CN112194477A - Preparation method of porous ceramic material and porous material obtained by same - Google Patents
Preparation method of porous ceramic material and porous material obtained by same Download PDFInfo
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- CN112194477A CN112194477A CN201910536095.1A CN201910536095A CN112194477A CN 112194477 A CN112194477 A CN 112194477A CN 201910536095 A CN201910536095 A CN 201910536095A CN 112194477 A CN112194477 A CN 112194477A
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011148 porous material Substances 0.000 title description 19
- 239000000919 ceramic Substances 0.000 claims abstract description 75
- 239000004575 stone Substances 0.000 claims abstract description 29
- 238000005245 sintering Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000003571 electronic cigarette Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 230000008569 process Effects 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 23
- 239000002243 precursor Substances 0.000 claims description 23
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 7
- 239000004926 polymethyl methacrylate Substances 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 229910052629 lepidolite Inorganic materials 0.000 claims description 5
- 229910052709 silver Inorganic materials 0.000 claims description 5
- 239000004332 silver Substances 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 239000010433 feldspar Substances 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 229910052656 albite Inorganic materials 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 2
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000011425 bamboo Substances 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 239000011368 organic material Substances 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 241001330002 Bambuseae Species 0.000 claims 1
- 239000005909 Kieselgur Substances 0.000 claims 1
- 239000011162 core material Substances 0.000 abstract description 17
- 239000002245 particle Substances 0.000 abstract description 12
- 238000000889 atomisation Methods 0.000 abstract description 8
- 238000010304 firing Methods 0.000 abstract description 8
- 239000012752 auxiliary agent Substances 0.000 abstract description 6
- 239000011521 glass Substances 0.000 abstract description 4
- 238000005452 bending Methods 0.000 abstract description 3
- 231100000701 toxic element Toxicity 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 17
- 239000002994 raw material Substances 0.000 description 12
- 239000000779 smoke Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000000227 grinding Methods 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 6
- 238000000498 ball milling Methods 0.000 description 6
- 235000019504 cigarettes Nutrition 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000000443 aerosol Substances 0.000 description 5
- 238000000748 compression moulding Methods 0.000 description 5
- 238000004659 sterilization and disinfection Methods 0.000 description 5
- 229920000049 Carbon (fiber) Polymers 0.000 description 4
- 229920002522 Wood fibre Polymers 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 239000004917 carbon fiber Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 238000005485 electric heating Methods 0.000 description 4
- 239000002025 wood fiber Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000208125 Nicotiana Species 0.000 description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229960002715 nicotine Drugs 0.000 description 2
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000009777 vacuum freeze-drying Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 244000082204 Phyllostachys viridis Species 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 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
- 238000004458 analytical method Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- UHZZMRAGKVHANO-UHFFFAOYSA-M chlormequat chloride Chemical compound [Cl-].C[N+](C)(C)CCCl UHZZMRAGKVHANO-UHFFFAOYSA-M 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- -1 iron-chromium-aluminum Chemical compound 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910001120 nichrome Inorganic materials 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 230000002618 waking effect Effects 0.000 description 1
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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
- C04B35/16—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 silicates other than clay
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- 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
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- C04B38/0635—Compounding ingredients
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention relates to a preparation method of a porous ceramic material for electronic cigarettes, the porous ceramic material prepared by the method and application of the porous ceramic material in an electronic cigarette atomizer. The preparation method of the invention uses natural medical stone as the main aggregate of the porous ceramic, can be fired and formed under normal pressure under the conventional atmospheric condition, has mild sintering condition, can adopt a two-step firing process of insulating heat for 0.5-3 hours at 450-550 ℃ and then heating to 800-950 ℃ for insulating and sintering for 0.3-2 hours, and does not need to introduce auxiliary agents such as low-melting-point glass powder and the like. The medical stone particles have a large number of micropores and mesopore structures, and the porosity of more than 90 percent can be obtained by combining with pore-forming agents, and the bending strength of more than 20MPa is also achieved. The obtained porous ceramic is used as an electronic cigarette atomization core material, and toxic elements are released in a zero mode.
