CN116409984A - Porous ceramic and preparation method and application thereof - Google Patents
Porous ceramic and preparation method and application thereof Download PDFInfo
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- CN116409984A CN116409984A CN202111669997.6A CN202111669997A CN116409984A CN 116409984 A CN116409984 A CN 116409984A CN 202111669997 A CN202111669997 A CN 202111669997A CN 116409984 A CN116409984 A CN 116409984A
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- 239000000919 ceramic Substances 0.000 title claims abstract description 315
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011148 porous material Substances 0.000 claims abstract description 52
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 48
- 239000010431 corundum Substances 0.000 claims abstract description 48
- 239000000843 powder Substances 0.000 claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 238000005245 sintering Methods 0.000 claims abstract description 32
- 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 17
- 239000002245 particle Substances 0.000 claims abstract description 17
- 238000001746 injection moulding Methods 0.000 claims description 56
- 239000002002 slurry Substances 0.000 claims description 39
- 238000002156 mixing Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 24
- 239000011230 binding agent Substances 0.000 claims description 23
- 239000002270 dispersing agent Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- 239000002994 raw material Substances 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 239000000443 aerosol Substances 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 7
- 239000007924 injection Substances 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 6
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 claims description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 2
- 239000004014 plasticizer Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 66
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 229910052814 silicon oxide Inorganic materials 0.000 abstract description 4
- 238000000889 atomisation Methods 0.000 description 29
- 239000001993 wax Substances 0.000 description 26
- 239000012188 paraffin wax Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 10
- 230000001276 controlling effect Effects 0.000 description 8
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 7
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 7
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 7
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 7
- 239000005642 Oleic acid Substances 0.000 description 7
- 235000021355 Stearic acid Nutrition 0.000 description 7
- 238000000498 ball milling Methods 0.000 description 7
- 238000004140 cleaning Methods 0.000 description 7
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 7
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 7
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 7
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 7
- 239000008117 stearic acid Substances 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000001802 infusion Methods 0.000 description 6
- 239000000758 substrate Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 238000007569 slipcasting Methods 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000011449 brick Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000009172 bursting Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000004018 waxing Methods 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
- C04B35/10—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 aluminium oxide
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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
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- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/3418—Silicon oxide, silicic acids, or oxide forming salts thereof, e.g. silica sol, fused silica, silica fume, cristobalite, quartz or flint
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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
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Abstract
The invention provides porous ceramic and a preparation method and application thereof. The porous ceramic provided by the invention comprises the following components in percentage by mass: 30-50% of corundum, 5-20% of alumina, 15-35% of silicon oxide and 10-20% of sintering aid. The porous ceramic provided by the invention uses corundum particles as aggregate, and has excellent strength, pore diameter, porosity, liquid locking capacity and liquid guiding performance. On one hand, the porous ceramic provided by the invention has higher strength, and can prevent the porous ceramic from powder falling, thereby prolonging the service life and improving the use safety; on the other hand, the porous ceramic provided by the invention has excellent liquid locking and guiding capabilities on the premise of not using pore-forming agents, can realize rapid liquid guiding and liquid locking, and effectively avoids dry burning failure of the heating position of the ceramic atomizing core due to insufficient liquid supply.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to porous ceramic, and a preparation method and application thereof.
Background
Currently, in an atomizer of an aerosol generating device manufactured by using the joule heating principle, an atomization core generally adopts a structure of combining a porous ceramic with a heating wire or a heating circuit, and the structure heats an aerosol forming substrate stored in the porous ceramic by utilizing heat generated after the heating wire or the heating circuit is electrified, so that the purpose of atomizing the aerosol forming substrate is achieved. However, the atomization core adopting the porous ceramic-heating wire or heating circuit combination structure generally has the problems of contradiction and incompatibility between the pore size and the strength, the liquid locking and the liquid guiding capability of the porous ceramic. Thus, not only is the liquid and liquid guiding capacity of the porous ceramic insufficient, but also the liquid and liquid are difficult to realize, the aerosol forming substrate is heated unevenly and the heating position of the atomizing core is dry-burned to fail, the strength of the porous ceramic is low, the powder falling of the porous ceramic of the atomizing core is easy to occur during suction, the service life of the atomizing core is shortened, and the use safety of the atomizing core is reduced.
Disclosure of Invention
The embodiment of the invention aims to provide porous ceramic which can realize rapid liquid guide and liquid locking and has high strength, so as to solve the technical problems of low strength and non-ideal liquid locking and liquid guide of the existing porous ceramic.
In order to achieve the above purpose, the invention adopts the following technical scheme: providing a porous ceramic, which comprises the following components in percentage by mass:
optionally, the sintering aid comprises 50-70% of silicon dioxide, 10-20% of high-activity aluminum oxide and 20-30% of alkaline earth metal oxide by taking the total mass percentage of the sintering aid as 100%.
