WO2023065702A1 - Porous ceramic atomizing core and preparation method therefor, and electronic cigarette - Google Patents
Porous ceramic atomizing core and preparation method therefor, and electronic cigarette Download PDFInfo
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- WO2023065702A1 WO2023065702A1 PCT/CN2022/100427 CN2022100427W WO2023065702A1 WO 2023065702 A1 WO2023065702 A1 WO 2023065702A1 CN 2022100427 W CN2022100427 W CN 2022100427W WO 2023065702 A1 WO2023065702 A1 WO 2023065702A1
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- atomizing core
- porous ceramic
- green body
- ceramic atomizing
- powder
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- 239000000919 ceramic Substances 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 55
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 52
- 238000010438 heat treatment Methods 0.000 claims abstract description 51
- 239000011230 binding agent Substances 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 34
- 230000008569 process Effects 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000005238 degreasing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 48
- 239000011148 porous material Substances 0.000 claims description 36
- 239000002245 particle Substances 0.000 claims description 34
- 230000004907 flux Effects 0.000 claims description 24
- 239000003623 enhancer Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 12
- 238000004898 kneading Methods 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 10
- 239000000395 magnesium oxide Substances 0.000 claims description 10
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 8
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 8
- 239000004698 Polyethylene Substances 0.000 claims description 7
- 235000021355 Stearic acid Nutrition 0.000 claims description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 7
- 239000012188 paraffin wax Substances 0.000 claims description 7
- 239000008188 pellet Substances 0.000 claims description 7
- 239000008117 stearic acid Substances 0.000 claims description 7
- 239000011787 zinc oxide Substances 0.000 claims description 7
- 239000004927 clay Substances 0.000 claims description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical group O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- 239000004113 Sepiolite Substances 0.000 claims description 4
- 229910052849 andalusite Inorganic materials 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 229910052878 cordierite Inorganic materials 0.000 claims description 4
- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 4
- 239000010433 feldspar Substances 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- 229910052624 sepiolite Inorganic materials 0.000 claims description 4
- 235000019355 sepiolite Nutrition 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims 3
- 238000002347 injection Methods 0.000 claims 3
- 239000007924 injection Substances 0.000 claims 3
- 238000004321 preservation Methods 0.000 claims 3
- 239000011162 core material Substances 0.000 description 46
- 230000000052 comparative effect Effects 0.000 description 12
- 238000001035 drying Methods 0.000 description 9
- 239000005995 Aluminium silicate Substances 0.000 description 7
- 235000012211 aluminium silicate Nutrition 0.000 description 7
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 7
- 239000010439 graphite Substances 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000005909 Kieselgur Substances 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 4
- -1 that is Substances 0.000 description 4
- 238000000889 atomisation Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910052656 albite Inorganic materials 0.000 description 1
- DLHONNLASJQAHX-UHFFFAOYSA-N aluminum;potassium;oxygen(2-);silicon(4+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Si+4].[Si+4].[Si+4].[K+] DLHONNLASJQAHX-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 229910052613 tourmaline Inorganic materials 0.000 description 1
- 239000011032 tourmaline Substances 0.000 description 1
- 229940070527 tourmaline Drugs 0.000 description 1
- 229910052902 vermiculite Inorganic materials 0.000 description 1
- 239000010455 vermiculite Substances 0.000 description 1
- 235000019354 vermiculite Nutrition 0.000 description 1
Images
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- 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
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/068—Carbonaceous materials, e.g. coal, carbon, graphite, hydrocarbons
-
- 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
-
- 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
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/64—Burning or sintering processes
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- 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
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6562—Heating rate
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/66—Specific sintering techniques, e.g. centrifugal sintering
- C04B2235/661—Multi-step sintering
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Definitions
- the present application relates to the technical field of ceramic materials, and more specifically, to a porous ceramic atomizing core, a preparation method thereof, and an electronic cigarette.
- the raw materials of the existing porous ceramic atomizing core mainly include ceramic aggregate, binder, flux and pore-forming agent.
- the preparation method usually includes four steps: mixing, molding, degreasing and sintering. Among them, degreasing is used to remove the pore-forming agent and binder to form a porous structure. Sintering mainly improves the strength of porous ceramics through high temperature. As the sintering temperature increases, the texture of ceramics becomes more and more dense, thereby increasing the strength. However, in order to maintain the porosity of the porous structure, and The sintering temperature is not allowed to be too high, otherwise, with the increase of the sintering temperature, the porous structure will shrink more and more, and the porosity will become smaller.
- the porous structure is prone to collapse during the shrinkage process. Therefore, the existing porous ceramic atomization It is difficult for the core to meet high strength under the condition of high porosity, and the strength is low.
- the atomizing core is not only easy to drop powder, which affects the taste of the suction, but also easy to be damaged during assembly, which affects the product yield.
- the purpose of the present application is to overcome the above-mentioned defects in the prior art, and provide a high-strength and high-porosity porous ceramic atomizing core, a preparation method thereof, and an electronic cigarette.
- a method for preparing a porous ceramic atomizing core comprising the following processes:
- the raw materials include: ceramic aggregate, binder, flux and pore-forming agent, wherein the pore-forming agent is selected from one or both of graphite powder and carbon powder;
- the sintered green body is placed in an oxygen-containing atmosphere for a heating reaction, the temperature of the heating reaction is 400°C to 800°C, the pore-forming agent reacts with the oxygen in the oxygen-containing atmosphere, and the A pore-forming agent to obtain the porous ceramic atomizing core.
- the present application also provides a porous ceramic atomizing core prepared by the above preparation method.
- the present application also provides an electronic cigarette, including a main body and the above-mentioned porous ceramic atomizing core, and the porous ceramic atomizing core is installed on the main body.
- graphite and/or carbon powder are used as pore-forming agents.
- the pore-forming agents are resistant to high temperatures and cannot be removed during degreasing and sintering, so that the strength of ceramics can be improved by setting a higher sintering temperature; Heating reaction after sintering, the pore-forming agent graphite and/or carbon powder can react with oxygen in the oxygen-containing atmosphere at a lower temperature of 400 ° C to 800 ° C lower than the sintering temperature, and remove the gas that generates carbon oxides , since the step of removing the pore-forming agent is arranged after the sintering step, and the heating temperature is lower than the sintering temperature, the texture of the ceramic will no longer shrink during the process of removing the pore-forming agent, and the resulting porosity and pore size will basically not change.
- the porosity and pore size are easy to control, so the present application can obtain a porous ceramic atomizing core with high strength and high porosity.
- the ultra-high temperature sintering process of the present application can effectively remove the residual organic matter of the binder in the porous ceramic, so that the obtained porous ceramic atomizing core is purer and healthier.
- Fig. 1 is a SEM image of the porous ceramic atomizing core prepared in Example 1 of the present application.
- the present application discloses a preparation method of a porous ceramic atomizing core, comprising the following steps:
- Step 1 Provide raw materials, including: ceramic aggregate, binder, flux and pore-forming agent, wherein the pore-forming agent is selected from one or both of graphite powder and carbon powder.
- Step 2 wet mixing the ceramic aggregate, binder, flux and pore forming agent to obtain a mixture.
- Step 3 molding the mixture to obtain a green body.
- Step 4 degreasing the green body, removing the binder, and obtaining a degreased green body.
- Step 5 Put the degreased green body in a vacuum or an oxygen-free atmosphere for sintering.
- the sintering temperature is 1100°C-1500°C.
- the pore-forming agent is sintered at this temperature without melting to obtain a sintered green body.
- Step 6 Put the sintered body in an oxygen-containing atmosphere for heating reaction, the temperature of the heating reaction is 400°C-800°C, the pore-forming agent reacts with the oxygen in the oxygen-containing atmosphere, removes the pore-forming agent, and obtains porous ceramics atomizing core.
- the present application uses graphite and/or carbon powder as a pore-forming agent, which is resistant to high temperatures and cannot be removed during degreasing and sintering, so that the strength of ceramics can be improved by setting a higher sintering temperature; through sintering After the heating reaction, the pore-forming agent graphite and/or carbon powder can react with the oxygen in the oxygen-containing atmosphere at a lower temperature of 400 ° C to 800 ° C lower than the sintering temperature, and the gas that generates carbon oxides is removed.
- the step of removing the pore-forming agent is set after the sintering step, and the heating temperature is lower than the sintering temperature.
- the ceramic texture will no longer shrink, and the resulting porosity and pore size will basically not change.
- the porosity And the pore size is easy to control, so the present application can obtain a porous ceramic atomizing core with high strength and high porosity.
- the average particle size of the pore-forming agent is 10 ⁇ m to 50 ⁇ m, specifically 20 ⁇ m, 30 ⁇ m or 40 ⁇ m, etc. Since the preparation method of the present application is to sinter first and then create pores, the size of the ceramic shrinks when creating pores Therefore, the obtained pore size is basically about the size of the pore-forming agent, that is, pores with a pore size of 10 ⁇ m to 50 ⁇ m can be obtained. Therefore, the particle size of the pore-forming agent determines the pore size of the porous ceramic atomizing core. By controlling the particle size of the pore-forming agent, the pore size can be controlled, which facilitates mass production and obtains a consistent atomizing core.
- the reason why the porosity can be passed by controlling the mass ratio of the pore-forming agent to the ceramic aggregate and the flux is that in the preparation method of sintering first and then pore-forming in the present application, the removal of the pore-forming agent will not cause Variations in ceramic volume and morphology, therefore, porosity can be controlled by the aforementioned mass ratios.
- High porosity can increase the amount of smoke and the degree of reduction of the atomizing core to the atomization of e-liquid, and improve the taste of smoking.
- the ceramic aggregate, pore forming agent, flux and strength enhancer are all dried raw materials.
- Conditions for drying the ceramic aggregate, pore forming agent, flux and strength enhancer may be as follows: the drying temperature is 80°C-120°C, and the drying time is 8h-24h.