Description
Technical Field
The invention relates to the field of electronic cigarettes, in particular to a preparation method of a porous ceramic material for an atomizing core and a porous material prepared by the method.
Background
A device for converting an atomized liquid containing nicotine or the like into an aerosol by means of heating and atomizing an atomizing core is an electronic product simulating a cigarette, and the generated aerosol has smoke, taste and feeling similar to those of a cigarette. The aerosol containing nicotine produced by atomization does not contain harmful carcinogenic substances such as tar and the like commonly existing in the smoke of common cigarettes, and is considered to be a cigarette substitute which is beneficial to the health of traditional smokers. Meanwhile, the electronic device has the characteristics of good portability, no naked flame, no second-hand smoke and environmental protection, and is popular with many smokers.
The heating atomization technology of aerosol generating device, there are two main types that are widely used at present: 1) cotton or fiber bundles are used as an oil guide body, and the electric heating wire is wound on the oil guide body to directly heat the tobacco tar for atomization; 2) the honeycomb ceramics is used as an oil guide body, and the tobacco tar is atomized by heating in modes of an electric heating wire or an electric heating belt and the like.
The porous ceramic with good high-temperature resistance is a preferred material for manufacturing the atomizing core in the electronic cigarette industry at the present stage. The porous ceramic is generally prepared by sintering components such as aggregate, a binder, a pore-forming agent and the like, has a large number of pore channel structures which are communicated with each other and the surface of the material in the porous ceramic, has excellent performances such as stable chemical property, low thermal conductivity, high temperature resistance, corrosion resistance and the like, and has a plurality of applications in the fields of biology, energy, environmental protection and the like.
At present, high-temperature sintering ceramics are mostly used as aggregates in the manufacture of ceramic atomizing cores for electronic cigarettes, for example, related patents of WO2015192300A1 and CN05294140B use alumina, silicon dioxide and the like as aggregates, and the sintering temperature is 1000-1400 ℃. Generally, the heating wire arranged inside the ceramic atomizing core close to the surface or the electric heating material arranged on the atomizing surface is mostly nichrome or iron-chromium-aluminum alloy and the like, which is softened and seriously deformed at the temperature of over 1000 ℃; therefore, the glass powder and other auxiliary agents are required to be added, the sintering temperature of the ceramic is reduced, and the atomization core is fired at a low temperature, and the introduction of the glass powder sintering auxiliary agent inevitably leads to the introduction of harmful metal elements such as lead and the like.
The medical stone is a natural silicate porous material, is mainly produced in China, is widely applied to water treatment, household cookers and the like at present, and mainly utilizes the natural porous microstructure characteristic and the characteristic of being rich in various health beneficial elements. The medical stone is called as 'east Shenshi' and 'Yashi'; as early as the Ming Dynasty, Li Shizhen written "compendium of materia Medica" is well documented. Modern scientific analysis results show that the microstructure of the medical stone particles is porous like a sponge, has physiological activity, has adsorption and ion exchange effects, and contains mineral elements indispensable to human bodies. CN105768230A adopts a ceramic tube containing medical stone as a cigarette waking device to reduce harmful substances such as tar in cigarette smoke. In the field of electronic cigarettes, CN205512363U uses medical stones as an alternative for adsorbing smoke oil in a smoke channel; CN105813815A uses medical stone as an alternative ceramic matrix material for preparing the porous ceramic heating element for the electronic cigarette, but the firing temperature of the ceramic body in the patent application is still as high as more than 1100-14 ℃, and the beneficial effect of natural ore materials such as medical stone and the like as main ceramic skeleton materials on the formation of the porous ceramic material is not disclosed.
The atomizing core is a core component for generating aerosol smoke in the electronic cigarette, and has extremely high requirements on the oil absorption capacity, the oil locking capacity and the oil guiding capacity of the porous ceramic. When a new unused commercial electronic cigarette is placed for a period of time, leaked smoke oil is often visible at the air inlet and the smoke outlet, so that an atomization core which has excellent oil absorption, oil locking and oil guiding capabilities and prevents oil leakage needs to be developed.
