CN117658609A - Preparation method of porous ceramic matrix, atomization core and aerosol forming device - Google Patents
Preparation method of porous ceramic matrix, atomization core and aerosol forming device Download PDFInfo
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- CN117658609A CN117658609A CN202311584707.7A CN202311584707A CN117658609A CN 117658609 A CN117658609 A CN 117658609A CN 202311584707 A CN202311584707 A CN 202311584707A CN 117658609 A CN117658609 A CN 117658609A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 186
- 239000011159 matrix material Substances 0.000 title claims abstract description 94
- 239000000443 aerosol Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title abstract description 21
- 238000000889 atomisation Methods 0.000 title abstract description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000000034 method Methods 0.000 claims abstract description 43
- 239000011268 mixed slurry Substances 0.000 claims abstract description 42
- 238000005245 sintering Methods 0.000 claims abstract description 40
- 238000005266 casting Methods 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011812 mixed powder Substances 0.000 claims abstract description 30
- 239000003960 organic solvent Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 239000011787 zinc oxide Substances 0.000 claims abstract description 24
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 21
- 239000003292 glue Substances 0.000 claims abstract description 19
- 238000007599 discharging Methods 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000011029 spinel Substances 0.000 claims abstract description 16
- 229910052596 spinel Inorganic materials 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000010453 quartz Substances 0.000 claims description 20
- 239000012298 atmosphere Substances 0.000 claims description 18
- 230000001590 oxidative effect Effects 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000011230 binding agent Substances 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 11
- 239000004014 plasticizer Substances 0.000 claims description 9
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 8
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000011701 zinc Substances 0.000 claims description 7
- 229910052725 zinc Inorganic materials 0.000 claims description 7
- -1 zinc aluminate Chemical class 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- 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 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- ZPIRTVJRHUMMOI-UHFFFAOYSA-N octoxybenzene Chemical compound CCCCCCCCOC1=CC=CC=C1 ZPIRTVJRHUMMOI-UHFFFAOYSA-N 0.000 claims description 3
- 229920000058 polyacrylate Polymers 0.000 claims description 3
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims description 3
- 229910001950 potassium oxide Inorganic materials 0.000 claims description 3
- 235000019353 potassium silicate Nutrition 0.000 claims description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical class CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 14
- 239000011148 porous material Substances 0.000 abstract description 11
- 229910000611 Zinc aluminium Inorganic materials 0.000 abstract description 9
- HXFVOUUOTHJFPX-UHFFFAOYSA-N alumane;zinc Chemical compound [AlH3].[Zn] HXFVOUUOTHJFPX-UHFFFAOYSA-N 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 9
- 239000013078 crystal Substances 0.000 abstract description 5
- 238000000465 moulding Methods 0.000 abstract description 5
- 238000001035 drying Methods 0.000 description 13
- 238000001746 injection moulding Methods 0.000 description 9
- 239000010408 film Substances 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 230000033001 locomotion Effects 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical group O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
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- 238000004321 preservation Methods 0.000 description 2
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- 230000002035 prolonged effect Effects 0.000 description 2
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- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 1
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
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- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical group [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The application provides a preparation method of a porous ceramic matrix, an atomization core and an aerosol forming device, wherein the preparation method of the porous ceramic matrix comprises the steps of providing zinc oxide, aluminum hydroxide, a filler and a pore-forming agent, mixing to obtain mixed powder material, providing an organic solvent and deionized water, mixing the mixed powder material, the organic solvent and water to obtain mixed slurry, casting the mixed slurry to obtain a ceramic green body, and performing glue discharging and sintering on the ceramic green body to form the porous ceramic matrix with a zinc-aluminum spinel structure. The internal stress of the porous ceramic matrix prepared by the water-based casting molding method is smaller, the surface of the porous ceramic matrix is smooth after the ceramic green body formed by casting is sintered, the pore size distribution is uniform, the use effect is better, zinc oxide and aluminum hydroxide form a zinc aluminum spinel structure with a regular octahedral crystal form in the sintering process, and the strength and the service life of the porous ceramic matrix can be improved.
Description
Technical Field
The application belongs to the technical field of aerosol forming devices, and particularly relates to a preparation method of a porous ceramic matrix, an atomization core and an aerosol forming device.
Background
In the related art, the porous ceramic is molded by injection molding, and the density of the ceramic blank is not uniform due to the existence of the glue injection port in the injection molding mode, so that the pore size distribution of the sintered ceramic blank is not uniform, and the use effect of the prepared porous ceramic is affected.
Disclosure of Invention
The purpose of the application is to provide a preparation method of a porous ceramic matrix, an atomization core and an aerosol forming device, so as to solve the technical problem that the use effect of the porous ceramic prepared by injection molding is poor.
In a first aspect, the present application provides a method for preparing a porous ceramic matrix, the method for preparing a porous ceramic matrix comprising:
providing zinc oxide, aluminum hydroxide, a filler and a pore-forming agent, and mixing to obtain a mixed powder material;
providing an organic solvent and deionized water, and mixing the mixed powder material, the organic solvent and water to obtain mixed slurry;
casting the mixed slurry to obtain a ceramic green body;
and discharging glue from the ceramic green body, and sintering to form the porous ceramic matrix with the zinc aluminate spinel structure.