- step 2 all components can be mixed together at the same time, or some components can be mixed first to form a uniform premix, and then the premix can be mixed with the remaining components to obtain the final mixture.
- the method of grinding and mixing can also be used to grind and mix the components with the same particle size together to make the powder particle size more uniform.
- molding includes the following steps:
- Step 31 Banbury or knead the mixed material to obtain banbury/kneaded material.
- the mixed material can be placed in a banbury mixer for banburying to obtain a banbury, or the mixed material can be placed in a kneader for kneading to obtain a kneaded material.
- the conditions for banburying or kneading can be: The rotation speed is 200 rpm to 1500 rpm, the temperature is 70 ° C to 150 ° C, and the time is 1 h to 10 h, in order to make the mixture soft, dense, uniform, smooth and tough, easy to shape, and make the final product The resulting ceramics are of better quality.
- Step 32 Granulate or crush the banburying/kneading material to obtain granules.
- Step 33 Injection molding the pellets to obtain a green body.
- step 4 The main purpose of step 4 is to remove the binder.
- the removal mentioned here can be incomplete removal with a small amount of residue, because the binder is mainly an organic solvent with a low boiling point, and it can also be used in the subsequent sintering and pore-making processes. It is further removed by heating and volatilization.
- the process of degreasing is: heating up to 150°C-190°C at a heating rate of 0.01°C/min-5°C/min, keeping it warm for 1h-10h, and then heating at a rate of 0.05°C/min-2°C Raise the temperature to 200°C-240°C at a heating rate of /min, keep it warm for 1h-10h, and obtain a degreased green body after cooling.
- Different temperature sections adopt different heating rates, so that different binder components can be completely decomposed and volatilized at different temperature sections.
- step 5 the degreased body obtained in step 4 can be placed in a vacuum sintering furnace for sintering, or placed in an atmosphere sintering furnace for sintering under the protection of an oxygen-free atmosphere. It is worth noting that, during the whole sintering process, it should be carried out under vacuum conditions or under the protection of an oxygen-free atmosphere.
- the vacuum degree should always be kept below 10Pa.
- the oxygen-free atmosphere can specifically be argon, nitrogen or argon-hydrogen mixed gas.
- the sintering process may be as follows: heating up to 1100°C-1500°C at a heating rate of 1°C/min-20°C/min, keeping the temperature for 1h-10h, and cooling to obtain a sintered green body .
- the heating reaction process can be as follows: heating up to 400°C-800°C at a heating rate of 1°C/min-5°C/min, keeping the temperature for 1h-5h, cooling Finally, a porous ceramic atomizing core is obtained.
- the raw materials of the porous ceramic atomizing core include 10%-60% ceramic aggregate, 2%-40% flux, 5%-40% binder and 10% ⁇ 70% pore former.
- the raw material also includes a strength enhancer, and the strength enhancer can be selected from one of aluminum oxide, zinc oxide, magnesium oxide, calcium carbonate and calcium oxide.
- the strength enhancer is mainly used to form a porous ceramic atomizing core together with ceramic aggregate and flux to enhance the strength of the porous ceramic atomizing core material itself.
- the average particle size of the strength enhancer is 1 nm to 10 ⁇ m. More preferably, the strength enhancer is a nanoscale powder, that is, the average particle size is 1 nm to 100 nm. In addition to the properties of the material itself, it also has The activity, large specific surface area, and strong adsorption brought by the nanoscale size can further enhance the strength of the porous ceramic atomizing core material itself.
- the nano-scale powder also has the function of fluxing. The smaller the particle size, the lower the melting point and the greater the fluidity, which can make the component distribution of each raw material more uniform during the sintering process, the texture is tighter, and the strength is higher.
- nano-scale powder also has bonding properties. Ceramic aggregates are usually micron-scale powders, and nano-scale powders are dispersed in micron-scale powders, which can make the bonding performance between components stronger and make the texture tighter. .
- the raw materials of the porous ceramic atomizing core include 10% to 60% of ceramic aggregate, 2% to 40% of flux, 5% to 40% of binder, 10% %-70% pore forming agent and 0.1%-5% strength enhancer, using the raw materials of this embodiment, combined with the preparation method of this application, can greatly increase the compressive strength of the porous ceramic atomizing core.
- the ceramic aggregate can be selected from aluminum oxide powder, sepiolite powder, cordierite powder, diatomaceous earth, feldspar (such as potassium feldspar, albite), quartz powder and andalusite powder, etc.
- feldspar such as potassium feldspar, albite
- quartz powder and andalusite powder etc.
- diatomite is porous, high temperature resistant, strong and wear-resistant, which can ensure the strength, toughness and adsorption of the porous ceramic atomizing core, and is a porous ceramic atomizing core aggregate with excellent performance.
- the fluxing agent can be selected from one or both of low-temperature glass powder and clay, wherein the clay can be kaolin, tourmaline, vermiculite, etc.
- the function of the fluxing agent is mainly to reduce the sintering temperature of the ceramic aggregate, so that the green body The texture is tighter during sintering.
- the binder can be selected from one or more of paraffin wax, polyethylene or ethylene-vinyl acetate copolymer and stearic acid.
- the binder is mainly used for wet mixing and is easy to shape into a green body.
- the average particle size of the fluxing agent is 1 nm-1 ⁇ m, more preferably 1 nm-100 nm, and the nano-scale powder has greater fluidity and can have a more significant fluxing effect.
- the average particle diameter of the ceramic aggregate is 10 ⁇ m ⁇ 100 ⁇ m.
- the present application also discloses a porous ceramic atomizing core prepared by the above preparation method.
- the porosity of the porous ceramic atomizing core can be 60% to 75%, the average pore size can be 10 ⁇ m to 30 ⁇ m, and the compressive strength can be compared with the existing Technology can be improved by 1 to 2 times.
- the present application also discloses an electronic cigarette, which includes a host and the above-mentioned porous ceramic atomizing core.
- the porous ceramic atomizing core is installed on the host, and the host provides power and atomization control for the atomizing core.
- the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours.
- 480g graphite powder 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin.
- the particle size of diatomite is 30 ⁇ m
- the particle size of graphite powder is 30 ⁇ m
- the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale
- the particle size of kaolin is 10 ⁇ m.
- the obtained degreased green body was placed in a vacuum sintering furnace to keep the vacuum below 10Pa throughout the process, and the temperature was raised to 1400°C at a heating rate of 5°C/min, kept for 2h, and then lowered to room temperature. Put the sintered green body in an atmospheric sintering furnace, raise the temperature to 600°C at a rate of 1°C/min, keep it warm for 3 hours, cool to room temperature and take it out to obtain a high-strength porous ceramic atomizing core.
- the strength, porosity and pore size of the obtained porous ceramic atomizing core are shown in Table 2. Finally, the obtained ceramic body is combined with heating resistance wire or resistance slurry, and after sintering, a ceramic atomizing core for electronic cigarette field is obtained.
- Example 2 Compared with Example 1, the difference between Examples 2-8 is that the percentages of each component are different.
- the components and the parameters of each step are the same as in Example 1.
- the percentages of each component are shown in Table 1.
- the obtained porous ceramic atomized The strength, porosity and pore size of the core are shown in Table 2.
- Example 9 The only difference between Example 9 and Example 2 is that the particle size of the graphite in Example 9 is 20 ⁇ m, which is smaller than that of Example 2, 30 ⁇ m, and the rest are the same.
- the strength, porosity and pore size of the porous ceramic atomizing core obtained are As shown in table 2.
- Example 9 As can be seen from Table 2: comparing Example 9 with Example 2, the pore diameter of Example 9 is 15 ⁇ 5 ⁇ m, which is less than 18 ⁇ 5 ⁇ m of Example 2, and the porosity of Example 9 is approximately equal to the porosity of Example 2 ratio, are 70 ⁇ 2%, it can be seen that the pore diameter of the pores in the porous ceramic structure obtained in Example 9 is small, and the number is large. Compared with Example 9, the pore diameter of the pores in the porous ceramic structure obtained in Example 2 is large, and the number is small. . In addition, it can also be seen from Table 2 that the compressive strength of Example 9 is 530 ⁇ 50N/mm 2 , which is greater than 500 ⁇ 50N/mm 2 of Example 2. It can be seen that the porosity is close, and the smaller the pore diameter, the higher the compressive strength. bigger.
- Figure 1 shows the SEM image of the porous ceramic atomizing core prepared in Example 1. From the image in Figure 1, it can be seen that after high-temperature sintering, a complete skeleton is formed between the ceramic particles, which greatly improves the ceramic overall strength.
- the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours.
- 480g graphite powder 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin.
- the particle size of diatomite is 30 ⁇ m
- the particle size of graphite powder is 30 ⁇ m
- the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale
- the particle size of kaolin is 10 ⁇ m.
- Comparative Example 1 differs in that the degreased green body obtained in Comparative Example 1 is not sintered at a high temperature in a vacuum or an oxygen-free atmosphere, but is directly placed in the atmosphere for sintering, that is, sintering and pore making At the same time, referring to Table 2, comparing Example 1 and Comparative Example 1, the compressive strength of the porous ceramic atomizing core prepared in Comparative Example 1 was reduced to 260 ⁇ 40N/mm 2 , compared to 550 ⁇ 40N/mm 2 in Example 1. 50N/mm 2 , almost a 50% drop.
- the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours.
- 480g graphite powder 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin.
- the particle size of diatomite is 30 ⁇ m
- the particle size of graphite powder is 30 ⁇ m
- the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale
- the particle size of kaolin is 10 ⁇ m.
- the degreased green body obtained was placed in an atmospheric sintering furnace, and the temperature was raised to 1400° C. at a heating rate of 5° C./min, kept for 2 hours, and then lowered to room temperature to obtain a porous ceramic atomizing core.
