WO2015192300A1 - 多孔陶瓷的制备方法、多孔陶瓷及电子烟 - Google Patents

多孔陶瓷的制备方法、多孔陶瓷及电子烟 Download PDF

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WO2015192300A1
WO2015192300A1 PCT/CN2014/079963 CN2014079963W WO2015192300A1 WO 2015192300 A1 WO2015192300 A1 WO 2015192300A1 CN 2014079963 W CN2014079963 W CN 2014079963W WO 2015192300 A1 WO2015192300 A1 WO 2015192300A1
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Prior art keywords
porous ceramic
precursor
premix
ceramic according
hours
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PCT/CN2014/079963
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English (en)
French (fr)
Inventor
刘平昆
周宏明
李荐
夏庆路
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深圳麦克韦尔股份有限公司
湖南省正源储能材料与器件研究所
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Application filed by 深圳麦克韦尔股份有限公司, 湖南省正源储能材料与器件研究所 filed Critical 深圳麦克韦尔股份有限公司
Priority to US14/414,114 priority Critical patent/US9861129B2/en
Priority to EP14814656.6A priority patent/EP3162778B1/en
Priority to PCT/CN2014/079963 priority patent/WO2015192300A1/zh
Publication of WO2015192300A1 publication Critical patent/WO2015192300A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62625—Wet mixtures
    • C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/40—Constructional details, e.g. connection of cartridges and battery parts
    • A24F40/44—Wicks
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/70—Manufacture
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/14—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silica
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • 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
    • C04B35/62605—Treating the starting powders individually or as mixtures
    • C04B35/62685—Treating the starting powders individually or as mixtures characterised by the order of addition of constituents or additives
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0051—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity
    • C04B38/0054—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof characterised by the pore size, pore shape or kind of porosity the pores being microsized or nanosized
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    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
    • A—HUMAN NECESSITIES
    • A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
    • A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
    • A24F40/10—Devices using liquid inhalable precursors
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M11/00—Sprayers or atomisers specially adapted for therapeutic purposes
    • A61M11/04—Sprayers or atomisers specially adapted for therapeutic purposes operated by the vapour pressure of the liquid to be sprayed or atomised
    • A61M11/041—Sprayers or atomisers specially adapted for therapeutic purposes operated by the vapour pressure of the liquid to be sprayed or atomised using heaters
    • A61M11/042—Sprayers or atomisers specially adapted for therapeutic purposes operated by the vapour pressure of the liquid to be sprayed or atomised using heaters electrical
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M15/00—Inhalators
    • A61M15/06—Inhaling appliances shaped like cigars, cigarettes or pipes
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61M—DEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M2205/00—General characteristics of the apparatus
    • A61M2205/02—General characteristics of the apparatus characterised by a particular materials
    • A61M2205/0211—Ceramics
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • 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
    • C04B2235/3201—Alkali metal oxides or oxide-forming salts thereof
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • 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
    • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • 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
    • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
    • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3418—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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    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34—Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3427—Silicates other than clay, e.g. water glass
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    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
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    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Definitions

  • the invention relates to a method for preparing a porous ceramic, a porous ceramic and the use thereof in an electronic cigarette.
  • Porous ceramics are ceramic materials which are generally sintered by high temperature from aggregates, binders and pore formers, and have a large number of pore structures which communicate with each other and with the surface of the material. Porous ceramics have many applications in metallurgy, biology, energy, environmental protection and other fields due to their high porosity, chemical stability, large specific surface area, small bulk density, low thermal conductivity and high temperature and corrosion resistance.
  • the atomizer of the electronic cigarette is the main component for storing the smoke liquid and generating the smoke in the electronic cigarette, and it is necessary to ensure that the storage liquid does not leak and achieve a certain amount of smoke generation.
  • the porous ceramics prepared by the conventional method for preparing porous ceramics cannot balance strength and porosity, and thus cannot be applied to electronic cigarettes.
  • a method for preparing a porous ceramic comprising the steps of:
  • the amorphous silica, the aluminum oxide and the ferric oxide are uniformly mixed to obtain a mixture, wherein the amorphous silica accounts for 80% to 98% by mass percent, and the third oxidation Al2O accounts for 1% ⁇ 10%, and the ferric oxide accounts for 1% ⁇ 10%;
  • the mixture is calcined at 1000 ° C to 1400 ° C for 0.5 hour to 3 hours to obtain a precursor, and the precursor is ground to obtain a precursor powder.
