WO2024245035A1 - 一种雾化芯、雾化器及电子雾化装置 - Google Patents

一种雾化芯、雾化器及电子雾化装置 Download PDF

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Publication number
WO2024245035A1
WO2024245035A1 PCT/CN2024/094269 CN2024094269W WO2024245035A1 WO 2024245035 A1 WO2024245035 A1 WO 2024245035A1 CN 2024094269 W CN2024094269 W CN 2024094269W WO 2024245035 A1 WO2024245035 A1 WO 2024245035A1
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WO
WIPO (PCT)
Prior art keywords
glass
measurement area
atomizer
porous
main element
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2024/094269
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English (en)
French (fr)
Inventor
王建国
肖令荣
南博
唐根初
罗洪梁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenzhen Smoore Technology Ltd
Smoore International Holdings Ltd
Original Assignee
Shenzhen Smoore Technology Ltd
Smoore International Holdings Ltd
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Filing date
Publication date
Application filed by Shenzhen Smoore Technology Ltd, Smoore International Holdings Ltd filed Critical Shenzhen Smoore Technology Ltd
Priority to EP24814234.1A priority Critical patent/EP4721601A1/en
Publication of WO2024245035A1 publication Critical patent/WO2024245035A1/zh
Priority to US19/404,363 priority patent/US20260083169A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • A24F40/10—Devices using liquid inhalable precursors
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/42—Cartridges or containers for inhalable precursors
    • 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
    • A24F40/44—Wicks
    • 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
    • A24F40/48—Fluid transfer means, e.g. pumps
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C11/00—Multi-cellular glass ; Porous or hollow glass or glass particles
    • C03C11/007—Foam glass, e.g. obtained by incorporating a blowing agent and heating
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • C03C3/087—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal containing calcium oxide, e.g. common sheet or container glass
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B3/00—Ohmic-resistance heating
    • H05B3/20—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater
    • H05B3/22—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater non-flexible
    • H05B3/26—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base
    • H05B3/265—Heating elements having extended surface area substantially in a two-dimensional [2D] plane, e.g. plate-heater non-flexible heating conductor mounted on insulating base the insulating base being an inorganic material, e.g. ceramic
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/013—Heaters using resistive films or coatings
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
    • H05B2203/00—Aspects relating to Ohmic resistive heating covered by group H05B3/00
    • H05B2203/021—Heaters specially adapted for heating liquids

Definitions

  • the present application relates to the field of electronic atomization technology, and in particular to an atomization core, an atomizer and an electronic atomization device.
  • the advantage of electronic cigarettes is that they reduce harmful substances such as tar and CO in smoke.
  • the atomization method of electronic cigarettes on the market is mainly resistance heating atomization, which atomizes the electronic cigarette oil through the heat of the atomizer core.
  • the existing atomizer core usually includes a porous matrix and a heating element.
  • the porous matrix usually uses materials with a porous structure such as cotton core and porous ceramics to achieve the function of guiding the atomized medium to the heating element.
  • ceramic materials are usually prepared using materials such as diatomaceous earth.
  • the components of traditional ceramic materials such as diatomaceous earth are complex, resulting in poor strength of the porous matrix of the electronic cigarette, poor thermal shock resistance, and easy local detachment and fracture, which in turn affects its service life.
  • the purpose of the present application is to overcome the defect in the prior art that the porous matrix of the atomizer core has poor strength, which affects its service life, and further provide an atomizer core, an atomizer and an electronic atomization device.
  • the present application provides an atomizer core, the atomizer core comprising a porous substrate and a heating element;
  • the porous substrate is a porous glass-ceramic substrate, and any two measurement areas on the porous glass-ceramic substrate are respectively recorded as a first measurement area and a second measurement area, and in terms of atomic percentage, the main element content of the first measurement area is recorded as Ma at%, and the corresponding main element content of the second measurement area is recorded as Na at%, wherein
  • the length of the measuring area is at least greater than 1 ⁇ m; the main element is an element with a large content in the porous glass ceramic matrix. Elements with an element content of 20 at%.
  • the main element content in the first measurement area is recorded as Ma at%, and the corresponding main element content in the second measurement area is recorded as Na at%, where
  • the main elements include a first main element and a second main element; in terms of atomic percentage, the content of the first main element in the porous glass-ceramic matrix is 55-64 at %; the content of the second main element is 20-36 at %.
  • the first main element is oxygen, and the second main element is silicon;
  • any two measurement areas on the porous glass-ceramic substrate are respectively recorded as the first measurement area and the second measurement area.
  • the O element content in the first measurement area is recorded as Ma at%, and the corresponding O element content in the second measurement area is recorded as Na at%, wherein
  • the Si element content in the first measurement area is recorded as M’at%, and the corresponding Si element content in the second measurement area is recorded as N’at%, wherein
  • the length of the measurement area is at least greater than 1 ⁇ m.
  • the elements in the porous glass-ceramic matrix further include at least one of sodium, magnesium, aluminum and calcium.
  • the average pore size of the porous glass-ceramic matrix is 15-45 ⁇ m.
  • the length of the measurement area is at least twice the average pore diameter.
  • the compressive strength of the porous glass-ceramic matrix is greater than 1.5 MPa;
  • the compressive strength of the porous glass-ceramic matrix is 6-18 MPa.
  • the porous glass-ceramic matrix includes a crystalline phase and an amorphous phase
  • the crystalline phase accounts for more than 50wt%
  • the crystalline phase includes a quartz phase.
  • the measurement area is at least one of circular, elliptical or rectangular.
  • the heating element is a metal heating film.
  • the present application provides an atomizer, wherein the atomizer comprises the atomizer core described above.
  • the present application also provides an electronic atomization device, wherein the atomizer described above in the electronic atomization device further includes a battery assembly.
  • the present application adopts a porous glass ceramic substrate as the porous substrate of the atomizer core, and simultaneously controls the main element content between any two measurement areas of the porous glass ceramic substrate.
  • Any two measurement areas on the porous glass ceramic substrate are respectively recorded as the first measurement area and the second measurement area.
  • the main element content of the first measurement area is recorded as Mat%
  • the corresponding main element content of the second measurement area is recorded as Nat%, wherein
  • FIG1 is a physical picture of the atomizer core of Example 1 of the present application.
  • FIG2 is a physical picture of the porous substrate of the atomizer core of Example 1 of the present application.
  • FIG3 is a SEM image of the porous substrate of the atomizer core of Example 2 of the present application and the measurement area selected in Test Example 1;
  • FIG4 is a selected measurement area of the porous substrate of Example 2 in Test Example 1 of the present application.
  • FIG5 is a schematic structural diagram of the atomizer of the present application.
  • FIG6 is a schematic structural diagram of the electronic atomization device of the present application.
  • ceramic materials are usually prepared using materials such as diatomaceous earth.
  • materials such as diatomaceous earth.
  • the components of traditional ceramic materials such as diatomaceous earth are complex, and the porous matrix prepared therefrom has poor strength and poor thermal shock resistance, and is prone to detachment and breakage, thereby affecting its service life.
  • the present application provides an atomizer core, which includes a porous substrate and a heating element; the porous substrate is a porous glass ceramic substrate, and any two measurement areas on the porous glass ceramic substrate are respectively recorded as a first measurement area and a second measurement area, and in terms of atomic percentage, the main element content of the first measurement area is recorded as Mat%, and the corresponding main element content of the second measurement area is recorded as Mat%.