- Comparative Example 2 differs in that the degreased green body obtained in Comparative Example 2 is not sintered at a high temperature in a vacuum or an oxygen-free atmosphere, but is directly placed in the atmosphere for sintering, and the sintering conditions are different from Compared with the staged temperature rise and lower sintering temperature (1200°C) of Example 1, the faster heating rate and higher sintering temperature (1500°C) in the vacuum sintering step of Example 1 were adopted, and the sintering and pore formation also At the same time, however, part of the porous ceramic atomizing core produced in Comparative Example 2 collapsed, and the product was scrapped.
- the reason may be that the heating rate was too fast, or the sintering temperature was too high, which caused the ceramic volume to shrink too much, resulting in collapse. Visible , sintering and pore making are carried out at the same time, the heating rate cannot be too fast, and the sintering temperature cannot be too high.
- Table 2 Strength, porosity and pore diameter of porous ceramic atomizing cores obtained in various examples and comparative examples
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Abstract
A porous ceramic atomizing core and a preparation method therefor, and an electronic cigarette. The preparation method comprises the following process: providing raw materials, the raw materials comprising a ceramic aggregate, a binder, a fluxing agent, and a pore-forming agent, wherein the pore-forming agent is selected from one or two of graphite powder and carbon powder; performing wet mixing on the ceramic aggregate, the binder, the fluxing agent, and the pore-forming agent to obtain a mixture; molding the mixture to obtain a green body; degreasing the green body, and removing the binder to obtain a degreased green body; placing the degreased green body in a vacuum or oxygen-free atmosphere for sintering, the temperature of the sintering being 1100°C-1500°C, and thus obtaining a sintered green body; placing the sintered green body in an oxygen-containing atmosphere for heating reaction, the temperature of the heating reaction being 400°C-800°C, the pore-forming agent reacting with oxygen in the oxygen-containing atmosphere, and removing the pore-forming agent to obtain the porous ceramic atomizing core. According to the preparation method, the porous ceramic atomizing core having high strength and high porosity can be obtained.
Description
本申请涉及陶瓷材料技术领域,更具体地,涉及一种多孔陶瓷雾化芯及其制备方法和电子烟。The present application relates to the technical field of ceramic materials, and more specifically, to a porous ceramic atomizing core, a preparation method thereof, and an electronic cigarette.
现有多孔陶瓷雾化芯的原料主要包括陶瓷骨料、粘结剂、助熔剂和造孔剂,制备方法通常包括混料、成型、脱脂和烧结四大步骤,其中,脱脂用于去除造孔剂和粘结剂,形成多孔结构,烧结主要通过高温提高多孔陶瓷的强度,随着烧结温度的增加,陶瓷质地越来越密实,从而提高强度,然而,要想维持多孔结构的孔隙率,又不允许烧结温度过高,否则,随着烧结的温度的增加,多孔结构越来越收缩,孔隙率变小,另,多孔结构收缩过程中,也易发生坍塌,因此,现有多孔陶瓷雾化芯在满足高孔隙率条件下难以满足高强度,强度低,雾化芯不仅易掉粉,影响抽吸口感,而且装配时易损坏,影响产品良率。The raw materials of the existing porous ceramic atomizing core mainly include ceramic aggregate, binder, flux and pore-forming agent. The preparation method usually includes four steps: mixing, molding, degreasing and sintering. Among them, degreasing is used to remove the pore-forming agent and binder to form a porous structure. Sintering mainly improves the strength of porous ceramics through high temperature. As the sintering temperature increases, the texture of ceramics becomes more and more dense, thereby increasing the strength. However, in order to maintain the porosity of the porous structure, and The sintering temperature is not allowed to be too high, otherwise, with the increase of the sintering temperature, the porous structure will shrink more and more, and the porosity will become smaller. In addition, the porous structure is prone to collapse during the shrinkage process. Therefore, the existing porous ceramic atomization It is difficult for the core to meet high strength under the condition of high porosity, and the strength is low. The atomizing core is not only easy to drop powder, which affects the taste of the suction, but also easy to be damaged during assembly, which affects the product yield.
发明内容Contents of the invention
本申请的目的在于克服现有技术存在的上述缺陷,提供一种高强度且高孔隙率的多孔陶瓷雾化芯及其制备方法和电子烟。The purpose of the present application is to overcome the above-mentioned defects in the prior art, and provide a high-strength and high-porosity porous ceramic atomizing core, a preparation method thereof, and an electronic cigarette.
为实现上述目的,本申请的技术方案如下:In order to achieve the above object, the technical scheme of the present application is as follows:
一种多孔陶瓷雾化芯的制备方法,包括以下过程:A method for preparing a porous ceramic atomizing core, comprising the following processes:
提供原料,所述原料包括:陶瓷骨料、粘结剂、助熔剂和造孔剂,其中,所述造孔剂选自石墨粉和碳粉中的一种或两种;Provide raw materials, the raw materials include: ceramic aggregate, binder, flux and pore-forming agent, wherein the pore-forming agent is selected from one or both of graphite powder and carbon powder;
将所述陶瓷骨料、所述粘结剂、所述助熔剂和所述造孔剂进行湿法混合,得到混合料;wet mixing the ceramic aggregate, the binder, the flux and the pore-forming agent to obtain a mixture;
将所述混合料进行成型,得到坯体;molding the mixture to obtain a green body;
将所述坯体进行脱脂,去除所述粘结剂,得到脱脂后的坯体;Degreasing the green body, removing the binder, and obtaining a degreased green body;
将所述脱脂后的坯体置于真空或无氧气氛中进行烧结,所述烧结的温度为1100℃~1500℃,得到烧结后的坯体;Sintering the degreased green body in a vacuum or an oxygen-free atmosphere at a temperature of 1100°C to 1500°C to obtain a sintered green body;
将所述烧结后的坯体置于含氧气氛中进行加热反应,所述加热反应的温度为400℃~800℃,所述造孔剂与所述含氧气氛中的氧气反应,去除所述造孔剂,得到所述多孔陶瓷雾化芯。The sintered green body is placed in an oxygen-containing atmosphere for a heating reaction, the temperature of the heating reaction is 400°C to 800°C, the pore-forming agent reacts with the oxygen in the oxygen-containing atmosphere, and the A pore-forming agent to obtain the porous ceramic atomizing core.
本申请还提供了一种上述制备方法制得的多孔陶瓷雾化芯。The present application also provides a porous ceramic atomizing core prepared by the above preparation method.
本申请还提供了一种电子烟,包括主机以及上述的多孔陶瓷雾化芯,所述多孔陶瓷雾化芯安装于所述主机上。The present application also provides an electronic cigarette, including a main body and the above-mentioned porous ceramic atomizing core, and the porous ceramic atomizing core is installed on the main body.
实施本申请实施例,将具有如下有益效果:Implementing the embodiment of the present application will have the following beneficial effects:
本申请实施例通过以石墨和/或碳粉为造孔剂,该造孔剂耐高温,在脱脂和烧结过程中均不能被去除,使得能通过设置较高的烧结温度提高陶瓷的强度;通过在烧结后进行加热反应,造孔剂石墨和/或碳粉能够在低于烧结温度的较低温度400℃~800℃下,与含氧气氛中的氧气 反应,生成碳氧化物的气体脱除,由于脱除造孔剂的步骤设置在烧结步骤之后,且加热温度小于烧结温度,因此,去除造孔剂过程中,陶瓷质地不再收缩,造成的孔隙率和孔隙大小基本不会发生变化,孔隙率和孔隙大小易控,故本申请能够得到高强度且高孔隙率的多孔陶瓷雾化芯。In the embodiment of the present application, graphite and/or carbon powder are used as pore-forming agents. The pore-forming agents are resistant to high temperatures and cannot be removed during degreasing and sintering, so that the strength of ceramics can be improved by setting a higher sintering temperature; Heating reaction after sintering, the pore-forming agent graphite and/or carbon powder can react with oxygen in the oxygen-containing atmosphere at a lower temperature of 400 ° C to 800 ° C lower than the sintering temperature, and remove the gas that generates carbon oxides , since the step of removing the pore-forming agent is arranged after the sintering step, and the heating temperature is lower than the sintering temperature, the texture of the ceramic will no longer shrink during the process of removing the pore-forming agent, and the resulting porosity and pore size will basically not change. The porosity and pore size are easy to control, so the present application can obtain a porous ceramic atomizing core with high strength and high porosity.
本申请的超高温烧结过程,可以有效去除多孔陶瓷中的粘结剂有机物残留,使得到的多孔陶瓷雾化芯更纯净、更健康。The ultra-high temperature sintering process of the present application can effectively remove the residual organic matter of the binder in the porous ceramic, so that the obtained porous ceramic atomizing core is purer and healthier.
为了更清楚地说明本申请实施例或现有技术中的技术方案,下面将对实施例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,下面描述中的附图仅仅是本申请的一些实施例,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。In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present application. Those skilled in the art can also obtain other drawings based on these drawings without creative work.
其中:in:
图1是本申请实施例1制得的多孔陶瓷雾化芯的SEM图像。Fig. 1 is a SEM image of the porous ceramic atomizing core prepared in Example 1 of the present application.
下面将结合本申请实施例中的附图,对本申请实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本申请一部分实施例,而不是全部的实施例。基于本申请中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例,都属于本申请保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the application with reference to the drawings in the embodiments of the application. Apparently, the described embodiments are only some of the embodiments of the application, not all of them. Based on the embodiments in this application, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of this application.
本申请公开了一种多孔陶瓷雾化芯的制备方法,包括以下步骤:The present application discloses a preparation method of a porous ceramic atomizing core, comprising the following steps:
步骤1:提供原料,原料包括:陶瓷骨料、粘结剂、助熔剂和造孔剂,其中,造孔剂选自石墨粉和碳粉中的一种或两种。Step 1: Provide raw materials, including: ceramic aggregate, binder, flux and pore-forming agent, wherein the pore-forming agent is selected from one or both of graphite powder and carbon powder.