In the preparation method of the porous ceramic matrix, zinc oxide, aluminum hydroxide, filler and pore-forming agent are mixed to obtain mixed powder material, the mixed powder material, an organic solvent and water are stirred to obtain mixed slurry, the mixed slurry is cast and molded to obtain a ceramic green body, and the ceramic green body is subjected to glue discharging and sintering to form the porous ceramic matrix with a zinc-aluminum spinel structure. Compared with the traditional injection molding method, the porous ceramic matrix prepared by the water-based casting method has smaller internal stress, uniform powder particle distribution in the mixed slurry, smooth surface of the porous ceramic matrix after sintering the cast ceramic green body, uniform pore size distribution and better use effect. In addition, zinc oxide and aluminum hydroxide form a zinc aluminum spinel structure with a regular octahedral crystal form in the sintering process, so that the strength of the porous ceramic matrix can be improved, the thermal expansion coefficient of the porous ceramic matrix is reduced, the porous ceramic matrix can be matched with a heating element, and the heating element is not broken and the service life is shortened due to the fact that the thermal expansion coefficient difference of the porous ceramic matrix and the heating element is large in the heating element atomization process.
The filler comprises high-purity quartz powder, and the pore-forming agent comprises graphite powder, wherein the high-purity quartz powder is a plurality of spherical quartz particles, the diameter range is 50-150 mu m, the graphite powder is a plurality of spherical graphite, and the diameter range is 100-200 mu m.
Wherein the organic solvent comprises a dispersing agent, a plasticizer and a binder, and the dispersing agent comprises one of ammonium polyacrylate and polyethylene glycol octyl phenyl ether; the plasticizer comprises one of dibutyl phthalate and polyethylene glycol; the binder comprises one or more of water glass, sodium carboxymethyl cellulose, polyvinyl alcohol, and B-76 of the polyvinyl butyral series.
Wherein, in the step of providing zinc oxide, aluminum hydroxide, filler and pore-forming agent, mixing to obtain mixed powder material, the method further comprises the following steps:
providing a sintering aid, wherein the sintering aid comprises one or more of magnesium oxide, potassium oxide, calcium oxide and sodium oxide;
and providing glass powder, and mixing to obtain the mixed powder material.
In the mixed slurry, the mass percentage range of zinc oxide is 3% -6%, the mass percentage range of aluminum hydroxide is 3% -6%, the mass percentage range of filler is 20% -25%, the mass percentage range of pore-forming agent is 30% -40%, the mass percentage range of sintering aid is 3% -5%, the mass percentage range of glass powder is 3% -7%, the mass percentage range of dispersing agent is 0.5% -2.5%, the mass percentage range of binder is 1% -3%, the mass percentage range of plasticizer is 1% -3%, and the mass percentage range of deionized water is 10% -35%.
Wherein, in the process of providing zinc oxide, aluminum hydroxide, filler and pore-forming agent, mixing to obtain mixed powder material, the mixing time is 2-4 h;
stirring the mixed powder material, the organic solvent and water to obtain mixed slurry, wherein the mixing time is 15-30 min;
and in the process of casting and forming the mixed slurry to obtain the ceramic green body, the casting temperature is 80-90 ℃ and the casting time is 20-100 min.
Wherein, after the mixed slurry is cast and molded to obtain a ceramic green body, the method comprises the following steps:
and (3) superposing the multilayer ceramic green bodies and then pressurizing, wherein the pressurizing pressure is 10-35 Mpa, and the pressurizing time is 5-10 min.
Wherein, the steps of discharging glue and sintering the ceramic green body to form the porous ceramic matrix with a zinc aluminate spinel structure include:
placing the ceramic green body into an oxidizing atmosphere furnace for glue discharging, wherein the temperature in the oxidizing atmosphere furnace is increased to a first temperature at a first heating rate, the first heating rate is 0.5 ℃/min-1.5 ℃/min, and the first temperature range is 400 ℃ -500 ℃;
and increasing the temperature in the oxidizing atmosphere furnace to sinter the ceramic green body, wherein the temperature in the oxidizing atmosphere furnace is increased to a second temperature at a second heating rate, wherein the second heating rate is 5 ℃/min-8 ℃/min, and the first temperature is in the range of 1200 ℃ -1300 ℃.
In a second aspect, the present application provides an atomization core comprising a heating element, and a ceramic matrix produced by the method of producing a porous ceramic matrix, the heating element being disposed on the ceramic matrix.
