WO2022135010A1 - Porous ceramic atomization core and preparation method therefor, and electronic cigarette - Google Patents
Porous ceramic atomization core and preparation method therefor, and electronic cigarette Download PDFInfo
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- WO2022135010A1 WO2022135010A1 PCT/CN2021/132966 CN2021132966W WO2022135010A1 WO 2022135010 A1 WO2022135010 A1 WO 2022135010A1 CN 2021132966 W CN2021132966 W CN 2021132966W WO 2022135010 A1 WO2022135010 A1 WO 2022135010A1
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- porous ceramic
- atomizing core
- mass percentage
- ceramic atomizing
- kneading
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- 239000000919 ceramic Substances 0.000 title claims abstract description 181
- 239000003571 electronic cigarette Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000889 atomisation Methods 0.000 title abstract description 11
- 238000005245 sintering Methods 0.000 claims abstract description 56
- 238000004898 kneading Methods 0.000 claims abstract description 47
- 238000005238 degreasing Methods 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 30
- 239000000843 powder Substances 0.000 claims abstract description 29
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011230 binding agent Substances 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 19
- 238000001746 injection moulding Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims description 51
- 238000000034 method Methods 0.000 claims description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000004793 Polystyrene Substances 0.000 claims description 11
- 229920002223 polystyrene Polymers 0.000 claims description 11
- 239000005995 Aluminium silicate Substances 0.000 claims description 8
- 235000021355 Stearic acid Nutrition 0.000 claims description 8
- 235000012211 aluminium silicate Nutrition 0.000 claims description 8
- 235000013871 bee wax Nutrition 0.000 claims description 8
- 239000012166 beeswax Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 8
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 8
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 8
- 239000012188 paraffin wax Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000008117 stearic acid Substances 0.000 claims description 8
- 239000006004 Quartz sand Substances 0.000 claims description 6
- 239000004203 carnauba wax Substances 0.000 claims description 6
- -1 polyethylene Polymers 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000010433 feldspar Substances 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
- 229920000573 polyethylene Polymers 0.000 claims description 5
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 229910052613 tourmaline Inorganic materials 0.000 claims description 5
- 239000011032 tourmaline Substances 0.000 claims description 5
- 229940070527 tourmaline Drugs 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 239000011162 core material Substances 0.000 description 85
- 239000011148 porous material Substances 0.000 description 24
- 229910010293 ceramic material Inorganic materials 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 6
- 238000000465 moulding Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000005469 granulation Methods 0.000 description 3
- 230000003179 granulation Effects 0.000 description 3
- 238000011031 large-scale manufacturing process Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 238000001272 pressureless sintering Methods 0.000 description 3
- 229910052656 albite Inorganic materials 0.000 description 2
- 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 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000004512 die casting Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229920001684 low density polyethylene Polymers 0.000 description 2
- 239000004702 low-density polyethylene Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010345 tape casting Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000004506 ultrasonic cleaning Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910052878 cordierite Inorganic materials 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 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 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000030279 gene silencing Effects 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000009747 swallowing Effects 0.000 description 1
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- 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
- C04B38/067—Macromolecular compounds
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/70—Manufacture
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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
- C04B35/01—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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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3427—Silicates other than clay, e.g. water glass
- C04B2235/3463—Alumino-silicates other than clay, e.g. mullite
- C04B2235/3472—Alkali metal alumino-silicates other than clay, e.g. spodumene, alkali feldspars such as albite or orthoclase, micas such as muscovite, zeolites such as natrolite
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Definitions
- the present application relates to the technical field of ceramic materials, in particular to a porous ceramic atomizing core and a preparation method thereof, and an electronic cigarette.
- Porous ceramic material is a kind of porous ceramic material with open pore diameter and high open porosity, which is made of high-quality raw materials such as corundum sand, silicon carbide, cordierite, etc., and is prepared by molding and special high-temperature sintering process.
- High temperature, high pressure, acid, alkali and organic medium corrosion resistance, good biological inertness, controllable pore structure and high open porosity, long service life, good product regeneration performance, etc. can be suitable for precision filtration of various media And separation, high pressure gas exhaust silencing, gas distribution and electrolytic diaphragm, etc.
- the atomizer As the heating element of electronic cigarette, the atomizer is one of the important components. When inhaling, it achieves the effect of "swallowing clouds and mist".
- the carrier used to adsorb e-liquid in the atomizer mainly adopts inorganic non-metal atomizing core material, which not only has strong adsorption capacity, but also is non-toxic, harmless, safe and reliable, non-flammable and stable. Therefore, the porous ceramic atomizing core is one of the good materials suitable for absorbing smoke oil. Further, the porosity, strength, pore size and distribution of the porous ceramic atomizing core have an important impact on the atomization effect and smoking experience of the electronic cigarette.
- the main methods for preparing porous ceramic atomizing cores include dry pressing, tape casting, hot die casting, and grouting.
- the main difficulty lies in precisely controlling the pore size, pore morphology and pore size of the porous ceramic atomizing core distribution, increase the porosity as much as possible, improve the atomization efficiency of e-liquid and reduce the cost.
- dry pressing, hot die casting, grouting, and tape casting have complex processes, high cost, low strength of the prepared porous ceramic atomizing core, and low forming efficiency, which are not conducive to automated production, so they are not conducive to industrial large-scale production.
- the size and density of the aggregate of the porous ceramic atomizing core, the binder and the pore-forming agent are quite different, which is easy to cause poor material uniformity during the preparation process; and the dry pressing method requires high press pressure, low production efficiency, and poor performance. unstable.
- the present application provides a porous ceramic atomizing core and its preparation method and electronic cigarette, adopting the following technical solutions:
- a preparation method of a porous ceramic atomizing core, the porous ceramic atomizing core being applied to an electronic cigarette atomizing core comprising the following steps:
- Banburying or kneading the premix, binder and dispersant to obtain banbury/kneading material granulating or crushing the banburying/kneading material to obtain granular ceramic feed;
- the ceramic green body is subjected to degreasing treatment with preset degreasing conditions under the condition of burying powder of calcined alumina;
- the ceramic blank obtained by degreasing is sintered under the atmospheric conditions under the preset sintering conditions to obtain the porous ceramic atomizing core.
- the particle size of the calcined alumina is 20-70 ⁇ m
- the burying condition of the calcined alumina is that the burying depth is 20-70 ⁇ m. 3 to 4 cm.
- the degreasing conditions are: heating from room temperature to 140-160°C for 0.5 ⁇ 1.5h, then heated to 240-260°C at a heating rate of 0.1-0.2°C/min, then heated to 440-460°C at a heating rate of 0.2-0.3°C/min for 1.5-2.5h, and then heated to 2.4-2.6°C
- the heating rate was raised to 890-910 °C for 0.5-1.5 h at a heating rate of /min, and finally cooled with the furnace.
- the sintering conditions are as follows: the temperature is raised from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5- 1.5h, then the temperature was raised to 1100-1200°C at a heating rate of 1.5-2.5°C/min for 1.5-2.5h, and finally cooled with the furnace.
- the drying treatment conditions are drying at 115-125° C. for 2-4 hours.
- the conditions for banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
- the injection temperature in the injection molding is 50°C-70°C.
- the mass percentage of the ceramic aggregate is ⁇ 45-60%
- the mass percentage of the sintering aid is 20-25%
- the The mass percentage of the pore agent is 20-30%.
- the total amount of banburying/kneading material is 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, and the mass percentage of the binder is 30-40%, so The mass percentage of the dispersant is 1-5%.
- the ceramic aggregate includes at least one of diatomite, feldspar, and quartz sand, all of which have firm,
- the sintering aid includes at least one of low temperature lead-free glass powder, kaolin and tourmaline, which can play The sintering temperature is lowered to promote the densification of the ceramic body
- the binder includes at least one of paraffin wax, beeswax, palm wax, and polyethylene, which can keep the body from deformation and reduce ceramic defects caused by thermal stress.
- the pore-forming agent includes at least one of polymethyl methacrylate, polyvinyl alcohol, and polystyrene, which can control the pore size and pore size of the porous ceramic atomizing core rate, to obtain the interpenetrating pore structure in the porous ceramic atomizing core;
- the dispersing agent including stearic acid can ensure that the powder is fully mixed and dispersed during banburying and maintains uniformity.
- a porous ceramic atomizing core is prepared by the above-mentioned preparation method of the porous ceramic atomizing core.
- the porous ceramic atomizing core has a micropore diameter of 10-30 ⁇ m, a density of 0.8-1.2 g/cm 3 , and a porosity of 50 ⁇ m. ⁇ 70%.
- the sintering conditions are as follows: the temperature is raised from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5-1.5h, Then, the temperature is raised to 1100-1200°C at a heating rate of 1.5-2.5°C/min for 1.5-2.5h, and finally cooled with the furnace.
- the conditions of the drying treatment are drying at 115-125°C for 2-4 hours.
- the conditions of banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
- the injection temperature in the injection molding is 50°C-70°C.
- the porous ceramic atomizing core in the step of mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix, Taking the total amount of the premix to be 100%, in terms of mass percentage, the mass percentage of the ceramic aggregate is 45-60%, the mass percentage of the sintering aid is 20-25%, and the mass percentage of the pore-forming agent is 20-25%. The percentage is 20 to 30%.
- the total amount of Banbury/kneading material is 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, the mass percentage of the binder is 30-40%, and the dispersant is The mass percentage is 1 to 5%.
- the ceramic aggregate includes at least one of diatomite, feldspar, and quartz sand;
- the sintering aid includes low-temperature lead-free At least one of glass powder, kaolin and tourmaline;
- the binder includes at least one of paraffin, beeswax, palm wax and polyethylene;
- the pore-forming agent includes polymethyl methacrylate, polyvinyl alcohol , at least one of polystyrene;
- the dispersant includes stearic acid.
- An electronic cigarette includes a main unit and the above-mentioned porous ceramic atomizing core, wherein the porous ceramic atomizing core is installed on the main unit.