Optionally, the alkaline earth metal oxide comprises at least one of magnesium oxide, calcium oxide, and barium oxide.
Another object of the embodiment of the invention is to provide a preparation method of porous ceramics with high strength, which can realize rapid liquid guiding and liquid locking, so as to solve the technical problems of low strength and non-ideal liquid locking and liquid guiding of the existing porous ceramics.
In order to achieve the above purpose, the invention adopts the following technical scheme: the preparation method of the porous ceramic comprises the following steps:
weighing raw materials of each component according to the components contained in the porous ceramic, and performing premix treatment on each raw material to obtain a ceramic premix;
mixing the ceramic premix, the binder and the dispersing agent, stirring, defoaming and mixing to obtain ceramic injection molding slurry;
injection molding the ceramic injection molding slurry into a ceramic green body;
performing wax removal treatment on the ceramic green body;
and sintering the ceramic green body subjected to the wax removal treatment at a high temperature to obtain a porous ceramic finished product with required pores, pore diameters and strength.
Optionally, the ceramic premix uses corundum as aggregate, wherein the aggregate is formed by mixing any two of 200-mesh, 300-mesh and 400-mesh corundum according to a mass ratio of 1:1, or the aggregate is formed by mixing 200-mesh, 300-mesh and 400-mesh corundum according to a mass ratio of 1:2:2.
Optionally, the conditions for mixing the ceramic injection molding slurry are as follows: according to the mass percentage, 60-80% of the ceramic premix, 20-35% of the binder and 2-5% of the dispersing agent are stirred for 4-8 hours at the temperature of 100-150 ℃ at the stirring speed of 1000r/min, and the uniform ceramic injection molding slurry is formed by mixing.
Optionally, the injection molding conditions of the ceramic green body are: the temperature of the ceramic injection molding slurry is controlled at 75-95 ℃, the injection molding pressure is controlled at 0.4-0.6 MPa, and the pressure maintaining time is controlled at 2-3 s.
Optionally, the ceramic green body is wax removed in the following manner: and (3) laying graphite at the bottom of the tray, placing the ceramic green body on the surface of the graphite, covering a layer of graphite on the ceramic green body so as to embed the ceramic green body in the graphite, and preserving heat for 2-4 hours at the temperature of 180-250 ℃.
Optionally, the ceramic green body sintering curve after the wax removal is controlled at 250-1300 ℃, and the temperature rising process at 250-1300 ℃ comprises three temperature rising stages: the first heating stage is heated up to 250 ℃ rapidly at a heating rate of 5-10 ℃/min, the second heating stage is heated up to 500 ℃ slowly at a heating rate of 1.5-3 ℃/min, the temperature is kept for 30-60 min, and the third heating stage is heated up to 1180-1300 ℃ rapidly at a heating rate of 10 ℃/min, and the temperature is kept for 2-4 h.
Another object of the embodiment of the invention is to provide a ceramic atomization piece with high strength porous ceramic, which can realize rapid liquid guiding and liquid locking and is provided by any scheme, so as to solve the technical problems of low strength and non-ideal liquid locking and liquid guiding of the porous ceramic of the existing ceramic atomization piece.
In order to achieve the above purpose, the invention adopts the following technical scheme: there is provided a ceramic atomizer for an aerosol generating device, the ceramic atomizer comprising a porous ceramic provided in any one of the above aspects or a porous ceramic prepared by the porous ceramic preparation method provided in any one of the above aspects.
Compared with the prior art, the one or more technical schemes in the embodiment of the invention have at least one of the following beneficial effects:
the porous ceramic in the embodiment of the invention takes corundum powder as aggregate, alumina, silica and sintering aid are used for synthesizing a second phase together, and granular aggregate and the second phase are mixed and can be piled to form a pore structure. Thus, the porous ceramic provided by the embodiment of the invention has a pore structure with proper pore diameter and good porosity on the basis of higher strength, so that the porous ceramic has excellent performances in the aspects of strength, pores, pore diameter, liquid locking capacity and liquid guiding capacity. As the porous ceramic uses corundum particles as aggregate, the strength of the porous ceramic can be enhanced, the porous ceramic is prevented from falling powder to improve the service life and the use safety, the liquid locking capacity and the liquid guiding capacity of the porous ceramic can be improved, the quick liquid guiding and liquid locking can be realized, and the dry burning failure of the heating position of the ceramic atomizing core due to insufficient liquid supply can be effectively avoided.