In addition, the existing raw materials and manufacturing methods for manufacturing porous ceramics, especially the method of firing high-temperature sintering ceramics at low temperature by using auxiliary agents, are difficult to take into account the basic parameters such as strength, porosity and micropore size distribution; on the other hand, harmful elements such as lead, cadmium and the like brought along with the auxiliary agent are separated out and enter a human body along with steam smoke at the working temperature of the atomizing core close to 300 ℃, and the design aim of reducing harm of the electronic cigarette is deviated.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a preparation method of a porous ceramic material for an atomizing core by using medical stone as a main matrix material and the porous ceramic material prepared by the method.
In a first aspect, the invention provides a preparation method of porous ceramic for an atomizing core, which takes medical stone as aggregate and comprises the following steps:
s1, uniformly mixing the ceramic base material and the stabilizer to obtain main material dry powder; wherein the ceramic base material comprises at least 50 wt% of medical stone based on the total weight of the ceramic base material;
s2: adding a pore-forming agent into the main material dry powder and uniformly mixing to obtain a precursor mixture;
s3: forming the precursor mixture to obtain a ceramic blank;
s4: and sintering the ceramic body to obtain the porous ceramic.
Further, the ceramic base material further comprises at least one of hexacyclic stone, diatomite, potassium feldspar, albite and lepidolite.
Further, the stabilizing agent is sodium silicate and/or sodium carboxymethyl cellulose.
Further, the pore-forming agent is powder and/or short fiber, for example, any one selected from wood, bamboo, carbon, organic materials such as polymethyl methacrylate.
Further, in the step S1, silver powder is added to obtain a silver-containing main material dry powder.
Further, the precursor mixture contains 0.5 wt% to 4 wt% of a stabilizer, 0 wt% to 60 wt% of metal silver powder, 2.5 wt% to 35 wt% of a pore-forming agent and the balance of a ceramic base material, wherein the weight of the stabilizer, the metal silver powder and the pore-forming agent is calculated by the total weight of the precursor mixture.
Further, the ceramic base material comprises 5-10 wt% of hexacyclic stone, 5-10 wt% of diatomite, 5-12 wt% of feldspar and 3-8 wt% of lepidolite, based on the total weight of the ceramic base material.
Further, the molding includes compression molding.
Further, the sintering temperature of the sintering is lower than 1000 ℃.
Further, the sintering comprises heating the ceramic blank to 450-550 ℃, preserving heat for 0.5-3 hours, and then heating to 800-950 ℃, preserving heat and sintering for 0.3-2 hours.
The preparation method of the porous ceramic adopts natural medical stone as the aggregate of the porous ceramic, can be fired and formed under normal pressure under the conventional atmospheric condition, has mild sintering condition, does not need to introduce auxiliary agents such as glass powder with low melting point and the like, is directly fired and formed under the low temperature condition, is used as an atomization core material of the electronic cigarette, and releases toxic elements in zero.
The medical stone particles have a large number of micro-porous and mesoporous structures, and the two-step firing process provided by the invention, which is characterized in that the heat preservation is carried out at 450-550 ℃ for 0.5-3 hours, and then the temperature is raised to 800-950 ℃ for heat preservation and sintering for 0.3-2 hours, ensures the microstructure integrity of the porous ceramic, can obtain more than 90% of porosity, and has the bending strength of more than 20 MPa.
The raw material mixing can adopt the common ceramic raw material mixing process, such as ball milling, stirring, kneading and the like; the grinding balls can be made of ceramic and/or metal materials, such as ZrO2 grinding balls, silicon nitride grinding balls, alumina grinding balls, hard alloy grinding balls, and the like, and the ball-to-material ratio and the grinding ball diameter grading can be easily determined by a person skilled in the art through experiments as long as the ceramic raw materials can be uniformly mixed. Suitably, the ball milling process may be dry ball milling or wet ball milling, such as adding ethanol and water.