  • the element content is recorded as N at%, where
  • the overall strength of the prepared porous matrix is uniform and the composition is uniform.
  • the stability of the porous matrix is also stronger, and it is not easy to cause local cracks, damage, etc. due to different components, and its pore structure is easy to control, the oil conduction effect is good, it is not easy to produce smoke stains, and it does not affect the taste. Therefore, the atomizer core prepared by the porous matrix has a longer service life, a better oil conduction effect, and does not affect the taste.
  • the first measurement area and the second measurement area may or may not intersect with each other.
  • the first measurement area and the second measurement area do not intersect with each other.
  • the main element content in the first measurement area is recorded as Ma at%, and the corresponding main element content in the second measurement area is recorded as Na at%, where
  • the main elements include a first main element and a second main element; optionally, in terms of atomic percentage, the content of the first main element in the porous glass-ceramic matrix is 55-64at%; the content of the second main element is 20-36at%.
  • the content of the first main element can be 55at%, 57at%, 59at%, 60at%, 61at%, 63at%, 64at%
  • the content of the second main element can be 20at%, 21at%, 22at%, 24at%, 26at%, 27at%, 28at%, 29at%, 30at%, 31at%, 32at%, 33at%, 34at%, 35at%, 36at%.
  • the first main element is oxygen (O) and the second main element is silicon (Si).
  • any two measurement areas on the porous glass-ceramic substrate are respectively recorded as the first measurement area and the second measurement area.
  • the O element content in the first measurement area is recorded as Ma at%
  • the corresponding O element content in the second measurement area is recorded as Na at%, wherein
  • the Si element content in the first measurement area is recorded as M’at%
  • the corresponding Si element content in the second measurement area is recorded as N’at%, wherein
  • the length of the measuring area is at least greater than 1 ⁇ m.
  • the elements in the porous glass-ceramic matrix also include at least one element of sodium, magnesium, aluminum, and calcium.
  • the elements in the porous glass-ceramic matrix also include at least one element of sodium 2.4-6at%, magnesium 0.13-3.18at%, aluminum 0.23-2.42at%, and calcium 1.35-6at%.
  • the porous glass-ceramic matrix includes a crystalline phase and an amorphous phase, and the crystalline phase accounts for 50wt% or more.
  • the crystalline phase can be selected to account for 50wt%, 55wt%, 60wt%, 65wt%, 66wt%, 70wt%, 75wt%, 80wt%, 85wt%, 90wt%, 95wt%.
  • the crystalline phase includes a quartz phase.
  • the matrix material of the porous glass-ceramic matrix prepared in the present application is essentially glass-ceramic, which has excellent mechanical and thermal properties such as corrosion resistance, high temperature resistance, thermal shock resistance, and adjustable thermal expansion. In particular, it is used in atomization cores. Good corrosion resistance determines its good safety and is not easy to precipitate harmful components; good high temperature resistance and thermal shock resistance determine that it has good mechanical stability and reliability under repeated high temperature shocks.
  • the average pore size of the porous glass-ceramic matrix is 15-45 ⁇ m.
  • the average pore size of the porous glass-ceramic matrix can be 15 ⁇ m, 16 ⁇ m, 17 ⁇ m, 18 ⁇ m, 19 ⁇ m, 20 ⁇ m, 21 ⁇ m, 22 ⁇ m, 23 ⁇ m, 24 ⁇ m, 25 ⁇ m, 26 ⁇ m, 27 ⁇ m, 28 ⁇ m, 29 ⁇ m, 30 ⁇ m, 31 ⁇ m, 32 ⁇ m, 33 ⁇ m, 34 ⁇ m, 35 ⁇ m, 36 ⁇ m, 37 ⁇ m, 38 ⁇ m, 39 ⁇ m, 40 ⁇ m, 41 ⁇ m, 42 ⁇ m, 43 ⁇ m, 44 ⁇ m, 45 ⁇ m.
  • the pore size range is moderate, and it has both the effect of guiding and locking liquid. It should be noted that the pore size of the porous glass-ceramic matrix can also be controlled and adjusted by the selection of raw glass bubbles. Through appropriate screening, raw glass bubbles of the required particle size can be obtained. Through suitable raw glass bubbles and preparation process, the pore structure of the porous glass-ceramic matrix can be controlled.
  • D50 glass ceramic bubble particle size corresponds to the particle size corresponding to the cumulative particle size distribution percentage of glass ceramic bubbles reaching 50%. Its physical meaning is that glass ceramic bubbles with a particle size larger than it account for 50%, and glass ceramic bubbles with a particle size smaller than it also account for 50%. D50 is also called the median diameter or median particle size; similarly, D50 pore size corresponds to the pore size corresponding to the cumulative pore size distribution percentage of the porous glass ceramic matrix reaching 50%. Its physical meaning is that pores with a pore size larger than it account for 50%, and pores with a pore size smaller than it also account for 50%.
  • the length of the measurement area is at least twice the average pore size; for example, the length of the measurement area can be selected to be at least 2 times, 3 times, 5 times, 10 times, 20 times, 30 times, 50 times, 100 times, 150 times, or 200 times the average pore size.
  • the aspect ratios of the selected measurement areas are all less than 2. The inventors have found that the measurement area selected within this range can effectively improve the strength of the matrix by controlling its main content components, while achieving the strength uniformity of the porous matrix.
  • the present application adopts the method of glass bubble sintering to obtain the matrix material, and the composition of the porous matrix is uniform within a specific range, so that its structure can be controlled, and the strength, strength consistency and reliability of the finished product are higher.
  • the compressive strength of the porous glass-ceramic matrix is greater than 1.5 MPa; further optionally, the compressive strength of the porous glass-ceramic matrix is 6-18 MPa.
  • the compressive strength of the porous glass-ceramic matrix can be 6 MPa, 6.1 MPa, 6.3 MPa, 6.5 MPa, 6.6 MPa, 6.7 MPa, 6.8 MPa, 6.9 MPa, 7 MPa, 7.1 MPa, 7.3 MPa, 7.4 MPa, 7.5 MPa, 7.6 MPa, 7.8 MPa, 7.9 MPa, 8 MPa, 8.5 MPa, 9 MPa, 9.5 MPa, 10 MPa, 10.5 MPa, 11 MPa, 11.5 MPa, 12 MPa, 12.5 MPa, 13 MPa, 13.5 MPa, 14MPa, 14.5MPa, 15MPa, 15.5MPa, 16MPa, 16.5MPa, 17MPa, 17.5MPa, 18MPa.
  • the porous glass-ceramic matrix includes a crystalline phase and an amorphous phase, and the crystalline phase accounts for more than 50%.
  • the crystalline phase can be selected to account for 50%, 55%, 60%, 65%, 66%, 70%, 75%, 80%, 85%, 90%, 95%, 99%, 100%.
  • the crystalline phase includes a quartz phase.
  • the porosity in the porous glass-ceramic matrix is 50-90%; for example, the porosity in the porous glass-ceramic matrix can be 50%, 55%, 60%, 65%, 66%, 70%, 75%, 80%, 85%, or 90%.