- the ceramic aggregate, sintering aid and pore-forming agent are mixed, and then the binder and dispersing agent are used for banburying or kneading, injection molding, degreasing and sintering to obtain high porosity.
- the present application solves the problems of low strength and low forming efficiency of the porous ceramic atomizing core prepared by the existing process, which is not conducive to automatic production.
- the porous ceramic atomizing core provided by the present application has high strength, strong material uniformity, high production efficiency, and improved The strength of the ceramic atomizing core improves production efficiency.
- the porous ceramic atomizing core prepared by the preparation method of the present application forms uniformly distributed micropores of 10-30 ⁇ m, the density is 0.8-1.2 g/cm3, and the porosity reaches 50-70%. It is applied to electronic cigarettes and atomized. The effect is good and the taste is full.
- FIG. 1 is a schematic diagram of the porous ceramic atomizing core prepared in Example 1 of the application under an electron scanning microscope.
- the embodiment of the present application provides a preparation of a porous ceramic atomizing core The method, wherein the porous ceramic atomizing core is applied to an electronic cigarette atomizing core.
- the preparation method of the porous ceramic atomizing core includes the following steps: (1) drying; (2) mixing; (3) banburying/kneading and granulation/crushing; (3) injection molding; (5) Degreasing treatment; (6) sintering treatment.
- the step (1) is specifically: drying the ceramic aggregate and the sintering aid.
- the ceramic aggregate and sintering aid are placed in a drying oven at 120°C for 2-4 hours, and the moisture adsorbed by the powder is discharged.
- the step (2) is specifically: mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix.
- the dried ceramic aggregate, sintering aid and pore-forming agent are weighed according to the mass ratio and placed on a three-dimensional mixer or ball mill for mixing.
- the step (3) is specifically as follows: banburying or kneading the premix, binder and dispersant to obtain banbury/kneading material; and then granulating or crushing the banburying/kneading material. , get granular ceramic feed.
- the premix and the binder are placed in a kneader or an internal mixer for kneading or internal mixing. It should be noted that after melting the binder first, add the premix consisting of ceramic aggregate, sintering aid and pore-forming agent powder, knead or banbury at 80°C-140°C for 2- 4h. Next, the muddy material obtained after banburying, namely banburying/kneading material, is placed in a granulator for granulation or cooled and then placed in a crusher for crushing.
- the step (4) is specifically as follows: injecting the granular ceramic feedstock to obtain a ceramic green body.
- the crushed granular ceramic feed is added to a special injection molding machine for ceramics for injection molding, and the injection temperature is 50°C-70°C.
- the step (5) is specifically as follows: degreasing the ceramic green body under the condition of burying the calcined alumina.
- the degreasing condition of the degreasing treatment is to heat up from room temperature to 140 to 160° C. for 0.5 to 1.5 h at a heating rate of 0.4 to 0.6° C./min, and then to heat at a temperature of 0.1 to 0.2° C./min for 0.5 to 1.5 hours.
- the temperature is increased to 240 ⁇ 260°C at a rate of 0.2 ⁇ 0.3°C/min, then the temperature is increased to 440 ⁇ 460°C for 1.5 ⁇ 2.5h at a heating rate of 0.2 ⁇ 0.3°C/min, and then the temperature is increased to 890 ⁇ 910°C at a heating rate of 2.4 ⁇ 2.6°C/min for 0.5 hours. ⁇ 1.5h, and finally cooled with the furnace.
- Different heating rates are used in different temperature sections, which can better allow different raw materials to be decomposed and released at appropriate temperature sections, and further provide the dimension of the ceramic embryo, avoiding the problem of collapse due to incomplete decomposition caused by a single heating rate or rapid heating.
- the degreasing treatment is carried out under the condition of burying powder of calcined ⁇ - Al 2 O 3 (alumina ) .
- the capillary effect of the fine powder increases the rate of debinding, and prevents the ceramic from collapsing due to its own gravity during debinding by the above-mentioned specific debinding conditions, so as to maintain the overall dimension of the product.
- the step (6) is specifically: sintering the ceramic blank obtained by degreasing under atmospheric conditions to obtain a porous ceramic atomizing core.
- the sintering process is to heat up from room temperature to 890-910°C for 0.5-1.5 h at a heating rate of 4-6°C/min, and then heat up at a heating rate of 1.5-2.5°C/min To 1100 ⁇ 1200 °C heat preservation for 1.5 ⁇ 2.5h, and finally cooling with the furnace.
- the binder, pore-forming agent, and dispersing agent described in the present application are completely volatilized and decomposed during the degreasing and sintering process, and are completely removed from the ceramic matrix, so as to avoid organic residues and maintain a good porosity.
- the porous ceramic atomizing core prepared by the preparation method of the present application forms uniformly distributed micropores of 10-30 ⁇ m, the density is 0.8-1.2 g/cm 3 , and the porosity reaches 50-70%. The effect is good and the taste is full.
- the ceramic aggregate, sintering aid and pore-forming agent are mixed, and then the binder and dispersing agent are used for banburying or kneading, injection molding, degreasing and sintering to obtain high porosity.
- the present application solves the problems of low strength and low forming efficiency of the porous ceramic atomizing core prepared by the existing process, which is not conducive to automatic production.
- the porous ceramic atomizing core provided by the present application has high strength, strong material uniformity, high production efficiency, and improved The strength of the ceramic atomizing core improves production efficiency.
- the total amount of premix is 100%
- the mass percentage of the ceramic aggregate is 45-60%
- the sintering aid is 45-60% by mass.
- the mass percentage is 20-25%
- the mass percentage of the pore-forming agent is 20-30%.
- the total amount of Banbury/kneading material is 100%, and the mass percentage of the premix is 55-65% by mass percentage, and the adhesive
- the mass percentage of the agent is 30-40%, and the mass percentage of the dispersing agent is 1-5%.
- the ceramic aggregate includes at least one of diatomaceous earth, feldspar (such as potassium feldspar, albite), and quartz sand;
- feldspar such as potassium feldspar, albite
- quartz sand The advantages of wide range and low cost can ensure the strength and toughness of the porous ceramic atomizing core
- the sintering aid includes at least one of low-temperature lead-free glass powder, kaolin or tourmaline, which can reduce the sintering temperature and promote the ceramic blank.
- the binder includes at least one of paraffin wax, beeswax, palm wax, and polyethylene, which can keep the green body from deformation, can reduce the ceramic defects caused by thermal stress, and is conducive to improving the porous ceramic mist.
- the yield of the atomizing core; the pore-forming agent includes at least one of polymethyl methacrylate, polyvinyl alcohol, and polystyrene, which can control the pore size and porosity of the porous ceramic atomizing core, and obtain the porous ceramic atomizing core.
- the interpenetrating pore structure in the core; the dispersant includes stearic acid, which can ensure that the powder is fully mixed and dispersed during banburying and maintains uniformity.
- ultrasonic cleaning is further included: ultrasonic cleaning is performed on the degreasing and sintered porous ceramic atomizing core, and finally, the finished product is obtained by drying in an oven.
- This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
- Kneading and crushing by mass percentage, add 60% of premix, 25% of paraffin, 5% of beeswax, 5% of low-density polyethylene and 5% of stearic acid into the kneader, and mix at 145°C Kneading for 3 hours, and cooling after kneading to obtain bulk ceramic kneading material, which is then put into a jaw crusher for crushing to obtain granular ceramic feedstock with uniform size;
- the ceramic green body is obtained by the injection molding process.
- the process parameters are: the molding pressure is 20bar, the speed is 20cm 3 /s, the injection temperature is 100°C, and the mold temperature is 30°C to obtain a ceramic green body. blank;
- Degreasing treatment The ceramic green body is placed in an alumina saggar, and calcined alumina powder with a thickness of 3 cm is buried. The particle size of the alumina powder is 70um, and the saggar is placed in a degreasing furnace. The heating rate per min was raised from room temperature to 150°C, held for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min The heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
- Sintering treatment take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering.
- the sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1150 °C for 2 h at a heating rate of 2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
- Figure 1 shows the pore structure of the porous ceramic atomizing core prepared in this example under an electron scanning microscope. It can be seen from the figure that the porous ceramic atomizing core prepared in this example has uniformly distributed pores.
- This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
- the ceramic green body is obtained by the injection molding process.
- the process parameters are: the molding pressure is 20bar, the speed is 20cm 3 /s, the injection temperature is 55°C, and the mold temperature is 26°C to obtain a ceramic green body. blank;
- Degreasing treatment The ceramic green body is placed in an alumina sagger, and calcined alumina powder with a thickness of 2 cm is buried. The particle size of the alumina powder is 50 ⁇ m. The saggar is placed in a degreasing furnace.
- the degreasing conditions are: 0.5 ° C
- the heating rate per min was raised from room temperature to 150°C, held for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min
- the heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
- Sintering treatment take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering.
- the sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1100 °C for 2 h at a heating rate of 2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
- This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
- Kneading and crushing by mass percentage, add 60% of premix, 25% of paraffin, 5% of beeswax, 5% of low-density polyethylene and 5% of stearic acid into the kneader, and mix at 140°C Kneading for 3 hours, and cooling after kneading to obtain bulk ceramic kneading material, which is then put into a jaw crusher for crushing to obtain granular ceramic feedstock with uniform size;
- the ceramic green body is obtained by the injection molding process.
- the process parameters are as follows: the molding pressure is 20 bar, the speed is 20 cm 3 /s, the injection temperature is 60 °C, and the mold temperature is 30 °C, and the ceramic green body is obtained. blank;
- Degreasing treatment The ceramic green body is placed in an alumina sagger, and calcined alumina powder with a thickness of 3 cm is buried. The particle size of the alumina powder is 70 ⁇ m. The saggar is placed in a degreasing furnace.
- the degreasing conditions are: 0.5 ° C
- the heating rate was raised from room temperature to 150°C/min, kept for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min
- the heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
- Sintering treatment take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering.