In some embodiments, the ceramic raw material may be a commercially available powder with a particle size of 200-500 mesh, or may be processed into 200-500 mesh powder by using natural ore for standby.
In some embodiments, the pre-mix or post-mix ceramic raw materials are preferably screened through a 50-300 mesh screen, which is effective in breaking up agglomerates formed during the mixing process and preventing the presence of large particles in the mixture from affecting the pore distribution of the material.
Pore formers have the meaning generally known in the art, occupy the space of the ceramic body and gradually decompose and/or gasify during the heating and sintering process to form a micro-pore structure. In some embodiments, the pore former is wood fiber, short carbon fiber, carbon powder, polymethyl methacrylate powder, or the like. In some embodiments, the wood fibers and the short carbon fibers have a diameter of 20 to 100 μm and a length of 60 to 500 μm, and the carbon powder and the polymethyl methacrylate powder have a particle size of 50 to 500 mesh. The micro-porous structure generated by the decomposition of the pore agent and the mesoporous structure of the medical stone particles jointly form the micro-composite pore structure of the porous ceramic.
The precursor mixture is preferably dried, for example, by vacuum drying, freeze drying or the like to remove water.
In some embodiments, the precursor mixture can be subjected to thermal plasticizing and compression molding, for example, after the precursor mixture is sieved, the precursor mixture is subjected to thermal plasticizing and compression molding at 130-180 ℃ to obtain a ceramic green body, and the molding pressure is, for example, 0.6-35 MPa. In some embodiments, the precursor mixture is formed by pugging with a liquid such as deionized water and other conventional methods.
In some embodiments, the sintering temperature rise rate is 10 ℃ to 100 ℃/min.
In some embodiments, the porosity of the porous ceramic may be adjusted in a range of 10% to 90% and the average pore size may be adjusted in a range of 10 μm to 150 μm, based on the application purpose of the porous ceramic device. In some embodiments, the adjustment can be made, for example, by pore former addition and pore former particle size selection.
Another aspect of the invention is the porous ceramic material obtained by the preparation method.
Another aspect of the invention is the use of a porous ceramic material in an electronic smoke atomizer.
Drawings
FIG. 1 is a schematic view of the manufacturing process of the porous ceramic special for the electronic cigarette atomizing core of the invention;
FIG. 2 is an example of a firing process curve of the porous ceramic for the electronic cigarette atomizing core according to the present invention;
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings. The embodiments are only for clear understanding of technical features, objects and effects of the present invention, and do not limit the present invention.
The purpose of the invention is: the preparation method of the porous ceramic material which is beneficial to human health and has excellent oil absorption, oil locking and oil guiding capabilities, the porous ceramic and the application of the porous ceramic in the electronic cigarette atomization core are provided.
Referring to fig. 1, a process for manufacturing a porous ceramic for an atomizing core includes the following steps:
and step S1, mixing and grinding the ceramic main materials. The method comprises the steps of preparing and blending Chinese medical stone, hexacyclic stone, diatomite, potash feldspar, albite, lepidolite, sodium silicate and/or sodium carboxymethylcellulose with the granularity of 200-500 meshes and optional metal silver powder, mixing the mixture with deionized water and ZrO2 grinding balls according to the mass ratio of 1:2:3, and carrying out ball milling on a planetary ball mill for 1-8 hours to obtain main material dry powder.
Roller ball mill can also be used for mixing. Of course, other mixing methods may be used, provided that the raw materials are uniformly mixed, for example, a kneader or a stirrer may be used to stir the dry mixture for 30 minutes to 2 hours.
Sodium silicate and sodium carboxymethyl cellulose are analytically pure.
The metal silver powder is added to endow the porous ceramic with a disinfection function, and the preferable mass ratio of the metal silver powder is 0-60 wt%. The specific blending mass ratio is preferably determined depending on the functional properties of the porous ceramic member to be manufactured in the embodiment.