In a third aspect, the present application provides an aerosol-forming device, comprising a housing, a core assembly, and an atomizing core, the core assembly and the atomizing core being disposed in the housing, and the core assembly being electrically connected to the atomizing core, the core assembly being configured to provide energy to the atomizing core and control atomizing parameters, the atomizing core being configured to heat and atomize an aerosol substrate in the housing.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flowchart of a method for preparing a porous ceramic substrate according to an embodiment of the present application;
FIG. 2 is a second flowchart of a method for preparing a porous ceramic substrate according to an embodiment of the present disclosure;
FIG. 3 is a flowchart III of a method for preparing a porous ceramic substrate according to an embodiment of the present application;
FIG. 4 is a flowchart IV of a method for preparing a porous ceramic substrate according to an embodiment of the present application;
fig. 5 is a flowchart of a method for preparing an atomizing core according to an embodiment of the present disclosure.
Detailed Description
The following description of the embodiments of the present application will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without undue burden, are within the scope of the present application.
Reference herein to "an embodiment" or "an implementation" means that a particular feature, structure, or characteristic described in connection with the embodiment or implementation may be included in at least one embodiment of the present application. The appearances of such phrases in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments. Those of skill in the art will explicitly and implicitly appreciate that the embodiments described herein may be combined with other embodiments.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between different objects and not for describing a particular sequential order. Furthermore, the terms "comprise" and "have," as well as any variations thereof, are intended to cover a non-exclusive inclusion.
In the present specification, for convenience, words such as "middle", "upper", "lower", "front", "rear", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, which indicate an azimuth or a positional relationship, are used to describe positional relationships of constituent elements with reference to the drawings, only for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or elements referred to must have a specific azimuth, be configured and operated in a specific azimuth, and thus are not to be construed as limiting the present disclosure. The positional relationship of the constituent elements is appropriately changed according to the direction of the described constituent elements. Therefore, the present invention is not limited to the words described in the specification, and may be appropriately replaced according to circumstances.
In this specification, the terms "mounted," "connected," and "connected" are to be construed broadly, unless explicitly stated or limited otherwise. For example, it may be a fixed connection, a removable connection, or an integral connection; may be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intermediate members, or may be in communication with the interior of two elements. The meaning of the above terms in the present disclosure can be understood by one of ordinary skill in the art as appropriate.
In the related art, the porous ceramic is molded by injection molding, and the density of the ceramic blank is not uniform due to the existence of the glue injection port in the injection molding mode, so that the pore size distribution of the sintered ceramic blank is not uniform, and the use effect of the prepared porous ceramic is affected.
Referring to fig. 1, the present application is directed to a method for preparing a porous ceramic substrate, so as to solve the technical problem of poor use effect of the porous ceramic prepared by injection molding.
The preparation method of the porous ceramic substrate includes, but is not limited to, steps S100, S200, S300 and S400, and the detailed description of steps S100, S200, S300 and S400 is as follows.
S100: providing zinc oxide, aluminum hydroxide, filler and pore-forming agent, and mixing to obtain mixed powder.
Specifically, in the present embodiment, the zinc oxide has a chemical formula of ZnO, and the aluminum hydroxide has a chemical formula of Al (OH) 3. Zinc oxide and aluminum hydroxide are capable of forming a zincate structure with an octahedral crystal form in a silica matrix (filler) during sintering. The porous ceramic matrix is provided with a zinc aluminate spinel structure, so that the strength of the porous ceramic matrix can be improved, the thermal expansion coefficient of the porous ceramic matrix is reduced, the porous ceramic matrix can be matched with a heating element, and the heating element is not broken and the service life is shortened due to the fact that the thermal expansion coefficient difference between the porous ceramic matrix and the heating element is large in the heating element atomization process.
The filler includes high purity quartz powder, specifically, the high purity quartz powder is a high purity quartz powder, in other words, in the present embodiment, the purity of the high purity quartz powder is more than 99%. Further, the high-purity quartz powder is a plurality of spherical quartz particles, and the diameter of the high-purity quartz powder particles ranges from 50 mu m to 150 mu m.
The diameter of the high-purity quartz powder particles can directly influence the subsequent sintering process of the porous ceramic matrix. Specifically, the quartz powder with smaller particle diameter has higher sintering activity, so that the sintering process of the porous ceramic matrix can be promoted, and the quartz powder with larger particle diameter is opposite. Therefore, in the preparation method of the porous ceramic matrix, the diameter of the particles in the high-purity quartz powder ranges from 50 mu m to 150 mu m, so that the effect of promoting the sintering of the porous ceramic matrix is achieved.
Further, smaller particles in the high-purity quartz powder can obtain higher density and finer grain boundaries, the diameter range of the high-purity quartz powder particles in the preparation of the porous ceramic matrix is 50-150 mu m, the mechanical properties of the porous ceramic matrix can be improved, and the strength, toughness, wear resistance and other properties of the prepared porous ceramic matrix can be further improved.
Alternatively, in the present embodiment, the high purity quartz powder may have a diameter of 50 μm, or 62 μm, or 75 μm, or 80 μm, or 88 μm, or 91 μm, or 100 μm, or 111 μm, or 123 μm, or 130 μm, or 144 μm, or 150 μm, or other diameter values within 50 μm-150 μm, which is not limited in this application.