- the sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1180 °C for 2 h at a heating rate of 2.2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
- This embodiment provides an electronic cigarette, which includes a main body and a porous ceramic atomizing core, and the porous ceramic atomizing core is installed on the main body.
- the porous ceramic atomizing core can be the porous ceramic atomizing core prepared by any of the methods in Examples 1-3.
- the porous ceramic atomizing core used in this embodiment has high porosity, uniform pore size, high green body strength, strong material uniformity, and uniform pore size. When applied to electronic cigarettes, the atomization effect is good and the taste is full.
Abstract
Disclosed are a porous ceramic atomization core and a preparation method therefor, and an electronic cigarette. The preparation method for a porous ceramic atomization core comprises the following steps: carrying out a drying treatment on a ceramic aggregate and a sintering aid; mixing the dried ceramic aggregate, the dried sintering aid and a pore-forming agent to obtain a premix; internally mixing or kneading the premix, a binder and a dispersant to obtain an internally mixed/kneaded material; granulating or crushing the internally mixed/kneaded material to obtain a granular ceramic feed; carrying out injection molding on the granular ceramic feed to obtain a ceramic green body; carrying out a degreasing treatment on the ceramic green body under a powder burying condition of calcined alumina under a preset degreasing condition; and sintering a degreased ceramic blank, which is under an atmospheric condition, under a preset sintering condition to obtain a porous ceramic atomization core. The porous ceramic atomization core provided in the present application has a high strength, high material uniformity and high production efficiency, thereby improving the strength of the ceramic atomization core, and improving the production efficiency.
Description
本申请要求于2020年12月25日提交中国专利局、申请号为2020115651617,申请名称为“一种多孔陶瓷雾化芯及其制备方法和电子烟”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。This application claims the priority of the Chinese patent application filed on December 25, 2020 with the application number 2020115651617 and titled "A Porous Ceramic Atomizing Core and Its Preparation Method and Electronic Cigarette", the entire contents of which are Incorporated herein by reference.
本申请涉及陶瓷材料技术领域,特别是涉及了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, in particular to a porous ceramic atomizing core and a preparation method thereof, and an electronic cigarette.
多孔陶瓷材料是以刚玉砂、碳化硅、堇青石等优质原料为主料、经过成型和特殊高温烧结工艺制备的一种具有开孔孔径、高开口气孔率的一种多孔性陶瓷材料、具有耐高温,高压、抗酸、碱和有机介质腐蚀,良好的生物惰性、可控的孔结构及高的开口孔隙率、使用寿命长、产品再生性能好等优点,可以适用于各种介质的精密过滤与分离、高压气体排气消音、气体分布及电解隔膜等。Porous ceramic material is a kind of porous ceramic material with open pore diameter and high open porosity, which is made of high-quality raw materials such as corundum sand, silicon carbide, cordierite, etc., and is prepared by molding and special high-temperature sintering process. High temperature, high pressure, acid, alkali and organic medium corrosion resistance, good biological inertness, controllable pore structure and high open porosity, long service life, good product regeneration performance, etc., can be suitable for precision filtration of various media And separation, high pressure gas exhaust silencing, gas distribution and electrolytic diaphragm, etc.
雾化器作为电子烟的加热元器件,是重要组成部件之一,其原理是:通过电池供电发热,使雾化器中储存的烟油挥发,产生一定量的烟雾,从而让消费者在抽吸的时候达到“吞云吐雾”的效果。随着技术的发展,雾化器中用于吸附烟油的载体主要采用无机非金属雾化芯材料,其不仅具有强大的吸附能力,还具有无毒无害、安全可靠、无可燃性、稳定性等优点,因而,多孔陶瓷雾化芯是适合用于吸附烟油的良好材料之一。进一步地,多孔陶瓷雾化芯的孔隙率、强度、孔径大小及分布对电子烟的雾化效果、抽吸体验起到了重要影响。As the heating element of electronic cigarette, the atomizer is one of the important components. When inhaling, it achieves the effect of "swallowing clouds and mist". With the development of technology, the carrier used to adsorb e-liquid in the atomizer mainly adopts inorganic non-metal atomizing core material, which not only has strong adsorption capacity, but also is non-toxic, harmless, safe and reliable, non-flammable and stable. Therefore, the porous ceramic atomizing core is one of the good materials suitable for absorbing smoke oil. Further, the porosity, strength, pore size and distribution of the porous ceramic atomizing core have an important impact on the atomization effect and smoking experience of the electronic cigarette.
现行技术中,制备多孔陶瓷雾化芯的主要方法有干压成型、流延成型、热压铸成型、注浆成形方法,主要难点在于精确控制多孔陶瓷雾化芯的孔径大小、孔形貌及孔分布,尽可能地提高孔隙率、提高烟油雾化效率进而降低成本。但是干压成型、热压铸成型和注浆成型、流延成型工艺复杂,成本高,制备的多孔陶瓷雾化芯强度较低,成型效率低,不利于自动化生产,故而不利于工业上规模化生产应用,多孔陶瓷雾化芯的骨料与结合剂、造孔剂的大小和密度均相差大,在制备过程中易造成材料均匀性差;而且干压法需要压机压力大,生产效率低,性能不稳定。In the current technology, the main methods for preparing porous ceramic atomizing cores include dry pressing, tape casting, hot die casting, and grouting. The main difficulty lies in precisely controlling the pore size, pore morphology and pore size of the porous ceramic atomizing core distribution, increase the porosity as much as possible, improve the atomization efficiency of e-liquid and reduce the cost. However, dry pressing, hot die casting, grouting, and tape casting have complex processes, high cost, low strength of the prepared porous ceramic atomizing core, and low forming efficiency, which are not conducive to automated production, so they are not conducive to industrial large-scale production. Application, the size and density of the aggregate of the porous ceramic atomizing core, the binder and the pore-forming agent are quite different, which is easy to cause poor material uniformity during the preparation process; and the dry pressing method requires high press pressure, low production efficiency, and poor performance. unstable.
鉴于此,克服以上现有技术中的缺陷,提供一种新的电子烟用多孔陶瓷雾化芯及其制备方法成为本领域亟待解决的技术问题。In view of this, it is an urgent technical problem to be solved in the art to provide a new porous ceramic atomizing core for electronic cigarette and a preparation method thereof to overcome the above defects in the prior art.
申请内容Application content
基于此,有必要针对上述技术问题,提供一种多孔陶瓷雾化芯及其制备方法和电子烟,以解决现有工艺制备的多孔陶瓷雾化芯强度较低,成型效率低,不利于自动化生产的问题。Based on this, it is necessary to provide a porous ceramic atomizing core, a preparation method thereof, and an electronic cigarette in view of the above technical problems, so as to solve the problem that the porous ceramic atomizing core prepared by the existing process has low strength and low molding efficiency, which is not conducive to automatic production. The problem.
为了解决上述技术问题,本申请提供一种多孔陶瓷雾化芯及其制备方法和电子烟,采用了如下所述的技术方案:In order to solve the above-mentioned technical problems, the present application provides a porous ceramic atomizing core and its preparation method and electronic cigarette, adopting the following technical solutions:
一种多孔陶瓷雾化芯的制备方法,所述多孔陶瓷雾化芯应用于电子烟雾化芯,其包括以下步骤:A preparation method of a porous ceramic atomizing core, the porous ceramic atomizing core being applied to an electronic cigarette atomizing core, comprising the following steps:
将陶瓷骨料和助烧剂进行干燥处理;Dry the ceramic aggregate and sintering aid;
将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料;Mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix;
将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料;对所述密炼/捏合料进行造粒或破碎,得到颗粒状陶瓷喂料;Banburying or kneading the premix, binder and dispersant to obtain banbury/kneading material; granulating or crushing the banburying/kneading material to obtain granular ceramic feed;
将所述颗粒状陶瓷喂料通过注射成型,得到陶瓷生坯;injecting the granular ceramic feedstock to obtain a ceramic green body;
将所述陶瓷生坯在煅烧氧化铝的埋粉条件下,以预设的脱脂条件进行脱 脂处理;The ceramic green body is subjected to degreasing treatment with preset degreasing conditions under the condition of burying powder of calcined alumina;
将脱脂得到的陶瓷坯于大气条件下,以预设的烧结条件进行烧结,得到多孔陶瓷雾化芯。The ceramic blank obtained by degreasing is sintered under the atmospheric conditions under the preset sintering conditions to obtain the porous ceramic atomizing core.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述煅烧氧化铝的粒径为20~70μm,所述煅烧氧化铝的埋粉条件是埋粉深度为3~4cm。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in the present application, the particle size of the calcined alumina is 20-70 μm, and the burying condition of the calcined alumina is that the burying depth is 20-70 μm. 3 to 4 cm.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述脱脂条件为:以0.4~0.6℃/min的升温速率从室温升温至140~160℃保温0.5~1.5h,接着以0.1~0.2℃/min的升温速率升温至240~260℃,再以0.2~0.3℃/min的升温速率升温至440~460℃保温1.5~2.5h,然后以2.4~2.6℃/min的升温速率升温至890~910℃保温0.5~1.5h,最后随炉冷却。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in the present application, the degreasing conditions are: heating from room temperature to 140-160°C for 0.5~ 1.5h, then heated to 240-260°C at a heating rate of 0.1-0.2°C/min, then heated to 440-460°C at a heating rate of 0.2-0.3°C/min for 1.5-2.5h, and then heated to 2.4-2.6°C The heating rate was raised to 890-910 °C for 0.5-1.5 h at a heating rate of /min, and finally cooled with the furnace.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述烧结条件为:以4~6℃/min的升温速率从室温升温至890~910℃保温0.5~1.5h,接着以1.5~2.5℃/min的升温速率升温至1100~1200℃保温1.5~2.5h,最后随炉冷却。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in the present application, the sintering conditions are as follows: the temperature is raised from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5- 1.5h, then the temperature was raised to 1100-1200°C at a heating rate of 1.5-2.5°C/min for 1.5-2.5h, and finally cooled with the furnace.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述干燥处理的条件为115~125℃干燥2-4h。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in the present application, the drying treatment conditions are drying at 115-125° C. for 2-4 hours.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述密炼或捏合的条件是在80℃-140℃条件下捏合或密炼2-4h。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in this application, the conditions for banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述注射成型中注射温度为50℃-70℃。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in the present application, the injection temperature in the injection molding is 50°C-70°C.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,在所述将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料的步骤中,以预混料总量为100%,按质量百分比计,所述陶瓷骨料的质量百分比为~45~60%,所述助烧剂的质量百分比为20~25%,所述造孔剂的质量百 分比为20~30%。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in this application, in the process of mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premixed In the step, taking the total amount of premix as 100%, in terms of mass percentage, the mass percentage of the ceramic aggregate is ~45-60%, the mass percentage of the sintering aid is 20-25%, and the The mass percentage of the pore agent is 20-30%.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,在所述将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料的步骤中,以密炼/捏合料总量为100%,按质量百分比计,所述预混料的质量百分比为55~65%,所述粘结剂的质量百分比为30~40%,所述分散剂的质量百分比为1~5%。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in this application, in the process of banburying or kneading the premix with a binder and a dispersant to obtain banbury/kneading material In the step of mixing/kneading, the total amount of banburying/kneading material is 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, and the mass percentage of the binder is 30-40%, so The mass percentage of the dispersant is 1-5%.