步骤2:将陶瓷骨料、粘结剂、助熔剂和造孔剂进行湿法混合,得到混合料。Step 2: wet mixing the ceramic aggregate, binder, flux and pore forming agent to obtain a mixture.
步骤3:将混合料进行成型,得到坯体。Step 3: molding the mixture to obtain a green body.
步骤4:将坯体进行脱脂,去除粘结剂,得到脱脂后的坯体。Step 4: degreasing the green body, removing the binder, and obtaining a degreased green body.
步骤5:将脱脂后的坯体置于真空或无氧气氛中进行烧结,烧结的温度为1100℃~1500℃,造孔剂在该温度下烧结不发生熔融,得到烧结后的坯体。Step 5: Put the degreased green body in a vacuum or an oxygen-free atmosphere for sintering. The sintering temperature is 1100°C-1500°C. The pore-forming agent is sintered at this temperature without melting to obtain a sintered green body.
步骤6:将烧结后的坯体置于含氧气氛中进行加热反应,加热反应的温度为400℃~800℃,造孔剂与含氧气氛中的氧气反应,去除造孔剂,得到多孔陶瓷雾化芯。Step 6: Put the sintered body in an oxygen-containing atmosphere for heating reaction, the temperature of the heating reaction is 400°C-800°C, the pore-forming agent reacts with the oxygen in the oxygen-containing atmosphere, removes the pore-forming agent, and obtains porous ceramics atomizing core.
本申请通过以石墨和/或碳粉为造孔剂,该造孔剂耐高温,在脱脂和烧结过程中均不能被去除,使得能通过设置较高的烧结温度提高陶瓷的强度;通过在烧结后进行加热反应,造孔剂石墨和/或碳粉能够在低于烧结温度的较低温度400℃~800℃下,与含氧气氛中的氧气反应,生成碳氧化物的气体脱除,由于脱除造孔剂的步骤设置在烧结步骤之后,且加热温度小于烧结温度,因此,去除造孔剂过程中,陶瓷质地不再收缩,造成的孔隙率和孔隙大小基本不会发生变化,孔隙率和孔隙大小易控,故本申请能够得到高强度且高孔隙率的多孔陶瓷雾化芯。The present application uses graphite and/or carbon powder as a pore-forming agent, which is resistant to high temperatures and cannot be removed during degreasing and sintering, so that the strength of ceramics can be improved by setting a higher sintering temperature; through sintering After the heating reaction, the pore-forming agent graphite and/or carbon powder can react with the oxygen in the oxygen-containing atmosphere at a lower temperature of 400 ° C to 800 ° C lower than the sintering temperature, and the gas that generates carbon oxides is removed. The step of removing the pore-forming agent is set after the sintering step, and the heating temperature is lower than the sintering temperature. Therefore, during the process of removing the pore-forming agent, the ceramic texture will no longer shrink, and the resulting porosity and pore size will basically not change. The porosity And the pore size is easy to control, so the present application can obtain a porous ceramic atomizing core with high strength and high porosity.
在一具体实施例中,造孔剂的平均粒径为10μm~50μm,具体还可以为20μm、30μm或40μm等,由于本申请的制备方法是先烧结再造孔,造孔时,陶瓷的尺寸收缩较小,因此, 得到的孔隙大小基本约为造孔剂的大小,即可以得到孔径大小为10μm~50μm的孔隙。因此,造孔剂的粒径决定了多孔陶瓷雾化芯的孔隙大小,通过控制造孔剂的粒径可以控制孔隙的大小,便于批量生产,以及便于得到一致性的雾化芯。In a specific embodiment, the average particle size of the pore-forming agent is 10 μm to 50 μm, specifically 20 μm, 30 μm or 40 μm, etc. Since the preparation method of the present application is to sinter first and then create pores, the size of the ceramic shrinks when creating pores Therefore, the obtained pore size is basically about the size of the pore-forming agent, that is, pores with a pore size of 10 μm to 50 μm can be obtained. Therefore, the particle size of the pore-forming agent determines the pore size of the porous ceramic atomizing core. By controlling the particle size of the pore-forming agent, the pore size can be controlled, which facilitates mass production and obtains a consistent atomizing core.
进一步的,在一具体实施例中,造孔剂的质量:陶瓷骨料和助熔剂的质量和=0.6~0.8,使得孔隙率可以达到60%~80%的高孔隙率。之所以能通过控制造孔剂与陶瓷骨料和助熔剂的质量和的质量比来通过孔隙率,是因为本申请的先烧结后造孔的制备方法中,造孔剂的脱除不会引起陶瓷体积和形态的变化,因此,可以通过上述质量比来控制孔隙率。高孔隙率可以提升雾化芯对烟油雾化的烟雾量及还原度,提升抽吸口感。Further, in a specific embodiment, the quality of the pore-forming agent: the sum of the quality of the ceramic aggregate and the flux = 0.6-0.8, so that the porosity can reach a high porosity of 60%-80%. The reason why the porosity can be passed by controlling the mass ratio of the pore-forming agent to the ceramic aggregate and the flux is that in the preparation method of sintering first and then pore-forming in the present application, the removal of the pore-forming agent will not cause Variations in ceramic volume and morphology, therefore, porosity can be controlled by the aforementioned mass ratios. High porosity can increase the amount of smoke and the degree of reduction of the atomizing core to the atomization of e-liquid, and improve the taste of smoking.
在步骤1中,陶瓷骨料、造孔剂、助熔剂以及强度增强剂均为干燥后的原料。对陶瓷骨料、造孔剂、助熔剂以及强度增强剂进行干燥的条件可以为:干燥温度为80℃~120℃,干燥时间为8h~24h。In step 1, the ceramic aggregate, pore forming agent, flux and strength enhancer are all dried raw materials. Conditions for drying the ceramic aggregate, pore forming agent, flux and strength enhancer may be as follows: the drying temperature is 80°C-120°C, and the drying time is 8h-24h.
在步骤2中,可以将所有组份同时加入一起混合,也可以先将部分组份混合得均匀的预混料,然后再将预混料与余下组份混合得最终的混合料。也可以采用研磨混合的方法,使具有相同粒径的组份一起研磨混合,使粉末粒径更均匀。In step 2, all components can be mixed together at the same time, or some components can be mixed first to form a uniform premix, and then the premix can be mixed with the remaining components to obtain the final mixture. The method of grinding and mixing can also be used to grind and mix the components with the same particle size together to make the powder particle size more uniform.
在一较优实施例中,成型包括以下步骤:In a preferred embodiment, molding includes the following steps:
步骤31:将混合料进行密炼或捏合得到密炼/捏合料。Step 31: Banbury or knead the mixed material to obtain banbury/kneaded material.
在本步骤中,可以将混合料置于密炼机中进行密炼得到密炼料,或将混合料置于捏合机中进行捏合得到捏合料,具体的,密炼或捏合的条件可以为:转速为200转/小时~1500转/小时,温度为70℃~150℃,时间为1h~10h,以使混合料柔软、密实、均匀、光滑、有韧性为目的,便于成型,以及使最终制得的陶瓷质量更好。In this step, the mixed material can be placed in a banbury mixer for banburying to obtain a banbury, or the mixed material can be placed in a kneader for kneading to obtain a kneaded material. Specifically, the conditions for banburying or kneading can be: The rotation speed is 200 rpm to 1500 rpm, the temperature is 70 ° C to 150 ° C, and the time is 1 h to 10 h, in order to make the mixture soft, dense, uniform, smooth and tough, easy to shape, and make the final product The resulting ceramics are of better quality.
步骤32:将密炼/捏合料进行造粒或破碎,得到颗粒料。Step 32: Granulate or crush the banburying/kneading material to obtain granules.
步骤33:将颗粒料通过注塑成型,得到坯体。Step 33: Injection molding the pellets to obtain a green body.
步骤4的主要目的是去除粘结剂,这里所说的去除可以是留有少量残余的不完全去除,因为粘结剂主要为有机溶剂,沸点较低,还可以在后续的烧结以及造孔工艺中进一步通过加热挥发而去除。The main purpose of step 4 is to remove the binder. The removal mentioned here can be incomplete removal with a small amount of residue, because the binder is mainly an organic solvent with a low boiling point, and it can also be used in the subsequent sintering and pore-making processes. It is further removed by heating and volatilization.
具体的,在一具体实施例中,脱脂的过程为:以0.01℃/min~5℃/min的升温速率升温至150℃~190℃,保温1h~10h,然后以0.05℃/min~2℃/min的升温速率升温至200℃~240℃,保温1h~10h,冷却后得到脱脂后的坯体。不同温度段采用不同的升温速率,便于不同的粘结剂组份分别在不同的温度段完全分解挥发。Specifically, in a specific embodiment, the process of degreasing is: heating up to 150°C-190°C at a heating rate of 0.01°C/min-5°C/min, keeping it warm for 1h-10h, and then heating at a rate of 0.05°C/min-2°C Raise the temperature to 200°C-240°C at a heating rate of /min, keep it warm for 1h-10h, and obtain a degreased green body after cooling. Different temperature sections adopt different heating rates, so that different binder components can be completely decomposed and volatilized at different temperature sections.
在步骤5中,可以将步骤4得到的脱脂后的坯体置于真空烧结炉中进行烧结,也可以置于气氛烧结炉中在无氧气氛的保护下进行烧结。值得注意的是,在整个烧结过程中,应一直处于真空条件下或一直处于无氧气氛的保护下进行。In step 5, the degreased body obtained in step 4 can be placed in a vacuum sintering furnace for sintering, or placed in an atmosphere sintering furnace for sintering under the protection of an oxygen-free atmosphere. It is worth noting that, during the whole sintering process, it should be carried out under vacuum conditions or under the protection of an oxygen-free atmosphere.
