WO2024239803A1 - 一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器 - Google Patents

一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器 Download PDF

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Publication number
WO2024239803A1
WO2024239803A1 PCT/CN2024/085494 CN2024085494W WO2024239803A1 WO 2024239803 A1 WO2024239803 A1 WO 2024239803A1 CN 2024085494 W CN2024085494 W CN 2024085494W WO 2024239803 A1 WO2024239803 A1 WO 2024239803A1
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Prior art keywords
porous glass
microns
glass material
pore
uniform
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PCT/CN2024/085494
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English (en)
French (fr)
Inventor
杨聪明
龙继才
周前远
付磊
张蛟
周宏明
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Shenzhen Smoore Technology Ltd
Smoore International Holdings Ltd
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Shenzhen Smoore Technology Ltd
Smoore International Holdings Ltd
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Priority to EP24810051.3A priority Critical patent/EP4714917A1/en
Publication of WO2024239803A1 publication Critical patent/WO2024239803A1/zh
Priority to US19/391,383 priority patent/US20260068948A1/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
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/48—Fluid transfer means, e.g. pumps
    • A24F40/485—Valves; Apertures
    • 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
    • A24F40/10—Devices using liquid inhalable precursors
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/08—Other methods of shaping glass by foaming
    • 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
    • C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
    • C03C14/002—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of fibres, filaments, yarns, felts or woven material
    • 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
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • 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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
    • C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
    • 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
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
    • C04B38/0058—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity open porosity
    • 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
    • H05B3/40—Heating elements having the shape of rods or tubes
    • H05B3/42—Heating elements having the shape of rods or tubes non-flexible
    • 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
    • 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
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/02—Fibres; Filaments; Yarns; Felts; Woven material
    • C03C2214/03—Fibres; Filaments; Yarns; Felts; Woven material surface treated, e.g. coated
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/36—Glass starting materials for making ceramics, e.g. silica 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/522—Oxidic
    • C04B2235/5228—Silica and alumina, including aluminosilicates, e.g. mullite
    • 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
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/522—Oxidic
    • C04B2235/5236—Zirconia

Definitions

  • the present application belongs to the technical field of porous materials, and in particular relates to a porous glass material with uniform pore channels, an atomization core and an electronic atomizer.
  • An electronic atomizer is a product that uses atomization and other means to turn atomization media into vapor for users to inhale.
  • the atomizer core is the core component of the electronic atomizer and plays a vital role in the taste, aerosol volume and other performance of the electronic atomizer.
  • porous ceramics As the atomization core. Most of them use diatomaceous earth, silicon oxide, aluminum oxide, etc. as raw materials, add glass powder, pore-forming agent, etc., and produce porous ceramics by sintering the prepared particles.
  • the use of porous ceramics as the atomization core has the characteristics of good uniformity, long life, delicate taste, and high degree of mechanization.
  • the porous ceramic heating element has a certain proportion of semi-closed pores and fine pores, which easily cause the adsorption of low-viscosity components in the atomization medium, thereby affecting the suction taste and aroma restoration.
  • the microscopic surface of the porous ceramic heating element is rough and has low continuity, and it cannot be matched with a thin film heating film.
  • porous glass Compared with porous ceramics, porous glass has the characteristics of smooth and continuous microstructure, low proportion of micro-nanopores, and is not easy to adsorb the atomizing medium, which improves the performance of electronic atomizers to a certain extent. Taste and aroma restoration.
  • the porous glass in the prior art has an uneven pore structure and the size of the pore channels varies greatly, which makes the transmission speed of the atomized liquid matrix vary greatly. In the area where the atomized liquid matrix transmission speed is slow, insufficient oil supply is likely to occur, resulting in local overheating, local coking, and carbon deposition. As the inhalation proceeds, the customer's inhalation experience is seriously affected and the failure of the electronic cigarette is accelerated. In addition, the liquid conduction speed needs to be further improved.
  • the technical problem to be solved by the present application is to overcome the above-mentioned defects of the porous glass material in the prior art, especially a series of problems caused by large differences in pore channels and the need to improve the liquid conduction speed, so as to provide a porous glass material with uniform pore channels, an atomization core and an electronic atomizer.
  • the present application provides a porous glass material with uniform pore channels, comprising a skeleton and multi-directional interconnected pores, wherein the multi-directional interconnected pores are interconnected by pore throats, wherein:
  • the average diameter of the pore throats is 25-45 microns, and the pore throats are distributed in the region of 5-60 microns, wherein more than 50% of the pore throats are distributed in the region of 20-45 microns.
  • the average diameter of the pore throats is 28-36 microns, the pore throats are distributed in the 10-55 micron region, and more than 90% of the pore throats are distributed in the 20-45 micron region.
  • the average diameter of the pore throats is about 29-35 microns, the pore throats are distributed in the 12-50 micron region, and the pore throats distributed in the 20-45 micron region account for more than 95%;
  • the pore throats are distributed between 20-45 microns.
  • the skeleton is a glass-coated fiber scaffolding structure, including a scaffolding body and a connector connecting the scaffolding body: the average diameter of the scaffolding body is 20 to 45 microns, and the average length is 60 to 100 microns.
  • the multi-directional interconnected holes have a diameter of 70-100 microns.
  • the porosity of the porous glass material is 65-80%, optionally 70-74%.
  • the porous glass material has a liquid conduction rate of 0.09 mm/s or more at room temperature for an atomized matrix with a viscosity of 230 cP; optionally, the liquid conduction rate at room temperature is 0.10 mm/s or more; further optionally, the liquid conduction rate at room temperature is 0.12 mm/s or more.
  • the present application also provides an atomizing core, which uses the above-mentioned porous glass material as a substrate, and a heating unit is arranged on the substrate.
  • the temperature field deviation of the atomization core is less than 10°C.
  • the present application also provides an electronic atomizer, comprising the above-mentioned atomization core.
  • the porous glass substrate can be a flat rectangular parallelepiped, a cylindrical shape, or a special-shaped structure, with a thickness of 0.5-4 mm on the atomized surface, and optionally, a thickness of 1.5-2.5 mm.
  • the porous glass substrate has an outer dimension of 9.0 mm in length, 4.0 mm in width, and a thickness of 1.6 ⁇ 0.1 (mm), 2.0 ⁇ 0.2 (mm), or 2.4 ⁇ 0.1 (mm); or, the porous glass substrate has an outer dimension of 7.4 mm in length, 4.0 mm in width, and a thickness of 1.6 ⁇ 0.1 (mm), 2.0 ⁇ 0.2 (mm), or 2.4 ⁇ 0.1 (mm).
