CN112321286A - Multilayer porous ceramic material and preparation method thereof - Google Patents

Multilayer porous ceramic material and preparation method thereof Download PDF

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Publication number
CN112321286A
CN112321286A CN202011215480.5A CN202011215480A CN112321286A CN 112321286 A CN112321286 A CN 112321286A CN 202011215480 A CN202011215480 A CN 202011215480A CN 112321286 A CN112321286 A CN 112321286A
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porous ceramic
ceramic
ceramic material
pore
porous
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刘翔
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Shenzhen Tianshili Shentong materia medica Technology Development Co.,Ltd.
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Shenzhen Buddy Technology Development Co Ltd
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Abstract

The invention provides a multilayer porous ceramic material and a preparation method thereof, and particularly relates to the field of atomizers. The material is composed of a plurality of layers of porous ceramics with different porosities and different thermal conductivities, and an integrated composite material is formed among the layers through an inorganic connecting layer formed by sintering. The ceramic material is formed by mutually overlapping a plurality of layers of porous ceramics, and an inorganic connecting layer is formed in the sintering process, so that the prepared multilayer ceramics form a whole, and the porous ceramic material is prevented from cracking and deforming. The composite material is ensured to form a unified whole, and the service performance of the material is improved.

Description

Multilayer porous ceramic material and preparation method thereof
Technical Field
The invention relates to the field of atomizers, in particular to a multilayer porous ceramic material and a preparation method thereof.
Background
The porous ceramic material has the advantages of high temperature resistance, high pressure resistance, acid and alkali corrosion resistance and the like, is widely applied to the fields of environmental protection, biological medicine, food and medicine, new energy and the like at present, and has great research and use values.
In the field of atomization equipment, an atomization core is a core component, and the atomization core mainly comprises two types of traditional cellucotton atomization cores and emerging ceramic atomization cores. Compared with the traditional atomization of cellucotton, the atomization effect of the porous ceramic atomization core is better and finer, the original taste of the atomized liquid is highly reduced, the reduction degree is high, and the continuity is better. Meanwhile, the consumption of electric quantity can be saved, and the battery service time of the equipment can be prolonged. However, the commercially available porous ceramic atomizing cores used at present have the following disadvantages: (1) the pore diameter of the atomizing core is single, and the atomizing core is not uniformly distributed, so that the tobacco tar is not uniformly distributed, and the atomizing amount effect is not good. (2) The oil locking and guiding capacity of the atomizing core is weak, atomized liquid is not smoothly supplied in the atomizing process, and the adsorption self-locking capacity is poor. (3) The porous ceramic has low thermal conductivity, the temperature of the heating wire in the atomizing core shows the distribution trend of high temperature near the heating wire and low edge temperature, and the porous ceramic has inconsistent heat transmission, so that the temperature field distribution is not uniform, and the physicochemical effect of the atomized liquid is influenced.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a multilayer porous ceramic material and a preparation method thereof, and solves at least one technical problem in the background art.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
in one aspect, a multi-layered porous ceramic material is provided, the material being composed of a plurality of layers of porous ceramics of different porosities and different thermal conductivities, with an inorganic connection layer formed by sintering between the layers forming an integrated composite material.
Preferably, the porosity is controlled based on the composition and composition of the ceramic material.
Preferably, the pore size D of the multilayer porous ceramic material502-15 μm, and the porosity of the porous layer is 50-70%.
Preferably, the porous ceramic comprises at least one of alumina, zirconia, silica, yttria, silicon carbide, boron nitride, aluminum nitride and silicon nitride, and the ceramic powder has a particle size D50Is 1-30 μm.
Preferably, micro-nano high-thermal-conductivity materials are added into each layer of porous ceramic material, the micro-nano high-thermal-conductivity materials comprise alloy powder with the surface subjected to anti-oxidation treatment, the addition amount of the alloy powder is 1% -10% of the mass of the ceramic powder, and the particle size D of the alloy powder is500.1 to 10 μm.