作为本申请提供的所述的多孔陶瓷雾化芯的制备方法的一种优选实施方式,所述陶瓷骨料包括硅藻土、长石、石英砂中的至少一种,以上物质都具有坚固、耐磨、耐高温、来源广泛,成本低廉的优点,可确保多孔陶瓷雾化芯的强度和韧性;所述助烧剂包括低温无铅玻璃粉、高岭土和电气石中的至少一种,起到降低烧结温度,促进陶瓷坯体致密化的作用;所述粘结剂包括石蜡、蜂蜡、棕榈蜡、聚乙烯中的至少一种,能够保持坯体不变形,能够减小热应力产生的陶瓷缺陷,有利于提高多孔陶瓷雾化芯的良品率;所述造孔剂包括聚甲基丙烯酸甲酯、聚乙烯醇、聚苯乙烯中的至少一种,能够控制多孔陶瓷雾化芯的孔径及孔隙率,得到多孔陶瓷雾化芯中互相贯穿的孔道结构;所述分散剂包括硬脂酸能够保证密炼中粉体充分混合分散,维持均匀性。As a preferred embodiment of the method for preparing the porous ceramic atomizing core provided in this application, the ceramic aggregate includes at least one of diatomite, feldspar, and quartz sand, all of which have firm, The advantages of wear resistance, high temperature resistance, wide source and low cost can ensure the strength and toughness of the porous ceramic atomizing core; the sintering aid includes at least one of low temperature lead-free glass powder, kaolin and tourmaline, which can play The sintering temperature is lowered to promote the densification of the ceramic body; the binder includes at least one of paraffin wax, beeswax, palm wax, and polyethylene, which can keep the body from deformation and reduce ceramic defects caused by thermal stress. , which is beneficial to improve the yield of the porous ceramic atomizing core; the pore-forming agent includes at least one of polymethyl methacrylate, polyvinyl alcohol, and polystyrene, which can control the pore size and pore size of the porous ceramic atomizing core rate, to obtain the interpenetrating pore structure in the porous ceramic atomizing core; the dispersing agent including stearic acid can ensure that the powder is fully mixed and dispersed during banburying and maintains uniformity.
一种多孔陶瓷雾化芯,其采用上述多孔陶瓷雾化芯的制备方法制得。A porous ceramic atomizing core is prepared by the above-mentioned preparation method of the porous ceramic atomizing core.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述多孔陶瓷雾化芯的微孔孔径为10~30μm,密度为0.8~1.2g/cm
3,孔隙率为50~70%。
As a preferred embodiment of the porous ceramic atomizing core provided in this application, the porous ceramic atomizing core has a micropore diameter of 10-30 μm, a density of 0.8-1.2 g/cm 3 , and a porosity of 50 μm. ~70%.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述烧结条件为:以4~6℃/min的升温速率从室温升温至890~910℃保温0.5~1.5h,接着以1.5~2.5℃/min的升温速率升温至1100~1200℃保温1.5~2.5h,最后随炉冷却。As a preferred embodiment of the porous ceramic atomizing core provided in this application, the sintering conditions are as follows: the temperature is raised from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5-1.5h, Then, the temperature is raised to 1100-1200°C at a heating rate of 1.5-2.5°C/min for 1.5-2.5h, and finally cooled with the furnace.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述干 燥处理的条件为115~125℃干燥2-4h。As a preferred embodiment of the porous ceramic atomizing core provided in the present application, the conditions of the drying treatment are drying at 115-125°C for 2-4 hours.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述密炼或捏合的条件是在80℃-140℃条件下捏合或密炼2-4h。As a preferred embodiment of the porous ceramic atomizing core provided in this application, the conditions of banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述注射成型中注射温度为50℃-70℃。As a preferred embodiment of the porous ceramic atomizing core provided in this application, the injection temperature in the injection molding is 50°C-70°C.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,在所述将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料的步骤中,以预混料总量为100%,按质量百分比计,所述陶瓷骨料的质量百分比为45~60%,所述助烧剂的质量百分比为20~25%,所述造孔剂的质量百分比为20~30%。As a preferred embodiment of the porous ceramic atomizing core provided in this application, in the step of mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix, Taking the total amount of the premix to be 100%, in terms of mass percentage, the mass percentage of the ceramic aggregate is 45-60%, the mass percentage of the sintering aid is 20-25%, and the mass percentage of the pore-forming agent is 20-25%. The percentage is 20 to 30%.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,在所述将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料的步骤中,以密炼/捏合料总量为100%,按质量百分比计,所述预混料的质量百分比为55~65%,所述粘结剂的质量百分比为30~40%,所述分散剂的质量百分比为1~5%。As a preferred embodiment of the porous ceramic atomizing core provided in this application, in the step of banburying or kneading the premix with a binder and a dispersant to obtain banbury/kneading material , the total amount of Banbury/kneading material is 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, the mass percentage of the binder is 30-40%, and the dispersant is The mass percentage is 1 to 5%.
作为本申请提供的所述的多孔陶瓷雾化芯的一种优选实施方式,所述陶瓷骨料包括硅藻土、长石、石英砂中的至少一种;所述助烧剂包括低温无铅玻璃粉、高岭土和电气石中的至少一种;所述粘结剂包括石蜡、蜂蜡、棕榈蜡、聚乙烯中的至少一种;所述造孔剂包括聚甲基丙烯酸甲酯、聚乙烯醇、聚苯乙烯中的至少一种;所述分散剂包括硬脂酸。As a preferred embodiment of the porous ceramic atomizing core provided in this application, the ceramic aggregate includes at least one of diatomite, feldspar, and quartz sand; the sintering aid includes low-temperature lead-free At least one of glass powder, kaolin and tourmaline; the binder includes at least one of paraffin, beeswax, palm wax and polyethylene; the pore-forming agent includes polymethyl methacrylate, polyvinyl alcohol , at least one of polystyrene; the dispersant includes stearic acid.
一种电子烟,其包括主机以及如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。An electronic cigarette includes a main unit and the above-mentioned porous ceramic atomizing core, wherein the porous ceramic atomizing core is installed on the main unit.
与现有技术相比,本申请有以下有益效果:Compared with the prior art, the present application has the following beneficial effects:
本申请通过改进的配方设计,将陶瓷骨料、助烧剂与造孔剂进行混料后,再借助粘结剂和分散剂进行密炼或捏合、注射成型、脱脂烧结等工序获得孔 隙率高、孔径均匀的多孔陶瓷雾化芯,其坯体强度高,材料均一性强,孔径均匀,应用于电子烟上,雾化效果好,口感饱满,并且生产效率高,利于规模化生产。本申请解决现有工艺制备的多孔陶瓷雾化芯强度较低,成型效率低,不利于自动化生产的问题,本申请提供的多孔陶瓷雾化芯强度高,材料均一性强,生产效率高,提升陶瓷雾化芯强度,提升生产效率。本申请制备方法制得的所述多孔陶瓷雾化芯形成10-30μm均匀分布的微孔,其密度在0.8-1.2g/cm3,孔隙率达到50~70%,应用到电子烟上,雾化效果好,口感饱满。In the present application, through the improved formula design, the ceramic aggregate, sintering aid and pore-forming agent are mixed, and then the binder and dispersing agent are used for banburying or kneading, injection molding, degreasing and sintering to obtain high porosity. , Porous ceramic atomizing core with uniform pore size, high green body strength, strong material uniformity, uniform pore size, applied to electronic cigarettes, good atomization effect, full taste, and high production efficiency, which is conducive to large-scale production. The present application solves the problems of low strength and low forming efficiency of the porous ceramic atomizing core prepared by the existing process, which is not conducive to automatic production. The porous ceramic atomizing core provided by the present application has high strength, strong material uniformity, high production efficiency, and improved The strength of the ceramic atomizing core improves production efficiency. The porous ceramic atomizing core prepared by the preparation method of the present application forms uniformly distributed micropores of 10-30 μm, the density is 0.8-1.2 g/cm3, and the porosity reaches 50-70%. It is applied to electronic cigarettes and atomized. The effect is good and the taste is full.
为了更清楚地说明本申请或现有技术中的方案,下面将对实施例或现有技术描述中所需要使用的附图作一个简单介绍,显而易见地,下面描述中的附图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 illustrate the solutions in the present application or the prior art more clearly, the following will briefly introduce the accompanying drawings that need to be used in the description of the embodiments or the prior art. Obviously, the drawings in the following description belong to the present application. In some embodiments, for those of ordinary skill in the art, other drawings can also be obtained according to these drawings without any creative effort.