  • premix contains 60% to 90% by mass of the precursor powder, and the sodium silicate 0 ⁇ 20%, the pore former accounts for 10% ⁇ 40%;
  • the green compact is first incubated at 200 ° C to 600 ° C for 1 hour to 6 hours, and then sintered at 700 ° C to 1200 ° C for 0.5 hour to 3 hours to obtain the porous ceramic.
  • the precursor is ground and passed through a 50 mesh standard sieve to obtain the precursor powder.
  • the pore former is selected from at least one of sucrose, starch, wood fibers, and short carbon fibers.
  • the sucrose and the starch have a particle diameter of 10 ⁇ m to 150 ⁇ m
  • the wood fibers and the short carbon fibers have a diameter of 50 ⁇ m to 300 ⁇ m and a length of 300 ⁇ m to 3000 ⁇ m.
  • the mass ratio of the premix to the water is from 3:1 to 6:1.
  • the press molding is carried out at 0.5 MPa to 20 MPa.
  • the compact when the green compact is kept at 200 ° C to 600 ° C, the compact is heated to a temperature of 200 ° C to 600 ° C at a heating rate of 1 ° C / min to 10 ° C / min.
  • the porous ceramic has a porosity of 40% to 80% and a pore diameter of 10 ⁇ m to 300 ⁇ m.
  • the preparation method of the above porous ceramic adopts amorphous silica, aluminum oxide and iron oxide as porous ceramic aggregate, and can be sintered at a lower temperature, an air atmosphere and a normal pressure, and the sintering condition is mild; the aggregate is aggregated After pre-firing after mixing, the obtained precursor has a certain loose structure, and does not cause pores blocking the liquid phase in the subsequent sintering process, and at the same time, a certain porosity is generated, and this part of the pores is difficult to be damaged by pressure during the press forming process, thereby ensuring The porosity of the porous ceramic; the physical structure of the pre-fired precursor is stable, which is beneficial to increase the strength of the porous ceramic, so that the prepared porous ceramic has higher porosity and better strength.
  • FIG. 1 is a flow chart showing a method of preparing a porous ceramic according to an embodiment
  • FIG. 2 is a perspective view of an electronic cigarette according to an embodiment
  • FIG. 3 is a schematic cross-sectional view of the electronic cigarette shown in FIG. 2.
  • FIG. 1 a method for preparing a porous ceramic, comprising the following steps:
  • Step S110 mixing amorphous silica, aluminum oxide and ferric oxide to obtain a mixture, and calcining the mixture at 1000 ° C to 1400 ° C for 0.5 hour to 3 hours to obtain a precursor, and grinding the precursor to obtain a precursor. powder.
  • the amorphous silicon dioxide (SiO 2 ) accounts for 80% to 98%
  • the aluminum oxide (Al 2 O 3 ) accounts for 1% to 10%
  • the ferric oxide (Fe 2 O) 3 ) 1% to 10%.
  • the amorphous silica, the aluminum oxide and the ferric oxide are all analytically pure.
  • the precursor is ground and passed through a 50 mesh standard sieve to obtain a precursor powder.
  • the precursor powder can also be screened by other methods as long as the particle size of the precursor powder can be ensured.
  • the calcination is carried out in a high temperature atmospheric pressure oxidation furnace.
  • the amorphous silica, the aluminum oxide and the ferric oxide are mixed and mixed by a roller ball mill or a planetary ball mill for 0.5 hour to 8 hours.
  • a roller ball mill or a planetary ball mill for 0.5 hour to 8 hours.
  • the mixture is pre-sintered, and the resulting precursor has a loose structure.
  • step S120 the precursor powder, the sodium silicate and the pore former are uniformly mixed to obtain a premix.
  • the precursor powder accounts for 60% to 90%
  • the sodium silicate accounts for 0-20%
  • the pore former accounts for 10% to 40%.
  • sodium silicate (Na 2 SiO 3 ) is in the form of an aqueous solution of Na 2 SiO 3 , sodium silicate hydrate (Na 2 SiO 3 •9H 2 O) or sodium silicate having a modulus of 1.5-3.5. mixed with an aqueous solution of the precursor powder and the pore former, as long as nine hydrated sodium silicate (Na 2 SiO 3 • 9H 2 O) or sodium silicate modulus of 1.5 to 3.5 in the Na 2 SiO 3 and the other two The mass ratio of the raw material (precursor powder and pore former) may be sufficient.