  • the method for preparing the atomizer core comprises the following steps:
  • step 2) subjecting the green body in step 1) to a first sintering, a second sintering and a third sintering to obtain a porous glass-ceramic matrix;
  • the glass raw material is selected from at least one of glass bubbles and glass powder
  • the binder can be an organic binder; specifically, the binder is selected from at least one of methyl cellulose, hydroxyethyl cellulose, and hydroxypropyl methyl cellulose
  • the lubricant can be an aliphatic hydrocarbon lubricant, such as paraffin, metal stearate; specifically, the lubricant is sodium stearate.
  • the pressure of the extrusion molding in step 1) is 1-40 bar. Most of the glass bubbles do not break during the extrusion molding process, and the single glass bubble maintains a complete spherical shape. Therefore, the extrusion molding pressure can be appropriately adjusted according to the compressive strength of the selected glass bubble.
  • the first temperature of the first sintering in step 2) is at least 200° C., such as 300° C. to 400° C., and/or the first residence time is at least 1 minute, such as 1 to 10 hours. During the sintering process at this temperature, substances such as solvents and binders in the green body are removed.
  • the second temperature of the second sintering is greater than 400°C and less than the softening point of the glass of the glass bubbles; for example, 500°C, 600°C, 700°C, etc., and the second residence time is at least 1 minute, for example, 1 to 10 hours.
  • the second temperature is higher than 400°C and lower than the softening point of the glass of the glass bubbles/glass powder. Its purpose is to keep the original shape of the blank unchanged. At the same time, because the temperature is already higher than 400°C, the glass component in the glass bubbles/glass powder begins to undergo a phase change, and the disordered glass phase partially crystallizes into a crystalline phase within this temperature range.
  • the glass bubbles are transformed into glass ceramic bubbles or the proportion of the crystalline phase in the glass bubbles begins to increase. At the same time, due to this transformation, some glass bubbles begin to break and have at least one opening. Therefore, the sintering time within this temperature range can be appropriately adjusted to adjust the crystallinity of the porous glass ceramics. It can be understood that the raw glass bubbles/glass powder itself can also contain a certain proportion of crystalline phases, which can be Shorten the sintering time in this process.
  • the third temperature of the third sintering is greater than the softening point of the glass.
  • the softening point temperature of the glass is less than 900°C.
  • the third residence time can be at least 1 minute, for example, 1 to 10 hours.
  • the glass component has fluidity, so the adjacent glass-ceramic bubbles are directly bonded to each other, and the glass-ceramic bubbles are bonded to form a porous glass-ceramic matrix of an integral structure; at the same time, because the glass-ceramic bubbles still have crystalline phase components, the crystalline phase components serve as a skeleton so that their morphology does not collapse, and they still maintain a basically complete morphology.
  • the glass-ceramic bubbles further crack to form a large number of openings, which are interconnected to form pores, and the pores extend through the porous glass-ceramic matrix and reach the surface of the porous glass-ceramic matrix.
  • the third temperature is higher than the softening point of the glass of the glass bubble.
  • the glass ceramic bubble is heated to at least the softening temperature of the amorphous glass in the glass ceramic bubble, so that most of the glass ceramic bubbles are opened due to the expansion of the gas in the bubble, and the adjacent glass ceramic bubbles are sintered together by heating to form a bond. From the overall point of view, the bonded open glass ceramic bubbles form pores in the porous glass ceramic matrix, which can be used in atomizers and electronic atomization devices to effectively improve the atomization efficiency and liquid guiding effect.
  • the mass ratio of glass raw material to binder, lubricant and water is (100-200): (10-50): (1-10): (50-150); optionally, the glass raw material is selected from glass bubbles and glass powder; optionally, the mass ratio of glass bubbles to glass powder is (1-100): (0-100).
  • the raw material of the heating element can be at least one of electronic paste (metal paste), heating wire or heating mesh.
  • the electronic paste can be directly coated on the surface of the porous glass-ceramic substrate in a preset shape by silk-screen printing, and sintered at a preset temperature.
  • the sintering temperature can be adaptively adjusted according to the type of bonding phase and metal components in the electronic paste, and the sintering temperature is usually 400-800°C.
  • the heating element can also be evaporated/deposited on the substrate by physical vapor deposition (PVD) or chemical vapor deposition (CVD).
  • PVD physical vapor deposition
  • CVD chemical vapor deposition
  • the metal wire or metal mesh is directly welded/attached to the surface of the substrate.
  • the glass component in the glass bubble may be soda-lime silicate glass, borosilicate glass or other glass.
  • the glass component may include: SiO 2 74-85%, CaO 6.5-10%, B 2 O 3 5-9%, Al 2 O 3 0.4-2%, Fe 2 O 3 0.01-1%, Na 2 O 1-3%, K 2 O 0.1-0.5%.
  • step 1) further includes adding a pore former.
  • the pore former is selected from at least one of starch, polymethyl methacrylate (PMMA), polystyrene (PS), and graphite.
  • the particle size range of the pore former can be 1-150 ⁇ m. It can be understood that the addition of the pore former can further improve the porosity of the porous glass ceramic matrix while ensuring the strength of the raw glass bubble.
  • step 1) further includes a second inorganic material.
  • the second inorganic material can be at least one of clay, talc, silica, and alumina.
  • the melting point or softening point of the above materials is higher than the softening point of the glass in the glass bubble.
  • the particle size range of the pore former can be 1-200 ⁇ m.
  • the mass ratio of glass raw material to binder, lubricant, water, pore former and second inorganic material is (100-200): (10-50): (1-10): (50-150): (0-125): (0-9); optionally, the glass raw material is selected from glass bubbles and glass powder; optionally, the mass ratio of glass bubbles to glass powder is (1-100): (0-100).
  • the present application further provides an atomizer, wherein the atomizer includes the atomizer core described above.
  • the atomizer includes a shell, and a liquid storage tank and an atomization cavity are formed in the shell.
  • the liquid storage tank is used to store liquid atomization medium, and the atomization cavity is used to accommodate the atomization core described above.
  • the atomization core can atomize the liquid atomization medium.
  • the present application further provides an electronic atomization device, which includes the atomizer 1 described above and a battery assembly 2.
  • the battery assembly and the atomizer may be an integrated structure or a detachable structure.
  • the battery assembly is used to power the atomizer according to a preset mode, so that the atomizer atomizes the liquid atomization medium according to the preset mode.
  • the glass bubbles of the present application are made of soda-lime silicate glass, and the following embodiments all use glass bubbles of the same composition.
  • the raw material parameters are shown in Table 1, and the specific implementation is described as follows.
  • This embodiment provides an atomizer core, and a preparation method thereof includes the following steps:
  • step 2) subjecting the green body in step 1) to a first sintering, a second sintering and a third sintering to obtain a porous glass ceramic substrate, wherein the first sintering temperature is 230° C., the first sintering time is 1 hour, the second sintering temperature is 650° C., the second sintering time is 2 hours; the third sintering temperature is 1050° C., the third sintering time is 1 hour; finally, the green body is naturally cooled in the furnace to obtain a porous glass ceramic substrate;
  • step 2) Printing the heating element slurry on the porous glass ceramic substrate in step 2), sintering and forming, the sintering temperature is 620° C., the sintering time is 1 hour, and the atomization core is obtained.
  • the heating element slurry is stainless steel.
  • the porous matrix of the prepared atomizer core is a porous glass ceramic matrix (as shown in FIG. 2 ), and the porous matrix has a pore structure that is interconnected.