The preparation method of the porous ceramic comprises the steps of preparing raw materials of components contained in the porous ceramic into a ceramic premix, adding a binder and a dispersing agent, stirring, defoaming, mixing to obtain ceramic injection slurry, and performing injection molding to obtain a ceramic green body by an injection molding process, wherein the ceramic green body is subjected to wax removal and sintering to obtain a porous ceramic finished product with required pore diameters, pore diameters and strength. According to the preparation method of the porous ceramic, disclosed by the embodiment of the invention, corundum powder is used as aggregate, the second phase consisting of alumina, silica and a sintering aid is only required to be uniformly dispersed in the aggregate, and the granular aggregate can be mixed and piled to form a pore structure, so that the porous ceramic has a pore structure with proper pore diameter and good porosity on the basis of higher strength without using a pore-forming agent, and therefore, the porous ceramic has excellent performances in the aspects of strength, pore diameter, liquid locking capacity and liquid guiding capacity.
The ceramic atomization piece in the embodiment of the invention contains the porous ceramic or the porous ceramic prepared by the preparation method of the porous ceramic, so that the ceramic atomization piece has excellent properties in the aspects of compressive strength, pores, pore diameter, liquid locking capacity and liquid guiding capacity, the ceramic atomization piece can be prevented from falling powder, the service life of a ceramic atomization core and the use safety can be improved, the liquid locking capacity and the liquid guiding capacity of the ceramic atomization piece can be improved, and the dry burning failure of a heating position of the ceramic atomization piece due to insufficient liquid supply can be effectively avoided.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM photograph of a porous ceramic prepared by the method for preparing a porous ceramic of example 1 of the present invention;
FIG. 2 is an SEM photograph of a porous ceramic prepared by the method of preparing a porous ceramic according to example 2 of the present invention;
FIG. 3 is an SEM photograph of a porous ceramic prepared by the method of preparing a porous ceramic according to example 3 of the present invention;
FIG. 4 is an SEM photograph of a porous ceramic prepared by the method of preparing a porous ceramic according to example 4 of the present invention;
fig. 5 is an SEM photograph of the porous ceramic prepared by the preparation method of the porous ceramic of example 5 of the present invention.
Detailed Description
The objects, technical solutions and advantages of the present invention will become more apparent, and the present invention will be further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides porous ceramic which has high strength and can realize rapid liquid guiding and liquid locking. The porous ceramic provided by the embodiment of the invention comprises the following components in percentage by mass:
specifically, the purity of the raw materials selected in the embodiment of the invention is more than 99.9 percent. In this way, the porous ceramic provided by the embodiment of the invention uses corundum particles as aggregate, and uses alumina, silica and sintering aid to synthesize a second phase (mullite phase). The corundum particles are used as the aggregate, so that the second phase can be uniformly dispersed in the aggregate, and the granular aggregate is mixed and piled to form a pore structure, and a pore forming agent is not needed, so that the porous ceramic provided by the embodiment of the invention has a pore structure with the pore diameter of 20-80 mu m and the porosity of 45-60% on the basis of higher strength, and therefore, the porous ceramic is very excellent in pores, pore diameter, liquid locking capacity and liquid guiding capacity, the liquid locking capacity and liquid guiding capacity of the porous ceramic are improved, rapid liquid guiding and liquid locking can be realized, and the failure caused by uneven heating of an aerosol forming matrix and dry burning of a heating position of an atomization core is effectively avoided. In addition, as corundum particles are used as aggregate, the porous ceramic has higher strength, so that the powder falling of the porous ceramic with an atomization core during suction is prevented, and the service life and the use safety of the atomization core are improved.
In some embodiments, the corundum may be white corundum or brown corundum, and the specific type of the corundum may be reasonably selected and set according to practical use needs, which is not limited only herein. Wherein, the particle size of the corundum is 200-400 meshes. In some embodiments, the aggregate is a particle-matched aggregate formed by mixing any two of 200 mesh, 300 mesh and 400 mesh corundum according to a mass ratio of 1:1. In other embodiments, the aggregate is a granule-matched aggregate formed by mixing 200 mesh, 300 mesh, 400 mesh corundum in a mass ratio of 1:2:2. The adjustment and improvement of the strength, the porosity and the pore diameter of the porous ceramic provided by the embodiment of the invention are realized by adjusting and controlling the particle size of the aggregate component of the porous ceramic provided by the embodiment of the invention and combining the adjustment and control of the forming and sintering process (such as sintering temperature).
In some of these embodiments, the burn-aid comprises, based on 100% total mass of the burn-aid, 50% to 70% silica, 10% to 20% highly active alumina, and 20% to 30% alkaline earth metal oxide. Because the sintering temperature of the porous ceramic is higher and the strength of the porous ceramic is relatively poorer, the sintering temperature of the porous ceramic can be reduced by adding the sintering aid, and the sintering aid can form glass under the high-temperature condition, so that the strength of the porous ceramic can be improved, and the porous ceramic has higher strength. In some embodiments, the alkaline earth metal comprises any one or a mixture of two or more of magnesium oxide, calcium oxide, and barium oxide.