The pore-forming agent comprises graphite powder, specifically, the graphite powder is a plurality of spherical graphites, and the particle diameter of the graphite powder ranges from 100 mu m to 200 mu m.
In this embodiment, the impurity content of the graphite powder is less than 1%. The graphite powder is easy to sinter at high temperature, and is helpful for promoting the sintering process of the porous ceramic matrix. And in addition, graphite powder is used as a pore-forming agent to prepare the porous ceramic matrix, and in the process of discharging glue to form a porous structure, the product formed by combining the graphite powder and oxygen element is carbon dioxide, so that the product generated in the preparation process of the porous ceramic matrix is more economic and environment-friendly. In addition, the graphite powder has high strength and high toughness, can enhance the mechanical property of the porous ceramic matrix, has low price compared with other pore formers, and can reduce the manufacturing cost of the porous ceramic matrix.
Further, in this embodiment, the particle diameter of the graphite powder ranges from 100 μm to 200 μm, so that a pore structure communicating with each other can be formed in the porous ceramic matrix, which is beneficial to improving the air permeability of the porous ceramic matrix.
Alternatively, the particle diameter of the graphite powder may be 100 μm, or 110 μm, or 120 μm, or 135 μm, or 150 μm, or 161 μm, or 172 μm, or 180 μm, or 190 μm, or 200 μm, or other diameter values within the range of 100 μm to 200 μm, which is not limited by the present application. Likewise, in other embodiments, the diameter range of the graphite powder particles may also be adjusted according to the specifications of the porous ceramic matrix, and should not be construed as limiting the present application.
Mixing zinc oxide, aluminum hydroxide, filler and pore-forming agent to obtain mixed powder. Specifically, zinc oxide, aluminum hydroxide, filler and pore-forming agent are poured into a three-dimensional mixer for mixing, and the mixing time is 2-4 hours, so that the components in the mixed powder material are ensured to be uniformly mixed. Alternatively, the mixing time may be 2h, or 2.1h, or 2.3h, or 2.5h, or 2.8h, or 3.0h, or 3.2h, or 3.4h, or 3.6h, or 3.9h, or 4h, or other times within 2h-4h, as the application is not limited.
The three-dimensional mixer is a container rotary mixer, and a charged barrel is driven by a driving shaft to do repeated translation, rotation, rolling and other repeated movements, so that materials are driven to do three-way compound movements in the circumferential direction, the radial direction and the axial direction along the barrel, and therefore the purposes of flowing, diffusing, accumulating and doping various materials mutually are achieved, and the purpose of uniformly mixing mixed powder materials is achieved.
S200: providing an organic solvent and deionized water, and stirring the mixed powder material, the organic solvent and water to obtain mixed slurry.
Specifically, the organic solvent comprises a dispersing agent, a plasticizer and a binder. The dispersing agent is added into the organic solvent and mixed to form mixed slurry, so that the wettability of solid particles can be improved, the dispersion of the mixed slurry is promoted, the mixed slurry has proper viscosity, and the ceramic material performance is improved. The dispersing agent is added into the organic solvent and mixed to form mixed slurry, so that the overall plasticity of the ceramic green body prepared subsequently can be improved, the ceramic green body is ensured to have certain strength, and the ceramic green body is kept in the original shape before sintering. The binder is added into the organic solvent and mixed to form mixed slurry, so that the green strength of the ceramic prepared later can be improved or powder segregation can be prevented.
Further, the dispersant includes one of ammonium polyacrylate, polyethylene glycol octyl phenyl ether. The plasticizer includes one of dibutyl phthalate (DBP), polyethylene glycol (PEG). The binder comprises one or more of water glass, sodium carboxymethylcellulose (CMC), polyvinyl alcohol (PVA), B-76 of the polyvinyl butyral PVB series.
Deionized water, which is pure water from which impurities in the form of ions are removed, is also included in the mixed slurry.
And stirring the organic solvent, deionized water and the mixed powder to obtain mixed slurry. Specifically, the organic solvent and the deionized water are poured into a three-dimensional mixer which is mixed with the mixed powder material, the mixing time is 15-30 min, and the vacuum mixing can be used for defoaming the mixed slurry and improving the mixing uniformity of the organic solvent, the deionized water and the mixed powder material. Alternatively, the stirring time may be 15min, or 16min, or 17min, or 19min, or 20min, or 22min, or 24min, or 25min, or 28min, or 30min, or other time within 15min-30min, which is not limited in this application.
S300: and (5) casting the mixed slurry to obtain a ceramic green body.
The casting forming is a special material processing method, and can prepare high-quality and ultrathin ceramic, glass and other materials.
Specifically, in this embodiment, the casting molding is to flow the mixed slurry with proper viscosity and good dispersibility from the edge of the slurry tank of the casting machine to the base belt, spread the mixed slurry by the relative motion of the base belt and the doctor blade, and form a blank film with a smooth upper surface under the action of surface tension, and the thickness of the blank film is mainly controlled by the gap between the doctor blade and the base belt. The blank film enters a drying chamber along with the base band, part of the organic solvent evaporates, a network structure is formed among solid particles in the mixed slurry under the action of the organic solvent such as a binder and the like, a ceramic green body with certain strength and flexibility is formed, and a reel is used after the dried ceramic green body is stripped from the base band, and then the ceramic green body can be cut, punched or perforated according to a required shape.