当处于真空条件下,真空度应始终保持在10Pa以下,当处于无氧气氛的保护下时,无氧气氛具体可以为氩气、氮气或氩氢混合气等。When under vacuum conditions, the vacuum degree should always be kept below 10Pa. When under the protection of an oxygen-free atmosphere, the oxygen-free atmosphere can specifically be argon, nitrogen or argon-hydrogen mixed gas.
具体的,在一具体实施例中,烧结的过程可以为:以1℃/min~20℃/min的升温速率升温至1100℃~1500℃,保温1h~10h,冷却后得到烧结后的坯体。Specifically, in a specific embodiment, the sintering process may be as follows: heating up to 1100°C-1500°C at a heating rate of 1°C/min-20°C/min, keeping the temperature for 1h-10h, and cooling to obtain a sintered green body .
在步骤6中,具体的,在一较优实施例中,加热反应的过程可以为:以1℃/min~5℃/min的升温速率升温至400℃~800℃,保温1h~5h,冷却后得到多孔陶瓷雾化芯。In step 6, specifically, in a preferred embodiment, the heating reaction process can be as follows: heating up to 400°C-800°C at a heating rate of 1°C/min-5°C/min, keeping the temperature for 1h-5h, cooling Finally, a porous ceramic atomizing core is obtained.
在一具体实施例中,多孔陶瓷雾化芯的原料按质量百分比计,包括10%~60%的陶瓷骨料、2%~40%的助熔剂、5%~40%粘结剂以及10%~70%的造孔剂。In a specific embodiment, the raw materials of the porous ceramic atomizing core include 10%-60% ceramic aggregate, 2%-40% flux, 5%-40% binder and 10% ~70% pore former.
本申请为了进一步增强多孔陶瓷雾化芯的强度,在一具体实施例中,原料还包括强度增强剂,强度增强剂可以选自氧化铝、氧化锌、氧化镁、碳酸钙和氧化钙中的一种或两种以上,强度增强剂主要用于和陶瓷骨料、助熔剂一起形成多孔陶瓷雾化芯,增强多孔陶瓷雾化芯材料本身的强度。In order to further enhance the strength of the porous ceramic atomizing core in the present application, in a specific embodiment, the raw material also includes a strength enhancer, and the strength enhancer can be selected from one of aluminum oxide, zinc oxide, magnesium oxide, calcium carbonate and calcium oxide. The strength enhancer is mainly used to form a porous ceramic atomizing core together with ceramic aggregate and flux to enhance the strength of the porous ceramic atomizing core material itself.
在一具体实施例中,强度增强剂的平均粒径为1nm~10μm,更优选的,强度增强剂为纳米级粉末,即平均粒径为1nm~100nm,除了具有材料本身的性能外,还具有纳米级尺寸带来的活性、比表面积大、吸附性强等作用,能够进一步增强多孔陶瓷雾化芯材料本身的强度。另,纳米级粉末还具有助熔的作用,粒径越小,熔点越低,流动性越大,可以使各原料在烧结过程中组份分布更均匀,质地更紧密,以及强度更高。还有,纳米级粉末还具有粘结的性能,陶瓷骨料通常为微米级粉末,纳米级粉末分散在微米级粉末中,可以使各组份之间的粘结性能更强,使质地更紧密。In a specific embodiment, the average particle size of the strength enhancer is 1 nm to 10 μm. More preferably, the strength enhancer is a nanoscale powder, that is, the average particle size is 1 nm to 100 nm. In addition to the properties of the material itself, it also has The activity, large specific surface area, and strong adsorption brought by the nanoscale size can further enhance the strength of the porous ceramic atomizing core material itself. In addition, the nano-scale powder also has the function of fluxing. The smaller the particle size, the lower the melting point and the greater the fluidity, which can make the component distribution of each raw material more uniform during the sintering process, the texture is tighter, and the strength is higher. In addition, nano-scale powder also has bonding properties. Ceramic aggregates are usually micron-scale powders, and nano-scale powders are dispersed in micron-scale powders, which can make the bonding performance between components stronger and make the texture tighter. .
在一较优实施例中,多孔陶瓷雾化芯的原料按质量百分比计,包括10%~60%的陶瓷骨料、2%~40%的助熔剂、5%~40%粘结剂、10%~70%的造孔剂以及0.1%~5%的强度增强剂,采用本实施例的原料,结合本申请的制备方法,可以大幅提高多孔陶瓷雾化芯的抗压强度。In a preferred embodiment, the raw materials of the porous ceramic atomizing core include 10% to 60% of ceramic aggregate, 2% to 40% of flux, 5% to 40% of binder, 10% %-70% pore forming agent and 0.1%-5% strength enhancer, using the raw materials of this embodiment, combined with the preparation method of this application, can greatly increase the compressive strength of the porous ceramic atomizing core.
上述各实施例中,陶瓷骨料可以选自氧化铝粉、海泡石粉、堇青石粉、硅藻土、长石(如钾长石、钠长石)、石英粉和红柱石粉等中的一种或两种以上。其中,硅藻土多孔、耐高温、坚固、耐磨,可确保多孔陶瓷雾化芯的强度、韧性、吸附性,是一种性能较优异的多孔陶瓷雾化芯骨料。In each of the above-mentioned embodiments, the ceramic aggregate can be selected from aluminum oxide powder, sepiolite powder, cordierite powder, diatomaceous earth, feldspar (such as potassium feldspar, albite), quartz powder and andalusite powder, etc. One or more than two. Among them, diatomite is porous, high temperature resistant, strong and wear-resistant, which can ensure the strength, toughness and adsorption of the porous ceramic atomizing core, and is a porous ceramic atomizing core aggregate with excellent performance.
助熔剂可以选自低温玻璃粉和粘土中的一种或两种,其中,粘土可以是高岭土、电气石、蛭石等,助熔剂的作用主要是降低陶瓷骨料的烧结温度,使坯体在烧结过程中质地更紧密。The fluxing agent can be selected from one or both of low-temperature glass powder and clay, wherein the clay can be kaolin, tourmaline, vermiculite, etc. The function of the fluxing agent is mainly to reduce the sintering temperature of the ceramic aggregate, so that the green body The texture is tighter during sintering.
粘结剂可以选自石蜡、聚乙烯或乙烯-醋酸乙烯共聚物和硬脂酸中的一种或两种以上,粘结剂主要用于湿法混合,易造型成坯体。The binder can be selected from one or more of paraffin wax, polyethylene or ethylene-vinyl acetate copolymer and stearic acid. The binder is mainly used for wet mixing and is easy to shape into a green body.
在一具体实施例中,助熔剂的平均粒径为1nm~1μm,更优选的为1nm~100nm,纳米级粉末的流动性更大,能够起到更显著的助熔效果。In a specific embodiment, the average particle size of the fluxing agent is 1 nm-1 μm, more preferably 1 nm-100 nm, and the nano-scale powder has greater fluidity and can have a more significant fluxing effect.
在一具体实施例中,陶瓷骨料的平均粒径为10μm~100μm。In a specific embodiment, the average particle diameter of the ceramic aggregate is 10 μm˜100 μm.
本申请还公开了一种上述制备方法制得的多孔陶瓷雾化芯,多孔陶瓷雾化芯的孔隙率可以为60%~75%,平均孔径可以为10μm~30μm,抗压强度相比现有技术可以提高1~2倍。The present application also discloses a porous ceramic atomizing core prepared by the above preparation method. The porosity of the porous ceramic atomizing core can be 60% to 75%, the average pore size can be 10 μm to 30 μm, and the compressive strength can be compared with the existing Technology can be improved by 1 to 2 times.
本申请还公开了一种电子烟,包括主机以及上述的多孔陶瓷雾化芯,多孔陶瓷雾化芯安装于主机上,主机为雾化芯提供电源及雾化控制。The present application also discloses an electronic cigarette, which includes a host and the above-mentioned porous ceramic atomizing core. The porous ceramic atomizing core is installed on the host, and the host provides power and atomization control for the atomizing core.
以下为具体实施例。The following are specific examples.
实施例1Example 1
将硅藻土粉料置于干燥箱中进行干燥,设置温度为100℃,干燥12h。使用高精度天平称取此硅藻土480g。然后称取480g石墨粉,100g低温玻璃粉,10g氧化镁粉,10g氧化锌粉以及120g高岭土。其中,硅藻土粒径为30μm,石墨粉粒径为30μm,低温玻璃粉、氧化镁、氧化锌均为纳米级,高岭土粒径为10μm。将以上称量好的粉料置于三维混料机均匀混合4h得到预混料。称取600g石蜡,100g聚乙烯以及100g硬脂酸作为粘结剂。粘结剂及预混料一起置于密炼机中进行密炼,转速设置为500转/h,温度为130℃,时间为6h,得到密炼料。将制备得到的密炼料冷却至室温后倒入造粒机中造粒,得到均匀颗粒料。然后将此颗粒料采用注塑成型方法得到坯体。将坯体摆放于烧秸坩埚中,并一起放置于脱脂炉进行脱脂,炉温以0.05℃/min的升温速率至160℃,保温5h。然后以1℃/min的升温速率至210℃,保温5h,降至室温,取出。将得到的脱脂后的坯体,置于真空烧结炉中全程保持真空度在10Pa以下,以5℃/min的升温速率升温至1400℃,保温2h,降至室温。将此烧结后的坯体置于大气烧结炉中,以1℃/min的升温速率升温至600℃,保温3h,冷却至室温取出,得到高强度多孔陶瓷雾化芯。得到的多孔陶瓷雾化芯的强度、孔隙率和孔径如表2所示。最后将得到的陶瓷体与加热电阻丝或电阻浆料复合,烧结后得到电子烟领域用陶瓷雾化芯。Put the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours. Use high precision balance to weigh this diatomite 480g. Then weigh 480g graphite powder, 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin. Among them, the particle size of diatomite is 30 μm, the particle size of graphite powder is 30 μm, the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale, and the particle size of kaolin is 10 μm. Place the above-weighed powder in a three-dimensional mixer and mix it uniformly for 4 hours to obtain a premix. Weigh 600g paraffin, 100g polyethylene and 100g stearic acid as binder. The binder and the premix are put together in an internal mixer for internal mixing, the speed is set at 500 rpm, the temperature is 130° C., and the time is 6 hours to obtain the internal mixing material. The prepared banburying material is cooled to room temperature and then poured into a granulator for granulation to obtain uniform granules. Then the pellets are used for injection molding to obtain green bodies. Place the green body in a straw-burning crucible, and place it together in a degreasing furnace for degreasing. The furnace temperature is raised to 160°C at a rate of 0.05°C/min, and kept for 5 hours. Then increase the temperature to 210°C at a rate of 1°C/min, keep it warm for 5 hours, cool down to room temperature, and take it out. The obtained degreased green body was placed in a vacuum sintering furnace to keep the vacuum below 10Pa throughout the process, and the temperature was raised to 1400°C at a heating rate of 5°C/min, kept for 2h, and then lowered to room temperature. Put the sintered green body in an atmospheric sintering furnace, raise the temperature to 600°C at a rate of 1°C/min, keep it warm for 3 hours, cool to room temperature and take it out to obtain a high-strength porous ceramic atomizing core. The strength, porosity and pore size of the obtained porous ceramic atomizing core are shown in Table 2. Finally, the obtained ceramic body is combined with heating resistance wire or resistance slurry, and after sintering, a ceramic atomizing core for electronic cigarette field is obtained.