  • the pore forming agent is at least one selected from the group consisting of sucrose, starch, wood fiber, and short carbon fiber.
  • sucrose and the starch have a particle diameter of 10 ⁇ m to 150 ⁇ m
  • the wood fiber and the short carbon fiber have a diameter of 50 ⁇ m to 300 ⁇ m and a length of 300 ⁇ m to 3000 ⁇ m.
  • the precursor powder, the sodium silicate and the pore former are mixed and mixed by a roller ball mill or a planetary ball mill for 0.5 hour to 8 hours.
  • a roller ball mill or a planetary ball mill for 0.5 hour to 8 hours.
  • it can also be stirred and mixed for 10 minutes to 2 hours using a mixer or a kneader.
  • a large-sized complex organic or inorganic material such as starch, sucrose, wood fiber and short carbon fiber is used as a pore-forming agent, and the pore diameter and porosity of the finally formed porous ceramic can be controlled according to requirements, and is suitable for storage, A communicating pore structure that conducts liquid and generates smoke.
  • Step S130 mixing the premix with water and pressing and molding to obtain a compact.
  • the mass ratio of the premix to water is from 3:1 to 6:1.
  • the press molding is carried out at 0.5 MPa to 20 MPa.
  • the premix is mixed with water to obtain a semi-wet material, and the semi-wet material is placed in a cylindrical mold, and pressed into a cylindrical green compact under a pressure of 0.5 MPa to 20 MPa.
  • the shape of the green compact depends on the shape of the final product, and is not limited to being cylindrical.
  • step S140 the green compact is first heated at 200 ° C to 600 ° C for 1 hour to 6 hours, and then sintered at 700 ° C to 1200 ° C for 0.5 hour to 3 hours to obtain a porous ceramic.
  • the green compact is heated and sintered at a heating rate of 1 ° C / min to 10 ° C / min until the temperature is raised to 200 ° C ⁇ 600 ° C, and then held at 200 ° C ⁇ 600 ° C for 1 hour ⁇ 6 hours.
  • both the heat preservation and the sintering are carried out in a high temperature atmospheric pressure oxidation furnace.
  • the resulting porous ceramic has a porosity of 40% to 80% and a pore diameter of 10 ⁇ m to 300 ⁇ m.
  • the preparation method of the above porous ceramic adopts amorphous silica, aluminum oxide and iron oxide as porous ceramic aggregate, and can be sintered at a lower temperature, an air atmosphere and a normal pressure, and the sintering condition is mild; the aggregate is aggregated After pre-firing after mixing, the obtained precursor has a certain loose structure, and does not cause pores blocking the liquid phase in the subsequent sintering process, and at the same time, a certain porosity is generated, and this part of the pores is difficult to be damaged by pressure during the press forming process, thereby ensuring The porosity of the porous ceramic; the physical structure of the pre-fired precursor is stable, which is beneficial to increase the strength of the porous ceramic, so that the prepared porous ceramic has higher porosity and better strength, and the porous ceramic is applied to the atomization of the electronic cigarette.
  • the structure of the atomizer can be simplified, and the cost can be reduced, and the porous ceramic can store more smoke liquid and exert a better atomization effect.
  • the preparation method of the above porous ceramic is simple in production process, low in sintering temperature, safe and non-toxic.
  • the electronic cigarette 200 of an embodiment includes a housing 220, a mouthpiece cover 240, an atomizing assembly 260, and a power supply assembly 280.
  • the atomizing assembly 260 includes a reservoir 262, a liquid absorbing element 264, and a liquid absorbing element 264 having a generally circular shape that cooperates with the housing 220.
  • the liquid absorbing member 264 is a porous ceramic prepared by the above-described method for producing a porous ceramic.
  • the liquid absorbing member 264 is housed in the housing 220 and is located at one end of the reservoir 262.
  • the smoke liquid from the accumulator 262 can be uniformly dispersed to the inside and the surface of the liquid absorbing member 264 by capillary action.
  • An atomizing passage 265 communicating with the flue of the electronic cigarette 200 is opened inside the liquid absorbing member 264.
  • the heating element 266 is a spiral tubular heating wire housed in the atomizing passage 265.