  • This embodiment provides an atomizer core, and a preparation method thereof includes the following steps:
  • step 2) subjecting the green body in step 1) to a first sintering, a second sintering and a third sintering to obtain a porous glass ceramic substrate, wherein the first sintering temperature is 230° C., the first sintering time is 1 hour, the second sintering temperature is 650° C., the second sintering time is 2 hours; the third sintering temperature is 1210° C., the third sintering time is 1 hour; finally, the green body is naturally cooled in the furnace to obtain a porous glass ceramic substrate;
  • Step 3) is the same as in Example 1.
  • This embodiment provides an atomizer core, and a preparation method thereof includes the following steps:
  • Step 2) and step 3) are the same as in Example 1.
  • This embodiment provides an atomizer core, and a preparation method thereof includes the following steps:
  • Step 2) and step 3) are the same as in Example 1.
  • This embodiment provides an atomizer core, and a preparation method thereof includes the following steps:
  • Step 2) and step 3) are the same as in Example 1.
  • the porous glass ceramic matrix of the atomizer core of the embodiment of the present application was scanned by SEM and the element content was detected.
  • the element content was detected by energy dispersive spectrometer (EDS).
  • EDS energy dispersive spectrometer
  • the pore size was measured by mercury intrusion method (the test instrument was mercury intrusion instrument).
  • Figures 3 and 4 are respectively the SEM images of Example 2 and the EDS analysis of different measurement areas and different range sizes.
  • two different measurement areas are selected, and the aspect ratios of the selected measurement areas are less than 2, respectively marked as Area 1 (or marked as M) and Area 2 (or marked as N), and the element contents of each measurement area are detected as shown in Table 2.
  • the detection area is a rectangle, and the length of the detection area is 151.17 ⁇ m; the D50 of the raw material particles is 41 ⁇ m, and the average pore size of the finished porous glass-ceramic matrix is 23.07 ⁇ m.
  • the differences in the main elements of Area 1 (or marked as M) and Area 2 (or marked as N) are 1% (oxygen element) and 0% (silicon element), respectively.
  • the results shown in Table 2 are obtained by measuring other embodiments.
  • the measurement area length of region 1 is about 5 ⁇ m, and its width is about 3 ⁇ m; the difference between its main component oxygen content and that of region 2 is 8%, and the difference between another main component silicon and that of region 2 is 28%. Similarly, the difference between region 2 and region 3 is also very significant.
  • the above-mentioned composition difference is much greater than the composition difference in different embodiments in Table 1.
  • composition segregation occurred, but the composition segregation only occurred in a very small range, usually not exceeding the range of a single glass bubble; therefore, when the length/range of each different measurement area is greater than the length/range of a single glass bubble, the difference in its composition will be very small, that is, the composition is uniform and consistent.
  • the difference in its composition will be very large, that is, the composition is uneven and inconsistent, and the reason is that the different smaller areas may actually correspond to different compositions such as the crystal phase or glass phase in the matrix material, and the composition has significant differences.
  • the grain size in glass ceramics is less than 1 ⁇ m; therefore, when the length/range of the measurement area is greater than 1 ⁇ m, several crystalline phase areas and amorphous phase areas can be included in the measurement area in equal proportions, so that the test results of the composition tend to be consistent; that is, the composition of different measurement areas is uniform and consistent.
  • the flow of the liquid phase is usually only carried out in a small range between adjacent/adjacent monomer glass bubbles. Therefore, when the length/range of the measurement area is greater than 2 times the pore size of the matrix, at least several sub-areas with different compositions can be included in equal proportions, and the composition results of different measurement areas tend to be uniform and consistent.
  • the average pore size is used as the length/range standard of the glass ceramic bubbles in the matrix in this application. In the present application, the average pore size of the substrate is about 15-45 ⁇ m, and the corresponding measurement area length/range is greater than 30-90 ⁇ m.
  • the length of the measurement area is its major axis; similarly, when the measurement area is circular, the length of the measurement area is its diameter.
  • the aspect ratio of the measurement area should not be too large, and usually less than 2 can more accurately reflect the composition of the measurement area.
  • the porous glass-ceramic matrix includes a crystalline phase.
  • the crystalline phase includes a quartz phase.
  • the compressive strength test was carried out on the porous glass-ceramic matrix in the above embodiment. Five parallel samples were taken from the same embodiment and tested separately. The test method was referred to GB/T 4740-1999 "Test Method for Compressive Strength of Ceramic Materials". The pore size and porosity of the porous glass-ceramic matrix and other related parameters were measured by mercury intrusion method (the test instrument was a mercury intrusion instrument). The atomizer core in the above embodiment was tested for failure during the preset number of puffs (the preset number of puffs in this application was 500 puffs), and the life span was statistically recorded. The failure mainly included: 1. The resistance of the atomizer core changed significantly abnormally (such as: the resistance increased significantly due to the breakage and shedding of the heating element); 2.
  • the amount of fog was less than half of the initial atomization amount.
  • the above test conditions were 6.5W power, bare chip (not assembled as an atomizer), and each puff process (i.e., each puff) included: puffing for 3s and then pausing for 8s.
  • the test results are shown in Table 4.
  • the inventors analyzed and believed that the overall compressive strength of the porous glass-ceramic matrix is good, and all matrices are greater than 1.5MPa.
  • the porosity corresponding to Example 2 is 77.80%, which is very high and close to 80%, and can still maintain a high compressive strength.
  • the compressive strength is greater than 6Mpa, and the corresponding porosity is greater than 60%.
  • the inventors analyzed and believed that the composition uniformity is extremely high above the range of a single glass bubble or glass powder, so that The overall compressive strength of the matrix is improved, and the strength of each position of the matrix is uniform, without obvious local strength defects, that is, the effect of improving the uniformity of the strength of the porous matrix is achieved.
  • the stability of the porous matrix is also stronger under the condition of thermal shock during the atomization process, and it is not easy to cause local cracks and damage due to different compositions; and there are no heavy metals and other harmful substances that can be precipitated in the composition. Therefore, the service life of the atomizer core is longer, safer and more reliable.