图1为本申请实施例1制得的多孔陶瓷雾化芯在电子扫描显微镜下的示意图。FIG. 1 is a schematic diagram of the porous ceramic atomizing core prepared in Example 1 of the application under an electron scanning microscope.
为了使本技术领域的人员更好地理解本申请方案,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的实施例,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做出创造性劳动前提下所获得的所有其他实施例,都应当属于本申请保护的范围。In order to make those skilled in the art better understand the solutions of the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present application. Obviously, the described embodiments are only The embodiments are part of the present application, but not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative work shall fall within the scope of protection of the present application.
针对现有工艺制备的多孔陶瓷雾化芯强度较低,孔径不均匀,孔隙率低,成型效率低,不利于自动化生产的技术问题,本申请实施例提供了一种多孔 陶瓷雾化芯的制备方法,其中,所述多孔陶瓷雾化芯应用于电子烟雾化芯。具体地,所述多孔陶瓷雾化芯的制备方法包括以下步骤:(1)干燥;(2)混料;(3)密炼/捏合与造粒/破碎;(3)注射成型;(5)脱脂处理;(6)烧结处理。Aiming at the technical problems of low strength, non-uniform pore size, low porosity, low molding efficiency, and unfavorable automatic production of the porous ceramic atomizing core prepared by the existing technology, the embodiment of the present application provides a preparation of a porous ceramic atomizing core The method, wherein the porous ceramic atomizing core is applied to an electronic cigarette atomizing core. Specifically, the preparation method of the porous ceramic atomizing core includes the following steps: (1) drying; (2) mixing; (3) banburying/kneading and granulation/crushing; (3) injection molding; (5) Degreasing treatment; (6) sintering treatment.
于本实施例中,所述步骤(1)具体为:将陶瓷骨料和助烧剂进行干燥处理。即将陶瓷骨料、助烧剂放置于干燥箱内120℃干燥2-4h,排出粉体吸附的水分。In this embodiment, the step (1) is specifically: drying the ceramic aggregate and the sintering aid. The ceramic aggregate and sintering aid are placed in a drying oven at 120°C for 2-4 hours, and the moisture adsorbed by the powder is discharged.
于本实施例中,所述步骤(2)具体为:将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得预混料。即将干燥后的陶瓷骨料、助烧剂和造孔剂按照质量比称量后置于三维混料机或者球磨机上进行混料。In this embodiment, the step (2) is specifically: mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix. The dried ceramic aggregate, sintering aid and pore-forming agent are weighed according to the mass ratio and placed on a three-dimensional mixer or ball mill for mixing.
于本实施例中,所述步骤(3)具体为:将预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料;再对密炼/捏合料进行造粒或破碎,得到颗粒状陶瓷喂料。In this embodiment, the step (3) is specifically as follows: banburying or kneading the premix, binder and dispersant to obtain banbury/kneading material; and then granulating or crushing the banburying/kneading material. , get granular ceramic feed.
其中,将预混料与粘结剂置于捏合机或者密炼机中进行捏合或密炼。需要注意的是,先将粘结剂熔化后,再将陶瓷骨料、助烧剂和造孔剂的粉料组成的预混料加入,在80℃-140℃条件下捏合或密炼2-4h。接着,将密炼后得到的泥状物料即密炼/捏合料置于造粒机进行造粒或冷却后置于破碎机进行破碎。Wherein, the premix and the binder are placed in a kneader or an internal mixer for kneading or internal mixing. It should be noted that after melting the binder first, add the premix consisting of ceramic aggregate, sintering aid and pore-forming agent powder, knead or banbury at 80℃-140℃ for 2- 4h. Next, the muddy material obtained after banburying, namely banburying/kneading material, is placed in a granulator for granulation or cooled and then placed in a crusher for crushing.
于本实施例中,所述步骤(4)具体为:将颗粒状陶瓷喂料通过注射成型得到陶瓷生坯。即将破碎后的颗粒状陶瓷喂料加入到陶瓷专用注塑机上进行注射成型,注射温度50℃-70℃。In this embodiment, the step (4) is specifically as follows: injecting the granular ceramic feedstock to obtain a ceramic green body. The crushed granular ceramic feed is added to a special injection molding machine for ceramics for injection molding, and the injection temperature is 50°C-70°C.
于本实施例中,所述步骤(5)具体为:将陶瓷生坯在煅烧氧化铝的埋粉条件下进行脱脂处理。In this embodiment, the step (5) is specifically as follows: degreasing the ceramic green body under the condition of burying the calcined alumina.
在本申请其他实施例中,所述脱脂处理的脱脂条件为以0.4~0.6℃/min的升温速率从室温升温至140~160℃保温0.5~1.5h,接着以0.1~0.2℃/min的升 温速率升温至240~260℃,再以0.2~0.3℃/min的升温速率升温至440~460℃保温1.5~2.5h,然后以2.4~2.6℃/min的升温速率升温至890~910℃保温0.5~1.5h,最后随炉冷却。不同温度段采用不同的升温速率,能够更好让不同原料分别在合适的温度段分解脱出,进一步提供陶瓷胚体的维形性,避免单一升温速率或快速升温造成分解不完成存在坍塌的问题。In other embodiments of the present application, the degreasing condition of the degreasing treatment is to heat up from room temperature to 140 to 160° C. for 0.5 to 1.5 h at a heating rate of 0.4 to 0.6° C./min, and then to heat at a temperature of 0.1 to 0.2° C./min for 0.5 to 1.5 hours. The temperature is increased to 240~260℃ at a rate of 0.2~0.3℃/min, then the temperature is increased to 440~460℃ for 1.5~2.5h at a heating rate of 0.2~0.3℃/min, and then the temperature is increased to 890~910℃ at a heating rate of 2.4~2.6℃/min for 0.5 hours. ~1.5h, and finally cooled with the furnace. Different heating rates are used in different temperature sections, which can better allow different raw materials to be decomposed and released at appropriate temperature sections, and further provide the dimension of the ceramic embryo, avoiding the problem of collapse due to incomplete decomposition caused by a single heating rate or rapid heating.
具体地,脱脂处理是在煅烧α-Al
2O
3(氧化铝)的埋粉条件下进行,煅烧α-Al
2O
3的粒径在20μm-70μm之间,埋粉深度3-4cm,利用细粉的毛细管效应,提高脱脂的速率,以及通过上述特定的脱脂条件防止陶瓷在脱脂过程中由于自身重力而坍塌,以保持产品的整体维形。
Specifically, the degreasing treatment is carried out under the condition of burying powder of calcined α - Al 2 O 3 (alumina ) . The capillary effect of the fine powder increases the rate of debinding, and prevents the ceramic from collapsing due to its own gravity during debinding by the above-mentioned specific debinding conditions, so as to maintain the overall dimension of the product.
于本实施例中,所述步骤(6)具体为:将脱脂得到的陶瓷坯于大气条件下进行烧结,得到多孔陶瓷雾化芯。In this embodiment, the step (6) is specifically: sintering the ceramic blank obtained by degreasing under atmospheric conditions to obtain a porous ceramic atomizing core.
在本申请其他实施例中,所述烧结的工艺为以4~6℃/min的升温速率从室温升温至890~910℃保温0.5~1.5h,接着以1.5~2.5℃/min的升温速率升温至1100~1200℃保温1.5~2.5h,最后随炉冷却。In other embodiments of the present application, the sintering process is to heat up from room temperature to 890-910°C for 0.5-1.5 h at a heating rate of 4-6°C/min, and then heat up at a heating rate of 1.5-2.5°C/min To 1100 ~ 1200 ℃ heat preservation for 1.5 ~ 2.5h, and finally cooling with the furnace.
本申请所述粘结剂、造孔剂、分散剂在脱脂烧结过程中完全挥发分解,从陶瓷基体中完全脱出,避免有机物残留以及保持较好的孔隙率。本申请制备方法制得的所述多孔陶瓷雾化芯形成10-30μm均匀分布的微孔,其密度在0.8-1.2g/cm
3,孔隙率达到50~70%,应用到电子烟上,雾化效果好,口感饱满。
The binder, pore-forming agent, and dispersing agent described in the present application are completely volatilized and decomposed during the degreasing and sintering process, and are completely removed from the ceramic matrix, so as to avoid organic residues and maintain a good porosity. The porous ceramic atomizing core prepared by the preparation method of the present application forms uniformly distributed micropores of 10-30 μm, the density is 0.8-1.2 g/cm 3 , and the porosity reaches 50-70%. The effect is good and the taste is full.
本申请通过改进的配方设计,将陶瓷骨料、助烧剂与造孔剂进行混料后,再借助粘结剂和分散剂进行密炼或捏合、注射成型、脱脂烧结等工序获得孔隙率高、孔径均匀的多孔陶瓷雾化芯,其坯体强度高,材料均一性强,孔径均匀,应用于电子烟上,雾化效果好,口感饱满,并且生产效率高,利于规模化生产。本申请解决现有工艺制备的多孔陶瓷雾化芯强度较低,成型效率低,不利于自动化生产的问题,本申请提供的多孔陶瓷雾化芯强度高,材料均一性强,生产效率高,提升陶瓷雾化芯强度,提升生产效率。In the present application, through the improved formula design, the ceramic aggregate, sintering aid and pore-forming agent are mixed, and then the binder and dispersing agent are used for banburying or kneading, injection molding, degreasing and sintering to obtain high porosity. , Porous ceramic atomizing core with uniform pore size, high green body strength, strong material uniformity, uniform pore size, applied to electronic cigarettes, good atomization effect, full taste, and high production efficiency, which is conducive to large-scale production. The present application solves the problems of low strength and low forming efficiency of the porous ceramic atomizing core prepared by the existing process, which is not conducive to automatic production. The porous ceramic atomizing core provided by the present application has high strength, strong material uniformity, high production efficiency, and improved The strength of the ceramic atomizing core improves production efficiency.