The embodiment of the invention also provides a preparation method of the porous ceramic.
In some embodiments, the preparation method of the porous ceramic provided by the embodiment of the invention comprises the following steps:
step S01: weighing raw materials of each component according to the components contained in the porous ceramic, and performing premix treatment on each raw material to obtain a ceramic premix;
step S02: mixing a ceramic premix, a binder and a dispersing agent, stirring, defoaming, and mixing to obtain ceramic injection molding slurry;
step S03: injection molding the ceramic injection molding slurry into a ceramic green body;
step S04: carrying out wax removal treatment on the ceramic green body;
step S05: and sintering the ceramic green body subjected to the wax removal treatment at high temperature to obtain a porous ceramic finished product with required pores, pore diameters and strength.
Specifically, in the step S01, the porous component in the embodiment of the present invention is as above, and the porous component contains the following components in percentage by mass:
in the step S01, the raw materials of each component are weighed and subjected to a premix treatment, wherein the premix treatment can be performed according to a conventional mixing manner of mixing ceramic raw materials in the ceramic field. In some embodiments, the mixing process may be, but is not limited to, ball milling by a roller ball mill. In some specific embodiments, the ceramic premix takes corundum (the corundum can be white corundum and/or brown corundum) as aggregate, the aggregate is aggregate with matched particles formed by mixing any two of 200-mesh, 300-mesh and 400-mesh corundum according to the mass ratio of 1:1, or the aggregate is aggregate with matched particles formed by mixing 200-mesh, 300-mesh and 400-mesh corundum according to the mass ratio of 1:2:2. The adjustment and improvement of the strength, the porosity and the pore diameter of the porous ceramic provided by the embodiment of the invention are realized by adjusting and controlling the particle size of the aggregate component of the porous ceramic provided by the embodiment of the invention and combining the adjustment and control of the forming and sintering process (such as sintering temperature).
In the step S02, the method of mixing the ceramic premix, the binder and the dispersant in the step S01 may be a conventional mixing method in the process of preparing the ceramic slurry. In some embodiments, the step of formulating the ceramic slurry is: according to the mass percentage, 60-80% of ceramic premix, 20-35% of binder and 2-5% of dispersing agent are stirred for 4-8 hours at the stirring speed of 1000r/min in a stirring and defoaming machine at the temperature of 100-150 ℃ to carry out stirring and defoaming treatment, and finally, the ceramic injection molding slurry with uniform and consistent mixing and proper viscosity is formed, so that the injection molding of the ceramic injection molding slurry in the later stage is facilitated. The addition of the binder and the dispersing agent is beneficial to the injection molding of the ceramic injection molding slurry in the later stage, ensures that the molded blank has certain strength and plasticity, and is convenient for the operation and treatment of the subsequent procedures. In some embodiments, the binder comprises one or both of paraffin No. 52 and paraffin No. 62, and the dispersant is one or both of stearic acid and oleic acid. By adopting the paraffin of two types, the purpose is that the paraffin can be volatilized and discharged step by step in order to realize the later paraffin removal process, but not the explosive volatilization and discharge, thereby being beneficial to reducing the defects of the porous ceramic and further improving the yield of the porous ceramic.
In the step S03, the ceramic injection slurry is injection molded into a ceramic green body, and the ceramic injection slurry may be injection molded into a ceramic green body of a designed size by a mold by an injection molding machine. In some embodiments, the injection molding conditions of the ceramic green body are: the temperature of the ceramic injection molding slurry is controlled at 75-95 ℃, the injection molding pressure is controlled at 0.4-0.6 MPa, the dwell time is controlled at 2-3 s, and the ceramic injection molding slurry can be better injection molded into ceramic green bodies, thereby being beneficial to reducing the defects of porous ceramics.
In the step S04, the ceramic green body is subjected to a wax removal treatment, which may be a conventional wax removal treatment method for removing wax from the ceramic green body. In some embodiments, the binder contains No. 52 paraffin and No. 62 paraffin, so that paraffin can be volatilized and discharged gradually in the paraffin discharging process, instead of being volatilized and discharged in a bursting manner, which is beneficial to reducing defects of the porous ceramic and further improving the yield of the porous ceramic. In some embodiments, the ceramic green body is de-waxed by: spreading graphite to cover the bottom of the tray, placing ceramic green bricks on the surface of the graphite, covering a layer of graphite on the ceramic green bricks to embed the ceramic green bricks in the graphite, and preserving heat for 2-4 h at 180-250 ℃. The method for removing the wax of the porous ceramic further improves the strength of the ceramic blank after the wax removal by combining the condition control of the wax removal mode of the porous ceramic and the regulation and control of the sintering process, and is beneficial to later powder cleaning and placement (the operation is not fragile).