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Abstract

一种雾化芯、雾化器及电子雾化装置，雾化芯包括多孔基体及发热体，多孔基体为多孔玻璃陶瓷基体，多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域主元素含量记为Mat％，第二测量区域相应主元素含量记为Nat％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；测量区域的长度至少大于1μm；主元素为多孔玻璃陶瓷基体中元素含量大于20at％的元素。可有效提升多孔基体的强度，基体的稳定性更优，使用寿命得到有效延长。

Description

一种雾化芯、雾化器及电子雾化装置
相关申请的交叉引用
本申请要求在2023年6月1日提交中国专利局、申请号为202310647629.4、发明名称为“一种雾化芯、雾化器及电子雾化装置”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
技术领域
本申请涉及电子雾化技术领域，具体涉及一种雾化芯、雾化器及电子雾化装置。
背景技术
电子烟作为传统卷烟的良好替代品，其优势在于降低了烟气中的焦油、CO等有害物质。目前市售电子烟的雾化方式主要为电阻加热雾化，通过雾化芯发热使电子烟油雾化。现有的雾化芯通常包括多孔基体及发热体，多孔基体通常采用如棉芯、多孔陶瓷等具有多孔结构的材料来实现将雾化介质导向发热体的作用。
然而，现有技术中，陶瓷材料通常采用如硅藻土等制备，硅藻土等传统陶瓷材料的成分复杂，造成电子烟多孔基体的强度较差，使其抗热冲击性能较差，容易局部脱离、断裂，进而影响其使用寿命。
发明内容
本申请的目的在于克服现有技术中雾化芯其多孔基体的强度较差，影响其使用寿命的缺陷，进而提供一种雾化芯、雾化器及电子雾化装置。
为达到上述目的，本申请采用如下技术方案：
本申请提供一种雾化芯，所述雾化芯包括多孔基体及发热体；
所述多孔基体为多孔玻璃陶瓷基体，所述多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；
所述测量区域的长度至少大于1μm；所述主元素为多孔玻璃陶瓷基体中元素含量大 于20at％的元素。
可选的，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M小于5％和/或|M-N|/N小于5％。
可选的，所述主元素包括第一主元素和第二主元素；以原子百分比计，所述多孔玻璃陶瓷基体中第一主元素的含量为55-64at％；第二主元素的含量为20-36at％。
可选的，所述第一主元素为氧，所述第二主元素为硅；
可选的，所述多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域O元素含量记为M at％，第二测量区域相应O元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；第一测量区域Si元素含量记为M’at％，第二测量区域相应Si元素含量记为N’at％，其中|M’-N’|/M’小于10％和/或|M’-N’|/N’小于10％；所述测量区域的长度至少大于1μm。
可选的，所述多孔玻璃陶瓷基体中的元素还包括钠、镁、铝、钙中的至少一种元素。
可选的，所述多孔玻璃陶瓷基体的平均孔径为15-45μm。
可选的，所述测量区域的长度至少为所述平均孔径的2倍。
可选的，所述多孔玻璃陶瓷基体的抗压强度大于1.5MPa；
可选的，所述多孔玻璃陶瓷基体的抗压强度为6-18MPa。
可选的，所述多孔玻璃陶瓷基体包括晶相和非晶相；
可选的，所述晶相的占比为50wt％以上；
可选的，所述晶相包括石英相。
可选的，所述测量区域为圆形、椭圆形或矩形中的至少一种。
可选的，所述发热体为金属发热膜。
本申请提供一种雾化器，所述雾化器中包括上述所述的雾化芯。
本申请还提供一种电子雾化装置，所述电子雾化装置中上述所述的雾化器，还包括电池组件。
本申请的有益效果：
本申请采用多孔玻璃陶瓷基体作为雾化芯的多孔基体，同时控制多孔玻璃陶瓷基体的任意2个测量区域之间的主元素含量，所述多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；所述测量区域的长度至少大于1μm；所述主元素为多孔玻璃陶瓷基体中元素 含量大于20at％的元素。发明人发现通过控制上述条件可有效提升多孔基体和雾化芯的强度，基体的稳定性更优，其使用寿命得到有效延长。
附图说明
为了更清楚地说明本申请具体实施方式或现有技术中的技术方案，下面将对具体实施方式或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图是本申请的一些实施方式，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1本申请实施例1的雾化芯的实物图；
图2本申请实施例1的雾化芯多孔基体的实物图；
图3本申请实施例2的雾化芯多孔基体的SEM图及其在测试例1所选测量区域；
图4本申请测试例1中对实施例2的多孔基体所选测量区域；
图5本申请雾化器的结构示意图；
图6本申请电子雾化装置的结构示意图；
附图标记：1-雾化器、2-电池组件。
具体实施方式
提供下述实施例是为了更好地进一步理解本申请，并不局限于所述最佳实施方式，不对本申请的内容和保护范围构成限制，任何人在本申请的启示下或是将本申请与其他现有技术的特征进行组合而得出的任何与本申请相同或相近似的产品，均落在本申请的保护范围之内。
实施例中未注明具体实验步骤或条件者，按照本领域内的文献所描述的常规实验步骤的操作或条件即可进行。所用试剂或仪器未注明生产厂商者，均为可以通过市购获得的常规试剂产品。
现有技术中，陶瓷材料通常采用如硅藻土等制备，硅藻土等传统陶瓷材料的成分复杂，其制备的多孔基体强度较差，抗热冲击性能较差，容易产生脱离、断裂，进而影响其使用寿命。
为此，本申请提供一种雾化芯，雾化芯包括多孔基体及发热体；多孔基体为多孔玻璃陶瓷基体，多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主 元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；测量区域的长度至少大于1μm，主元素为多孔玻璃陶瓷基体中元素含量大于20at％的元素。发明人发现通过控制上述条件可有效提升多孔基体和包含该基体的雾化芯的强度，基体的稳定性更优，其使用寿命得到有效延长。此外，制备的多孔基体整体的强度均一，成分均匀，在雾化过程中热冲击情形下，多孔基体的稳定性也更强，不易因为成分不同造成局部出现裂纹、损坏等情况，而且其孔隙结构易控，导油效果好，不易产生烟垢，不影响口感。因此，由该多孔基体制备的雾化芯的使用寿命更长，导油效果更好，不影响口感。
