of the atomization cores 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:
1-a porous 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-groove.
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 capillary adsorption microporous structure 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 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, and the mass ratio of Ni/(Ni + Cr) is 0.2-0.9. According to the resistance calculation formula, the thickness of the heating layer 3 determines the resistance value of the heating layer 3, the thinner the heating layer 3 is, the larger the resistance value is, and the thicker the heating layer 3 is, the smaller the resistance value is, 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, so that the stability of the resistance value of the heating layer 3 is affected, 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 potential safety hazard of short circuit overload of the heating layer 3 exists, and the resistance of the heating layer 3 is too high, the problem that the required heating power cannot be reached is solved, 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 common resistance of the heat generating layer 3 being 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 nichrome layer, nichrome layer's thickness sets up to 1 ~ 5 mu m to make the resistance stability who generates heat layer 3 improve, generate heat layer 3's resistance and be in resistance range commonly used, and generate heat layer 3's formation time 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, thin film depositionThe 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/cm2The sputtering pressure is 0.1-0.3 Pa, and the sputtering time is 30-90 min. Thus, a nickel-chromium alloy layer with the thickness of 1-5 mu m is deposited and formed on at least part of the atomizing surface 11 of the porous substrate 1 through a magnetron sputtering process, and the nickel-chromium alloy layer forms the heating 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 deposited atoms, and is combined with other small islands to grow up 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 vacant porous substrate 1; 4. merging, growing up and filling: the formation and merging 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 films: 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 a thickness of 0.1-1 μm is deposited on at least part of the atomization surface 11 of the porous substrate 1 by 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, wherein the target power density of the magnetron sputtering process is 3-12W/cm2The 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 cannot 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 heating layer 3 under the action of an electric field; 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 roughness of the surface of the porous substrate 1 is reduced by the transition layer 2, sodium ions and potassium ions of the porous substrate 1 are prevented by the transition layer 2 from diffusing into the heat generating layer 3 under the action of an electric field, and the transition layer 2 adjusts the stress matching of the heat generating layer 3 and the surface of the porous substrate 1. Preferably, the transition will be madeThe thickness of the layer 2 is set to be 0.3-0.8 mu m, so that the roughness of the surface of the porous substrate 1 is reduced, and sodium ions and potassium ions of the porous substrate 1 are prevented from diffusing into the heating layer 3 under the action of an electric field.
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 0.5-3 μm is deposited on the side of the heat generating layer 3 away from the porous substrate 1 by a thin film deposition process. 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/cm2The 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. Synthesize the above-mentioned examinationThe 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. Preferably, the protective layer 4 is 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.
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 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 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 atomizing core of the atomizing core, where the method for preparing the atomizing 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, by a thin film deposition process;
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 0.1-1 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/cm2The 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 cannot 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 heating layer 3 under the action of an electric field; and when the thickness of transition layer 2 is too thick, transition layer 2 stress can appear increasing by a wide margin, causes transition layer 2 to suffer destruction in atomizing core circular telegram use microstructure, and transition layer 2 can't obstruct the diffusion of sodium, the potassium ion of porous substrate 1 and get into layer 3 that generates heat under the electric field effect, influences the stability of layer 3 resistance that generates heat. Therefore, the thickness of the transition layer 2 is set to be 0.1-1 μm, so that the roughness of the surface of the porous substrate 1 is reduced by the transition layer 2, sodium ions and potassium ions of the porous substrate 1 are prevented by the transition layer 2 from diffusing into the heat generating layer 3 under the action of an electric field, and the transition layer 2 adjusts the stress matching of 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, so that the roughness of the surface of the porous substrate 1 is reduced, and simultaneously, the sodium ions and the potassium ions of the porous substrate 1 are prevented from being influenced by an electric fieldDiffused into the heat generating layer 3. 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, 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 heating layer 3 is a nichrome layer, and the thickness of the nichrome layer is set to be 1-5 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, and the mass ratio of Ni/(Ni + Cr) is 0.2-0.9. According to the resistance calculation formula, the thickness of the heating layer 3 determines the resistance value of the heating layer 3, the thinner the heating layer 3 is, the larger the resistance value is, and the thicker the heating layer 3 is, the smaller the resistance value is, 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, so that the stability of the resistance value of the heating layer 3 is affected, 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 safety hazard of short-circuit overload of the heating layer 3 exists when the resistance of the heating layer 3 is too low, and the safety hazard of short-circuit overload of the heating layer 3 exists when the resistance of the heating layer 3 is too highThe required heating power, 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 correlation when forming time, and the resistance that commonly uses of layer 3 that combines to generate heat is 0.8 ~ 2 omega, synthesize the above-mentioned consideration, layer 3 that generates heat is nichrome layer, nichrome layer's thickness sets up to 1 ~ 5 mu m, so that the resistance stability of layer 3 that generates heat improves, the resistance of layer 3 that generates heat is in the resistance range that commonly uses, and the formation time of layer 3 that generates heat is moderate, and then make the resistance stability of atomizing core improve, atomizing core's the power of generating heat is great, atomizing core's atomizing 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 a target material of the magnetron sputtering process is 5-15W/cm2The sputtering pressure is 0.1-0.3 Pa, and the sputtering time is 30-90 min. Thus, a nickel-chromium alloy layer with the thickness of 1-5 mu m is deposited on at least part of the atomizing surface 11 of the porous substrate 1 through a magnetron sputtering process, and the nickel-chromium alloy 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 dense structure is deposited on a surface of the heat generating 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 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. Preferably, the protective layer 4 is 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:
step S4: and annealing and aging to perform annealing heat treatment on the atomizing core.