And step S2, preparing a pore-forming agent and obtaining a precursor mixture. And adding the pore-forming agent into the main material dry powder, continuing ball milling for 3-10 hours, and then placing the mixture in a drying oven to dry at 90 ℃ to obtain a precursor mixture.
The pore-forming agent can be any one of wood fiber, short carbon fiber, carbon powder, polymethyl methacrylate powder and the like. The pore-forming agent is preferably used in an amount of 5 to 70 wt%, preferably adjusted according to the porosity and average pore diameter of the target member to be manufactured.
Preferably, the wood fiber and the short carbon fiber have a diameter of 20 to 100 μm and a length of 60 to 500 μm, and the carbon powder and the polymethyl methacrylate powder have a particle size of 50 to 500 mesh. Preferably, the polymethylmethacrylate powder is analytically pure.
The drying of the precursor mixture to remove water may be carried out by other methods such as vacuum drying and freeze drying.
And step S3, preparing a precursor green body section by plasticizing and hot pressing, namely, sieving the precursor mixture, and heating, plasticizing and compression molding at 130-180 ℃ to obtain the precursor green body section.
Heating, plasticizing and compression molding, and performing the molding under the pressure of 0.6 to 35 MPa.
Or adding deionized water into the precursor powder, pugging, and other methods.
Preferably, the mass ratio of the precursor powder to the deionized water is 3: 1-6: 1. after pugging, the mixture can be molded under a pressure of 0.6MPa to 35MPa, for example, the mixture of the precursor and deionized water is mixed to obtain pugging material, the pugging material is put into a square sheet-shaped mold, and the pugging material is pressed under a pressure of 0.6MPa to 35MPa to obtain a ceramic blank. The shape and structure of the blank is not limited to a square sheet, depending on the properties of the target article.
And step S4, sintering the ceramic body into porous ceramic through a two-stage heating process. And heating the precursor blank section in a resistance furnace to 450-550 ℃, preserving heat for 0.5-3 hours, heating to 800-950 ℃, preserving heat and sintering for 0.3-2 hours to obtain the porous ceramic. Please refer to an example of a firing profile of the porous ceramic member shown in fig. 2.
Other heating and firing modes can also be adopted, such as gas heating and a matched ceramic firing kiln and the like.
Preferably, the temperature rise rate of the precursor blank profile is 10-100 ℃/min in the steps of preserving heat at 450-550 ℃ for 0.5-3 hours and preserving heat at 800-950 ℃ for 0.3-2 hours.
In the embodiment, the heat preservation sintering at 450-550 ℃ and 800-950 ℃ is carried out under atmospheric conditions and normal pressure.
By controlling and adjusting the raw material ratio, porous ceramics with different porosities and silver contents can be obtained, for example, as described in the following examples.
Example 1:
the raw materials are mixed according to the required proportion, then mixed with deionized water and ZrO2 grinding balls according to the mass ratio of 1:2:3, ball-milled for 18 hours on a planetary ball mill, dried in a drying box, made into sheet-shaped sections (wet method) after pugging, and fired according to the sintering process curve of figure 2.
The desired profile can also be formed by a thermoplastic extrusion process (dry process) and fired to form the target ceramic.
The purpose of adding 1 wt% of silver powder into the raw material at the air inlet end is to endow the material with the functions of disinfection and sterilization.
The porosity of the prepared medical stone-based ceramic porous material is 40-60%, and the average pore diameter is 20-30 microns.
Example 2:
the metal silver powder with the weight percent less than or equal to 0.5 percent is added into the raw materials to endow the oil guide body material with the function of disinfection and sterilization, and the change of the electrical insulation performance of the oil guide body by trace silver can be ignored.
The remaining process parameters were the same as for the manufacturing process of example 1.
The porosity of the prepared medical stone-based porous ceramic material is not lower than 85%, and the average pore diameter is 60-70 microns.