  • the preparation method of the porous glass material generally includes the steps of mixing glass powder, fiber components and pore-forming agent, preparing green body, debinding, sintering and the like.
  • the fiber component has a diameter of 3-30 ⁇ m and a length of 20-500 ⁇ m;
  • the fiber component has a diameter of 10-25 ⁇ m and a length of 20-150 ⁇ m.
  • the aspect ratio of the fiber component is 1-10, and optionally, the aspect ratio of the fiber with a length of 50-150 ⁇ m is 2-5;
  • fibers with a fiber length of more than 50 ⁇ m account for 25%, optionally, account for more than 40%; further optionally, account for 40-100%.
  • the glass powder accounts for 40-62%, and the fiber component accounts for 38-60%;
  • the amount of the pore former used is 0.3-2.5 times the total mass of the glass powder and fiber components.
  • the steps of the gel casting process are roughly as follows: first, the materials are mixed evenly, and then the mixed materials are added to the sol liquid, and stirred into a paste at a certain temperature. Then, the sol liquid is injected into a mold of a corresponding shape, and a green compact is formed after cooling.
  • the debinding temperature is 200-800°C, and the debinding time is 5-50h; optionally, the debinding temperature is 200-350°C.
  • the sintering temperature is 900-1250° C. or 1180-1320° C.
  • the sintering time is 10-180 min.
  • the method for preparing the porous glass satisfies at least one of the following (1)-(5):
  • the softening temperature of the glass powder is 600-1200°C; the softening point of the selected fiber raw material is above the sintering temperature in the preparation method and can play a skeleton role;
  • the particle size of the glass powder is less than 10 ⁇ m, and optionally, the particle size is less than 3000 mesh;
  • the fiber component is at least one of silicon carbide fiber, silicon nitride fiber, aluminum silicate fiber, quartz fiber, mullite fiber, alumina fiber, hydroxyapatite fiber, and zirconium oxide fiber;
  • the pore-forming agent material is carbon powder, polystyrene, polymethyl methacrylate, polylactic acid, polyvinyl alcohol, polyethylene terephthalate, engineering plastics, starch, cellulose, sawdust, graphite
  • One or a mixture of materials such as powders that can decompose, volatilize or burn at high temperatures;
  • the particle size of the pore former is 10-300 ⁇ m, and optionally, the average particle size of the pore former is 80 ⁇ m.
  • a porous glass material with better connectivity can be obtained by adjusting the addition ratio of pore formers with different diameters.
  • the glass raw materials and fiber materials are pretreated as follows:
  • the particle size of the glass powder raw material is less than 10 microns, and glass powder with a mesh size of less than 3000 can be used.
  • commercially available glass powder can be milled for 3-5 hours using ethanol as solvent and a high-energy planetary ball mill at a speed of 200-500r/min, and then dried and sieved before use.
  • the fiber can be mullite fiber, zirconia fiber or alumina fiber and other high temperature resistant fibers.
  • mullite fiber can be selected, with a fiber diameter of 10-25 microns, a length of less than 150 microns, and a fiber aspect ratio of 1-10.
  • commercially available 2-5mm chopped fibers are first crushed to less than 0.5mm by a crusher, and then ethanol is used as a solvent, stearic acid is used as a grinding aid, and high-energy planetary ball milling is performed for 2-8 hours at a ball milling speed of 100-400r/min.
  • ball milling is performed at 300r/min.
  • the ball-milled fibers are washed with ethanol and dried through a 100-mesh sieve to obtain the target fiber.
  • the ball milling time is 6 hours to obtain the target fiber.
  • the target fiber is a fiber between 300 mesh and 100 mesh sieved after ball milling for 6 hours.
  • a spherical pore former is selected, and the pore former has a particle size of 50 microns, 80 microns, or a mixture of multiple particles mixed in a certain proportion.
  • the porous glass in the present application is prepared by gel casting, and the preparation method is as follows:
  • Glass powder, fiber, and pore-forming agent are mixed in a certain proportion and mixed with a three-dimensional mixer for 2 hours until uniform.
  • the mixed materials are then added to agar polysaccharide sol at 80°C, slowly stirred until a uniform paste is formed, and then injected into a corresponding mold and cooled to obtain a green body.
  • the green body is first cured at 60°C for 1-5h, then heated to 200°C in 200 minutes, and then heated to 500°C at 0.5°C per minute, wherein a 2-hour heat preservation time is set at 240°C, 300°C, and 350°C, and then heated to 1150°C-1320°C at 5°C per minute, and kept for 15-30 minutes, and naturally cooled to room temperature to obtain a porous glass material.
  • a better debinding process can be obtained according to the thermogravimetric curve of the pore-forming agent.
  • the strength and sintering properties of the porous glass material can be improved by adding a glass powder binder or/and a ceramic fiber material; generally, the addition or increase of ceramic powder and non-effective ceramic fiber will reduce the porosity of the porous glass matrix.
  • the hollow glass microspheres, glass powder or/and ceramic fiber are mixed evenly in a three-dimensional mixer, and then the mixed material is added to an agar polysaccharide sol solution at 80°C, slowly stirred to a uniform paste, and then injected into the corresponding mold, and the green body is obtained after cooling.
  • the green body is first cured at 60°C for 1-5h, then heated to 200°C at 200 minutes, and then heated to 500°C at 0.5°C per minute, wherein the heat preservation time is set at 240°C and 350°C for 1 hour, and then heated to 1000°C-1150°C at 5°C per minute, kept warm for 30 minutes, and naturally cooled to room temperature to obtain a porous glass material.
  • the atomizer core provided in the present application is based on a porous glass material, and a heating unit is arranged on the substrate, and the heating unit is a heating wire, a heating net or a heating film.
  • the heating wire or the heating net needs to be embedded in the green body forming process, and then sintered together with the formed green body to obtain a porous glass atomizer core; when a heating film is used, a thick film resistive heating film can be printed on the porous glass substrate by screen printing or a thin film resistive heating film can be sprayed or magnetron sputtered, and the pattern of the heating film can be designed, and then the porous glass atomizer core can be obtained through a sintering step.
  • a thick film resistive heating film is prepared by screen printing technology.
  • the main components of the thick film are nickel-based alloys, iron-based alloys, silver alloys, titanium alloys, aluminum alloys, stainless steel, etc., including elements such as Fe, Cr, Ni, Ti, Pa, Pt, Al, Mo, Si, Ag, etc.