Preferably, the porous ceramic further comprises an additive, and the additive comprises at least one of alumina, silica, sodium carbonate, calcium carbonate, magnesium oxide and magnesium carbonate; the addition amount of the additive is 1-10% of the mass of the ceramic slurry, and the particle size D of the additive50Is 1-10 μm.
Preferably, the connection between the layers of the porous ceramic material is an inorganic material generated at the interface by porous ceramic sintering, the inorganic material includes aluminum phosphate, aluminum silicate and/or silicate, and the thickness of the inorganic material is 0.1 μm to 5 μm.
Preferably, the ceramic powder material also comprises a pore-forming agent, wherein the pore-forming agent comprises at least one of hollow glass, hollow silicon oxide, hollow aluminum oxide, hollow zirconium oxide, ammonium carbonate, ammonium bicarbonate and ammonium dihydrogen phosphate, and the addition amount of the pore-forming agent is 5 percent of the mass of the ceramic powder materialAbout 20% of the pore-forming agent, the particle diameter D of the pore-forming agent502-20 μm.
In another aspect, there is also provided a method for preparing a multilayer porous ceramic material, the method comprising:
ceramic powder, an additive, a cosolvent, a pore-forming agent and a nano high-heat-conductivity material are prepared into a ceramic blank body through ball milling, granulation and cold pressing forming processes;
pressing ceramic powder, an additive, a pore-forming agent and a nano high-thermal-conductivity material into ceramic slurry;
the ceramic slurry and the ceramic blank are sequentially and alternately distributed to obtain a pre-composite material;
and sintering the pre-composite material to prepare the multilayer porous ceramic composite material.
Preferably, the ceramic slurry is uniformly coated on the ceramic body by any one of a spray coating method, a spin coating method, a czochralski method, a screen printing method, a coating method, a 3d printing method, a casting method, and a casting method.
(III) advantageous effects
The invention provides a multilayer porous ceramic material and a preparation method thereof. Compared with the prior art, the method has the following beneficial effects:
(1) the invention provides a method for preparing a porous ceramic material, which is characterized in that a ceramic material comprises a plurality of layers of porous ceramics which are mutually overlapped to form an inorganic connecting layer in the sintering process, so that the prepared multilayer ceramics form a whole, and the porous ceramic material is prevented from cracking and deforming. The composite material is ensured to form a unified whole, and the service performance of the material is improved.
(2) According to the invention, the porous ceramic layer is formed on the surface of the ceramic material by using the additive preparation method, so that the composite porous ceramic composite material with controllable ceramic micropore size and porosity can be formed, and the service performance of the porous ceramic material is optimized. The size and the distribution of the micropores are controlled, so that the oil locking and oil guiding capacity of the porous ceramics is improved, and then a certain amount of high-heat-conduction materials which are uniformly distributed are added into the porous ceramics of each layer, so that the heat conductivity of the porous ceramics is improved, and the temperature distribution in the ceramic materials is regulated and controlled. The metal micro-nano powder is used as a heat transmission medium, so that the serious problem of uneven distribution of a thermal field of the porous ceramic material in the aspect of atomization heating is solved, each micro-nano powder can be used as a heating body after absorbing heat, the loss of ambient temperature can be greatly reduced, and the temperature field of the whole porous ceramic body is more uniform.
Drawings
FIG. 1 is a structural diagram of a multilayer composite porous ceramic material.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In one aspect, a multi-layered porous ceramic material is provided, the material being composed of a plurality of layers of porous ceramics of different porosities and different thermal conductivities, with an inorganic connection layer formed by sintering between the layers forming an integrated composite material.
In the above embodiment, as shown in fig. 1 below, the ceramic material is formed by stacking a plurality of porous ceramics, and the inorganic connection layer is formed in the sintering process, so that the prepared multilayer ceramics form a whole, thereby preventing the porous ceramic material from cracking and deforming. The composite material is ensured to form a unified whole, and the service performance of the material is improved.