  • the structure of the electronic cigarette and the structure of the liquid absorbing member are not limited to the structure of the electronic cigarette 200 described above, and other types of electrons.
  • the porous ceramic can be used as a liquid absorbing member in the smoke, and the shape of the porous ceramic can be changed according to the structure of the electronic cigarette.
  • the porous ceramic prepared by the above method has better pore diameter, porosity and strength, can store more smoke liquid and exert good atomization effect, and can reduce the cost of the electronic cigarette on the one hand, and can obtain good use effect on the other hand. And a long service life.
  • the method for testing the performance of the porous ceramic material prepared by the embodiment of the invention is as follows: the porosity of the porous ceramic block is determined by the Archimedes drainage method; and the bending strength of the sample by the electronic universal testing machine (GB/T) 4741-1999) Test; the average pore size of the porous ceramic was measured using a pore size distribution meter.
  • the ratio of 1:1 (mass ratio) is mixed with water and stirred for 5 minutes to obtain a wet material, which is put into a cylindrical mold and pressed into a desired compact under a pressure of 0.5 MPa; the compact is placed in a high-temperature atmospheric pressure resistance furnace to The temperature was raised to 600 ° C for 1 h at 2 ° C / min to remove the pore former and moisture; the sample was further heated to 1000 ° C for 1 h at a rate of 2 ° C / min, and the desired porous ceramic was obtained after cooling with the furnace.
  • the ceramic block was subjected to porosity, bending strength, and average pore diameter measurement.
  • the porous ceramic exhibits a porosity of 36.1%,
  • amorphous SiO 2 , 1 g of Al 2 O 3 , 1 g of Fe 2 O 3 , 1 h of planetary ball milling calcination in a high temperature furnace, calcination temperature 1000 ° C, calcination time 3 h, calcination and grinding 50
  • the temperature is raised to 200 ° C for 2 h at a rate of 1 ° C / min, and then heated to 600 ° C for 4 h at the same rate to remove the pore former and moisture; the sample is further heated to 700 ° C at a rate of 1 ° C / min. 3h, the desired porous ceramic is obtained after cooling with the furnace.
  • the ceramic block was subjected to porosity, bending strength, and average pore diameter measurement.
  • the porous ceramic has a porosity of 65.3%, a flexural strength of 10.53 MPa, and an average pore diameter of 20 ⁇ m.
  • the precursor powder was obtained by a 50 mesh standard sieve; 70 g of the precursor powder, 20 g of Na 2 SiO 3 , 10 g of the pore-forming agent short carbon fiber were weighed and the mixture was ball milled for 8 h to obtain a mixed premix, wherein the carbon fiber was obtained.
  • the compact is placed in a high-temperature atmospheric pressure resistance furnace, heated at a rate of 10 ° C / min to 300 ° C for 4 h, and then heated to 500 ° C for 2 h at the same rate to remove the pore former and moisture; the sample is further 10 ° C
  • the rate of /min was raised to 1200 ° C for 0.5 h, and the desired porous ceramic was obtained after cooling with the furnace.
  • the ceramic block was subjected to porosity, bending strength, and average pore diameter measurement. Under this condition, the porous ceramic exhibited a porosity of 54.3%, a flexural strength of 15.27 MPa, and an average pore diameter of 50 ⁇ m.
  • the porous ceramic prepared by the porous ceramic preparation method of the present invention has a high porosity and a good strength.