  • the protruding thickness of the thick film is 11-100 ⁇ m, the infiltration thickness is 10-100 ⁇ m, the line width is 250-450 ⁇ m, the line spacing is 300 ⁇ m-900 ⁇ m, and the patterns used are S, M, ⁇ , etc.
  • the sintering temperature of the heating film is 700-1200°C, and the sintering time is 0.5-3h.
  • the thin film resistive heating film is prepared by spraying or magnetron sputtering.
  • the main components of the film are nickel-based alloys, silver alloys, titanium alloys, aluminum alloys, stainless steel, etc., containing elements such as Fe, Cr, Ni, Ti, Pa, Pt, Al, Mo, Si, Ag, etc.
  • the protruding thickness of the film is 0.5-5 ⁇ m.
  • an atomizer core is prepared by sintering a printed film of porous glass material, and its heating unit is a porous heating membrane, wherein: the porous heating membrane includes a portion higher than the surface of the porous glass substrate and a portion infiltrated into the porous glass substrate, wherein the portion higher than the surface of the porous glass substrate is a porous structure with a pore size of 5-30 microns, the pores are interconnected and connected to the substrate pores, and its height is 30-100 microns, and the optional height is about 80 microns; the heating membrane infiltrated into the porous glass substrate has a maximum infiltration thickness of about 70 microns, and is embedded in the pores of the porous substrate, so that the entire porous heating membrane is firmly bonded to the porous glass substrate; the resistance of the heating membrane is 0.8-1.2 ohms.
  • the porous glass material with uniform pore channels provided in the present application includes a skeleton and multi-directional interconnected pores, and the multi-directional interconnected pores are interconnected by pore throats, wherein: the average diameter of the pore throat is 25-45 microns, and the pore throat is distributed in the 5-60 micron area, wherein more than 50% of the pore throats are distributed in 20-45 microns.
  • the present application limits the size of the pore throat to make the size of the connecting channel between the pores uniform, avoids the uneven liquid conduction speed and local overheating during the use of the atomizer core, avoids the generation of local coking and carbon deposition, and the amount of smoke is basically not attenuated during the suction process.
  • the prepared atomizer core is tested for its atomization temperature condition using an infrared thermal imager.
  • the temperature field is evenly distributed, there is no local high temperature point, and the atomization temperature is stably distributed between 235-245°C.
  • the porous glass matrix is not easy to deposit carbon after smoking an electronic cigarette.
  • the liquid conduction speed is significantly improved, and the liquid conduction speed can be increased by more than 33% compared with commercially available porous ceramic heating elements.
  • the porous glass material with uniform pore channels provided in the present application further improves the overall uniformity of the porous glass material by optimizing the design of parameters such as pore throats, skeletons, multi-directional interconnected pores, porosity and liquid conduction rate, and the oil conduction rate at each location is significantly improved with high consistency, while the temperature during the atomization process is increased.
  • the uniformity of the field can further reduce the occurrence of local coking and carbon deposition and improve its atomization effect.
  • FIG1 is a pore throat size distribution diagram of the porous glass materials provided in Examples 1-3 and Comparative Example 1 of the present application;
  • FIG2 is an appearance morphology diagram (left) and a microscopic morphology diagram (right) of the atomizer core provided by the present application;
  • FIG3 is a temperature field distribution and a temperature distribution diagram of Example 1 during the atomization process in the test example
  • FIG4 is a temperature field distribution and a temperature distribution diagram of Comparative Example 1 during the atomization process in the test example
  • FIG5 is a comparison diagram of carbon deposition between Example 1 of the present application and a commercially available ceramic heating element
  • FIG. 6 is a microscopic morphology diagram of the porous material provided in Example 1 of the present application.
  • This embodiment provides a porous glass material with uniform pore channels, and a specific preparation method thereof comprises the following steps:
  • the glass powder is ball milled at a speed of 300r/min in a planetary ball mill for 3h, dried and sieved to obtain glass powder with a particle size of 3-5 microns; the crushed mullite chopped fibers are planetarily ball milled at a speed of 300r/min for 6h with stearic acid as a grinding aid and ethanol as a solvent, washed with ethanol, dried, and sieved with 100 mesh to obtain fiber raw materials.
  • the green body was first cured in a 60°C oven for 4 hours, then heated to 200°C in 200 minutes, and then heated to 500°C at 0.5°C per minute, with a 2-hour insulation time at 240°C and 350°C, and then heated to 1180°C at 5°C per minute, and kept for 30 minutes, and naturally cooled to room temperature to obtain a porous glass material with a porosity of 71.6%, an average pore throat of 34 microns, and pore throats distributed between 16-55 microns.
  • the pore throats are similar to the normal distribution, and more than 50% of the pore throats are distributed between 25-42 microns.
  • the pore throat size distribution is shown in Figure 1a.
  • the average diameter of the skeleton is 25 microns, the average length is 100 microns, and the diameter of the multi-directional connected pores is 75 microns.
  • Figure 6 is a microscopic morphology of the porous glass material.
  • a porous glass material with a length of 9mm, a width of 4mm, and a height of 2.5mm was prepared, and its oil conduction speed was tested at room temperature.
  • the smoke oil with a viscosity of 230cP was selected, and the substrate was placed vertically (height 9mm). It took about 75s for the smoke oil to rise 9mm, and the oil conduction speed was 0.12mm/s. Under the same conditions, the commercially available porous ceramic substrate took 100s to raise the smoke oil by 9mm, and the oil conduction speed was 0.09mm/s. Compared with the commercially available ceramic heating element substrate, the oil conduction speed of the porous glass material was increased by more than 33%.
  • This embodiment provides a porous glass material with uniform pore channels, and the specific preparation method thereof includes the following steps: Next steps:
  • the glass powder was ball milled at a speed of 300r/min in a planetary ball mill for 3h, dried and sieved to obtain glass powder with a particle size of 3-5 microns; the crushed alumina chopped fibers were planetarily ball milled at a speed of 300r/min for 6h with stearic acid as a grinding aid and ethanol as a solvent, washed with ethanol, dried, and sieved with 100 mesh to obtain fiber raw materials.
  • the green body was first cured in a 60°C oven for 2 hours, then heated to 200°C in 200 minutes, and then heated to 500°C at 0.5°C per minute, with a 2-hour insulation time at 240°C and 350°C, and then heated to 1250°C at 5°C per minute, and kept for 30 minutes, and naturally cooled to room temperature to obtain a porous glass material.
  • the porous glass material has a porosity of 74.2%, an average pore throat of 40 microns, pore throats distributed between 7-56 microns, and more than 50% of the pore throat sizes distributed between 38-45 microns.