Preferably, the pore size D of the multilayer porous ceramic material502-15 μm, and the porosity of the porous layer is 50-70%.
In the embodiment, the porous ceramic layer is formed on the surface of the ceramic material by using the additive preparation method, so that the composite porous ceramic composite material with controllable ceramic micropore size and porosity can be formed, and the service performance of the porous ceramic material is optimized.
Preferably, the porous ceramic includes at least one of alumina, zirconia, silica, yttria, silicon carbide, boron nitride, aluminum nitride, and silicon nitride, and the ceramicParticle diameter D of powder50Is 1-30 μm.
Preferably, micro-nano high-thermal-conductivity materials are added into each layer of porous ceramic material, the micro-nano high-thermal-conductivity materials comprise alloy powder with the surface subjected to anti-oxidation treatment, the addition amount of the alloy powder is 1% -10% of the mass of the ceramic powder, and the particle size D of the alloy powder is500.1 to 10 μm.
In the embodiment, the metal micro-nano powder is used as a heat propagation medium, so that the serious problem of uneven distribution of a thermal field of the porous ceramic material in the aspect of atomization heating is solved, each micro-nano powder can be used as a heating body after absorbing heat, the loss of ambient temperature can be greatly reduced, and the temperature field of the whole porous ceramic body is more uniform.
Preferably, the porous ceramic further comprises an additive, and the additive comprises at least one of alumina, silica, sodium carbonate, calcium carbonate, magnesium oxide and magnesium carbonate; the addition amount of the additive is 1-10% of the mass of the ceramic slurry, and the particle size D of the additive50Is 1-10 μm.
Preferably, the connection between the layers of the porous ceramic material is an inorganic material generated at the interface by porous ceramic sintering, the inorganic material includes aluminum phosphate, aluminum silicate and/or silicate, and the thickness of the inorganic material is 0.1 μm to 5 μm.
Specifically, the raw materials such as alumina, silica, ammonium dihydrogen phosphate and the like added into the ceramic slurry can form inorganic substances such as phosphate, silicate and the like in the high-temperature sintering process, and the inorganic substances are equivalent to inorganic glue and can firmly fix surrounding substances, so that the porous ceramic is ensured to form a whole, and the mechanical property of the ceramic can be improved. Such as strength, hardness, etc.
Preferably, the ceramic powder material also comprises a pore-forming agent, wherein the pore-forming agent comprises at least one of hollow glass, hollow silicon oxide, hollow aluminum oxide, hollow zirconium oxide, ammonium carbonate, ammonium bicarbonate and ammonium dihydrogen phosphate, the addition amount of the pore-forming agent is 5-20% of the mass of the ceramic powder material, and the particle size D50 of the pore-forming agent is 2-20 μm.
Specifically, the porosity of the multilayer porous ceramic material in the above embodiment is precisely controlled by controlling the components and constituents of the ceramic material, and the porosities arranged in multiple layers form a certain relationship, so that the composite multilayer porous ceramic material having a certain arrangement rule is formed. According to the size of the pore-forming agent added to each layer, the porosity can be increased or decreased from inside to outside in sequence, or other designed porosity relations can be formed, and the porosity can be specifically selected according to needs.
In another aspect, there is also provided a method for preparing a multilayer porous ceramic material, the method comprising:
ceramic powder, an additive, a cosolvent, a pore-forming agent and a nano high-heat-conductivity material are prepared into a ceramic blank body through ball milling, granulation and cold pressing forming processes;
pressing ceramic powder, an additive, a pore-forming agent and a nano high-thermal-conductivity material into ceramic slurry;
the ceramic slurry and the ceramic blank are sequentially and alternately distributed to obtain a pre-composite material;
and sintering the pre-composite material to prepare the multilayer porous ceramic composite material.