Specifically, in the present embodiment, the thickness of the ceramic green body after casting molding is 0.2mm to 1.0mm, alternatively, the ceramic green body may be 0.2mm, or 0.3mm, or 0.4mm, or 0.5mm, or 0.6mm, or 0.7mm, or 0.8mm, or 0.9mm, or 1.0mm, or other thickness values within 0.2mm to 1.0 mm.
Further, in the present embodiment, in the step of casting the mixed slurry to obtain a ceramic green body, the casting temperature is 80 to 90 ℃. In other words, when the blank film enters the drying chamber along with the base band, the temperature in the drying chamber is 80-90 ℃.
If the temperature in the drying chamber is lower than 80 ℃, the ceramic green body can be possibly caused to be moist and adhered, and the subsequent processing of the ceramic green body is not facilitated; if the temperature in the drying chamber is higher than 90 ℃, the ceramic green body may be subjected to undesirable phenomena such as air bubbles and warpage, which affect the use effect.
Therefore, the temperature in the drying chamber is 80-90 ℃, so that the drying degree of the ceramic green body can be ensured not to influence the subsequent preparation, and the problems of more bubbles, warping and the like in the ceramic green body can be ensured. Alternatively, the temperature within the drying chamber may be 80 ℃, or 81 ℃, or 82 ℃, or 83 ℃, or 84 ℃, or 85 ℃, or 86 ℃, or 87 ℃, or 88 ℃, or 89 ℃, or 90 ℃, or other temperatures within 80 ℃ -90 ℃.
Further, in the present embodiment, in the step of casting the mixed slurry to obtain a ceramic green body, the casting time is 20min to 100min. In other words, when the blank film enters the drying chamber along with the base band, the length of the base band in the drying chamber is 10m-15m, and the transmission speed of the base band is 0.2m/min-2.5m/min.
Likewise, if the casting time is too short (less than 100 min), the length of the base band is too short (less than 15 m), and the transmission speed of the base band is relatively high (more than 2.5 m/min), the ceramic green body is possibly caused to be moist and adhered, which is not beneficial to the subsequent processing of the ceramic green body; if the casting time is too long (more than 100 min), the length of the base band is too long (more than 15 m), and the transmission speed of the base band is relatively slow (less than 0.2 m/min), adverse phenomena such as bubbles and warping of the ceramic green body, which affect the use effect, may be caused.
Therefore, the casting time of casting molding is 20-100 min, the length of the base band in the drying chamber is 10-15 m, and the transmission speed of the base band is 0.2-2.5 m/min, so that the drying degree of the ceramic green body can be ensured not to influence the subsequent preparation, and the problems of more bubbles, warping and the like in the ceramic green body can be ensured. Alternatively, the casting time of the casting molding may be 20min, or 30min, or 40min, or 50min, or 65min, or 70min, or 85min, or 90min, or 100min, or other time within 20min-100min, the length of the base band in the drying chamber may be 10m, or 11m, or 12m, or 13m, or 14m, or other dimension within 10m-15m, and the transmission speed of the base band may be 0.2m/min, or 1.5m/min, or 1.7m/min, or 1.0m/min, or 1.3m/min, or 1.8m/min, or 2.0m/min, or 2.3m/min, or 2.5m/min, or other speed within 0.2m/min-2.5m/min, which is not limited in this application.
In this embodiment, the organic solvent and deionized water are added into the mixed slurry, wherein the mass percentage of the deionized water ranges from 10% to 35%, so that the casting process is water-based casting.
S400: and discharging glue from the ceramic green body, and sintering to form the porous ceramic matrix with the zinc aluminate spinel structure.
The porous ceramic matrix is prepared by a water-based casting method, and compared with the traditional injection molding method, the preparation method of the porous ceramic matrix can reduce the use amount of an organic solvent, is safer and more environment-friendly, and has the advantages that the internal stress of the porous ceramic matrix prepared by the water-based casting method is smaller, powder particles in the mixed slurry are uniformly distributed, the sintered ceramic green body is smooth in surface and uniform in pore size distribution. When the porous ceramic matrix is applied to an atomization device, after thick film printing or thin film coating, the heating element can be well combined with the porous ceramic matrix, so that the atomization taste is improved, the use defects of the porous ceramic matrix are reduced, and the service life is prolonged.