  • the pore throat distribution is shown in Figure 1b.
  • the average diameter of the skeleton is 20 microns, the average length is 100 microns, and the diameter of the multi-directional connected pores is 80 microns.
  • a porous glass substrate with a length of 9 mm, a width of 4 mm, and a height of 2.5 mm was prepared, and its oil conduction speed was tested at room temperature.
  • a smoke oil with a viscosity of 230 cP was selected, and the substrate was placed vertically (height 9 mm). It took about 85 seconds for the smoke oil to rise 9 mm, and the oil conduction speed was 0.11 mm/s.
  • This embodiment provides a porous glass material with uniform pore channels, and a specific preparation method thereof comprises the following steps:
  • the glass powder was ball milled at 300r/min in a planetary ball mill for 3h, dried and sieved to obtain glass powder with a particle size of 3-5 microns; the crushed mullite chopped fibers were planetarily ball milled at 300r/min for 6h with stearic acid as a grinding aid and ethanol as a solvent, washed with ethanol, dried, and sieved with 100 mesh to obtain fiber raw materials.
  • PMMA (50 micron) pore former and 190 parts of PMMA (80 micron) pore former were mixed in three dimensions for 2 hours.
  • the mixed materials were added to 120 parts of 80°C agar polysaccharide sol solution, slowly stirred at 80°C to form a uniform paste, and then the paste was injected into a mold of the corresponding shape, and taken out after cooling to obtain a green body.
  • the green body was first cured in a 60°C oven for 1 hour, then heated to 200°C for 200 minutes, and then heated to 500°C at 0.5°C per minute, wherein the insulation time was set at 240°C and 350°C for 2 hours respectively, and then heated to 1220°C at 5°C per minute, and kept warm for 30 minutes, and naturally cooled to room temperature to obtain a porous glass material.
  • the porous glass material has a porosity of 67.7%, an average pore throat of 23 microns, and pore throats distributed between 12-39 microns.
  • the pore throats are similar to the normal distribution, and more than 50% of the pore throats are distributed between 22-28 microns.
  • the pore throat size distribution is shown in Figure 1c.
  • the average diameter of the skeleton is 25 ⁇ m, the average length is 95 ⁇ m, and the diameter of the multidirectional connected pore is 60 ⁇ m.
  • a porous glass substrate with a length of 9 mm, a width of 4 mm, and a height of 2.5 mm was prepared, and its oil conduction speed was tested at room temperature.
  • a smoke oil with a viscosity of 230 cP was selected, and the substrate was placed vertically (height 9 mm). It took about 80 seconds for the smoke oil to rise 9 mm, and the oil conduction speed was 0.11 mm/s.
  • This comparative example provides a porous glass material, and the preparation method thereof comprises the following steps:
  • the glass powder was ball milled at a speed of 300r/min in a planetary ball mill for 3h, dried and sieved to obtain glass powder with a particle size of 3-5 microns; the crushed mullite chopped fibers were planetarily ball milled at a speed of 300r/min for 6h with stearic acid as a grinding aid and ethanol as a solvent, washed with ethanol, dried, and sieved with 100 mesh to obtain fiber raw materials.
  • the green body was first cured in an oven at 60°C for 1 hour, then heated to 200°C in 200 minutes, and then heated to 500°C at 0.5°C per minute, with 2 hours of insulation time at 240°C and 350°C respectively, and then heated to 1180°C at 5°C per minute, and kept at this temperature for 30 minutes, and naturally cooled to room temperature to obtain a porous glass material.
  • the pore throat distribution is shown in Figure 1d.
  • the average diameter of the skeleton is 35 microns, the average length is 55 microns, and the diameter of the multidirectional connected pores is 60 microns.
  • a porous glass substrate with a length of 9 mm, a width of 4 mm, and a height of 2.5 mm was prepared, and its oil conduction speed was tested at room temperature.
  • a smoke oil with a viscosity of 230 cP was selected, and the substrate was placed vertically (height 9 mm). It took about 96 seconds for the smoke oil to rise 9 mm, and the oil conduction speed was 0.094 mm/s.
  • An atomizer core is prepared with the porous glass material prepared in the embodiment and the comparative example, and a porous iron-based heating membrane slurry is used (the specific composition is mainly metal Fe element, including some Ni, Cr, Mn, Mo, and W metal elements).
  • the film is printed and sintered to obtain a porous heating membrane.
  • the pore size of the porous heating membrane is 5-30 microns.
  • the pores are interconnected and penetrate the pores of the substrate. It is about 80 microns higher than the substrate and has a penetration thickness of about 70 microns.
  • the pattern is shown in Figure 2.
  • the line width is about 330 ⁇ m
  • the line spacing is about 650 ⁇ m
  • the line is about 800 microns away from the edge of the substrate
  • the sintering temperature is 980°C
  • the time is 30 min to obtain a porous glass atomizer core.
  • the atomization temperature of the porous glass atomization core was investigated using an infrared thermal imager. A 7.5W power board was used, and the atomization ability of the porous glass atomization core was evaluated using fruit-flavored e-liquid in a test mode of energizing for 3s and stopping for 27s. During the atomization process, the temperature field of the atomization core was evenly distributed without local high temperature points.
  • Example 1 The atomization temperature of Example 1 was stably distributed between 235-245°C, as shown in Figure 3.
  • the atomization temperature of Comparative Example 1 was unstably distributed between 240-310°C, as shown in Figure 4.
  • the test results of Examples 2-3 are similar to those of Example 1 and are no longer shown one by one.
  • the porous glass atomizer cores prepared in Examples 1-3 and Comparative Example 1 were tested for loading cigarettes. Under the conditions of 7.5W power battery and fruit-flavored e-liquid, the puffs were simulated by puffing for 3s and stopping for 27s. Compared with the commercially available ceramic heating element (Feelm heating element, Shenzhen McWell Technology Co., Ltd.), the porous glass atomizer core in Example 1 was not prone to carbon deposition after puffing. As shown in Figure 5, after 400 puffs, the porous glass atomizer core (left picture) had a significant advantage over the ceramic heating element (right picture) in terms of carbon deposition, while the commercially available ceramic heating element had serious carbon deposition after 400 puffs. Among them, the carbon deposition of Examples 2 and 3 was close to that of Example 1, and Comparative Example 1 was The carbon deposit condition is similar to that of commercially available ceramic heating elements, so pictures will not be shown one by one.