In the above embodiment, in the preparation method of the composite porous ceramic, the ceramic powder is at least one of alumina, zirconia, silica, yttria, silicon carbide, boron nitride, aluminum nitride, silicon nitride, and the like, and the particle diameter D of the ceramic powder is50Is 1-30 μm. The additive is alumina, silica, sodium carbonate, calcium carbonate, magnesium oxide, magnesium carbonate, etc., and has a particle diameter D50Is 1-10 μm. The pore-forming agent comprises hollow glass, hollow silicon oxide, hollow aluminum oxide, hollow zirconium oxide, ammonium carbonate, ammonium bicarbonate, ammonium dihydrogen phosphate, ammonium polyphosphate and the like, and the particle diameter D of the additive501-10 μm, and the addition amount is 1-10% of the mass of the ceramic powder. The high heat conduction material comprises micro-nano alloy powder, such as alloy powder consisting of at least two of Ag, Au, Al, Cu, Mg, Ni, Fe, Ti or Si. The addition amount is 1-10% of the mass of the ceramic powder, and the grain diameter D of the alloy powder500.1 to 10 μm. The organic material used for forming the ceramic slurry 2 includes an organic solvent (60 wt% to 90 wt%)Percent), dispersant (0.5 to 10 percent) and adhesive (1 to 20 percent). The organic solvent comprises at least one of pure water, methanol, ethanol, propanol, toluene, acetone, etc., and the dispersant comprises at least one of PSE series dispersant, SD-05, DA-50, FS-20, D3005, D9000, polyacrylic acid (PAA) ester, polymethylacrylic acid (PMAA) salt, etc. The binder comprises polyethylene, polystyrene, polyvinyl acetate, microcrystalline paraffin, organosilane and the like.
The laminated green bodies, namely the ceramic slurry and the ceramic green bodies are sequentially and alternately distributed, the ceramic slurry is coated on the surface of the ceramic green body, and the ceramic green bodies are placed and alternately distributed in a reciprocating way. The number of layers may be selected as desired. And then placing the laminated green body in a sintering furnace for binder removal and sintering, wherein the sintering mode is to carry out binder removal in the air atmosphere, the heating rate in the binder removal stage is 1-3 ℃/min, the heat preservation temperature is 600-1000 ℃, the heat preservation time is 1-48h, and then the sintering stage is carried out, the sintering temperature is 1000-1400 ℃, the heating rate is 3-5 ℃/min, and the heat preservation time is 12-48h
Preferably, the ceramic slurry 2 is uniformly coated on the ceramic body 1 by any one of a spray coating method, a spin coating method, a czochralski method, a screen printing method, a coating method, a 3d printing method, a casting method, and a casting method.
The following is a detailed description of the embodiments:
example 1:
(1) taking a certain amount of alumina powder with a powder particle diameter D50Is 5 μm, 8 wt% SiO28 wt% of hollow zirconia, 5 wt% of ammonium dihydrogen phosphate and 3 wt% of TiO2And 3 wt% MgO23 wt% of Al-Mg-Cu alloy powder and 65 wt% of absolute ethyl alcohol, and ball-milling the raw materials by using a ball mill for 2 hours at the rotating speed of 200 r/min.
(2) And drying the ball-milling slurry at 120 ℃ to obtain dried ceramic powder, adding a certain amount of 5% PVA solution, and then granulating, wherein the granulation particle size does not make special requirements, and the cold-pressed blank body can be ensured to have certain strength, and a pressed sample is not layered, has no defects and the like.
(3) And (3) preparing the granulated powder into a ceramic blank by using isostatic cool pressing or other forming methods.
(4) Taking a certain amount of alumina powder with a powder particle diameter D505 μm, 5 wt% SiO25 wt% of hollow alumina, 5 wt% of ammonium dihydrogen phosphate and 3 wt% of TiO2And 3 wt% MgO25 wt% of Al-Mg-Cu alloy powder, 50 wt% of absolute ethyl alcohol, 40 wt% of sodium polyacrylate and 10 wt% of 5% of PVA solution are added, the raw materials are subjected to ball milling by using a ball mill, the ball milling time is 2 hours, and the rotating speed is 200r/min, so that uniformly dispersed slurry is obtained.