In the step S05, the ceramic green body after the wax removal is sintered at high temperature, and a porous ceramic finished product with required pore, pore diameter and strength can be obtained. In some of these embodiments, the ceramic green body sintering temperature profile after de-waxing is controlled between 250 and 1300 ℃. In some embodiments, the temperature rising process between 250 and 1300 ℃ further comprises three temperature rising stages: the first heating stage is heated up to 250 ℃ rapidly at a heating rate of 5-10 ℃/min, the second heating stage is heated up to 500 ℃ slowly at a heating rate of 1.5-3 ℃/min, the temperature is kept for 30-60 min, and the third heating stage is heated up to 1180-1300 ℃ rapidly at a heating rate of 10 ℃/min, and the temperature is kept for 2-4 h. The sintering temperature of the porous ceramic provided by the embodiment of the invention is regulated and controlled, so that the strength, the porosity and the pore diameter of the porous ceramic provided by the embodiment of the invention are further improved, the porous ceramic is not easy to crack and deform, and the porous ceramic has good porosity and proper pore diameter.
Therefore, according to the preparation method of the porous ceramic, corundum particles are used as aggregate, and alumina, silica and a sintering aid are used for jointly synthesizing a second phase (mullite phase). The corundum particles are used as the aggregate, so that the second phase can be uniformly dispersed in the aggregate, and the granular aggregate is mixed and piled to form a pore structure, and a pore forming agent is not required to be used, so that the porous ceramic provided by the embodiment of the invention has a pore structure with the pore diameter of 20-60 mu m and the porosity of 45-60% on the basis of higher strength, and therefore, the porous ceramic is very excellent in pores, pore diameter, liquid locking capacity and liquid guiding capacity, the liquid locking capacity and liquid guiding capacity of the porous ceramic are improved, rapid liquid guiding and liquid locking can be realized, and the defects that aerosol forms a matrix and the heating position of an atomization core is dry-burned and loses efficacy are effectively avoided. In addition, the preparation method of the porous ceramic takes corundum particles as aggregate, so that the porous ceramic has higher strength, the powder falling of the porous ceramic with an atomization core during suction can be prevented, and the service life and the use safety of the atomization core are improved.
On the basis of the porous ceramic and the preparation method thereof, the embodiment of the invention also provides a ceramic atomization piece. In some of these embodiments, the ceramic atomizer comprises the porous ceramic provided by the embodiments of the invention described above or comprises a porous ceramic prepared by the porous ceramic preparation methods provided by the embodiments of the invention described above. Therefore, the porous ceramic has a pore structure with a pore diameter of 20-60 mu m and a porosity of 45-60% on the basis of higher strength, so that the ceramic atomization piece is very excellent in pores, pore diameter, liquid locking capacity and liquid guiding capacity, the liquid locking capacity and liquid guiding capacity of the ceramic atomization piece are improved, quick liquid guiding and liquid locking can be realized, and the defects that an aerosol forming substrate is heated unevenly and the heating position of the ceramic atomization piece is burnt dry to fail are effectively avoided. And because corundum particles are used as aggregate, the ceramic atomization piece has higher strength, powder falling of the ceramic atomization piece is prevented when the ceramic atomization piece is sucked, and the service life and the use safety of the ceramic atomization piece are improved.
In order that the details and operation of the above-described embodiments of the present invention may be clearly understood by those skilled in the art, and that the advanced properties of the porous ceramics of the present invention and the method of preparing the same may be significantly embodied, the embodiments of the present invention are illustrated by the following examples.
Example 1
This example 1 provides a porous ceramic and a method for preparing the same. The porous ceramic comprises the following components in percentage by mass:
respectively weighing 300g of 200-mesh corundum powder, 300g of 300-mesh corundum powder, 60g of alumina, 420g of silica, 60g of silica, 20g of high-activity alumina, 40g of magnesia, 400g of binder (No. 52 paraffin and/or No. 62 paraffin) and 36g of dispersing agent (stearic acid and/or oleic acid).