在一个可选的实施方式中，第一测量区域和第二测量区域之间可以交叉也可以不交叉，可选的，第一测量区域和第二测量区域之间不交叉。以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M和/或|M-N|/N小于5％；例如，可以选择的，|M-N|/M和/或|M-N|/N为0.01％、0.1％、0.2％、0.5％、0.7％、0.9％、1％、1.3％、1.4％、1.6％、1.8％、1.9％、2％、2.1％、2.6％、2.8％、2.9％、3％、3.4％、3.6％、3.7％、3.8％、3.9％、4％、4.2％、4.3％、4.5％、4.7％、4.8％、4.9％。发明人发现通过控制其中|M-N|/M和/或|M-N|/N小于5％可进一步提升多孔基体的强度均一性，基体的稳定性更优，其使用寿命得到进一步有效延长。
在一个可选的实施方式中，主元素包括第一主元素和第二主元素；可选的，以原子百分比计，多孔玻璃陶瓷基体中第一主元素的含量为55-64at％；第二主元素的含量为20-36at％。例如，可以选择的，第一主元素的含量为55at％、57at％、59at％、60at％、61at％、63at％、64at％，第二主元素的含量为20at％、21at％、22at％、24at％、26at％、27at％、28at％、29at％、30at％、31at％、32at％、33at％、34at％、35at％、36at％。进一步的，第一主元素为氧(O)，第二主元素为硅(Si)。
在一个可选的实施例中，多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域O元素含量记为M at％，第二测量区域相应O元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；第一测量区域Si元素含量记为M’at％，第二测量区域相应Si元素含量记为N’at％，其中|M’-N’|/M’小于10％和/或|M’-N’|/N’小于10％；测量区域的长度至少大于1μm。
在一个可选的实施方式中，多孔玻璃陶瓷基体中的元素还包括钠、镁、铝、钙中的至少一种元素。可选的，以原子百分比计，多孔玻璃陶瓷基体中的元素还包括钠2.4-6at％、镁0.13-3.18at％、铝0.23-2.42at％、钙1.35-6at％中的至少一种元素。
在一个可选的实施方式中，多孔玻璃陶瓷基体包括晶相和非晶相，晶相占比为 50wt％以上。例如，可以选择的，晶相占比为50wt％、55wt％、60wt％、65wt％、66wt％、70wt％、75wt％、80wt％、85wt％、90wt％、95wt％。进一步的，晶相包括石英相。本申请中所制备的多孔玻璃陶瓷基体的基体材料实质为玻璃陶瓷(Glass-ceramic)，玻璃陶瓷具有耐腐蚀、耐高温、抗热震、热膨胀可调等优异的力学和热学性能，特别是应用于雾化芯当中，耐腐蚀性良好决定了其安全性良好，不易析出有害成分；耐高温和抗热震性好，决定了其在反复的高温冲击下具有良好的机械稳定性和可靠性。
在一个可选的实施方式中，多孔玻璃陶瓷基体的平均孔径为15-45μm。例如，可以选择的，多孔玻璃陶瓷基体的平均孔径为15μm、16μm、17μm、18μm、19μm、20μm、21μm、22μm、23μm、24μm、25μm、26μm、27μm、28μm、29μm、30μm、31μm、32μm、33μm、34μm、35μm、36μm、37μm、38μm、39μm、40μm、41μm、42μm、43μm、44μm、45μm。孔径范围适中，兼具导液和锁液的效果。需要说明的是，多孔玻璃陶瓷基体的孔径同样可以通过原料玻璃泡的选择来进行控制调整，通过适当的筛分，即可得到需要粒径大小的原料玻璃泡，通过合适的原料玻璃泡及制备过程，使得多孔玻璃陶瓷基体的孔隙结构可控。
D50玻璃陶瓷泡粒径对应于玻璃陶瓷泡的累计粒径分布百分数达到50％时所对应的粒径。它的物理意义是粒径大于它的玻璃陶瓷泡占50％，小于它的玻璃陶瓷泡也占50％，D50也叫中位径或中值粒径；类似地，D50孔径对应于多孔玻璃陶瓷基体累计孔径分布百分数达到50％时所对应的孔径，它的物理意义是孔径大于它的孔占50％，小于它的孔也占50％。
在一个可选的实施方式中，测量区域的长度至少为平均孔径的2倍；例如，可以选择的，测量区域的长度至少为平均孔径的2倍、3倍、5倍、10倍、20倍、30倍、50倍、100倍、150倍、200倍。所选测量区域的长宽比均小于2。发明人发现在此范围内所选择的测量区域，通过控制其主含量成分可有效提升基体强度，同时实现多孔基体的强度均一性。本申请采用玻璃泡烧结的方式获得基体材料，多孔基体的成分组成在特定的范围内具有均一性，即可实现使其结构可控，成品的强度、强度一致性和可靠性更高。
在一个可选的实施方式中，多孔玻璃陶瓷基体的抗压强度大于1.5MPa；进一步可选的，多孔玻璃陶瓷基体的抗压强度为6-18MPa。例如，可以选择的，多孔玻璃陶瓷基体的抗压强度为6MPa、6.1MPa、6.3MPa、6.5MPa、6.6MPa、6.7MPa、6.8MPa、6.9MPa、7MPa、7.1MPa、7.3MPa、7.4MPa、7.5MPa、7.6MPa、7.8MPa、7.9MPa、8MPa、8.5MPa、9MPa、9.5MPa、10MPa、10.5MPa、11MPa、11.5MPa、12MPa、12.5MPa、13MPa、13.5MPa、 14MPa、14.5MPa、15MPa、15.5MPa、16MPa、16.5MPa、17MPa、17.5MPa、18MPa。
在一个可选的实施方式中，多孔玻璃陶瓷基体包括晶相和非晶相，晶相的占比为50％以上。例如，可以选择的，晶相的占比为50％、55％、60％、65％、66％、70％、75％、80％、85％、90％、95％、99％、100％。进一步的，晶相包括石英相。
在一个可选的实施方式中，多孔玻璃陶瓷基体中的孔隙率为50-90％；例如，可以选择的，多孔玻璃陶瓷基体中的孔隙率为50％、55％、60％、65％、66％、70％、75％、80％、85％、90％。
下面结合制备方法对本申请进行进一步的说明。
在一些可选的实施方式中，雾化芯的制备方法，包括如下步骤：
1)将玻璃原料与粘结剂、增滑剂、水混合并挤压成型得到坯体；
2)将步骤1)中的坯体经第一烧结、第二烧结和第三烧结，得到多孔玻璃陶瓷基体；
3)将发热体原料制备在步骤2)中的多孔玻璃陶瓷基体上，烧结成型。
在一些可选的实施方式中，步骤1)中：玻璃原料选自玻璃泡、玻璃粉体中的至少一种；粘结剂可以选择有机粘结剂；具体的，粘结剂选自甲基纤维素、羟乙基纤维素、羟丙甲基纤维素中的至少一种；增滑剂可以为脂肪烃类增滑剂，如：石蜡、金属硬脂酸盐；具体的，增滑剂为硬质酸钠。
在一些可选的实施方式中，步骤1)中挤压成型的压力为1-40bar。其中，大部分的玻璃泡在挤压成型过程中不发生碎裂；保持单体玻璃泡完整的球形。因此，可以依据所选择的玻璃泡的抗压强度对挤压成型的压力进行适当的调整。
在一些可选的实施方式中，步骤2)中第一烧结的第一温度是至少200℃，例如300℃至400℃，和/或其中第一停留时间是至少1分钟，例如1至10小时。该温度下的烧结过程中，坯体中溶剂、粘结剂等物质被去除。