In the preparation method of the porous ceramic matrix, zinc oxide, aluminum hydroxide, a filler and a pore-forming agent are mixed to obtain mixed powder, the organic solvent and water are stirred to obtain mixed slurry, the mixed slurry is cast and molded to obtain a ceramic green body, and the ceramic green body is subjected to glue discharging and sintering to form the porous ceramic matrix with a zinc-aluminum spinel structure. Compared with the traditional injection molding method, the porous ceramic matrix prepared by the water-based casting method has smaller internal stress, uniform powder particle distribution in the mixed slurry, smooth surface of the porous ceramic matrix after sintering the cast ceramic green body, better use effect and uniform pore size distribution. In addition, zinc oxide and aluminum hydroxide form a zinc aluminum spinel structure with a regular octahedral crystal form in the sintering process, so that the strength of the porous ceramic matrix can be improved, the thermal expansion coefficient of the porous ceramic matrix is reduced, the porous ceramic matrix can be matched with a heating element, and the heating element is not broken and the service life is shortened due to the fact that the thermal expansion coefficient difference of the porous ceramic matrix and the heating element is large in the heating element atomization process.
Referring to fig. 2, the step S100 of providing zinc oxide, aluminum hydroxide, filler, and pore-forming agent, mixing to obtain a mixed powder material further includes steps S110 and S120, and the steps S110 and S120 are described in detail below.
S110: a burn aid is provided, wherein the burn aid comprises one or more of magnesium oxide, potassium oxide, calcium oxide, sodium oxide.
The present application is illustrated with the burn aid as magnesium oxide and should not be construed as limiting the present application. The magnesium oxide is added into the mixed powder material, so that the sintering temperature of the ceramic green body can be reduced in the sintering process, the sintering time is shortened, the zinc aluminum spinel can be produced more quickly, and the sintering efficiency is improved.
S120: and providing glass powder, and mixing to obtain the mixed powder material.
The glass powder has a lower melting point and higher viscosity, can play a role of a binder in the sintering process of the porous ceramic matrix, and can fill gaps among particles of the porous ceramic matrix to promote densification of the porous ceramic matrix.
Further, in the present embodiment, in the mixed slurry, the mass percentage range of the zinc oxide is 3% -6%, the mass percentage range of the aluminum hydroxide is 3% -6%, the mass percentage range of the filler is 20% -25%, the mass percentage range of the pore-forming agent is 30% -40%, the mass percentage range of the sintering aid is 3% -5%, the mass percentage range of the glass frit is 3% -7%, the mass percentage range of the dispersing agent is 0.5% -2.5%, the mass percentage range of the binder is 1% -3%, the mass percentage range of the plasticizer is 1% -3%, and the mass percentage range of the deionized water is 10% -35%.
In the present embodiment, the porous ceramic matrix prepared based on the mixed slurry and the preparation process in the above ratio has a porosity of 50 to 65%, an average pore diameter of 40 to 110 μm, and a flexural strength of 8 to 28Mpa. Alternatively, the porosity of the porous ceramic matrix may be 50%, or 51%, or 52%, or 55%, or 57%, or 58%, or 60%, or 65%, or other proportions within 50% -65%, and the average pore diameter of the porous ceramic matrix may be 45 μm, or 50 μm, or 60 μm, or 78 μm, or 80 μm, or 90 μm, or 100 μm, or other dimensions within 40 μm-110 μm, and the flexural strength of the porous ceramic matrix may be 10Mpa, or 12Mpa, or 15Mpa, or 17Mpa, or 20Mpa, or 23Mpa, or 25Mpa, or 26Mpa, or other values within 8Mpa-28, depending on the fine tuning of the proportions of the above components.
Referring to fig. 3, step S310 is further included after the step S300 of casting the mixed slurry to obtain a ceramic green body, and the detailed description of step S310 is as follows.
S310: and (3) superposing the multilayer ceramic green bodies and then pressurizing, wherein the pressurizing pressure is 10-35 Mpa, and the pressurizing time is 5-10 min.
According to the thickness required by the product matched with the porous ceramic matrix, the multi-layer ceramic green bodies can be pressed and bonded into a whole after being overlapped, so that the thickness required by the product matched with the porous ceramic matrix can be met.
Alternatively, the pressurization pressure may be 10Mpa, or 15Mpa, or 17Mpa, or 20Mpa, or 23Mpa, or 27Mpa, or 30Mpa, or 35Mpa, or other values within 10Mpa-35Mpa, and the pressurization time may be 5min, or 6min, or 7min, or 8min, or 9min, or 10min, or other times within 5min-10min.
Referring to fig. 4, the step S400 of discharging glue from the ceramic green body and sintering the ceramic green body to form the porous ceramic matrix with a zinc-aluminum spinel structure further includes steps S410 and S420, and the steps S410 and S420 are described in detail below.
S410: and placing the ceramic green body into an oxidizing atmosphere furnace for glue discharging, wherein the temperature in the oxidizing atmosphere furnace is increased to a first temperature at a first heating rate, the first heating rate is 0.5 ℃/min-1.5 ℃/min, and the first temperature range is 400 ℃ -500 ℃.
The ceramic green body is placed into an oxidizing atmosphere furnace for discharging glue, and mainly aims to discharge deionized water, part of organic solvents and part of inorganic matters in the ceramic green body so as to promote the follow-up sintering process.
Further, after the temperature in the oxidizing atmosphere furnace is raised to the first temperature at the first temperature rising rate, the ceramic green body is required to be placed in the oxidizing atmosphere furnace for heat preservation for 2-4 hours so as to ensure the glue discharging effect.