The preparation method of the porous ceramic comprises the following steps:
(1): according to the porous ceramic in the embodiment 1, the components contained in the porous ceramic are respectively weighed according to the proportion, the corresponding raw materials are mixed, and the ceramic premix powder is obtained after the roller ball milling treatment for 4 hours;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, stirring and defoaming are carried out for 4 hours, and the ceramic injection molding slurry is prepared by mixing;
(3): pouring the stirred ceramic injection molding slurry into an injection molding machine, maintaining the temperature of the ceramic injection molding slurry at 75 ℃, starting slip casting, controlling the molding pressure at 0.4Mpa, maintaining the pressure for 2s, and performing injection molding to form a ceramic green body;
(4): after injection molding to form a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 200 ℃ for 200 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1210 ℃ for 120 minutes, and preparing the porous ceramic.
The porous ceramic prepared in this example 1 was tested (as shown in FIG. 1), and had a porosity of 58%, a median pore diameter of 80. Mu.m, an infusion rate (liquid-conducting rate) of 22s, and a compressive strength of 18N/mm 2 。
Example 2
This example 2 provides a porous ceramic and a method for preparing the same. The porous ceramic comprises the following components in percentage by mass:
160g of 200-mesh corundum powder, 320g of 300-mesh corundum powder, 320g of 400-mesh corundum powder, 308g of alumina, 700g of silica, 237g of silica, 59g of high-activity alumina, 100g of magnesia, 616g of binder (No. 52 paraffin and/or No. 62 paraffin) and 88g of dispersing agent (stearic acid and/or oleic acid) are respectively weighed.
The preparation method of the porous ceramic comprises the following steps:
(1): according to the porous ceramic of the embodiment 2, the components contained in the porous ceramic are respectively weighed according to the proportion, the corresponding raw materials are mixed, and the ceramic premix powder is obtained after the roller ball milling treatment for 4 hours;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, stirring and defoaming are carried out for 4 hours, and the ceramic injection molding slurry is prepared by mixing;
(3): pouring the stirred ceramic injection molding slurry into an injection molding machine, keeping the temperature of the ceramic injection molding slurry at 80 ℃, starting slip casting, controlling the molding pressure at 0.5Mpa, keeping the pressure for 2.5s, and performing injection molding to form a ceramic green body;
(4): after injection molding to form a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 220 ℃ for 200 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1250 ℃ for 120 minutes, and preparing the porous ceramic.
The porous ceramic prepared in this example 2 was tested (as shown in FIG. 2), and had a porosity of 55%, a median pore diameter of 51. Mu.m, an infusion rate (liquid-conducting rate) of 27s, and a compressive strength of 23N/mm 2 。
Example 3
This example 3 provides a porous ceramic and a method for preparing the same. The porous ceramic comprises the following components in percentage by mass:
respectively weighing 120g of 200-mesh corundum powder, 240g of 300-mesh corundum powder, 240g of 400-mesh corundum powder, 400g of alumina, 600g of silicon oxide, 280g of silicon dioxide, 40g of high-activity alumina, 80g of magnesium oxide, 600g of binder (No. 52 paraffin and/or No. 62 paraffin) and 70g of dispersing agent (stearic acid and/or oleic acid).
The preparation method of the porous ceramic comprises the following steps:
(1): according to the porous ceramic of the embodiment 3, the components contained in the porous ceramic are respectively weighed according to the proportion, the corresponding raw materials are mixed, and the ceramic premix powder is obtained after the roller ball milling treatment for 4 hours;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, stirring and defoaming are carried out for 4 hours, and the ceramic injection molding slurry is prepared by mixing;
(3): pouring the stirred ceramic injection molding slurry into an injection molding machine, keeping the temperature of the ceramic injection molding slurry at 80 ℃, starting slip casting, controlling the molding pressure at 0.6Mpa, keeping the pressure for 2.5s, and performing injection molding to form a ceramic green body;
(4): after injection molding to form a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 220 ℃ for 200 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1180 ℃ for 120 minutes to prepare the porous ceramic.
The porous ceramic prepared in this example 3 was tested (as shown in FIG. 3), and had a porosity of 46%, a median pore diameter of 70. Mu.m, an infusion rate (liquid-conducting rate) of 29s, and a compressive strength of 20N/mm 2 。
Example 4
This example 4 provides a porous ceramic and a method for preparing the same. The porous ceramic comprises the following components in percentage by mass:
100g of 200-mesh corundum powder, 200g of 300-mesh corundum powder, 200g of 400-mesh corundum powder, 150g of alumina, 350g of silicon oxide, 150g of silicon dioxide, 50g of high-activity alumina, 50g of magnesium oxide, 350g of binder (No. 52 paraffin and/or No. 62 paraffin) and 50g of dispersing agent (stearic acid and/or oleic acid) are respectively weighed.