在一些可选的实施方式中，第二烧结的第二温度大于400℃且小于玻璃泡的玻璃的软化点；例如500℃、600℃、700℃等，其第二停留时间是至少1分钟，例如1至10小时。第二温度高于400℃且低于玻璃泡/玻璃粉体的玻璃的软化点，其目的在于保持坯体的原有形态不变，同时由于温度已经高于400℃，玻璃泡/玻璃粉体中的玻璃成分开始产生相变，无序的玻璃相在该温度范围内部分结晶为晶相，玻璃泡转变为玻璃陶瓷泡或者玻璃泡中的晶相的比例开始增大。同时，由于这一转变，部分玻璃泡开始破裂具有至少一开口。因此，可以适当的调整在该温度范围内的烧结时间，用于调整多孔玻璃陶瓷的结晶度。可以理解，原料玻璃泡/玻璃粉体中本身也可以含有一定比例的结晶相，可以 缩短在这一过程的烧结时间。
在一些可选的实施方式中，第三烧结的第三温度大于玻璃的软化点。具体的，玻璃的软化点温度小于900℃。第三停留时间可以是至少1分钟，例如1至10小时。该温度下，玻璃成分具有流动性，因此毗邻的玻璃陶瓷泡彼此直接粘结，并使得玻璃陶瓷泡粘结成为一体结构的多孔玻璃陶瓷基体；同时，由于玻璃陶瓷泡仍然具有晶相成分，晶相成分作为骨架使其形态并不发生塌陷，依旧保持基本完整形态。并且，玻璃陶瓷泡进一步开裂形成大量的开口，开口之间相互连通以形成孔隙，孔隙延伸穿过多孔玻璃陶瓷基体并到达多孔玻璃陶瓷基体的表面。
第三温度高于玻璃泡的玻璃的软化点。将玻璃陶瓷泡至少加热到玻璃陶瓷泡中无定形玻璃的软化温度，使得大部分的玻璃陶瓷泡因泡内的气体膨胀而开口，同时加热使得毗邻玻璃陶瓷泡彼此烧结在一起，形成粘结，从整体来看，粘结的开口玻璃陶瓷泡形成多孔玻璃陶瓷基体的孔隙，应用于雾化器、电子雾化装置中可以有效提高雾化效率和导液效果。
在一些可选的实施方式中，玻璃原料与粘结剂、增滑剂、水的质量比为(100-200)：(10-50)：(1-10)：(50-150)；可选的，玻璃原料选自玻璃泡和玻璃粉体；可选的，玻璃泡与玻璃粉体的质量比为(1-100)：(0-100)。
在一些可选的实施方式中，步骤3)中：发热体原料可以为电子浆料(金属浆料)、发热丝或发热网中的至少一种。电子浆料可以直接通过丝印的方式按照预设的外形涂覆于多孔玻璃陶瓷基体的表面，并且在预设温度下烧结成型。烧结温度依据电子浆料中粘结相和金属成分的种类可以进行适应性调整，通常烧结温度为400-800℃。可以选择的，在一些其他的实施方式中，还可以通过物理气相沉积(PVD)或化学气相沉积(CVD)的方式将发热体蒸镀/沉积在基体上。或者，直接将金属丝或金属网焊接/贴附于基体表面。
在一些可选的实施方式中，玻璃泡中玻璃成分可以是钠钙硅酸盐玻璃、硼硅酸盐玻璃或者其他玻璃。具体的，玻璃成分可以包括：SiO2 74-85％、CaO 6.5-10％、B2O3 5-9％、Al2O3 0.4-2％、Fe2O3 0.01-1％、Na2O 1-3％、K2O 0.1-0.5％。
在一些可选的实施方式中，步骤1)中还包括添加成孔剂。可选的，成孔剂选自淀粉、聚甲基丙烯酸甲酯(PMMA)、聚苯乙烯(PS)、石墨中的至少一种。可选的，成孔剂的粒径范围可以为1-150μm。可以理解，成孔剂的加入，可以保证原料玻璃泡强度的情况下，进一步提高多孔玻璃陶瓷基体的孔隙率。
在一些可选的实施方式中，步骤1)中还包括第二无机材料。第二无机材料可以是粘土、滑石、二氧化硅、氧化铝中的至少一种。上述材料的熔点或软化点高于玻璃泡中玻璃的软化点。可选的，成孔剂的粒径范围可以为1-200μm。
在一些可选的实施方式中，玻璃原料与粘结剂、增滑剂、水、成孔剂、第二无机材料的质量比为(100-200)：(10-50)：(1-10)：(50-150)：(0-125)：(0-9)；可选的，玻璃原料选自玻璃泡和玻璃粉体；可选的，玻璃泡与玻璃粉体的质量比为(1-100)：(0-100)。
如图5所示，本申请还提供一种雾化器，所述雾化器中包括上述所述的雾化芯。其中，雾化器包括外壳，外壳内形成储液仓和雾化腔，储液仓用于储存液态的雾化介质，雾化腔用于容置上述的雾化芯。雾化芯可以将液态的雾化介质进行雾化。
如图6所示，本申请还提供一种电子雾化装置，电子雾化装置包括上述所述的雾化器1，还包括电池组件2。电池组件与雾化器可以为一体结构或可拆卸式结构。电池组件用于按预设模式为雾化器供电，使雾化器按照预设模式雾化液体雾化介质。
以下结合具体实施例对本申请作进一步详细描述，这些实施例不能理解为限制本申请所要求保护的范围。
本申请玻璃泡成分采用钠钙硅酸盐玻璃，以下实施例均采用的同一成分的原料玻璃泡。其原料参数请参见表1，具体实施方式如下所述。
实施例1
本实施例提供一种雾化芯，其制备方法，包括如下步骤：
1)将100g玻璃泡与25g羟乙基纤维素、2.5g硬质酸钠、50g水混合并挤压成型得到坯体，成型压力为7bar；
2)将步骤1)中的坯体经第一烧结、第二烧结和第三烧结，得到多孔玻璃陶瓷基体，第一烧结温度230℃，第一烧结时间1小时，第二烧结温度650℃，第二烧结时间2小时；第三烧结温度1050℃，第三烧结时间1小时；最后，随炉自然冷却得到多孔玻璃陶瓷基体；
3)将发热体浆料印刷在步骤2)中的多孔玻璃陶瓷基体上，烧结成型，烧结温度620℃，烧结时间1小时，得到所述雾化芯。其中，发热体浆料为不锈钢。
如图1所示，制备得到的雾化芯，其多孔基体为多孔玻璃陶瓷基体(如图2)，多孔基体具有相互贯通的孔隙结构。
实施例2
本实施例提供一种雾化芯，其制备方法，包括如下步骤：
1)将100g玻璃泡与25g羟乙基纤维素、2.5g硬质酸钠、25g成孔剂、67g水混合并挤压成型得到坯体，成型压力为14bar。
2)将步骤1)中的坯体经第一烧结、第二烧结和第三烧结，得到多孔玻璃陶瓷基体，第一烧结温度230℃，第一烧结时间1小时，第二烧结温度650℃，第二烧结时间2小时；第三烧结温度1210℃，第三烧结时间1小时；最后，随炉自然冷却得到多孔玻璃陶瓷基体；
步骤3)与实施例1相同。
实施例3
本实施例提供一种雾化芯，其制备方法，包括如下步骤：
1)将100g玻璃泡与25g羟乙基纤维素、2.5g硬质酸钠、75g水混合并挤压成型得到坯体，成型压力为24bar。
步骤2)和步骤3)与实施例1相同。
实施例4
本实施例提供一种雾化芯，其制备方法，包括如下步骤：
1)将20g玻璃泡与80g玻璃粉体、25g羟乙基纤维素、2.5g硬质酸钠、50g成孔剂、75g水混合并挤压成型得到坯体，成型压力为13bar。其中，成孔剂为聚甲基丙烯酸甲酯(PMMA)。玻璃粉体内部无空穴的颗粒，玻璃粉体的玻璃种类与玻璃泡相同；玻璃粉体的粒径为1-20μm。
步骤2)和步骤3)与实施例1相同。
实施例5
本实施例提供一种雾化芯，其制备方法，包括如下步骤：
1)将20g玻璃泡与80g玻璃粉体、25g羟乙基纤维素、2.5g硬质酸钠、50g成孔剂、75g水混合并挤压成型得到坯体，成型压力为24bar。其中，成孔剂为聚甲基丙烯酸甲酯(PMMA)。玻璃粉体内部无空穴的颗粒，玻璃粉体的玻璃种类与玻璃泡相同；玻璃粉体的粒径为1-20μm。
步骤2)和步骤3)与实施例1相同。
表1实施例原料玻璃泡参数

测试例1
对本申请实施例雾化芯的多孔玻璃陶瓷基体进行SEM扫描，以及元素含量检测。其中，元素含量采用能谱仪(EDS,Energy Dispersive Spectrometer)进行检测。孔径采用压汞法测量(测试仪器为压汞仪)。