In some embodiments, the method for preparing an atomizing core of the atomizing core further comprises:
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 above step S4, the atomized core with the heat generating layer 3 is subjected to annealing heat treatment by using an annealing aging process. 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 stable state with lower free energy, and to realize the trend of changing to the stable state with lower free energy, the atoms of the conductive material need to have stronger diffusion capacity so as to complete the migration movement of the crystal grain boundary when the crystal grains grow, and the high-temperature annealing heat treatment is just making the condition. Therefore, the atomizing core with the heating layer 3 is subjected to annealing heat treatment, crystal grains in the microstructure of the heating layer 3 can be promoted to grow, the heating layer 3 is more compact, the stability of the resistance of the heating layer 3 in the electrifying use process is improved, and the stability of the resistance of the atomizing core in the electrifying use process is improved.
In some embodiments, the temperature of the annealing heat treatment of 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 step S4, the atomized core annealing heat treatment process 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 thermodynamic point of view, 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, the transition layer 2 or the protective layer 4 of the atomizing core is subjected to annealing heat treatment, so that 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 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 an atmospheric atmosphere, the heating layer 3 of the atomizing core is powered by a direct-current voltage-stabilizing power supply, 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 in example two differs from the atomizing core in example one 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 to 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 is 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 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 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, before the step of depositing the transition layer, the porous substrate 1 screen-printed with the electrode 5 is placed in a vacuum chamber, vacuum is applied to 0.003Pa, and the porous substrate 1 is ion-cleaned with a koffman type ion source for 2-10 min.
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 one 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 atomizing 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 20 min;
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/cm2The sputtering pressure is 0.3Pa, and the sputtering time is 30 min.
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 atomizing core prepared in the experimental example 1 is marked as S-1, and the atomizing core S-1, a battery and a cartridge are assembled into an electronic cigarette to be subjected to 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, the sodium ions and the 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 was varied, and the sputtering time in experimental example 2 was 60min 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 metal aluminum target material is 8W/cm2The sputtering time is 20 min. 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 aluminum nitride transition layer 2 is deposited, the same process steps as those in experimental example 1 are adopted, and the heating layer 3 is continuously deposited on the surface of the aluminum nitride 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 50 min. 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 atomized 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 100 min. 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/cm2The sputtering time is 40 min. The alumina protective layer in experimental example 7 was measured to have a thickness of 0.5 μm using a step meter, and the atomizing core prepared in experimental example 7 was marked as 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 90 min. 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 150 min. 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 10 min. 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 electrifying is continued 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 labeled as S-15, and the atomizing core S-15 was subjected to the cycle reliability test and the resistance value thereof was measured in the same manner as in experimental example 1.