The preparation method of the porous ceramic comprises the following steps:
(1): the components contained in the porous ceramic according to the comparative example are respectively weighed according to the proportion, the corresponding raw materials are mixed, and the ceramic premix powder is obtained after the roller ball milling treatment for 4 hours;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, and the stirring and the defoaming are carried out for 4 hours, and the ceramic slurry is prepared by mixing;
(3): pouring the stirred ceramic slurry into a dry pressing mold, controlling the dry pressing forming pressure to be 0.5Mpa and the dwell time to be 2.5s, and forming a ceramic green body;
(4): after forming a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 220 ℃ for 200 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1220 ℃, and preserving heat for 120 minutes to prepare the porous ceramic.
The porous ceramic prepared in this example 4 was tested (as shown in FIG. 4), and had a porosity of 52%, a median pore diameter of 32. Mu.m, an infusion rate (liquid-conducting rate) of 36s, and a compressive strength of 30N/mm 2 。
Example 5
This example 5 provides a porous ceramic and a method for preparing the same. The porous ceramic comprises the following components in percentage by mass:
respectively weighing 295g of 300-mesh corundum powder, 295g of 400-mesh corundum powder, 200g of alumina, 180g of silicon oxide, 100g of silicon dioxide, 40g of high-activity alumina, 60g of magnesium oxide, 420g of binder (No. 52 paraffin and/or No. 62 paraffin) and 60g of dispersing agent (stearic acid and/or oleic acid).
The preparation method of the porous ceramic comprises the following steps:
(1): according to the embodiment, the components contained in the porous ceramic are respectively weighed according to the proportion, the corresponding raw materials are mixed, and the ceramic premix powder is obtained after the roller ball milling treatment for 4 hours;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, and the stirring and the defoaming are carried out for 4 hours, and the ceramic slurry is prepared by mixing;
(3): pouring the stirred ceramic injection molding slurry into an injection molding machine, keeping the temperature of the ceramic injection molding slurry at 80 ℃, starting slip casting, controlling the molding pressure at 0.5Mpa, keeping the pressure for 3s, and performing injection molding to form a ceramic green body;
(4): after forming a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 210 ℃ for 180 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1230 ℃ for 120 minutes to prepare the porous ceramic.
The porous ceramic prepared in this example 5 was tested (as shown in FIG. 5), and had a porosity of 46%, a median pore diameter of 38. Mu.m, an infusion rate (liquid-conducting rate) of 24s, and a compressive strength of 27N/mm 2 。
Comparative example
The comparative example provides a porous ceramic and a preparation method thereof. The porous ceramic comprises the following components in percentage by mass:
374g of diatomite, 510g of glass powder, 320g of organic pore-forming agent with D50 of 50 μm, 458g of binder (No. 52 paraffin and/or No. 62 paraffin) and 50g of dispersing agent (stearic acid and/or oleic acid) are respectively weighed. Poured into a ball mill pot, and 1450g of zirconia balls with a diameter of 10mm were added and ball-milled and mixed for an hour.
The preparation method of the porous ceramic comprises the following steps:
(1): the porous ceramic of the comparative example comprises the following components, respectively weighing corresponding raw materials according to the proportion, mixing diatomite, glass powder and pore-forming agent, and performing roller ball milling treatment for 4 hours to obtain ceramic premix powder;
(2): after the binder and the dispersing agent are put into a stirring and defoaming machine to be melted for 1 hour, the premixed ceramic premix powder is added, and the stirring and the defoaming are carried out for 4 hours, and the ceramic slurry is prepared by mixing;
(3): pouring the stirred ceramic injection molding slurry into an injection molding machine, keeping the temperature of the ceramic injection molding slurry at 80 ℃, starting slip casting, controlling the molding pressure at 0.5Mpa, keeping the pressure for 2.5s, and performing injection molding to form a ceramic green body;
(4): after forming a ceramic green body, placing the ceramic green body in the middle of graphite powder, and preserving heat and removing wax at 220 ℃ for 200 minutes;
(5): after cleaning graphite powder on the surface of the green body, sintering the ceramic green body after wax removal at a high temperature of 1080 ℃ for 120 minutes, and preparing the porous ceramic.
The porous ceramics prepared in this comparative example were tested, with a porosity of 56%, a median pore diameter of 44 μm, an infusion rate (liquid-conducting rate) of 44s, and a compressive strength of 15N/mm 2 。
Porous ceramic related performance test:
the porous ceramics in examples 1 to 5 and comparative examples described above were respectively subjected to the tests of porosity, pore diameter, liquid-conducting rate and compressive strength, and the test results are shown in table 1 below.