于本实施例中,在所述步骤(2)中,以预混料总量为100%,按质量百分比计,所述陶瓷骨料的质量百分比为45~60%,所述助烧剂的质量百分比为20~25%,所述造孔剂的质量百分比为20~30%。In this embodiment, in the step (2), the total amount of premix is 100%, the mass percentage of the ceramic aggregate is 45-60%, and the sintering aid is 45-60% by mass. The mass percentage is 20-25%, and the mass percentage of the pore-forming agent is 20-30%.
于本实施例中,在所述步骤(3)中,以密炼/捏合料总量为100%,按质量百分比计,所述预混料的质量百分比为55~65%,所述粘结剂的质量百分比为30~40%,所述分散剂的质量百分比为1~5%。In this embodiment, in the step (3), the total amount of Banbury/kneading material is 100%, and the mass percentage of the premix is 55-65% by mass percentage, and the adhesive The mass percentage of the agent is 30-40%, and the mass percentage of the dispersing agent is 1-5%.
于本实施例中,所述陶瓷骨料包括硅藻土、长石(如钾长石、钠长石)、石英砂中的至少一种;以上物质都具有坚固、耐磨、耐高温、来源广泛,成本低廉的优点,可确保多孔陶瓷雾化芯的强度和韧性;所述助烧剂包括低温无铅玻璃粉、高岭土或电气石中的至少一种,起到降低烧结温度,促进陶瓷坯体致密化的作用;所述粘结剂包括石蜡、蜂蜡、棕榈蜡、聚乙烯中的至少一种,能够保持坯体不变形,能够减小热应力产生的陶瓷缺陷,有利于提高多孔陶瓷雾化芯的良品率;所述造孔剂包括聚甲基丙烯酸甲酯、聚乙烯醇、聚苯乙烯中的至少一种,能够控制多孔陶瓷雾化芯的孔径及孔隙率,得到多孔陶瓷雾化芯中互相贯穿的孔道结构;所述分散剂包括硬脂酸,能够保证密炼中粉体充分混合分散,维持均匀性。In this embodiment, the ceramic aggregate includes at least one of diatomaceous earth, feldspar (such as potassium feldspar, albite), and quartz sand; The advantages of wide range and low cost can ensure the strength and toughness of the porous ceramic atomizing core; the sintering aid includes at least one of low-temperature lead-free glass powder, kaolin or tourmaline, which can reduce the sintering temperature and promote the ceramic blank. The effect of body densification; the binder includes at least one of paraffin wax, beeswax, palm wax, and polyethylene, which can keep the green body from deformation, can reduce the ceramic defects caused by thermal stress, and is conducive to improving the porous ceramic mist. The yield of the atomizing core; the pore-forming agent includes at least one of polymethyl methacrylate, polyvinyl alcohol, and polystyrene, which can control the pore size and porosity of the porous ceramic atomizing core, and obtain the porous ceramic atomizing core. The interpenetrating pore structure in the core; the dispersant includes stearic acid, which can ensure that the powder is fully mixed and dispersed during banburying and maintains uniformity.
优选地,所述步骤(6)之后还包括超声清洗:将脱脂烧结后的多孔陶瓷雾化芯进行超声清洗,最后在烘箱内烘干即得成品。Preferably, after the step (6), ultrasonic cleaning is further included: ultrasonic cleaning is performed on the degreasing and sintered porous ceramic atomizing core, and finally, the finished product is obtained by drying in an oven.
为了使本技术领域的人员更好地理解本申请方案,下面将结合附图,对本申请实施例中的技术方案进行清楚、完整地描述。In order to make those skilled in the art better understand the solutions of the present application, the technical solutions in the embodiments of the present application will be described clearly and completely below with reference to the accompanying drawings.
实施例1:Example 1:
本实施例提供了一种电子烟雾化芯用多孔陶瓷雾化芯的制备方法,其包括如下步骤:This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
(1)干燥:将陶瓷骨料、助烧剂放置于干燥箱内120℃干燥2h,排出粉体吸附的水分;(1) Drying: The ceramic aggregate and sintering aid are placed in a drying oven at 120°C for 2 hours, and the moisture adsorbed by the powder is discharged;
(2)混料:按质量百分比计,分别称取硅藻土40%、钾长石10%、高岭土12%、玻璃粉8%和聚苯乙烯造孔剂30%放入三维混料机混合2h,混合均匀后形成预混料;该步骤中,控制聚苯乙烯造孔剂的平均粒径为50μm;(2) Mixing: by mass percentage, weigh 40% of diatomite, 10% of potassium feldspar, 12% of kaolin, 8% of glass powder and 30% of polystyrene pore-forming agent, respectively, and put them into a three-dimensional mixer to mix 2h, the premix is formed after mixing uniformly; in this step, the average particle size of the polystyrene pore-forming agent is controlled to be 50 μm;
(3)捏合与破碎:按质量百分比计,将预混料60%、石蜡25%、蜂蜡5%、低密度聚乙烯5%和硬脂酸5%加入捏合机中,145℃条件下进行混合捏合3h,捏合后冷却得到块状陶瓷捏合料,再放入颚式破碎机中进行破碎,获得大小均匀的颗粒状陶瓷喂料;(3) Kneading and crushing: by mass percentage, add 60% of premix, 25% of paraffin, 5% of beeswax, 5% of low-density polyethylene and 5% of stearic acid into the kneader, and mix at 145°C Kneading for 3 hours, and cooling after kneading to obtain bulk ceramic kneading material, which is then put into a jaw crusher for crushing to obtain granular ceramic feedstock with uniform size;
(4)注射成型:将陶瓷喂料采用注塑成型工艺得到陶瓷生坯,该过程参数为:成型压力为20bar,速度为20cm
3/s,注射温度为100℃,模具温度30℃,得到陶瓷生坯;
(4) Injection molding: The ceramic green body is obtained by the injection molding process. The process parameters are: the molding pressure is 20bar, the speed is 20cm 3 /s, the injection temperature is 100°C, and the mold temperature is 30°C to obtain a ceramic green body. blank;
(5)脱脂处理:将陶瓷生坯放置于氧化铝匣钵中,并埋3cm厚的煅烧氧化铝粉,氧化铝粉粒度为70um,匣钵放置于脱脂炉内,脱脂条件为:以0.5℃/min的升温速率从室温升温至150℃,保温1h,然后以0.1℃/min的速度升温至250℃,再以0.2℃/min的速度升温至450℃,保温2h,然后以2.5℃/min的升温速率升至900℃,保温1h,最后随炉冷却至室温;(5) Degreasing treatment: The ceramic green body is placed in an alumina saggar, and calcined alumina powder with a thickness of 3 cm is buried. The particle size of the alumina powder is 70um, and the saggar is placed in a degreasing furnace. The heating rate per min was raised from room temperature to 150°C, held for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min The heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
(6)烧结处理:将脱脂得到的陶瓷材料从脱脂炉内取出,清理表面的氧化铝粉后,将陶瓷材料放在氧化铝匣钵内,放置于大气烧结炉内,进行无压烧结。烧结工艺为:以5℃/min的升温速率从室温升温至900℃保温1h,接着以2℃/min的升温速率升温至1150℃保温2h,最后随炉冷却至室温,获得多孔陶瓷雾化芯。(6) Sintering treatment: take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering. The sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1150 °C for 2 h at a heating rate of 2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
将制得的多孔陶瓷雾化芯进行性能测试,具体实验数据如下:The performance of the prepared porous ceramic atomizing core is tested, and the specific experimental data are as follows:
孔隙率Porosity | 平均孔径Average pore size | 抗压强度Compressive strength | 密度density | 吸油时间Oil absorption time |
63.15%63.15% | 22um22um | 7.6MPa7.6MPa | 0.85g/cm 3 0.85g/ cm3 | 21s21s |
本实施例制得的多孔陶瓷雾化芯在电子扫描显微镜下观察孔结构如图1所示,从图中可以看出,本实施例制得的多孔陶瓷雾化芯获得均匀分布的孔。Figure 1 shows the pore structure of the porous ceramic atomizing core prepared in this example under an electron scanning microscope. It can be seen from the figure that the porous ceramic atomizing core prepared in this example has uniformly distributed pores.