图3和图4分别为实施例2的SEM图及不同测量区域、不同范围大小的EDS分析。如图3所示测量区域，选定两个不同的测量区域，所选测量区域的长宽比均小于2，分别标记为区域1(或者标记为M)和区域2(或者标记为N)，检测其各个测量区域的元素含量如表2所示。其中，以检测区域为矩形，检测区域的长度为151.17μm；原料颗粒的D50为41μm，成品多孔玻璃陶瓷基体的平均孔径为23.07μm。显然，区域1(或者标记为M)和区域2(或者标记为N)的主要元素的差异分别为1％(氧元素)和0％(硅元素)。同理，对其他实施例进行测量得到如表2所示的结果。
表2实施例元素含量
如图4所示，在实施例2所得到的多孔玻璃陶瓷基体中选择不同区域中进行测量。 其中，检测结果如表3所示。
表3实施例2不同区域元素含量
如表3所示，区域1的测量区域长度约为5μm，其宽度约为3μm；其主要成分氧含量与区域2的差异为8％，另一主要成分硅与区域2的差异为28％。同理，区域2与区域3的差异也十分显著。上述的成分差异远大与表1中不同实施例中的成分差异。本申请发明人分析认为，由于本申请玻璃泡或玻璃粉体在烧结过程中产生的相变，因此产生了成分偏析，但成分偏析仅发生在很小的范围内，通常不会超过一个单体玻璃泡的范围；因此，在各个不同的测量区域长度/范围大于一个单体玻璃泡的长度/范围时，其成分组成差异会很小，即显示成分组成均匀、一致。同理，在各个不同的测量区域长度/范围小于一个单体玻璃泡的长度/范围时，其成分组成差异会很大，即显示成分组成不均匀、不一致，其原因就在于，该不同较小的区域实质可能是对应于基体材料中的晶相或玻璃相等不同的组成，成分具有显著的差异。通常，玻璃陶瓷中的晶粒尺寸小于1μm；所以，当测量区域长度/范围大于1μm时，即可在测量区域内同等比例的包括若干晶相区域和非晶相区域，使得成分组成的测试结果趋于一致；即不同测量区域的成分均匀、一致。更进一步，由于本申请中没有形成完全熔融的液体环境，液相的流动通常仅在相邻/毗邻的单体玻璃泡之间的小范围内进行，因此在测量区域长度/范围大于基体孔径的2倍就能至少同等比例的包括若干有成分差异的子区域，其不同测量区域的成分结果就趋于均匀、一致。为了简单描述，本申请中以平均孔径作为基体中玻璃陶瓷泡的长度/范围标准。 本申请中基体的平均孔径约为15-45μm，对应的测量区域长度/范围大于30-90μm即可。需要说明的是，在测量区域为椭圆形的情形下，其测量区域的长度为其长轴；同理，测量区域选择为圆形时，其测量区域的长度为其直径。同时，测量区域的长宽比也不宜过大，通常小于2能较为准确反映该测量区域的成分组成。
其中，如图4中的区域1所示，其微观结构与周围组织差异明显，可见多孔玻璃陶瓷基体中包括了晶相。进一步的，晶相中包括石英相。
测试例2
对上述实施例中的多孔玻璃陶瓷基体进行抗压强度测试，相同实施例取5个平行样品分别测试，测试方法参考GB/T 4740-1999《陶瓷材料抗压强度试验方法》。多孔玻璃陶瓷基体的孔径及孔隙率等相关参数采用压汞法测量(测试仪器为压汞仪)。对上述实施例中的雾化芯在抽吸预设的口数(本申请中的预设口数为500口)，这一过程中测试是否具有失效的情形，并进行统计记录寿命情况，其中失效的情形主要包括：1、雾化芯的阻值显著异常变化(如：发热体断裂、脱落引起的阻值显著增大)；2、出雾量低于初始雾化量的二分之一。上述的测试条件为6.5W功率，裸片(未装配为雾化器)，每一个抽吸过程(即每一口)包括：抽吸3s然后暂停8s。测试结果如表4所示。
表4
如表4所示，发明人分析认为：多孔玻璃陶瓷基体的整体抗压强度较好，所有基体均大于1.5MPa。如实施例2对应的孔隙率为77.80％，孔隙率很高接近80％，依然能保持较高的抗压强度。一些实施例中，抗压强度大于6Mpa，对应的孔隙率大于60％。发明人分析认为，在大于单个玻璃泡或玻璃粉体范围之上，成分均匀性极高，因此，使得 基体的整体抗压强度提升，同时使基体各个位置的强度均匀，没有明显的局部强度缺陷，即实现提高多孔基体的强度均匀性的效果。同时，由于成分均匀，在雾化过程中热冲击情形下，多孔基体的稳定性也更强，不易因为成分不同造成局部出现裂纹、损坏等情况；并且成分中没有可以析出的重金属等有害物质。因此，雾化芯的使用寿命更长、更安全可靠。
显然，上述实施例仅仅是为清楚地说明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本申请的保护范围之中。

Claims (11)

  1. 一种雾化芯，其特征在于，所述雾化芯包括多孔基体及发热体；
    所述多孔基体为多孔玻璃陶瓷基体，所述多孔玻璃陶瓷基体上任意2个测量区域，分别记为第一测量区域和第二测量区域，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M小于10％和/或|M-N|/N小于10％；
    所述测量区域的长度至少大于1μm；所述主元素为多孔玻璃陶瓷基体中元素含量大于20at％的元素。
  2. 根据权利要求1所述的雾化芯，其特征在于，以原子百分比计，第一测量区域主元素含量记为M at％，第二测量区域相应主元素含量记为N at％，其中|M-N|/M小于5％和/或|M-N|/N小于5％。
  3. 根据权利要求1或2所述的雾化芯，其特征在于，所述主元素包括第一主元素和第二主元素；以原子百分比计，所述多孔玻璃陶瓷基体中第一主元素的含量为55-64at％；第二主元素的含量为20-36at％；
    优选的，所述第一主元素为氧，所述第二主元素为硅；
    优选的，所述多孔玻璃陶瓷基体中的元素还包括钠、镁、铝、钙中的至少一种元素。
  4. 根据权利要求1-3中任一项所述的雾化芯，其特征在于，所述多孔玻璃陶瓷基体的平均孔径为15-45μm。
  5. 根据权利要求4所述的雾化芯，其特征在于，所述测量区域的长度至少为所述平均孔径的2倍。
  6. 根据权利要求1-5中任一项所述的雾化芯，其特征在于，所述多孔玻璃陶瓷基体的抗压强度大于1.5MPa；
    优选的，所述多孔玻璃陶瓷基体的抗压强度为6-18MPa。
  7. 根据权利要求1-6中任一项所述的雾化芯，其特征在于，所述多孔玻璃陶瓷基体包括晶相和非晶相；
    优选的，所述晶相的占比为50wt％以上；
    优选的，所述晶相包括石英相。
  8. 根据权利要求1-7中任一项所述的雾化芯，其特征在于，所述测量区域为圆形、椭圆形或矩形中的至少一种。
  9. 根据权利要求1-8中任一项所述的雾化芯，其特征在于，所述发热体为金属发 热膜。
  10. 一种雾化器(1)，其特征在于，所述雾化器(1)中包括权利要求1-9中任一项所述的雾化芯。
  11. 一种电子雾化装置，其特征在于，所述电子雾化装置中包括权利要求10所述的雾化器(1)，还包括电池组件(2)。
PCT/CN2024/094269 2023-06-01 2024-05-20 一种雾化芯、雾化器及电子雾化装置 Ceased WO2024245035A1 (zh)

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