(5) Placing the ceramic blank into a special mold, pouring the slurry onto the surface of the ceramic blank by a pouring method to form a ceramic layer with the thickness of 5mm, and then placing the mold into a 300 ℃ for baking for 2-12 h to obtain the composite ceramic material.
(6) And (3) placing the composite ceramic material into a sintering furnace for removing glue and sintering. The sintering mode is that glue is discharged in the air atmosphere, the temperature rising speed is 1 ℃/min in the glue discharging stage, the heat preservation temperature is 800 ℃, the heat preservation time is 12h, then the sintering stage is carried out, the sintering temperature is 1200 ℃, the temperature rising speed is 3 ℃/min, and the heat preservation time is 48 h.
Example 2
(1) Taking a certain amount of ZrO2Particle size D of powder50Is 5 μm, 8 wt% SiO28 wt% of hollow glass powder, 5 wt% of ammonium dihydrogen phosphate, 3 wt% of Al-Mg-Cu alloy powder and 3 wt% of TiO2And 3 wt% MgO2And 65 wt% of absolute ethyl alcohol, and ball milling the raw materials by using a ball mill for 2 hours at the rotating speed of 200 r/min.
(2) And drying the ball-milling slurry at 120 ℃ to obtain dried ceramic powder, adding a certain amount of 5% PVA solution, and then granulating, wherein the granulation particle size does not make special requirements, and the cold-pressed blank body can be ensured to have certain strength, and a pressed sample is not layered, has no defects and the like.
(3) And (3) preparing the granulated powder into a ceramic blank by using isostatic cool pressing or other forming methods.
(4) Taking a certain amount of Si3N4Particle size D of powder505 μm, 5 wt% SiO25 wt% of hollow glass powder, 5 wt% of ammonium dihydrogen phosphate, 5 wt% of Cu-Ni-Zn alloy powder and 3 wt% of TiO2And 3 wt% MgO250 wt% of absolute ethyl alcohol, 40 wt% of sodium polyacrylate and 10 wt% of 5% of PVA solution are added, the raw materials are ball-milled by a ball mill for 2 hours at a rotating speed of 200r/min, and uniformly dispersed slurry is obtained.
(5) Placing the ceramic blank into a special mold, pouring the slurry onto the surface of the ceramic blank by a pouring method to form a ceramic layer with the thickness of 5mm, and then placing the mold into a 300 ℃ for baking for 2-12 h to obtain the composite ceramic material.
(6) And (3) placing the composite ceramic material into a sintering furnace for removing glue and sintering. The sintering mode is that glue is discharged in the air atmosphere, the heating rate is 1 ℃/min in the glue discharging stage, the heat preservation temperature is 800 ℃, the heat preservation time is 12h, then the sintering stage is carried out, the sintering temperature is 1300 ℃, the heating rate is 3 ℃/min, and the heat preservation time is 48 h.
The test method comprises the following steps:
and (3) porosity testing: reference GB/T1966-1996 porous ceramic apparent porosity and volume-weight test method
And (3) testing thermal conductivity: thermal conductivity of porous ceramic tested by laser thermal diffusion/thermal conductivity tester
Permeability: according to the permeability of the porous ceramic material in GB/T1969-1996 porous ceramic permeability test method. The detailed test results are shown in the following table:
Figure BDA0002760232600000071
the material prepared by the method has good performances in the aspects of heat conductivity, permeability, compressive strength and Vickers hardness.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A multi-layer porous ceramic material is characterized in that the material is composed of a plurality of layers of porous ceramics with different porosities and different thermal conductivities, and an integrated composite material is formed among the layers through inorganic connecting layers formed by sintering.
2. The multi-layer porous ceramic material of claim 1 wherein the porosity is controlled based on the composition and composition of the ceramic material.