实施例2:Example 2:
本实施例提供了一种电子烟雾化芯用多孔陶瓷雾化芯的制备方法,其包括如下步骤:This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
(1)干燥:将陶瓷骨料、助烧剂放置于干燥箱内120℃干燥3h,排出粉体吸附的水分;(1) Drying: Place the ceramic aggregates and sintering aids in a drying oven at 120 °C for 3 hours, and discharge the moisture adsorbed by the powder;
(2)混料:按质量百分比计,分别称取硅藻土35%、石英砂10%、高岭土10%、玻璃粉15%和聚苯乙烯造孔剂30%放入三维混料机混合2h,混合均匀后形成预混料;该步骤中,控制聚苯乙烯造孔剂的平均粒径为50μm;(2) Mixing: in terms of mass percentage, weigh 35% of diatomite, 10% of quartz sand, 10% of kaolin, 15% of glass powder and 30% of polystyrene pore-forming agent, respectively, put them into a three-dimensional mixer and mix for 2 hours , and the premix is formed after mixing evenly; in this step, the average particle size of the polystyrene pore-forming agent is controlled to be 50 μm;
(3)密炼与造粒/破碎:按质量百分比计,将预混料60%、石蜡25%、蜂蜡5%、棕榈蜡3%、乙烯-醋酸乙烯共聚物3%和硬脂酸4%加入密炼机中,80℃条件下进行密炼4h,冷却得到块状陶瓷密炼/捏合料,再放入颚式破碎机中进行破碎,获得大小均匀的颗粒状陶瓷喂料;(3) Banburying and granulation/crushing: by mass percentage, mix 60% of premix, 25% of paraffin, 5% of beeswax, 3% of palm wax, 3% of ethylene-vinyl acetate copolymer and 4% of stearic acid Add it into the mixer, carry out the mixer at 80°C for 4 hours, cool to get the bulk ceramic mixer/kneading material, and then put it into the jaw crusher for crushing to obtain the granular ceramic feed with uniform size;
(4)注射成型:将陶瓷喂料采用注塑成型工艺得到陶瓷生坯,该过程参数为:成型压力为20bar,速度为20cm
3/s,注射温度为55℃,模具温度26℃,得到陶瓷生坯;
(4) Injection molding: The ceramic green body is obtained by the injection molding process. The process parameters are: the molding pressure is 20bar, the speed is 20cm 3 /s, the injection temperature is 55°C, and the mold temperature is 26°C to obtain a ceramic green body. blank;
(5)脱脂处理:将陶瓷生坯放置于氧化铝匣钵中,并埋2cm厚的煅烧氧化铝粉,氧化铝粉粒度为50μm,匣钵放置于脱脂炉内,脱脂条件为:以0.5℃/min的升温速率从室温升温至150℃,保温1h,然后以0.1℃/min的速度升温至250℃,再以0.2℃/min的速度升温至450℃,保温2h,然后以2.5℃/min的升温速率升至900℃,保温1h,最后随炉冷却至室温;(5) Degreasing treatment: The ceramic green body is placed in an alumina sagger, and calcined alumina powder with a thickness of 2 cm is buried. The particle size of the alumina powder is 50 μm. The saggar is placed in a degreasing furnace. The degreasing conditions are: 0.5 ° C The heating rate per min was raised from room temperature to 150°C, held for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min The heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
(6)烧结处理:将脱脂得到的陶瓷材料从脱脂炉内取出,清理表面的氧化铝粉后,将陶瓷材料放在氧化铝匣钵内,放置于大气烧结炉内,进行无压烧结。烧结工艺为:以5℃/min的升温速率从室温升温至900℃保温1h,接着以2℃/min的升温速率升温至1100℃保温2h,最后随炉冷却至室温,获得多孔陶瓷雾化芯。(6) Sintering treatment: take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering. The sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1100 °C for 2 h at a heating rate of 2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
将制得的多孔陶瓷雾化芯进行性能测试,具体实验数据如下:The performance of the prepared porous ceramic atomizing core is tested, and the specific experimental data are as follows:
孔隙率Porosity | 平均孔径Average pore size | 抗压强度Compressive strength | 密度density | 吸油时间Oil absorption time |
66.94%66.94% | 17um17um | 6.9MPa6.9MPa | 0.81g/cm 3 0.81g/ cm3 | 17s17s |
实施例3:Example 3:
本实施例提供了一种电子烟雾化芯用多孔陶瓷雾化芯的制备方法,其包括如下步骤:This embodiment provides a preparation method of a porous ceramic atomizing core for an electronic cigarette atomizing core, which includes the following steps:
(1)干燥:将陶瓷骨料、助烧剂放置于干燥箱内120℃干燥4h,排出粉体吸附的水分;(1) Drying: Place the ceramic aggregates and sintering aids in a drying oven at 120 °C for 4 hours, and discharge the moisture absorbed by the powder;
(2)混料:按质量百分比计,分别称取硅藻土50%、钠长石10%、高岭土5%、玻璃粉15%和聚苯乙烯造孔剂20%放入卧室球磨机料罐中混合2h,混合均匀后形成预混料;该步骤中,控制聚苯乙烯造孔剂的平均粒径为50μm;(2) Mixing: by mass percentage, weigh 50% of diatomite, 10% of albite, 5% of kaolin, 15% of glass powder and 20% of polystyrene pore-forming agent and put them into the jar of the bedroom ball mill Mixing for 2 hours, the premix is formed after mixing uniformly; in this step, the average particle size of the polystyrene pore-forming agent is controlled to be 50 μm;
(3)捏合与破碎:按质量百分比计,将预混料60%、石蜡25%、蜂蜡5%、低密度聚乙烯5%和硬脂酸5%加入捏合机中,140℃条件下进行混合捏合3h,捏合后冷却得到块状陶瓷捏合料,再放入颚式破碎机中进行破碎,获得大小均匀的颗粒状陶瓷喂料;(3) Kneading and crushing: by mass percentage, add 60% of premix, 25% of paraffin, 5% of beeswax, 5% of low-density polyethylene and 5% of stearic acid into the kneader, and mix at 140°C Kneading for 3 hours, and cooling after kneading to obtain bulk ceramic kneading material, which is then put into a jaw crusher for crushing to obtain granular ceramic feedstock with uniform size;
(4)注射成型:将陶瓷喂料采用注塑成型工艺得到陶瓷生坯,该过程参数为:成型压力为20bar,速度为20cm
3/s,注射温度为60℃,模具温度30℃,得到陶瓷生坯;
(4) Injection molding: The ceramic green body is obtained by the injection molding process. The process parameters are as follows: the molding pressure is 20 bar, the speed is 20 cm 3 /s, the injection temperature is 60 °C, and the mold temperature is 30 °C, and the ceramic green body is obtained. blank;
(5)脱脂处理:将陶瓷生坯放置于氧化铝匣钵中,并埋3cm厚的煅烧氧化铝粉,氧化铝粉粒度为70μm,匣钵放置于脱脂炉内,脱脂条件为:以0.5℃/min的升温速率从室温升温至150℃,保温1h,然后以0.1℃/min的速度升温至250℃,再以0.2℃/min的速度升温至450℃,保温2h,然后以2.5℃/min的升温速率升至900℃,保温1h,最后随炉冷却至室温;(5) Degreasing treatment: The ceramic green body is placed in an alumina sagger, and calcined alumina powder with a thickness of 3 cm is buried. The particle size of the alumina powder is 70 μm. The saggar is placed in a degreasing furnace. The degreasing conditions are: 0.5 ° C The heating rate was raised from room temperature to 150°C/min, kept for 1 h, then heated to 250°C at a rate of 0.1°C/min, then heated to 450°C at a rate of 0.2°C/min, held for 2 hours, and then heated to 2.5°C/min The heating rate was raised to 900 °C, kept for 1 h, and finally cooled to room temperature with the furnace;
(6)烧结处理:将脱脂得到的陶瓷材料从脱脂炉内取出,清理表面的氧化铝粉后,将陶瓷材料放在氧化铝匣钵内,放置于大气烧结炉内,进行无压 烧结。烧结工艺为:以5℃/min的升温速率从室温升温至900℃保温1h,接着以2.2℃/min的升温速率升温至1180℃保温2h,最后随炉冷却至室温,获得多孔陶瓷雾化芯。(6) Sintering treatment: take out the degreasing ceramic material from the degreasing furnace, clean the alumina powder on the surface, put the ceramic material in an alumina sagger, and place it in an atmospheric sintering furnace for pressureless sintering. The sintering process is as follows: heating from room temperature to 900 °C for 1 h at a heating rate of 5 °C/min, then heating to 1180 °C for 2 h at a heating rate of 2.2 °C/min, and finally cooling to room temperature with the furnace to obtain a porous ceramic atomizing core .
将制得的多孔陶瓷雾化芯进行性能测试,具体实验数据如下:The performance of the prepared porous ceramic atomizing core is tested, and the specific experimental data are as follows:
孔隙率Porosity | 平均孔径Average pore size | 抗压强度Compressive strength | 密度density | 吸油时间Oil absorption time |
65.86%65.86% | 24um24um | 8.2MPa8.2MPa | 0.98g/cm 3 0.98g/cm 3 | 30s30s |
实施例4Example 4
本实施例提供了一种电子烟,其包括主机以及多孔陶瓷雾化芯,所述多孔陶瓷雾化芯安装于所述主机上。其中,所述多孔陶瓷雾化芯可以采用实施例1-3任一方法制得的多孔陶瓷雾化芯。This embodiment provides an electronic cigarette, which includes a main body and a porous ceramic atomizing core, and the porous ceramic atomizing core is installed on the main body. Wherein, the porous ceramic atomizing core can be the porous ceramic atomizing core prepared by any of the methods in Examples 1-3.
本实施例所用的多孔陶瓷雾化芯其孔隙率高、孔径均匀,坯体强度高,材料均一性强,孔径均匀,应用到电子烟上,雾化效果好,口感饱满。The porous ceramic atomizing core used in this embodiment has high porosity, uniform pore size, high green body strength, strong material uniformity, and uniform pore size. When applied to electronic cigarettes, the atomization effect is good and the taste is full.
显然,以上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,附图中给出了本申请的较佳实施例,但并不限制本申请的专利范围。本申请可以以许多不同的形式来实现,相反地,提供这些实施例的目的是使对本申请的公开内容的理解更加透彻全面。尽管参照前述实施例对本申请进行了详细的说明,对于本领域的技术人员来而言,其依然可以对前述各具体实施方式所记载的技术方案进行修改,或者对其中部分技术特征进行等效替换。凡是利用本申请说明书及附图内容所做的等效结构,直接或间接运用在其他相关的技术领域,均同理在本申请专利保护范围之内。Obviously, the above-described embodiments are only a part of the embodiments of the present application, rather than all of the embodiments. The accompanying drawings show the preferred embodiments of the present application, but do not limit the scope of the patent of the present application. This application may be embodied in many different forms, rather these embodiments are provided so that a thorough and complete understanding of the disclosure of this application is provided. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing specific embodiments, or perform equivalent replacements for some of the technical features. . Any equivalent structures made by using the contents of the description and drawings of this application, which are directly or indirectly used in other related technical fields, are all within the scope of protection of the patent of this application.