实施例2~8Embodiment 2-8
实施例2~8与实施例1相比,区别仅在于各组份的百分比不同,组份及各步骤参数均与实施例1相同,各组份的百分比参见表1,得到的多孔陶瓷雾化芯的强度、孔隙率和孔径如表2所示。Compared with Example 1, the difference between Examples 2-8 is that the percentages of each component are different. The components and the parameters of each step are the same as in Example 1. The percentages of each component are shown in Table 1. The obtained porous ceramic atomized The strength, porosity and pore size of the core are shown in Table 2.
表1:实施例1~8的各组份百分比/%Table 1: each component percentage/% of embodiment 1~8
实施例9Example 9
实施例9与实施例2的不同点仅在于,实施例9中的石墨的粒径为20μm,小于实施例2的30μm,其余均相同,得到的多孔陶瓷雾化芯的强度、孔隙率和孔径如表2所示。The only difference between Example 9 and Example 2 is that the particle size of the graphite in Example 9 is 20 μm, which is smaller than that of Example 2, 30 μm, and the rest are the same. The strength, porosity and pore size of the porous ceramic atomizing core obtained are As shown in table 2.
从表2可以看到:将实施例9与实施例2相比,实施例9的孔径为15±5μm,小于实施 例2的18±5μm,实施例9的孔隙率约等于实施例2的孔隙率,均为70±2%,可见,实施例9得到的多孔陶瓷结构中孔隙的孔径小,数量多,相比实施例9,实施例2得到的多孔陶瓷结构中孔隙的孔径大,数量小。另,由表2还可以看到:实施例9的抗压强度为530±50N/mm
2,大于实施例2的500±50N/mm
2,可见,孔隙率接近,孔径越小,抗压强度越大。
As can be seen from Table 2: comparing Example 9 with Example 2, the pore diameter of Example 9 is 15 ± 5 μm, which is less than 18 ± 5 μm of Example 2, and the porosity of Example 9 is approximately equal to the porosity of Example 2 ratio, are 70 ± 2%, it can be seen that the pore diameter of the pores in the porous ceramic structure obtained in Example 9 is small, and the number is large. Compared with Example 9, the pore diameter of the pores in the porous ceramic structure obtained in Example 2 is large, and the number is small. . In addition, it can also be seen from Table 2 that the compressive strength of Example 9 is 530±50N/mm 2 , which is greater than 500±50N/mm 2 of Example 2. It can be seen that the porosity is close, and the smaller the pore diameter, the higher the compressive strength. bigger.
实验例1Experimental example 1
参考图1,图1给出了实施例1制得的多孔陶瓷雾化芯的SEM图像,从图1的图像可以看到:经过高温烧结后,陶瓷颗粒之间形成完整骨架,大大提升了陶瓷整体强度。Referring to Figure 1, Figure 1 shows the SEM image of the porous ceramic atomizing core prepared in Example 1. From the image in Figure 1, it can be seen that after high-temperature sintering, a complete skeleton is formed between the ceramic particles, which greatly improves the ceramic overall strength.
对比例1Comparative example 1
将硅藻土粉料置于干燥箱中进行干燥,设置温度为100℃,干燥12h。使用高精度天平称取此硅藻土480g。然后称取480g石墨粉,100g低温玻璃粉,10g氧化镁粉,10g氧化锌粉以及120g高岭土。其中,硅藻土粒径为30μm,石墨粉粒径为30μm,低温玻璃粉、氧化镁、氧化锌均为纳米级,高岭土粒径为10μm。将以上称量好的粉料置于三维混料机均匀混合4h得到预混料。称取600g石蜡,100g聚乙烯以及100g硬脂酸作为粘结剂。粘结剂及预混料一起置于密炼机中进行密炼,转速设置为500转/h,温度为130℃,时间为6h,得到密炼料。将制备得到的密炼料冷却至室温后倒入造粒机中造粒,得到均匀颗粒料。然后将此颗粒料采用注塑成型方法得到坯体。将坯体摆放于烧秸坩埚中,并一起放置于脱脂炉进行脱脂,炉温以0.05℃/min的升温速率至160℃,保温5h。然后以1℃/min的升温速率至210℃,保温5h,降至室温,取出。将得到的脱脂后的坯体,置于大气烧结炉中,以1℃/min的升温速率升温至800℃,保温2h,然后以1℃/min的升温速率继续升温至1200℃,保温2h,冷却至室温取出,得到多孔陶瓷雾化芯。得到的多孔陶瓷雾化芯的强度、孔隙率和孔径如表2所示。Put the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours. Use high precision balance to weigh this diatomite 480g. Then weigh 480g graphite powder, 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin. Among them, the particle size of diatomite is 30 μm, the particle size of graphite powder is 30 μm, the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale, and the particle size of kaolin is 10 μm. Place the above-weighed powder in a three-dimensional mixer and mix it uniformly for 4 hours to obtain a premix. Weigh 600g paraffin, 100g polyethylene and 100g stearic acid as binder. The binder and the premix are put together in an internal mixer for internal mixing, the speed is set at 500 rpm, the temperature is 130° C., and the time is 6 hours to obtain the internal mixing material. The prepared banburying material is cooled to room temperature and then poured into a granulator for granulation to obtain uniform granules. Then the pellets are used for injection molding to obtain green bodies. Place the green body in a straw-burning crucible, and place it together in a degreasing furnace for degreasing. The furnace temperature is raised to 160°C at a rate of 0.05°C/min, and kept for 5 hours. Then increase the temperature to 210°C at a rate of 1°C/min, keep it warm for 5 hours, cool down to room temperature, and take it out. The degreased green body obtained was placed in an atmospheric sintering furnace, and the temperature was raised to 800°C at a heating rate of 1°C/min, and kept for 2 hours, and then continued to be heated at a heating rate of 1°C/min to 1200°C, and kept for 2 hours. Cool to room temperature and take out to obtain a porous ceramic atomizing core. The strength, porosity and pore size of the obtained porous ceramic atomizing core are shown in Table 2.
对比例1相比实施例1,区别在于,对比例1将得到的脱脂后的坯体未在真空或无氧气氛中进行高温烧结,而是直接置于大气中进行烧结,即烧结和造孔同时进行,参考表2,将实施例1和对比例1相比,对比例1制得的多孔陶瓷雾化芯的抗压强度降低至260±40N/mm
2,相比实施例1的550±50N/mm
2,几乎下降50%。
Compared with Example 1, Comparative Example 1 differs in that the degreased green body obtained in Comparative Example 1 is not sintered at a high temperature in a vacuum or an oxygen-free atmosphere, but is directly placed in the atmosphere for sintering, that is, sintering and pore making At the same time, referring to Table 2, comparing Example 1 and Comparative Example 1, the compressive strength of the porous ceramic atomizing core prepared in Comparative Example 1 was reduced to 260±40N/mm 2 , compared to 550±40N/mm 2 in Example 1. 50N/mm 2 , almost a 50% drop.