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Abstract

本申请属于多孔材料技术领域，具体涉及一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器。该孔通道均匀的多孔玻璃材料，包括骨架及多向连通孔，多向连通孔由孔喉相互连通，其中：所述孔喉的平均直径为25-45微米，孔喉分布于5-60微米区域，其中，50％以上孔喉分布于20-45微米。本申请通过对孔喉尺寸的限定，使孔与孔之间的连通通道尺寸均匀，避免了在雾化芯使用中出现导液速度不均匀，出现局部过热的情况，避免了局部焦化和积碳的产生，抽吸过程中烟雾量基本无衰减。对比市售陶瓷发热体，相同的条件下，多孔玻璃基体抽吸电子烟后不易积碳。同时，导液速度提升明显，相比于市售多孔陶瓷发热体，导液速度最高可提升33％以上。

Description

一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器
相关申请的交叉引用
本申请要求在2023年5月19日提交中国专利局、申请号为202310574687.9、发明名称为“一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器”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
本申请属于多孔材料技术领域，具体涉及一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器。
背景技术
电子雾化器是一种通过雾化等手段，将雾化介质等变成蒸汽，让用户吸食的一种产品。雾化芯是电子雾化器的核心部件，对电子雾化器的口感、气溶胶量等性能起到了至关重要的的作用。
封闭式电子雾化器大部分采用多孔陶瓷作为雾化芯，大多数采用硅藻土、氧化硅、氧化铝等为原料，加入玻璃粉、造孔剂等，通过烧结制备的颗粒堆积产生的多孔陶瓷。采用多孔陶瓷作雾化芯，具有均一性好，寿命长，口感细腻、械化程度高等特点。但是，多孔陶瓷发热体具有一定的比例的半闭孔和微细孔隙的特点，容易造成对雾化介质中低粘度成分的吸附，进而影响抽吸口感和香气还原度。同时，多孔陶瓷发热体微观表面粗糙、连续性较低，无法搭配薄膜发热膜。
与多孔陶瓷相比，多孔玻璃具有微观结构光滑连续、微纳孔比例较低的特点，不易对雾化介质产生吸附等特点，在一定程度上提升了电子雾化器的 口感和香气还原度。然而，现有技术中的多孔玻璃的孔结构不均匀，孔通道的大小差异较大，使得雾化液基质的传输速度差别较大，而在雾化液基质传递速度慢的区域容易产生供油不足的情况，导致局部过热，使得局部焦化，产生积碳，进而随着抽吸的进行，严重影响客户抽吸体验，加速电子烟的失效；另外，导液速度也有待进一步提升。
发明内容
因此，本申请要解决的技术问题在于克服现有技术中的多孔玻璃材料存在的上述缺陷，特别是孔通道差异大导致的一系列问题以及导液速度有待提升等缺陷，从而提供一种孔通道均匀的多孔玻璃材料、雾化芯和电子雾化器。
为此，本申请提供如下技术方案：
本申请提供一种孔通道均匀的多孔玻璃材料，包括骨架及多向连通孔，多向连通孔由孔喉相互连通，其中：
所述孔喉的平均直径为25-45微米，孔喉分布于5-60微米区域，其中，50％以上孔喉分布于20-45微米。
可选地，所述孔喉的平均直径为28-36微米，孔喉分布于10-55微米区域，90％以上孔喉分布于20-45微米。
可选地，所述孔喉的平均直径约29-35微米，孔喉分布于12-50微米区域，分布于20-45微米的孔喉占比高于95％；
可选地，孔喉均分布于20-45微米。
可选地，所述骨架为玻璃包覆纤维搭架结构，包括搭架体及连结搭架体的连接体：搭架体的平均直径为20～45微米，平均长度60-100微米。
可选地，所述多向连通孔的孔直径为70-100微米。
可选地，所述多孔玻璃材料的孔隙率为65-80％，可选地为70-74％。
可选地，所述多孔玻璃材料对于粘度为230cP的雾化基质，室温下的导液速率为0.09mm/s以上；可选地，室温下的导液速率为0.10mm/s以上；进一步可选地，室温下的导液速率为0.12mm/s以上。
本申请还提供一种雾化芯，以上述的多孔玻璃材料为基体，所述基体上设置有发热单元。
可选地，所述雾化芯在雾化过程中，温度场偏差小于10℃。
本申请还提供一种电子雾化器，包括上述的雾化芯。
所述多孔玻璃基体可以是平板长方体、圆柱体形状，也可以是异形结构形状，雾化面厚度0.5-4mm，可选地，厚度1.5～2.5mm。典型非限定性地，多孔玻璃基体外尺寸长9.0mm，宽4.0mm，厚度1.6±0.1(mm)、2.0±0.2(mm)、2.4±0.1(mm)；或者，多孔玻璃基体外尺寸长7.4mm，宽4.0mm，厚度1.6±0.1(mm)、2.0±0.2(mm)、2.4±0.1(mm)。
所述多孔玻璃材料的制备方法一般包括：将玻璃粉、纤维组分、造孔剂混合，制备生坯，经排胶，烧结等步骤。
可选地，所述纤维组分的直径为3-30μm，长度为20-500μm；
可选地，所述纤维组分的直径为10-25微米，长度为20-150μm。
可选地，所述纤维组分的长径比为1-10，可选地，长度为50-150μm的纤维的长径比为2-5；
和/或，纤维组分中，纤维长度在50μm以上的纤维占比在25％，可选地，占比在40％以上；进一步可选地，占比为40-100％。
以玻璃粉和纤维组分的总质量计，所述玻璃粉占40-62％，所述纤维组分占38-60％；
和/或，所述造孔剂的用量为玻璃粉和纤维组分总质量的0.3-2.5倍。
选用流延工艺，注塑工艺，干压工艺，凝胶注模工艺中的任一种制备生坯；
制备生坯的上述工艺均为领域内已知的，可根据选择的不同工艺添加使用相应的加工助剂。典型非限定性地，凝胶注模工艺的步骤大致为：先将材料混合均匀，再将混料后的材料加入至溶胶液中，于一定温度下搅拌成膏状。再将其注入至相应形状的模具中，冷却后形成生坯。
和/或，所述排胶温度为200-800℃，排胶时间为5-50h；可选地，所述排胶温度为200-350℃。