Table 1 porous ceramic-related Performance test tables in examples 1 to 5 and comparative example
| Test item | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example |
| Porosity (%) | 58 | 55 | 46 | 52 | 46 | 56 |
| Median pore diameter (μm) | 80 | 51 | 70 | 32 | 38 | 44 |
| Liquid transfer rate(s) | 22 | 27 | 29 | 36 | 24 | 44 |
| Compressive Strength (N/mm) 2 ) | 18 | 23 | 20 | 30 | 27 | 15 |
In summary, the porous ceramics of examples 1 to 5 of the present invention maintain excellent properties, particularly compressive strength, in terms of both liquid-locking ability and liquid-guiding ability without significant decrease in porosity and pore size, as compared with the porous ceramics of comparative examples. Therefore, the porous ceramics in the embodiments 1 to 5 of the invention can not only prevent the ceramic atomization piece from powder falling and improve the service life and the use safety of the ceramic atomization core, but also improve the liquid locking capability and the liquid guiding capability of the ceramic atomization piece, and effectively avoid the dry burning failure of the heating position of the ceramic atomization piece due to insufficient liquid supply. It should be noted that, compared with the porous ceramics in the comparative examples, the porous ceramics in examples 1 to 5 of the present invention have a small liquid guiding rate, which is more advantageous for the porous ceramics to enhance the liquid locking capability to avoid liquid leakage, and for the porous ceramics to sufficiently atomize the aerosol-forming substrate, so as to avoid insufficient atomization due to too fast supply of the aerosol-forming substrate, causing small particles of doped liquid in the smoke, and affecting the smoke sucking taste.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (10)
1. The porous ceramic is characterized by comprising the following components in percentage by mass:
2. the porous ceramic according to claim 1, wherein the sintering aid comprises 50 to 70% of silica, 10 to 20% of highly active alumina and 20 to 30% of alkaline earth metal oxide, based on 100% of the total mass of the sintering aid.
3. The porous ceramic of claim 2, wherein the alkaline earth metal oxide comprises at least one of magnesium oxide, calcium oxide, and barium oxide.
4. The preparation method of the porous ceramic is characterized by comprising the following steps:
the porous ceramic according to any one of claims 1 to 3, wherein each component is prepared by weighing each component raw material, and performing premix treatment on each raw material to obtain a ceramic premix;
mixing the ceramic premix, the binder and the plasticizer, and mixing the mixture into ceramic injection molding slurry after stirring and defoaming treatment;
injection molding the ceramic injection molding slurry into a ceramic green body;
performing wax removal treatment on the ceramic green body;
and sintering the ceramic green body subjected to the wax removal treatment at a high temperature to obtain a porous ceramic finished product with required pores, pore diameters and strength.
5. The method for preparing porous ceramic according to claim 4, wherein the ceramic premix uses corundum powder as aggregate, the aggregate is aggregate with particle matching formed by mixing any two of 200 mesh corundum, 300 mesh corundum and 400 mesh corundum according to a mass ratio of 1:1, or the aggregate is aggregate with particle matching formed by mixing 200 mesh corundum, 300 mesh corundum and 400 mesh corundum according to a mass ratio of 1:2:2.
6. The method of claim 4, wherein the mixing into the ceramic injection slurry is performed under the following conditions: according to the mass percentage, 60-80% of the ceramic premix, 20-35% of the binder and 2-5% of the dispersing agent are stirred for 4-8 hours at the temperature of 100-150 ℃ at the stirring speed of 1000r/min, and the uniform ceramic injection molding slurry is formed by mixing.
7. The method of producing a porous ceramic according to claim 4, wherein the injection molding conditions of the ceramic green body are: the temperature of the ceramic injection molding slurry is controlled at 75-95 ℃, the injection molding pressure is controlled at 0.4-0.6 MPa, and the pressure maintaining time is controlled at 2-3 s.
8. The method for preparing a porous ceramic according to claim 4, wherein the ceramic green body is dewaxed in the following manner: and (3) laying graphite at the bottom of the tray, placing the ceramic green body on the surface of the graphite, covering a layer of graphite on the ceramic green body so as to embed the ceramic green body in the graphite, and preserving heat for 2-4 hours at the temperature of 180-250 ℃.
9. The method for producing a porous ceramic according to claim 4, wherein the ceramic green body sintering temperature after the dewaxing treatment is controlled to 250 to 1300 ℃, and the temperature rising process of 250 to 1300 ℃ includes three temperature rising stages: the first heating stage is heated up to 250 ℃ at a heating rate of 5-10 ℃/min, the second heating stage is heated up to 500 ℃ at a heating rate of 1.5-3 ℃/min and is kept at the temperature for 30-60 min, and the third heating stage is heated up to 1180-1300 ℃ at a heating rate of 10 ℃/min and is kept at the temperature for 2-4 h.
10. A ceramic atomizer for an aerosol generating device, characterized in that it comprises the porous ceramic according to any one of claims 1 to 3 or the porous ceramic produced by the porous ceramic production method according to any one of claims 4 to 9.
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