If the first heating rate is lower than 0.5 ℃/min, the glue discharging efficiency is too low, which is not beneficial to the batch preparation of the porous ceramic matrix; if the first heating rate is higher than 1.5 ℃/min, the ceramic green body may be warped and bubble generated due to the internal stress problem.
Therefore, the first heating rate is 0.5 ℃/min-1.5 ℃/min, so that the glue discharging efficiency of the ceramic green body can be ensured, and the problems of more bubbles, warping and the like in the ceramic green body can be avoided. Alternatively, the first heating rate may be 0.5 ℃/min, or 0.6 ℃/min, or 0.7 ℃/min, or 0.8 ℃/min, or 0.9 ℃/min, or 1.0 ℃/min, or 1.2 ℃/min, or 1.5 ℃/min, or other heating rates within the range of 0.5 ℃/min-1.5 ℃/min.
Alternatively, the first temperature range may be 400 ℃, or 410 ℃, or 430 ℃, or 450 ℃, or 465 ℃, or 470 ℃, or 480 ℃, or 490 ℃, or 500 ℃, or other temperatures within 400 ℃ -500 ℃.
S420: and increasing the temperature in the oxidizing atmosphere furnace to sinter the ceramic green body, wherein the temperature in the oxidizing atmosphere furnace is increased to a second temperature at a second heating rate, wherein the second heating rate is 5 ℃/min-8 ℃/min, and the first temperature is in the range of 1200 ℃ -1300 ℃.
The ceramic green body is sintered in an oxidizing atmosphere furnace, namely, the ceramic green body is heated at high temperature, so that particles in the ceramic green body are combined with each other to form a compact porous ceramic matrix. The principle of sintering is to utilize sinterable components in the ceramic green body, melt or soften at high temperatures, fill voids between particles, and promote interdiffusion and bonding between particles. Meanwhile, the sintering can fully discharge gas, deionized water and organic solvent in the ceramic green body, and the compactness and performance of the porous ceramic matrix are improved.
Further, after the temperature in the oxidizing atmosphere furnace is raised to the second temperature at the second temperature raising rate, the ceramic green body needs to be placed in the oxidizing atmosphere furnace for heat preservation for 2-3 hours so as to ensure the sintering effect.
Alternatively, the second temperature rise rate may be 5 ℃/min, or 5.5 ℃/min, or 5.7 ℃/min, or 6.0 ℃/min, or 6.3 ℃/min, or 7.0 ℃/min, or 7.6 ℃/min, or 8 ℃/min, or other temperature rise rates within the range of 5 ℃/min-8 ℃/min, the second temperature range may be 1200 ℃, or 1210 ℃, or 1230 ℃, or 1250 ℃, or 1265 ℃, or 1270 ℃, or 1280 ℃, or 1290 ℃, or 1300 ℃, or other temperatures within the range of 1200 ℃ -1300 ℃.
Referring to fig. 5, the following provides a detailed description of the preparation method of the atomizing core according to the above embodiment, and the preparation method of the atomizing core includes, but is not limited to, steps S100, S200, S300, S400 and S500, and the detailed description of steps S100, S200, S300, S400 and S500 is as follows.
S100: providing zinc oxide, aluminum hydroxide, filler and pore-forming agent, and mixing to obtain mixed powder.
S200: providing an organic solvent and deionized water, and stirring the mixed powder material, the organic solvent and water to obtain mixed slurry.
S300: and (5) casting the mixed slurry to obtain a ceramic green body.
S400: and discharging glue from the ceramic green body, and sintering to form the porous ceramic matrix with the zinc aluminate spinel structure.
S500: and (3) putting the porous ceramic matrix into a printing jig, printing alloy slurry on the surface of the porous ceramic matrix, and performing vacuum sintering to obtain the atomization core.
The steps for preparing the porous ceramic matrix in the preparation method of the atomization core are the same as the steps for preparing the porous ceramic matrix, and are not described in detail herein.
The application also provides an atomization core, which comprises a heating element and a ceramic matrix prepared by the preparation method of the porous ceramic matrix, wherein the heating element is arranged on the ceramic matrix.
According to the atomization core provided by the embodiment, the surface of the porous ceramic matrix formed after the ceramic green body formed by casting is sintered is flat, the pore size distribution is uniform, and the heating element can be well combined with the porous ceramic matrix, so that the atomization taste is improved, the use defects of the porous ceramic matrix are reduced, and the service life is prolonged. In addition, zinc oxide and aluminum hydroxide form a zinc aluminum spinel structure with a regular octahedral crystal form in the sintering process, so that the strength of the porous ceramic matrix can be improved, the thermal expansion coefficient of the porous ceramic matrix is reduced, the porous ceramic matrix can be matched with a heating element, and the heating element is not broken and the service life is shortened due to the fact that the thermal expansion coefficient difference of the porous ceramic matrix and the heating element is large in the heating element atomization process.