和/或，所述烧结温度为900-1250℃或者1180-1320℃，烧结时间为10-180min。
可选地，所述的多孔玻璃的制备方法，满足以下(1)-(5)中的至少一项：
(1)所述玻璃粉的软化温度为600-1200℃；所选纤维原料的软化点在制备方法中的烧结温度以上即可起到骨架作用；
(2)所述玻璃粉的粒径在10μm以下，可选地，粒径在3000目以下；
(3)所述纤维组分为碳化硅纤维，氮化硅纤维，硅酸铝纤维，石英纤维，莫来石纤维，氧化铝纤维，羟基磷石灰纤维，氧化锆纤维中的至少一种；
(4)所述造孔剂材料为碳粉、聚苯乙烯、聚甲基丙烯酸甲酯、聚乳酸、聚乙烯醇、聚对苯二甲酸乙二醇酯、工程塑料、淀粉、纤维素、木屑、石墨 粉中等经高温能分解、挥发或燃烧的材料中的一种或混合物；
(5)所述造孔剂的粒径为10-300μm，可选地，所述造孔剂的平均粒径为80微米。可以通过调节不同直径造孔剂的加入比例来获得更好连通性的多孔玻璃材料。
为了获得该特殊孔隙结构的多孔玻璃材料，对玻璃原料及纤维材料做如下预处理：
1.玻璃粉体原料粒径小于10微米，可选使用3000目以下的玻璃粉末。为了获得均匀粒径的玻璃粉，可将市售的玻璃粉末，以乙醇为溶剂，使用高能行星球磨机以200-500r/min的转速，球磨3-5小时，烘干过筛后使用。
2.纤维可以使用莫来石纤维、氧化锆纤维或氧化铝等耐高温纤维，本案可选莫来石纤维，纤维直径10-25微米，长度小于150微米，纤维长径比1-10。一般的，先通过破碎机将市售的2-5mm的短切纤维破碎至0.5mm以下，再以乙醇为溶剂，硬脂酸为助磨剂，高能行星球磨2-8小时，球磨转速100-400r/min，可选的，以300r/min球磨，球磨后的纤维经乙醇洗涤，烘干过100目筛，获得目标纤维，可选地，球磨时间为6小时，获得目标纤维，更优地，目标纤维为球磨6h后筛分的300目～100目之间的纤维。
为了获得更均匀孔径的多孔玻璃基体，选择球形造孔剂，造孔剂为粒径为50微米，80微米中的一种，或按一定比例混合的多种混合物。
具体地，本申请中的多孔玻璃采用凝胶注模法制备获得，其制备方法如下：
将玻璃粉，纤维，以及造孔剂按照一定的比例配料，并用三维混炼机混料2小时至均匀。然后将混合后的材料加入至80℃的琼脂多糖溶胶液中，缓慢搅拌至均匀的膏体状，然后将其注入至相应的模具中，冷却后获得生坯。 生坯先于60℃下养护1-5h，然后按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，300℃，350℃设置2小时保温时间，然后按5℃每分钟升温至1150℃～1320℃，保温15-30分钟，自然冷却至室温，获得多孔玻璃材料。一般的，可以根据造孔剂的热重曲线来获得较优的排胶工艺。
或者，可以通过添加玻璃粉末粘结剂或/和陶瓷纤维材料提高多孔玻璃材料的强度及烧结性能；通常的，陶瓷粉末及非有效陶瓷纤维的加入或增加，将降低多孔玻璃基体的孔隙率。一般的,将空心玻璃微球、玻璃粉体或/和陶瓷纤维于三维混料机中混合均匀，然后将混合后的材料加入至80℃的琼脂多糖溶胶液中，缓慢搅拌至均匀的膏体状，然后将其注入至相应的模具中，冷却后获得生坯。生坯先于60℃下养护1-5h，然后按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，350℃设置1小时保温时间，然后按5℃每分钟升温至1000℃-1150℃，保温30分钟，自然冷却至室温，获得多孔玻璃材料。
典型非限定性的，本申请提供的雾化芯以多孔玻璃材料为基体，基体上设置有发热单元，所述发热单元为发热丝，发热网或发热膜。其中，发热丝或发热网需要在生坯成型过程中嵌入，然后与成型坯体一起进行烧结，得到多孔玻璃雾化芯；当采用发热膜的时候，可以在多孔玻璃基体上，采用丝网印刷的方式印刷厚膜电阻发热膜或者喷涂、磁控溅射薄膜电阻发热膜的形式，设计发热膜的图案，然后再经过烧结步骤得到多孔玻璃雾化芯。
典型非限定性的，采用丝网印刷工艺制备厚膜电阻发热膜，厚膜的主要成分为镍基合金、铁基合金、银合金、钛合金、铝合金、不锈钢等，包含Fe、Cr、Ni、Ti、Pa、Pt、Al、Mo、Si、Ag等元素，厚膜突出厚度为11-100μm，下渗厚度为10-100μm，线宽为250-450μm，线距为300μm-900μm，采用的图案S、M、Ω等图案，发热膜烧结温度为700-1200℃，烧结时间为0.5-3h。
典型非限定性的，采用喷涂或者磁控溅射制备薄膜电阻发热膜，薄膜的主要成分为镍基合金、银合金、钛合金、铝合金、不锈钢等，包含Fe、Cr、Ni、Ti、Pa、Pt、Al、Mo、Si、Ag等元素，薄膜突出厚度为0.5-5μm。
例如，一种基于多孔玻璃材料印膜烧结后制备的雾化芯，其发热单元为多孔发热膜，其中：多孔发热膜包括高于多孔玻璃基体表面部分和渗入多孔玻璃基体部分，其中，高于多孔玻璃基体表面部分为多孔结构，孔径5-30微米，孔与孔之间相互连通，并与基体孔贯通，其高度30-100微米，可选的高度约为80微米；渗入多孔玻璃基体部分的发热膜，最大渗入厚度约为70微米，其镶嵌于多孔基体孔道内，使整个多孔发热膜与多孔玻璃基体结合牢固；发热膜阻值0.8-1.2欧姆。
本申请技术方案，具有如下优点：
本申请提供的孔通道均匀的多孔玻璃材料，包括骨架及多向连通孔，多向连通孔由孔喉相互连通，其中：所述孔喉的平均直径为25-45微米，孔喉分布于5-60微米区域，其中，50％以上孔喉分布于20-45微米。本申请通过对孔喉尺寸的限定，使孔与孔之间的连通通道尺寸均匀，避免了在雾化芯使用中出现导液速度不均匀，出现局部过热的情况，避免了局部焦化和积碳的产生，抽吸过程中烟雾量基本无衰减。具体地，对所制备的雾化芯，使用红外热成像仪测试其雾化温度状况，该雾化芯雾化过程中，温度场分布均匀，无局部高温点，雾化温度稳定分布在235-245℃之间。对比市售陶瓷发热体，相同的条件下，多孔玻璃基体抽吸电子烟后不易积碳。同时，导液速度提升明显，相比于市售多孔陶瓷发热体，导液速度最高可提升33％以上。