Example 3:
the main purpose of adding 8 wt% of metal silver powder into the raw materials is to utilize the molten metal silver to strengthen the microcosmic connection between ceramic particles such as medical stone and the like, thereby improving the overall strength of the material and endowing the porous ceramic with certain conductive capability. In microcosmic view, the melting points of the 200-500-mesh silver powder and the medical stone particles are both low and are both between 700 and 800 ℃, and the co-sintering can be realized.
The process parameters were the same as in example 1, except that the sintering temperature in the second stage was 950 ℃ for 2 hours.
The porosity of the prepared medical stone-based porous ceramic is not lower than 80%, the average pore diameter is 50-69 micrometers, and the thickness is 0.5 mm.
The medical stone particles have a large number of micropores and mesopore structures, and the porosity of not less than 80-90% can be usually obtained only by adding a certain pore-forming amount, and the bending strength of more than 20MPa is also achieved.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. A preparation method of porous ceramic for an atomizing core is characterized in that a ceramic base material contains medical stone, and comprises the following steps:
s1, uniformly mixing the ceramic base material and the stabilizer to obtain main material dry powder; wherein the ceramic base material comprises at least 50 wt% of medical stone based on the total weight of the ceramic base material;
s2: adding a pore-forming agent into the main material dry powder and uniformly mixing to obtain a precursor mixture;
s3: forming the precursor mixture to obtain a ceramic blank;
s4: and sintering the ceramic body to obtain the porous ceramic.
2. The method of claim 1, wherein the ceramic base further comprises at least one of hexacyclic stone, diatomaceous earth, potash feldspar, albite, and lepidolite.
3. The preparation method according to claim 1, wherein the stabilizer is sodium silicate and/or sodium carboxymethyl cellulose; the pore-forming agent is powder and/or short fiber, for example, any one selected from wood, bamboo, carbon, organic materials such as polymethyl methacrylate.
4. The method according to claim 1, further comprising adding silver powder in step S1 to obtain a silver-containing main dry powder.
5. The preparation method of claim 1, further comprising 0.5 wt% to 4 wt% of a stabilizer, 0 wt% to 60 wt% of a silver metal powder, 2.5 wt% to 35 wt% of a pore-forming agent, and the balance of a ceramic binder, based on the total weight of the precursor mixture.
6. The preparation method according to claim 1, further comprising 5-10 wt% of hexacyclic stone, 5-10 wt% of diatomite, 5-12 wt% of feldspar and 3-8 wt% of lepidolite based on the total weight of the ceramic base.
7. The method of claim 1, further wherein the sintering temperature of the sintering is less than 1000 ℃.
8. The preparation method according to claim 9, further comprising the step of heating the ceramic body to 450-550 ℃ for 0.5-3 hours, and then heating to 800-950 ℃ for 0.3-2 hours.
9. Porous ceramic material obtainable by the process according to any one of claims 1 to 8.
10. Use of the porous ceramic material of claim 9 in an electronic cigarette.
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| CN112806613A (en) * | 2021-01-20 | 2021-05-18 | 珠海亿特立新材料有限公司 | Preparation method of porous ceramic with nano-silver, porous ceramic, electronic cigarette atomization core and electronic cigarette |
| CN113416089A (en) * | 2021-06-04 | 2021-09-21 | 深圳市华诚达精密工业有限公司 | Porous atomizing core capable of releasing negative ions and preparation method thereof |
| CN113754453A (en) * | 2021-08-23 | 2021-12-07 | 深圳市安芯精密组件有限公司 | Carbon fiber gain ceramic atomizing core and preparation method thereof |
| CN113880603A (en) * | 2021-11-11 | 2022-01-04 | 深圳市汉清达科技有限公司 | Porous ceramic composition and preparation method thereof |
| CN116283258A (en) * | 2023-03-06 | 2023-06-23 | 深圳市吉迩科技有限公司 | High heat conduction porous ceramic and porous ceramic atomizing core |
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Application publication date: 20210108 |