Testing the relevant performance of the atomizing core:
the atomizing cores in the above experimental examples 1 to 15 were subjected to a cycle reliability test, respectively, and their resistance values 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
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 mode, if the surface roughness of the porous substrate 1 is larger, and the heating layer 3 is thinner, the heating layer 3 is distributed in a discontinuous and loose shape, and the heating layer 3 is easily oxidized or carbonized in the using process to influence the stability of the resistance value. 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 from 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 was 0.67 Ω and the resistivity change was 53.6%, and in the atomizing cores S-4, the atomizing cores S-5 and the atomizing cores S-6 in experimental examples 4 to 6, the aluminum nitride transition layer 2 of the atomizing core S-4 in experimental example 4 had a thickness of 0.1 μm, the resistance change value in the cycle test was 0.53 Ω and the resistivity change was 42.7%, and the resistance value stability was 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 reason is that 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 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 referring to fig. 9, 13 and the test data in table 1, with the atomizing core S-5 in experimental example 5 as a comparative example, the resistance change value in 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 cycles, the resistance change value in the cycle test was 0.34 Ω and the resistivity change was 27%, the atomizing core S-8 in experimental example 8, after 3000 cycles, the resistance change value in 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 cycles, the resistance change value in the cycle test was 0.29 Ω and the resistivity change was 22.7%, and 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 clearly smaller than the atomizing core S-5 in experimental example 5, this is because the setting of aluminium oxide protective layer makes layer 3 that generates heat and aerosol formation matrix and the oxygen in the air keep apart, avoids generating heat in the long-term use layer 3 by high temperature carbonization and oxidation and influence the stability of resistance value to improve atomizing core's layer 3 that generates heat's resistance stability, and improve atomizing core's cycle life.
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 referring to fig. 9, 14 and the test data in table 1, with the atomizing core S-8 in experimental example 8 as a comparative example, the resistance change value in the cycle test was 0.24 Ω and the resistivity change was 18.9%, the atomizing core S-10 in experimental example 10, after 3000 cycles, the resistance change value in the cycle test was 0.18 Ω and the resistivity change was 13.5%, the atomizing core S-11 in experimental example 11, after 3000 cycles, the resistance change value in the cycle test was 0.13 Ω and the resistivity change was 9.7%, the atomizing core S-12 in experimental example 12, after 3000 cycles, the resistance change value in the cycle test was 0.21 Ω and the resistivity change was 15.4%, and the resistance change of the atomizing core S-10, the atomizing core S-11 and the atomizing core S-12 in experimental examples 10 to 12 was significantly smaller than the atomizing core S-8 in experimental example 8, the annealing heat treatment can reduce the micro defects of the transition layer 2, the heating layer 3 and the protective layer 4, so that the crystal grains in the microstructure of the heating layer 3 grow up, the heating layer 3 is more compact, and the stability of the resistance of the heating layer 3 of the atomizing core in the cycle test is improved.
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 atomized core S-11 in the experimental example 11 had a resistance change value of 0.13 Ω and a resistivity change value of 9.7% in the cycle test, and the atomized core S-11 in the experimental example 11 had a significantly improved resistance stability in the cycle test. 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, with the atomizing core S-11 of experimental example 11 as a comparative example, the resistance change value of the cycle test is 0.13 omega, the resistivity change is 9.7 percent, the atomizing core S-13 in the experimental example 13 is tested after 3000 cycles, the resistance change value of the cycle test is 0.1 omega, the resistivity change is 6.8 percent, the atomization core S-14 in the experimental example 14 is tested after 3000 cycles, the resistance change value of the cycle test was 0.07. omega. and the resistivity change was 4.8%, the resistance value changes of the atomizing core S-13 and the atomizing core S-14 in experimental examples 13 to 14 were significantly smaller than that of the atomizing core S-11 in experimental example 11, the electrical stability of the heating layer 3 can be improved by the electrifying heating aging treatment, and the purpose of improving and enhancing the stability of the resistance of the high heating layer 3 in the cycle test is achieved.
As can be seen from the test data in fig. 10, fig. 15 and table 1, with the atomizing core S-11 of experimental example 11 as a comparative example, the resistance value of change in cycle test was 0.13 Ω and the resistivity of change was 9.7%, and with the atomizing core S-13 of experimental example 13, the power of energization heating aging treatment was 5W, the resistance value of change in cycle test was 0.1 Ω and the resistivity of change was 6.8%, and the resistance value stability of cycle test of the atomizing core S-13 of experimental example 13 was not significantly improved as compared to the resistance value stability of cycle test of the atomizing core S-11 of experimental example 11 which was not subjected to annealing heat treatment. This is because the power of the electrification heating aging treatment is too low, the heating amount of the heating layer 3 is small, the microstructure improvement of the heating layer 3 is small, and thus 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 process is too high, and the larger the amount of heat generated by the heat generating layer 3 is, the microstructure of the heat generating layer 3 is destroyed by the excessive amount of heat generated, thereby lowering the stability of the resistance of the heat generating 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 (17)
1. An atomizing core, comprising:
a porous substrate, at least part of the outer surface of which is formed with an atomising surface for the heated atomisation of an aerosol-forming substrate, the porous substrate having within it a microporous structure for adsorbing and storing an aerosol-forming substrate, the aerosol-forming substrate adsorbed and stored by the porous substrate being transferable to the atomising surface via the microporous structure;
the transition layer is covered on at least part of the atomization surface;
the heating layer is used for heating and atomizing aerosol to form a matrix after being electrified, the heating layer is combined on one surface of the transition layer, which is far away from the porous substrate, and the heating layer is a nickel-chromium alloy layer; and
and the protective layer is arranged on one surface of the heating layer, which deviates from the transition layer.