对比例2Comparative example 2
将硅藻土粉料置于干燥箱中进行干燥,设置温度为100℃,干燥12h。使用高精度天平称取此硅藻土480g。然后称取480g石墨粉,100g低温玻璃粉,10g氧化镁粉,10g氧化锌粉以及120g高岭土。其中,硅藻土粒径为30μm,石墨粉粒径为30μm,低温玻璃粉、氧化镁、氧化锌均为纳米级,高岭土粒径为10μm。将以上称量好的粉料置于三维混料机均匀混合4h得到预混料。称取600g石蜡,100g聚乙烯以及100g硬脂酸作为粘结剂。粘结剂及预混料一起置于密炼机中进行密炼,转速设置为500转/h,温度为130℃,时间为6h,得到密炼料。将制备得到的密炼料冷却至室温后倒入造粒机中造粒,得到均匀颗粒料。然后将此颗粒料采用注塑成型方法得到坯体。将坯体摆放于烧秸坩埚中,并一起放置于脱脂炉进行脱脂,炉温以0.05℃/min的升温速率至160℃,保温5h。然后以1℃/min的升温速率至210℃,保温5h,降至室温,取出。将得到的脱脂后的坯体,置于大气烧结炉中,以5℃/min的升温速率升温至1400℃,保温2h,降至室温,得到多孔陶瓷雾化芯。Put the diatomaceous earth powder in a drying oven for drying, set the temperature at 100° C., and dry for 12 hours. Use high precision balance to weigh this diatomite 480g. Then weigh 480g graphite powder, 100g low-temperature glass powder, 10g magnesium oxide powder, 10g zinc oxide powder and 120g kaolin. Among them, the particle size of diatomite is 30 μm, the particle size of graphite powder is 30 μm, the particle size of low-temperature glass powder, magnesium oxide, and zinc oxide is nanoscale, and the particle size of kaolin is 10 μm. Place the above-weighed powder in a three-dimensional mixer and mix it uniformly for 4 hours to obtain a premix. Weigh 600g paraffin, 100g polyethylene and 100g stearic acid as binder. The binder and the premix are put together in an internal mixer for internal mixing, the speed is set at 500 rpm, the temperature is 130° C., and the time is 6 hours to obtain the internal mixing material. The prepared banburying material is cooled to room temperature and then poured into a granulator for granulation to obtain uniform granules. Then the pellets are used for injection molding to obtain green bodies. Place the green body in a straw-burning crucible, and place it together in a degreasing furnace for degreasing. The furnace temperature is raised to 160°C at a rate of 0.05°C/min, and kept for 5 hours. Then increase the temperature to 210°C at a rate of 1°C/min, keep it warm for 5 hours, cool down to room temperature, and take it out. The degreased green body obtained was placed in an atmospheric sintering furnace, and the temperature was raised to 1400° C. at a heating rate of 5° C./min, kept for 2 hours, and then lowered to room temperature to obtain a porous ceramic atomizing core.
对比例2相比实施例1,区别在于,对比例2将得到的脱脂后的坯体未在真空或无氧气氛中进行高温烧结,而是直接置于大气中进行烧结,且烧结条件不同于对比例1的分段升温以及较低的烧结温度(1200℃),而是采用了实施例1真空烧结步骤中较快的升温速率和较高的烧结温度(1500℃),烧结和造孔也同时进行,然而,对比例2制得的多孔陶瓷雾化芯部分出现坍塌现象,产品报废,原因可能在于,升温速率过快,或烧结温度过高,使陶瓷体积收缩过大,导致坍塌,可见,烧结和造孔同时进行,升温速率不能过快,且烧结温度不能太高。Compared with Example 1, Comparative Example 2 differs in that the degreased green body obtained in Comparative Example 2 is not sintered at a high temperature in a vacuum or an oxygen-free atmosphere, but is directly placed in the atmosphere for sintering, and the sintering conditions are different from Compared with the staged temperature rise and lower sintering temperature (1200°C) of Example 1, the faster heating rate and higher sintering temperature (1500°C) in the vacuum sintering step of Example 1 were adopted, and the sintering and pore formation also At the same time, however, part of the porous ceramic atomizing core produced in Comparative Example 2 collapsed, and the product was scrapped. The reason may be that the heating rate was too fast, or the sintering temperature was too high, which caused the ceramic volume to shrink too much, resulting in collapse. Visible , sintering and pore making are carried out at the same time, the heating rate cannot be too fast, and the sintering temperature cannot be too high.
表2:各实施例和对比例得到的多孔陶瓷雾化芯的强度、孔隙率和孔径Table 2: Strength, porosity and pore diameter of porous ceramic atomizing cores obtained in various examples and comparative examples
the | 平均抗压强度/N/mm 2 Average compressive strength/N/mm 2 | 平均孔径/μmAverage pore size/μm | 平均孔隙率/%Average porosity/% |
实施例1Example 1 | 550550 | 2020 | 6868 |
实施例2Example 2 | 500500 | 1818 | 7070 |
实施例3Example 3 | 620620 | 1818 | 6363 |
实施例4Example 4 | 600600 | 1616 | 6565 |
实施例5Example 5 | 600600 | 1515 | 6262 |
实施例6Example 6 | 500500 | 1818 | 6060 |
实施例7Example 7 | 470470 | 1515 | 6060 |
实施例8Example 8 | 420420 | 1515 | 5858 |
实施例9Example 9 | 530530 | 1515 | 7070 |
对比例1Comparative example 1 | 260260 | 2020 | 6060 |
对比例2Comparative example 2 | ———— | ———— | ———— |
以上所述实施例仅表达了本申请的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对申请专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本申请构思的前提下,还可以做出若干变形和改进,这些都属于本申请的保护范围。因此,本申请专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present application, and the description thereof is relatively specific and detailed, but should not be construed as limiting the scope of the patent application. It should be noted that those skilled in the art can make several modifications and improvements without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the scope of protection of the patent application should be based on the appended claims.
Claims (20)
- 一种多孔陶瓷雾化芯的制备方法,其中,包括以下过程:A method for preparing a porous ceramic atomizing core, which includes the following process:提供原料,所述原料包括:陶瓷骨料、粘结剂、助熔剂和造孔剂,其中,所述造孔剂选自石墨粉和碳粉中的一种或两种;Provide raw materials, the raw materials include: ceramic aggregates, binders, fluxes and pore-forming agents, wherein the pore-forming agents are selected from one or both of graphite powder and carbon powder;将所述陶瓷骨料、所述粘结剂、所述助熔剂和所述造孔剂进行湿法混合,得到混合料;wet mixing the ceramic aggregate, the binder, the flux and the pore-forming agent to obtain a mixture;将所述混合料进行成型,得到坯体;molding the mixture to obtain a green body;将所述坯体进行脱脂,去除所述粘结剂,得到脱脂后的坯体;Degreasing the green body, removing the binder, and obtaining a degreased green body;将所述脱脂后的坯体置于真空或无氧气氛中进行烧结,所述烧结的温度为1100℃~1500℃,得到烧结后的坯体;Sintering the degreased green body in a vacuum or an oxygen-free atmosphere at a temperature of 1100°C to 1500°C to obtain a sintered green body;将所述烧结后的坯体置于含氧气氛中进行加热反应,所述加热反应的温度为400℃~800℃,所述造孔剂与所述含氧气氛中的氧气反应,去除所述造孔剂,得到所述多孔陶瓷雾化芯。The sintered green body is placed in an oxygen-containing atmosphere for a heating reaction, the temperature of the heating reaction is 400°C to 800°C, the pore-forming agent reacts with the oxygen in the oxygen-containing atmosphere, and the A pore-forming agent to obtain the porous ceramic atomizing core.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述造孔剂的平均粒径为10μm~50μm。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the average particle diameter of the pore-forming agent is 10 μm-50 μm.
- 根据权利要求2所述的多孔陶瓷雾化芯的制备方法,其中,所述造孔剂的质量:所述陶瓷骨料和所述助熔剂的质量和=0.6~0.8。The method for preparing a porous ceramic atomizing core according to claim 2, wherein the mass of the pore forming agent: the mass sum of the ceramic aggregate and the flux = 0.6-0.8.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述烧结的过程为:以1℃/min~20℃/min的升温速率升温至1100℃~1500℃,保温1h~10h,冷却后得到所述烧结后的坯体;The preparation method of the porous ceramic atomizing core according to claim 1, wherein, the sintering process is: heating up to 1100°C-1500°C at a heating rate of 1°C/min-20°C/min, and holding the temperature for 1h-10h , to obtain the sintered green body after cooling;所述加热反应的过程为:以1℃/min~5℃/min的升温速率升温至400℃~800℃,保温1h~5h,冷却后得到所述多孔陶瓷雾化芯;The process of the heating reaction is: heating up to 400-800°C at a heating rate of 1°C/min-5°C/min, keeping the temperature for 1h-5h, and obtaining the porous ceramic atomizing core after cooling;所述脱脂的过程为:以0.01℃/min~5℃/min的升温速率升温至150℃~190℃,保温1h~10h,然后以0.05℃/min~2℃/min的升温速率升温至200℃~240℃,保温1h~10h,冷却后得到所述脱脂后的坯体。The degreasing process is as follows: heat up to 150°C-190°C at a heating rate of 0.01°C/min-5°C/min, keep warm for 1h-10h, and then heat up to 200°C at a heating rate of 0.05°C/min-2°C/min ℃~240℃, heat preservation for 1h~10h, and obtain the degreased green body after cooling.
- 根据权利要求2所述的多孔陶瓷雾化芯的制备方法,其中,所述烧结的过程为:以1℃/min~20℃/min的升温速率升温至1100℃~1500℃,保温1h~10h,冷却后得到所述烧结后的坯体;The method for preparing a porous ceramic atomizing core according to claim 2, wherein the sintering process is: heating up to 1100°C-1500°C at a heating rate of 1°C/min-20°C/min, and holding the temperature for 1h-10h , to obtain the sintered green body after cooling;所述加热反应的过程为:以1℃/min~5℃/min的升温速率升温至400℃~800℃,保温1h~5h,冷却后得到所述多孔陶瓷雾化芯;The process of the heating reaction is: heating up to 400-800°C at a heating rate of 1°C/min-5°C/min, keeping the temperature for 1h-5h, and obtaining the porous ceramic atomizing core after cooling;所述脱脂的过程为:以0.01℃/min~5℃/min的升温速率升温至150℃~190℃,保温1h~10h,然后以0.05℃/min~2℃/min的升温速率升温至200℃~240℃,保温1h~10h,冷却后得到所述脱脂后的坯体。The degreasing process is as follows: heat up to 150°C-190°C at a heating rate of 0.01°C/min-5°C/min, keep warm for 1h-10h, and then heat up to 200°C at a heating rate of 0.05°C/min-2°C/min ℃~240℃, heat preservation for 1h~10h, and obtain the degreased green body after cooling.