Claims (20)
- 一种多孔陶瓷雾化芯的制备方法,其包括以下步骤:A preparation method of a porous ceramic atomizing core, comprising the following steps:将陶瓷骨料和助烧剂进行干燥处理;Dry the ceramic aggregate and sintering aid;将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料;Mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix;将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料;对所述密炼/捏合料进行造粒或破碎,得到颗粒状陶瓷喂料;Banburying or kneading the premix, binder and dispersant to obtain banbury/kneading material; granulating or crushing the banburying/kneading material to obtain granular ceramic feed;将所述颗粒状陶瓷喂料通过注射成型,得到陶瓷生坯;injecting the granular ceramic feedstock to obtain a ceramic green body;将所述陶瓷生坯在煅烧氧化铝的埋粉条件下,以预设的脱脂条件进行脱脂处理;degreasing the ceramic green body under the condition of burying powder of calcined alumina with preset degreasing conditions;将脱脂得到的陶瓷坯于大气条件下,以预设的烧结条件进行烧结,得到多孔陶瓷雾化芯。The ceramic blank obtained by degreasing is sintered under the atmospheric conditions under the preset sintering conditions 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,所述煅烧氧化铝的粒径为20~70μm,所述煅烧氧化铝的埋粉条件是埋粉深度为3~4cm。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the particle size of the calcined alumina is 20-70 μm, and the burying condition of the calcined alumina is that the burying depth is 3-4 cm.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述脱脂条件为:以0.4~0.6℃/min的升温速率从室温升温至140~160℃保温0.5~1.5h,接着以0.1~0.2℃/min的升温速率升温至240~260℃,再以0.2~0.3℃/min的升温速率升温至440~460℃保温1.5~2.5h,然后以2.4~2.6℃/min的升温速率升温至890~910℃保温0.5~1.5h,最后随炉冷却。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the degreasing conditions are: heating from room temperature to 140-160°C at a heating rate of 0.4-0.6°C/min for 0.5-1.5h, and then heating with The heating rate is 0.1~0.2°C/min to 240~260°C, then the temperature is raised to 440~460°C at the heating rate of 0.2~0.3°C/min and the temperature is kept for 1.5~2.5h, and then the heating rate is 2.4~2.6°C/min. The temperature is raised to 890~910℃ and kept for 0.5~1.5h, and finally cooled with the furnace.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述烧结条件为:以4~6℃/min的升温速率从室温升温至890~910℃保温0.5~1.5h,接着以1.5~2.5℃/min的升温速率升温至1100~1200℃保温1.5~2.5h,最后随炉冷却。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the sintering conditions are: heating from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5-1.5h, and then heating at a temperature of 4-6°C/min. The heating rate of 1.5~2.5℃/min was heated to 1100~1200℃ and kept for 1.5~2.5h, and finally cooled with the furnace.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述干燥处理的条件为115~125℃干燥2-4h。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the drying treatment conditions are drying at 115-125° C. for 2-4 hours.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述密炼或捏合的条件是在80℃-140℃条件下捏合或密炼2-4h。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the conditions for banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
- 根据权利要求1所述的多孔陶瓷雾化芯的制备方法,其中,所述注射成型中注射温度为50℃-70℃。The method for preparing a porous ceramic atomizing core according to claim 1, wherein the injection temperature in the injection molding is 50°C-70°C.
- 根据权利要求1至7任意一项所述的多孔陶瓷雾化芯的制备方法,其中,在所述将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料的步骤中,以预混料总量为100%,按质量百分比计,所述陶瓷骨料的质量百分比为45~60%,所述助烧剂的质量百分比为20~25%,所述造孔剂的质量百分比为20~30%。The method for preparing a porous ceramic atomizing core according to any one of claims 1 to 7, wherein, in the process of mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premixed In the step, taking the total amount of premix as 100%, in terms of mass percentage, the mass percentage of the ceramic aggregate is 45-60%, the mass percentage of the sintering aid is 20-25%, and the pore-forming agent is 20-25%. The mass percentage of the agent is 20-30%.
- 根据权利要求1至7任意一项所述的多孔陶瓷雾化芯的制备方法,其中,在所述将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料的步骤中,以密炼/捏合料总量为100%,按质量百分比计,所述预混料的质量百分比为55~65%,所述粘结剂的质量百分比为30~40%,所述分散剂的质量百分比为1~5%。The method for preparing a porous ceramic atomizing core according to any one of claims 1 to 7, wherein the banburying/kneading material is obtained by banburying or kneading the premix with a binder and a dispersant. In the step of mixing/kneading, the total amount of banburying/kneading material is 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, and the mass percentage of the binder is 30-40%, so The mass percentage of the dispersant is 1-5%.
- 根据权利要求1至7任意一项所述的多孔陶瓷雾化芯的制备方法,其中,所述陶瓷骨料包括硅藻土、长石、石英砂中的至少一种;所述助烧剂包括低温无铅玻璃粉、高岭土和电气石中的至少一种;所述粘结剂包括石蜡、蜂蜡、棕榈蜡、聚乙烯中的至少一种;所述造孔剂包括聚甲基丙烯酸甲酯、聚乙烯醇、聚苯乙烯中的至少一种;所述分散剂包括硬脂酸。The method for preparing a porous ceramic atomizing core according to any one of claims 1 to 7, wherein the ceramic aggregate comprises at least one of diatomite, feldspar, and quartz sand; the sintering aid comprises At least one of low-temperature lead-free glass powder, kaolin and tourmaline; the binder includes at least one of paraffin, beeswax, palm wax, and polyethylene; the pore-forming agent includes polymethyl methacrylate, At least one of polyvinyl alcohol and polystyrene; the dispersant includes stearic acid.
- 一种多孔陶瓷雾化芯,采用权利要求1-3任一项所述的制备方法制得。A porous ceramic atomizing core is prepared by the preparation method described in any one of claims 1-3.
- 根据权利要求11所述多孔陶瓷雾化芯,其中,所述多孔陶瓷雾化芯的微孔孔径为10~30μm,密度为0.8~1.2g/cm 3,孔隙率为50~70%。 The porous ceramic atomizing core according to claim 11, wherein the micropore diameter of the porous ceramic atomizing core is 10-30 μm, the density is 0.8-1.2 g/cm 3 , and the porosity is 50-70%.
- 根据权利要求11所述多孔陶瓷雾化芯,其中,所述烧结条件为:以4~6℃/min的升温速率从室温升温至890~910℃保温0.5~1.5h,接着以1.5~2.5℃/min的升温速率升温至1100~1200℃保温1.5~2.5h,最后随炉冷却。The porous ceramic atomizing core according to claim 11, wherein the sintering conditions are: heating from room temperature to 890-910°C at a heating rate of 4-6°C/min for 0.5-1.5h, and then heating at 1.5-2.5°C for 0.5-1.5 hours. The heating rate was raised to 1100-1200 °C for 1.5-2.5 h at a heating rate of /min, and finally cooled with the furnace.
- 根据权利要求11所述多孔陶瓷雾化芯,其中,所述干燥处理的条 件为115~125℃干燥2-4h。The porous ceramic atomizing core according to claim 11, wherein the conditions of the drying treatment are drying at 115-125°C for 2-4 hours.
- 根据权利要求11所述多孔陶瓷雾化芯,其中,所述密炼或捏合的条件是在80℃-140℃条件下捏合或密炼2-4h。The porous ceramic atomizing core according to claim 11, wherein the conditions of banburying or kneading are kneading or banburying at 80°C-140°C for 2-4 hours.
- 根据权利要求11所述多孔陶瓷雾化芯,其中,所述注射成型中注射温度为50℃-70℃。The porous ceramic atomizing core according to claim 11, wherein the injection temperature in the injection molding is 50°C-70°C.
- 根据权利要求11至16任意一项所述多孔陶瓷雾化芯,其中,在所述将干燥后的陶瓷骨料、助烧剂和造孔剂进行混料,得到预混料的步骤中,以预混料总量为100%,按质量百分比计,所述陶瓷骨料的质量百分比为45~60%,所述助烧剂的质量百分比为20~25%,所述造孔剂的质量百分比为20~30%。The porous ceramic atomizing core according to any one of claims 11 to 16, wherein, in the step of mixing the dried ceramic aggregate, sintering aid and pore-forming agent to obtain a premix, The total amount of premix is 100%. In terms of mass percentage, the mass percentage of the ceramic aggregate is 45-60%, the mass percentage of the sintering aid is 20-25%, and the mass percentage of the pore-forming agent is 20-25%. 20 to 30%.
- 根据权利要求11至16任意一项所述多孔陶瓷雾化芯,其中,在所述将所述预混料与粘结剂、分散剂进行密炼或捏合得到密炼/捏合料的步骤中,以密炼/捏合料总量为100%,按质量百分比计,所述预混料的质量百分比为55~65%,所述粘结剂的质量百分比为30~40%,所述分散剂的质量百分比为1~5%。The porous ceramic atomizing core according to any one of claims 11 to 16, wherein, in the step of banburying or kneading the premix with a binder and a dispersant to obtain banbury/kneading material, Taking the total amount of Banbury/kneading materials as 100%, in terms of mass percentage, the mass percentage of the premix is 55-65%, the mass percentage of the binder is 30-40%, and the dispersant is 30-40%. The mass percentage is 1-5%.
- 根据权利要求11至16任意一项所述多孔陶瓷雾化芯,其中,所述陶瓷骨料包括硅藻土、长石、石英砂中的至少一种;所述助烧剂包括低温无铅玻璃粉、高岭土和电气石中的至少一种;所述粘结剂包括石蜡、蜂蜡、棕榈蜡、聚乙烯中的至少一种;所述造孔剂包括聚甲基丙烯酸甲酯、聚乙烯醇、聚苯乙烯中的至少一种;所述分散剂包括硬脂酸。The porous ceramic atomizing core according to any one of claims 11 to 16, wherein the ceramic aggregate comprises at least one of diatomite, feldspar, and quartz sand; and the sintering aid comprises low-temperature lead-free glass At least one of powder, kaolin and tourmaline; the binder includes at least one of paraffin, beeswax, palm wax, polyethylene; the pore-forming agent includes polymethyl methacrylate, polyvinyl alcohol, At least one of polystyrene; the dispersant includes stearic acid.
- 一种电子烟,包括主机以及如权利要求11-19任一项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 main unit and the porous ceramic atomizing core according to any one of claims 11-19, wherein the porous ceramic atomizing core is installed on the main unit.
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CN115925442A (en) * | 2022-12-29 | 2023-04-07 | 深圳市吉迩技术有限公司 | Porous ceramic atomizing core and preparation method and application thereof |
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