The application also provides an aerosol forming device, aerosol forming device includes casing, electric core subassembly, and the atomizing core, electric core subassembly with the atomizing core is located in the casing, just electric core subassembly electricity is connected the atomizing core, electric core subassembly is used for the atomizing core provides energy and control atomizing parameter, the atomizing core is used for heating and atomizing aerosol substrate in the casing.
The aerosol forming device provided by the embodiment adopts the atomization core provided by the application, and has better atomization effect and longer service life.
While the foregoing is directed to embodiments of the present application, it will be appreciated by those of ordinary skill in the art that numerous modifications and variations can be made without departing from the principles of the present application, and such modifications and variations are also considered to be within the scope of the present application.
Claims (10)
1. A method for preparing a porous ceramic matrix, the method comprising:
providing zinc oxide, aluminum hydroxide, a filler and a pore-forming agent, and mixing to obtain a mixed powder material;
providing an organic solvent and deionized water, and stirring the mixed powder material, the organic solvent and water to obtain mixed slurry;
casting the mixed slurry to obtain a ceramic green body;
and discharging glue from the ceramic green body, and sintering to form the porous ceramic matrix with the zinc aluminate spinel structure.
2. The method for preparing a porous ceramic matrix according to claim 1, wherein the filler comprises high-purity quartz powder and the pore-forming agent comprises graphite powder, wherein the high-purity quartz powder is a plurality of spherical quartz particles with a diameter ranging from 50 μm to 150 μm, the graphite powder is a plurality of spherical graphite with a diameter ranging from 100 μm to 200 μm.
3. The method of preparing a porous ceramic matrix according to claim 2, wherein the organic solvent comprises a dispersant, a plasticizer, and a binder, and the dispersant comprises one of ammonium polyacrylate and polyethylene glycol octyl phenyl ether; the plasticizer comprises one of dibutyl phthalate and polyethylene glycol; the binder comprises one or more of water glass, sodium carboxymethyl cellulose, polyvinyl alcohol, and B-76 of the polyvinyl butyral series.
4. The method according to claim 3, wherein the step of mixing the zinc oxide, the aluminum hydroxide, the filler, and the pore-forming agent to obtain a mixed powder material, further comprises:
providing a sintering aid, wherein the sintering aid comprises one or more of magnesium oxide, potassium oxide, calcium oxide and sodium oxide;
and providing glass powder, and mixing to obtain the mixed powder material.
5. The method according to claim 4, wherein in the mixed slurry, the zinc oxide is 3 to 6% by mass, the aluminum hydroxide is 3 to 6% by mass, the filler is 20 to 25% by mass, the pore-forming agent is 30 to 40% by mass, the sintering aid is 3 to 5% by mass, the glass frit is 3 to 7% by mass, the dispersant is 0.5 to 2.5% by mass, the binder is 1 to 3% by mass, the plasticizer is 1 to 3% by mass, and the deionized water is 10 to 35% by mass.
6. The method for preparing a porous ceramic matrix according to claim 1, wherein in the step of mixing the zinc oxide, the aluminum hydroxide, the filler and the pore-forming agent to obtain a mixed powder, the mixing time is 2-4 hours;
stirring the mixed powder material, the organic solvent and water to obtain mixed slurry, wherein the mixing time is 15-30 min;
and in the process of casting and forming the mixed slurry to obtain the ceramic green body, the casting temperature is 80-90 ℃ and the casting time is 20-100 min.
7. The method for producing a porous ceramic substrate according to claim 1, wherein after the casting of the mixed slurry to obtain a ceramic green body, comprising:
and (3) superposing the multilayer ceramic green bodies and then pressurizing, wherein the pressurizing pressure is 10-35 Mpa, and the pressurizing time is 5-10 min.
8. The method according to claim 1, wherein the step of discharging and sintering the ceramic green body to form the porous ceramic body having a zinc aluminate spinel structure comprises:
placing the ceramic green body into an oxidizing atmosphere furnace for glue discharging, wherein the temperature in the oxidizing atmosphere furnace is increased to a first temperature at a first heating rate, the first heating rate is 0.5 ℃/min-1.5 ℃/min, and the first temperature range is 400 ℃ -500 ℃;
and increasing the temperature in the oxidizing atmosphere furnace to sinter the ceramic green body, wherein the temperature in the oxidizing atmosphere furnace is increased to a second temperature at a second heating rate, wherein the second heating rate is 5 ℃/min-8 ℃/min, and the first temperature is in the range of 1200 ℃ -1300 ℃.
9. An atomizing core, characterized in that the atomizing core comprises a heating member provided to a ceramic substrate manufactured by the method for manufacturing a porous ceramic substrate according to any one of claims 1 to 8.
10. An aerosol-forming device comprising a housing, a core assembly, and an atomizing core according to claim 9, wherein the core assembly and the atomizing core are disposed in the housing, and the core assembly is electrically connected to the atomizing core, and the core assembly is configured to provide energy to the atomizing core and control atomizing parameters, and the atomizing core is configured to heat and atomize an aerosol substrate in the housing.
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