本申请提供的孔通道均匀的多孔玻璃材料，通过对孔喉、骨架、多向连通孔、孔隙率和导液速率等参数的优化设计，进一步提高了多孔玻璃材料的整体均匀性，各处导油速率提升明显且一致性高，同时提升雾化过程中温度 场的均匀性，能够进一步降低局部焦化和积碳的产生，提升其雾化效果。
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是本申请实施例1-3和对比例1所提供的多孔玻璃材料的孔喉尺寸分布图；
图2是本申请提供的雾化芯外观形貌图(左)及微观形貌图(右)；
图3是测试例中雾化过程中实施例1的温度场分布和温度分布图；
图4是测试例中雾化过程中对比例1的温度场分布和温度分布图；
图5是本申请实施例1和市售陶瓷发热体的积碳情况对比图；
图6是本申请实施例1提供多孔材料的微观形貌图。
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。
实施例1
本实施例提供一种孔通道均匀的多孔玻璃材料，其具体制备方法包含如下步骤：
以乙醇为溶剂，将玻璃粉末以300r/min的转速，于行星球磨机种球磨3h，烘干、过筛，获得粒径3-5微米的玻璃粉；将粉碎后的莫来石短切纤维，以硬脂酸为助磨剂，以乙醇为溶剂，以300r/min的转速，行星球磨6小时，乙醇洗涤后烘干、100目过筛，获得纤维原料。以48份玻璃粉、52份莫来石纤维、100份PMMA(80微米)造孔剂配料，三维混料2h，将混合后的材料加入至140份80℃的3.5％的琼脂多糖溶胶水溶液中(下同)，80℃下缓慢搅拌成均匀的膏状体，再将膏状体注入相应形状的模具中，冷却后取出，获得生坯。生坯先于60℃烘箱中养护4h，再按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，350℃设置2小时保温时间，然后按5℃每分钟升温至1180℃，保温30分钟，自然冷却至室温，获得多孔玻璃材料，多孔玻璃材料孔隙率71.6％，平均孔喉34微米，孔喉分布于16-55微米之间，孔喉似于正太分布，50％以上的孔喉分布于25-42微米之间。孔喉尺寸分布如图1a所示。骨架的平均直径为25微米，平均长度为100微米，多向连通孔的直径为75微米。图6为多孔玻璃材料的微观形貌图。
取制备的长度9mm，宽度4mm，高度2.5mm的多孔玻璃材料，室温下测试其导油速度，选取粘度为230cP的烟油，将基体竖直放置(高度9mm)，烟油升高9mm用时约75s，导油速度0.12mm/s，相同条件下，市售多孔陶瓷基体，烟油升高9mm用时100s，导油速度0.09mm/s，对比市售陶瓷发热体基体，多孔玻璃材料导油速度提升33％以上。
实施例2
本实施例提供一种孔通道均匀的多孔玻璃材料，其具体制备方法包含如 下步骤：
以乙醇为溶剂，将玻璃粉末以300r/min的转速，于行星球磨机种球磨3h，烘干、过筛，获得粒径3-5微米的玻璃粉；将粉碎后的氧化铝短切纤维，以硬脂酸为助磨剂，以乙醇为溶剂，以300r/min的转速，行星球磨6小时，乙醇洗涤后烘干、100目过筛，获得纤维原料。以40份玻璃粉、60份纤维、200份PMMA(80微米)造孔剂配料，三维混料2h，将混合后的材料加入至130份80℃的琼脂多糖溶胶液中，80℃下缓慢搅拌成均匀的膏状体，再将膏状体注入相应形状的模具中，冷却后取出，获得生坯。生坯先于60℃烘箱中养护2h，再按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，350℃设置2小时保温时间，然后按5℃每分钟升温至1250℃，保温30分钟，自然冷却至室温，获得多孔玻璃材料。多孔玻璃材料孔隙率74.2％，平均孔喉40微米，孔喉分布于7-56微米之间，50％以上的孔喉尺寸分布于38-45微米之间。孔喉分布如图1b所示。骨架的平均直径为20微米，平均长度为100微米，多向连通孔的直径为80微米。
取制备的长度9mm，宽度4mm，高度2.5mm的多孔玻璃基体，室温下测试其导油速度，选取粘度为230cP的烟油，将基体竖直放置(高度9mm)，烟油升高9mm用时约85秒，导油速度0.11mm/s。
实施例3
本实施例提供一种孔通道均匀的多孔玻璃材料，其具体制备方法包含如下步骤：
以乙醇为溶剂，将玻璃粉末以300r/min的转速，于行星球磨机种球磨3h，烘干、过筛，获得粒径3-5微米的玻璃粉；将粉碎后的莫来石短切纤维，以硬脂酸为助磨剂，以乙醇为溶剂，以300r/min的转速，行星球磨6小时，乙醇洗涤后烘干、100目过筛，获得纤维原料。以62份玻璃粉、38份纤维、50份 PMMA(50微米)造孔剂、190份PMMA(80微米)造孔剂配料，三维混料2h，将混合后的材料加入至120份80℃的琼脂多糖溶胶液中，80℃下缓慢搅拌成均匀的膏状体，再将膏状体注入相应形状的模具中，冷却后取出，获得生坯。生坯先于60℃烘箱中养护1h，再按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，350℃设置2小时保温时间，然后按5℃每分钟升温至1220℃，保温30分钟，自然冷却至室温，获得多孔玻璃材料。多孔玻璃材料孔隙率67.7％，平均孔喉23微米，孔喉分布于12-39微米之间，孔喉近似于正太分布，50％以上的孔喉分布于22-28微米之间。孔喉尺寸分布如图1c所示。骨架的平均直径为25微米，平均长度为95微米，多向连通孔的直径为60微米。
取制备的长度9mm，宽度4mm，高度2.5mm的多孔玻璃基体，室温下测试其导油速度，选取粘度为230cP的烟油，将基体竖直放置(高度9mm)，烟油升高9mm用时约80秒，导油速度0.11mm/s。
对比例1
本对比例提供一种多孔玻璃材料，其制备方法包含如下步骤：