- 根据权利要求3所述的多孔陶瓷雾化芯的制备方法,其中,所述烧结的过程为:以1℃/min~20℃/min的升温速率升温至1100℃~1500℃,保温1h~10h,冷却后得到所述烧结后的坯体;The preparation method of the porous ceramic atomizing core according to claim 3, wherein the sintering process is: raising the temperature to 1100°C-1500°C at a heating rate of 1°C/min-20°C/min, and holding the temperature for 1h-10h , to obtain the sintered green body after cooling;所述加热反应的过程为:以1℃/min~5℃/min的升温速率升温至400℃~800℃,保温 1h~5h,冷却后得到所述多孔陶瓷雾化芯;The process of the heating reaction is as follows: heating up to 400°C-800°C at a heating rate of 1°C/min-5°C/min, keeping the temperature for 1h-5h, and obtaining the porous ceramic atomizing core after cooling;所述脱脂的过程为:以0.01℃/min~5℃/min的升温速率升温至150℃~190℃,保温1h~10h,然后以0.05℃/min~2℃/min的升温速率升温至200℃~240℃,保温1h~10h,冷却后得到所述脱脂后的坯体。The degreasing process is as follows: heat up to 150°C-190°C at a heating rate of 0.01°C/min-5°C/min, keep warm for 1h-10h, and then heat up to 200°C at a heating rate of 0.05°C/min-2°C/min ℃~240℃, heat preservation for 1h~10h, and obtain the degreased green body after cooling.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述原料还包括强度增强剂,所述强度增强剂选自氧化铝、氧化锌、氧化镁、碳酸钙和氧化钙中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 1, wherein, the raw material also includes a strength enhancer, and the strength enhancer is selected from aluminum oxide, zinc oxide, magnesium oxide, calcium carbonate and calcium oxide one or more;按质量百分比计,所述陶瓷骨料的质量百分比为10%~60%,所述助熔剂的质量百分比为2%~40%,所述粘结剂的质量百分比为5%~40%,所述造孔剂的质量百分比为10%~70%,所述强度增强剂的质量百分比为0.1%~5%。In terms of mass percentage, the mass percentage of the ceramic aggregate is 10% to 60%, the mass percentage of the flux is 2% to 40%, and the mass percentage of the binder is 5% to 40%. The mass percentage of the pore forming agent is 10%-70%, and the mass percentage of the strength enhancer is 0.1%-5%.
- 根据权利要求2所述的多孔陶瓷雾化芯的制备方法,其中,所述原料还包括强度增强剂,所述强度增强剂选自氧化铝、氧化锌、氧化镁、碳酸钙和氧化钙中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 2, wherein, the raw material also includes a strength enhancer, and the strength enhancer is selected from aluminum oxide, zinc oxide, magnesium oxide, calcium carbonate and calcium oxide one or more;按质量百分比计,所述陶瓷骨料的质量百分比为10%~60%,所述助熔剂的质量百分比为2%~40%,所述粘结剂的质量百分比为5%~40%,所述造孔剂的质量百分比为10%~70%,所述强度增强剂的质量百分比为0.1%~5%。In terms of mass percentage, the mass percentage of the ceramic aggregate is 10% to 60%, the mass percentage of the flux is 2% to 40%, and the mass percentage of the binder is 5% to 40%. The mass percentage of the pore forming agent is 10%-70%, and the mass percentage of the strength enhancer is 0.1%-5%.
- 根据权利要求3所述的多孔陶瓷雾化芯的制备方法,其中,所述原料还包括强度增强剂,所述强度增强剂选自氧化铝、氧化锌、氧化镁、碳酸钙和氧化钙中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 3, wherein, the raw material also includes a strength enhancer, and the strength enhancer is selected from aluminum oxide, zinc oxide, magnesium oxide, calcium carbonate and calcium oxide one or more;按质量百分比计,所述陶瓷骨料的质量百分比为10%~60%,所述助熔剂的质量百分比为2%~40%,所述粘结剂的质量百分比为5%~40%,所述造孔剂的质量百分比为10%~70%,所述强度增强剂的质量百分比为0.1%~5%。In terms of mass percentage, the mass percentage of the ceramic aggregate is 10% to 60%, the mass percentage of the flux is 2% to 40%, and the mass percentage of the binder is 5% to 40%. The mass percentage of the pore forming agent is 10%-70%, and the mass percentage of the strength enhancer is 0.1%-5%.
- 根据权利要求7所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料选自氧化铝粉、海泡石粉、堇青石粉、硅藻土、长石、石英粉和红柱石粉中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 7, wherein the ceramic aggregate is selected from alumina powder, sepiolite powder, cordierite powder, diatomite, feldspar, quartz powder and andalusite powder one or more of them;所述助熔剂选自低温玻璃粉和粘土中的一种或两种以上;The flux is selected from one or more of low-temperature glass powder and clay;所述粘结剂选自石蜡、聚乙烯或乙烯-醋酸乙烯共聚物和硬脂酸中的一种或两种以上。The binder is selected from one or more of paraffin wax, polyethylene or ethylene-vinyl acetate copolymer and stearic acid.
- 根据权利要求8所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料选自氧化铝粉、海泡石粉、堇青石粉、硅藻土、长石、石英粉和红柱石粉中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 8, wherein the ceramic aggregate is selected from alumina powder, sepiolite powder, cordierite powder, diatomite, feldspar, quartz powder and andalusite powder one or more of them;所述助熔剂选自低温玻璃粉和粘土中的一种或两种以上;The flux is selected from one or more of low-temperature glass powder and clay;所述粘结剂选自石蜡、聚乙烯或乙烯-醋酸乙烯共聚物和硬脂酸中的一种或两种以上。The binder is selected from one or more of paraffin wax, polyethylene or ethylene-vinyl acetate copolymer and stearic acid.
- 根据权利要求9所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料选自氧化铝粉、海泡石粉、堇青石粉、硅藻土、长石、石英粉和红柱石粉中的一种或两种以上;The preparation method of the porous ceramic atomizing core according to claim 9, wherein the ceramic aggregate is selected from alumina powder, sepiolite powder, cordierite powder, diatomite, feldspar, quartz powder and andalusite powder one or more of them;所述助熔剂选自低温玻璃粉和粘土中的一种或两种以上;The flux is selected from one or more of low-temperature glass powder and clay;所述粘结剂选自石蜡、聚乙烯或乙烯-醋酸乙烯共聚物和硬脂酸中的一种或两种以上。The binder is selected from one or more of paraffin wax, polyethylene or ethylene-vinyl acetate copolymer and stearic acid.
- 根据权利要求7所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料的平均粒径为10μm~100μm;The method for preparing a porous ceramic atomizing core according to claim 7, wherein the average particle size of the ceramic aggregate is 10 μm to 100 μm;所述强度增强剂的平均粒径为1nm~10μm;The average particle diameter of the strength enhancer is 1 nm to 10 μm;所述助熔剂的平均粒径为1nm~1μm。The average particle diameter of the flux is 1 nm˜1 μm.
- 根据权利要求8所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料的平均粒径 为10μm~100μm;The preparation method of the porous ceramic atomizing core according to claim 8, wherein the average particle diameter of the ceramic aggregate is 10 μm to 100 μm;所述强度增强剂的平均粒径为1nm~10μm;The average particle diameter of the strength enhancer is 1 nm to 10 μm;所述助熔剂的平均粒径为1nm~1μm。The average particle diameter of the flux is 1 nm˜1 μm.
- 根据权利要求9所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料的平均粒径为10μm~100μm;The method for preparing a porous ceramic atomizing core according to claim 9, wherein the average particle size of the ceramic aggregate is 10 μm to 100 μm;所述强度增强剂的平均粒径为1nm~10μm;The average particle diameter of the strength enhancer is 1 nm to 10 μm;所述助熔剂的平均粒径为1nm~1μm。The average particle diameter of the flux is 1 nm˜1 μm.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述成型包括以下过程:The preparation method of the porous ceramic atomizing core according to claim 1, wherein said molding comprises the following process:将所述混合料进行密炼或捏合得到密炼/捏合料;Banburying or kneading the mixture to obtain banburying/kneading;将所述密炼/捏合料进行造粒或破碎,得到颗粒料;Granulating or crushing the banburying/kneading material to obtain granules;将所述颗粒料通过注塑成型,得到所述坯体。The pellets are injection molded to obtain the green body.
- 根据权利要求2所述的多孔陶瓷雾化芯的制备方法,其中,所述成型包括以下过程:The preparation method of the porous ceramic atomizing core according to claim 2, wherein said forming comprises the following process:将所述混合料进行密炼或捏合得到密炼/捏合料;Banburying or kneading the mixture to obtain banburying/kneading;将所述密炼/捏合料进行造粒或破碎,得到颗粒料;Granulating or crushing the banburying/kneading material to obtain granules;将所述颗粒料通过注塑成型,得到所述坯体。The pellets are injection molded to obtain the green body.
- 根据权利要求3所述的多孔陶瓷雾化芯的制备方法,其中,所述成型包括以下过程:The preparation method of the porous ceramic atomizing core according to claim 3, wherein said forming comprises the following process:将所述混合料进行密炼或捏合得到密炼/捏合料;Banburying or kneading the mixture to obtain banburying/kneading;将所述密炼/捏合料进行造粒或破碎,得到颗粒料;Granulating or crushing the banburying/kneading material to obtain granules;将所述颗粒料通过注塑成型,得到所述坯体。The pellets are injection molded to obtain the green body.
- 一种多孔陶瓷雾化芯,其中,采用如权利要求1所述的制备方法制得。A porous ceramic atomizing core, which is produced by the preparation method as claimed in claim 1.
- 一种电子烟,其中,包括主机以及如权利要求19所述的多孔陶瓷雾化芯,所述多孔陶瓷雾化芯安装于所述主机上。An electronic cigarette, comprising a host and the porous ceramic atomizing core according to claim 19, the porous ceramic atomizing core is installed on the host.
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