3. The multi-layered porous ceramic material according to claim 1, wherein the pore size D of the multi-layered porous ceramic material502-15 μm, and the porosity of the porous layer is 50-70%.
4. The multi-layer porous ceramic material of claim 1, wherein the porous ceramic comprises alumina, zirconia, silica, yttria, carbonAt least one of silicon nitride, boron nitride, aluminum nitride and silicon nitride, and the ceramic powder particle diameter D50Is 1-30 μm.
5. The multilayer porous ceramic material of claim 4, wherein micro-nano high thermal conductivity material is added in each layer of porous ceramic material, the micro-nano high thermal conductivity material comprises alloy powder with surface anti-oxidation treatment, the addition amount is 1-10% of the mass of the ceramic powder, and the particle size D of the alloy powder500.1 to 10 μm.
6. The multi-layer porous ceramic material of claim 4 wherein the porous ceramic further comprises an additive and the additive comprises at least one of alumina, silica, sodium carbonate, calcium carbonate, magnesium oxide, magnesium carbonate; the addition amount of the additive is 1-10% of the mass of the ceramic slurry, and the particle size D of the additive50Is 1-10 μm.
7. The multi-layered porous ceramic material as claimed in claim 1, wherein the connection between the layers of the porous ceramic material is an inorganic material formed at the interface by sintering of the porous ceramic, the inorganic material comprising aluminum phosphate, aluminum silicate and/or silicate, and the inorganic material has a thickness of 0.1 μm to 5 μm.
8. The multi-layer porous ceramic material of claim 1, further comprising a pore-forming agent, wherein the pore-forming agent comprises at least one of hollow glass, hollow silica, hollow alumina, hollow zirconia, ammonium carbonate, ammonium bicarbonate and ammonium dihydrogen phosphate, the addition amount of the pore-forming agent is 5-20% of the mass of the ceramic powder, and the particle size D of the pore-forming agent is502-20 μm.
9. A method for preparing a multilayer porous ceramic material according to any of claims 1 to 8, comprising:
ceramic powder, additives, pore-forming agents and nano high-heat-conducting materials are prepared into a ceramic blank body (1) through ball milling, granulation and cold pressing forming processes;
forming ceramic slurry (2) by using ceramic powder, additives, pore-forming agents and nano high-thermal-conductivity materials;
the ceramic slurry (2) and the ceramic blank body (1) are sequentially and alternately distributed to obtain a pre-composite material;
and sintering the pre-composite material to prepare the multilayer porous ceramic composite material.
10. The method for preparing a multi-layered porous ceramic material according to claim 9, wherein the ceramic slurry (2) is uniformly applied to the ceramic body (1) by any one of a spray coating method, a spin coating method, a czochralski method, a screen printing method, a coating method, a 3d printing method, a casting method, and a tape casting method.
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CN114213139A (en) * 2021-12-31 2022-03-22 深圳市吉迩科技有限公司 Preparation method of ceramic heating element and ceramic heating element
CN114315333A (en) * 2022-02-10 2022-04-12 刘松青 Novel porous ceramic atomizing core production process
CN114804842A (en) * 2022-05-11 2022-07-29 西安交通大学 Preparation method of ceramic core with controllable pore distribution and atmosphere
CN114804842B (en) * 2022-05-11 2022-12-09 西安交通大学 Preparation method of ceramic core with controllable pore distribution and atmosphere
CN116375496A (en) * 2023-03-14 2023-07-04 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) Submillimeter-grade porous ceramic microsphere and preparation method thereof
CN116947470A (en) * 2023-08-19 2023-10-27 福建德化瓷国文化股份有限公司 Shaving pattern ceramic with imitation old and black cloud imprinting effects and preparation method thereof
CN116947470B (en) * 2023-08-19 2024-03-19 福建德化瓷国文化股份有限公司 Shaving pattern ceramic with imitation old and black cloud imprinting effects and preparation method thereof

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