2. The atomizing core according to claim 1, further comprising two electrodes for electrically connecting the heat generating layer and a power supply device, wherein the electrodes are formed on the atomizing surface by a thick film deposition process, and the electrodes are at least 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.
3. The atomizing core of claim 1, wherein the protective layer 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.
4. The atomizing core of claim 1, wherein the protective layer has a thickness of 0.5 to 3 μm.
5. The atomizing core according to claim 1, wherein the heat-generating layer has a thickness of 1 to 5 μm.
6. The atomizing core of claim 1, wherein the transition layer is at least one of an aluminum nitride layer, a silicon nitride layer, a chromium nitride layer, and a chromium carbide layer.
7. The atomizing core of any one of claims 1 to 6, wherein the transition layer has a thickness of 0.1 to 1 μm.
8. The atomizing core of claim 2, wherein the electrodes are arranged in pairs and spaced apart in a first region on the atomizing surface, the transition layer overlies a second region on the atomizing surface that is outside the first region, such that the first and second regions are continuous regions on the atomizing surface, and the thickness of the electrodes is greater than the sum of the thickness of the heat generating layer and the thickness of the transition layer.
9. The atomizing core according to claim 8, wherein a groove is formed between the two electrodes, the transition layer, the heating portion of the heating layer, and the protective layer are sequentially stacked from bottom to top from the inner bottom surface of the groove, and the thickness of the electrode is greater than the sum of the thicknesses of the transition layer, the heating portion, and the protective layer.
10. The atomizing core according to claim 8, wherein the heat-generating layer includes a heat-generating portion formed in the second region, a first connecting portion formed on at least a part of a surface of one of the electrodes, and a second connecting portion formed on at least a part of a surface of the other of the electrodes, and the first connecting portion and the second connecting portion are connected to the heat-generating portion, respectively.
11. The atomizing core according to claim 10, wherein the first connecting portion includes a first joining portion formed on a face of one of the electrodes facing away from the porous substrate, the second connecting portion includes a second joining portion formed on a face of the other of the electrodes facing away from the porous substrate, a corresponding side of the first joining portion is joined to a corresponding side of the heat-generating portion, and a corresponding side of the second joining portion is joined to a corresponding side of the heat-generating portion.
12. The atomizing core of claim 2, wherein the electrode has a thickness of 20 to 60 μm.
13. An atomizer, characterized in that it comprises an atomizing core according to any one of claims 1 to 12.
14. An aerosol generating device comprising an atomising core according to any of claims 1 to 12 or an atomiser according to claim 13.
15. The preparation method of the atomization core is characterized by comprising the following steps:
depositing a transition layer: depositing a transition layer on at least part of the atomization surface of the porous substrate by a thin film deposition process;
depositing a heating layer: depositing a heating layer on one surface of the transition layer, which is far away from the porous substrate, by a thin film deposition process, wherein the heating layer is a nickel-chromium alloy layer;
depositing a protective layer: and depositing to form a protective layer on one surface of the heating layer, which is far away from the transition layer, by a thin film deposition process.
16. The method of manufacturing an atomizing core according to claim 15, wherein the mass ratio of Ni/(Ni + Cr) in the nichrome material of the heat generating layer is 0.2 to 0.9.
17. The method of preparing an atomizing core according to claim 15, wherein the porosity of the porous substrate is 30 to 80%, and the pore diameter of the porous substrate is 10 to 30 μm.
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| PCT/CN2022/111313 WO2023045598A1 (en) | 2021-09-22 | 2022-08-10 | Atomizing core, atomizer, aerosol generating device, and atomizing core preparation method |
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