以乙醇为溶剂，将玻璃粉末以300r/min的转速，于行星球磨机种球磨3h，烘干、过筛，获得粒径3-5微米的玻璃粉；将粉碎后的莫来石短切纤维，以硬脂酸为助磨剂，以乙醇为溶剂，以300r/min的转速，行星球磨6小时，乙醇洗涤后烘干、100目过筛，获得纤维原料。以70份玻璃粉、30份纤维、200份PMMA(80微米)造孔剂配料，三维混料2h，将混合后的材料加入至120份80℃的琼脂多糖溶胶液中，80℃下缓慢搅拌成均匀的膏状体，再将膏状体注入相应形状的模具中，冷却后取出，获得生坯。生坯先于60℃烘箱中养护1h，再按200分钟升温至200℃，再以0.5℃每分钟升温至500℃，其中分别于240℃，，350℃设置2小时保温时间，然后按5℃每分钟升温至1180℃，保温30分钟，自然冷却至室温，获得多孔玻璃材料。多孔玻璃材料孔隙率 47.7％，平均孔喉15.2微米，孔喉分布于3-30微米之间，50％以上的孔喉分布于7-15微米之间。孔喉分布如图1d所示。骨架的平均直径为35微米，平均长度为55微米，多向连通孔的直径为60微米。
取制备的长度9mm，宽度4mm，高度2.5mm的多孔玻璃基体，室温下测试其导油速度，选取粘度为230cP的烟油，将基体竖直放置(高度9mm)，烟油升高9mm用时约96秒，导油速度0.094mm/s。
测试例
以实施例和对比例所制备的多孔玻璃材料制备雾化芯，采用多孔铁基发热膜浆料(具体组成主要为金属Fe元素，包含部分Ni,Cr,Mn,Mo,W金属元素)，印膜烧结获得多孔发热膜，多孔发热膜孔径5-30微米，孔与孔相互连通，并与基体孔贯通，高于基体约80微米，下渗厚度约为70微米，图案如图2所示，线宽约为330μm，线距约为650μm，线与基体边缘相距约800微米，烧结温度为980℃，时间为30min，得到多孔玻璃雾化芯。使用红外热成像仪考察该多孔玻璃雾化芯雾化温度状况，使用7.5W功率板，按照通电3s,停27s的测试方式，使用水果味烟油评价该多孔玻璃雾化芯的雾化能力，雾化过程中，雾化芯温度场分布均匀，无局部高温点，其中，实施例1的雾化温度稳定分布在235-245℃之间，如图3所示。对比例1的雾化温度不稳定分布在240-310℃之间，如图4所示。实施例2-3与实施例1的测试结果接近不再一一展示。
对实施例1-3和对比例1制备的多孔玻璃雾化芯装烟检测，7.5W功率电池，水果味烟油下，按照抽3s停27s模拟抽吸方式抽吸，与市售陶瓷发热体(深圳市麦克韦尔科技有限公司，Feelm发热体)相比，实施例1多孔玻璃雾化芯抽吸后不易积碳，如图5所示，抽吸400口后，多孔玻璃雾化芯(左图)在积碳方面比陶瓷发热体(右图)有显著优势，而市售陶瓷发热体在测试400口后因积碳严重。其中，实施例2和3的积碳情况与实施例1接近，对比例1 的积碳情况与市售陶瓷发热体接近，不再一一展示图片。
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 (14)

  1. 一种孔通道均匀的多孔玻璃材料，其特征在于，包括骨架及多向连通孔，多向连通孔由孔喉相互连通，其中：
    所述孔喉的平均直径为25-45微米，孔喉分布于5-60微米区域，其中，50％以上孔喉分布于20-45微米。
  2. 根据权利要求1所述的孔通道均匀的多孔玻璃材料，其特征在于，所述孔喉的平均直径为28-36微米，孔喉分布于10-55微米区域，90％以上孔喉分布于20-45微米。
  3. 根据权利要求2所述的孔通道均匀的多孔玻璃材料，其特征在于，所述孔喉的平均直径约29-35微米，孔喉分布于12-50微米区域，分布于20-45微米的孔喉占比高于95％。
  4. 根据权利要求3所述的孔通道均匀的多孔玻璃材料，其特征在于，孔喉均分布于20-45微米。
  5. 根据权利要求1-4任一项所述的孔通道均匀的多孔玻璃材料，其特征在于，所述骨架为玻璃包覆纤维搭架结构，包括搭架体及连结搭架体的连接体：搭架体的平均直径为20～45微米，平均长度60-100微米。
  6. 根据权利要求5所述的孔通道均匀的多孔玻璃材料，其特征在于，所述多向连通孔的孔直径为70-100微米。
  7. 根据权利要求1-4任一项所述的孔通道均匀的多孔玻璃材料，其特征在于，所述多孔玻璃材料的孔隙率为65-80％。
  8. 根据权利要求7所述的孔通道均匀的多孔玻璃材料其特征在于，所述多 孔玻璃材料的孔隙率为70-74％。
  9. 根据权利要求7或8所述的孔通道均匀的多孔玻璃材料，其特征在于，所述多孔玻璃材料对于粘度为230cP的雾化基质，室温下的导液速率为0.09mm/s以上。
  10. 根据权利要求9所述的孔通道均匀的多孔玻璃材料，其特征在于，室温下的导液速率为0.10mm/s以上。
  11. 根据权利要求9所述的孔通道均匀的多孔玻璃材料，其特征在于，室温下的导液速率为0.12mm/s以上。
  12. 一种雾化芯，其特征在于，以权利要求1-11任一项所述的多孔玻璃材料为基体，所述基体上设置有发热单元。
  13. 根据权利要求12所述的雾化芯，其特征在于，雾化过程中，温度场偏差小于10℃。
  14. 一种电子雾化器，其特征在于，包括权利要求12或13所述的雾化芯。
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KR920017967A (ko) * 1991-03-25 1992-10-21 최영중 큰 개방기공용적을 갖는 다공질 소결유리의 제조방법
CN110194662A (zh) * 2019-06-05 2019-09-03 阿特麦哲(东莞)科技有限公司 雾化芯及其制备方法和电子烟
CN114804639A (zh) * 2022-05-25 2022-07-29 深圳麦克韦尔科技有限公司 一种多孔玻璃及其制备方法和应用

Patent Citations (3)

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KR920017967A (ko) * 1991-03-25 1992-10-21 최영중 큰 개방기공용적을 갖는 다공질 소결유리의 제조방법
CN110194662A (zh) * 2019-06-05 2019-09-03 阿特麦哲(东莞)科技有限公司 雾化芯及其制备方法和电子烟
CN114804639A (zh) * 2022-05-25 2022-07-29 深圳麦克韦尔科技有限公司 一种多孔玻璃及其制备方法和应用

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