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Abstract

一种多孔陶瓷的制备方法、多孔陶瓷及该多孔陶瓷在电子烟中的应用。该制备方法包括以下步骤：将无定型二氧化硅，三氧化二铝及三氧化二铁混合均匀得到混合物，将混合物在1000℃～1400℃下煅烧0.5小时～3小时得到前驱体，将前驱体研磨得到前驱体粉末，其中，混合物中按质量百分比计，无定型二氧化硅占80％～98％，三氧化二铝占1％～10％，三氧化二铁占1％～10％；将前驱体粉末、硅酸钠以及造孔剂混合均匀得到预混料；将预混料与水混合均匀后压制成型得到压坯；及将压坯先在200℃～600℃下保温1小时～6小时，再在700℃～1200℃下烧结0.5小时～3小时，得到多孔陶瓷。

Description

多孔陶瓷的制备方法、多孔陶瓷及电子烟
【技术领域】
本发明涉及一种多孔陶瓷的制备方法、多孔陶瓷及其在电子烟中的应用。
【背景技术】
多孔陶瓷是一般由骨料、粘结剂及造孔剂等组分由高温烧结的陶瓷材料，内部具有大量彼此连通并与材料表面连通的孔道结构。由于多孔陶瓷具有孔隙率高、化学性质稳定、比表面积大、体积密度小、导热性低以及耐高温耐腐蚀等优良性能，在冶金、生物、能源、环保等领域有着众多应用。
电子烟的雾化器是电子烟中储存烟液和产生烟雾的主要部件，需要保证储存液体不泄露并达到一定的烟雾产生量。然而现有的多孔陶瓷的制备方法制备的多孔陶瓷无法兼顾强度及孔隙率，从而无法应用于电子烟。
【发明内容】
基于此，有必要提供具有较高孔隙率且强度较好的多孔陶瓷的制备方法、多孔陶瓷及其在电子烟中的应用。
一种多孔陶瓷的制备方法，包括以下步骤：
将无定型二氧化硅，三氧化二铝及三氧化二铁混合均匀得到混合物，其中，所述混合物中按质量百分比计，所述无定型二氧化硅占80%~98%，所述三氧化二铝占1%~10%，所述三氧化二铁占1%~10%；
将所述混合物在1000℃~1400℃下煅烧0.5小时~3小时得到前驱体，将所述前驱体研磨得到前驱体粉末，
将所述前驱体粉末、硅酸钠以及造孔剂混合均匀得到预混料，其中所述预混料中按质量百分比计，所述前驱体粉末占60%~90%，所述硅酸钠占0~20%，所述造孔剂占10%~40%；
将所述预混料与水混合均匀后压制成型得到压坯；及
将所述压坯先在200℃~600℃下保温1小时~6小时，再在700℃~1200℃下烧结0.5小时~3小时，得到所述多孔陶瓷。
在其中一个实施例中，将所述前驱体研磨后过50目标准筛得到所述前驱体粉末。
在其中一个实施例中，所述造孔剂选自蔗糖、淀粉、木纤维及短碳纤维中的至少一种。
在其中一个实施例中，所述蔗糖及所述淀粉的粒径为10μm~150μm，所述木纤维及所述短碳纤维的直径为50μm~300μm，长度为300μm~3000μm。
在其中一个实施例中，所述预混料与所述水的质量比为3:1~6:1。
在其中一个实施例中，所述压制成型在0.5MPa~20MPa下进行。
在其中一个实施例中，所述压坯在200℃~600℃下保温时，将所述压坯以1℃/min~10℃/min的升温速率升温至200℃~600℃。
一种上述任一项所述的多孔陶瓷的制备方法制备的多孔陶瓷。
在其中一个实施例中，所述多孔陶瓷的孔隙率为40%~80%，孔径为10μm~300μm。
上述任一项所述的多孔陶瓷在电子烟中的应用。
上述多孔陶瓷的制备方法，采用无定型二氧化硅、三氧化二铝及氧化铁作为多孔陶瓷骨料，可以在较低温度、空气气氛及常压下烧结，烧结的条件较为温和；将骨料混合后进行预烧，得到的前驱体具有一定疏松结构，在后续的烧结过程中不会产生阻塞液相的孔隙，同时产生一定孔隙率，在压制成型过程中这部分孔隙难以被压力破坏，保证了多孔陶瓷的孔隙率；预烧得到的前驱体物理结构稳定，有利于提高多孔陶瓷的强度，从而制备的多孔陶瓷具有较高孔隙率且强度较好。
【附图说明】
图1为一实施方式的多孔陶瓷的制备方法的流程图；
图2为一实施方式的电子烟的立体示意图；
图3为图2所示电子烟的剖面示意图。
【具体实施方式】
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合实施例对本发明的具体实施方式做详细的说明。在下面的描述中阐述了很多具体细节以便于充分理解本发明。但是本发明能够以很多不同于在此描述的其它方式来实施，本领域技术人员可以在不违背本发明内涵的情况下做类似改进，因此本发明不受下面公开的具体实施的限制。
请参阅图1，一种多孔陶瓷的制备方法，包括以下步骤：
步骤S110、将无定型二氧化硅，三氧化二铝及三氧化二铁混合均匀得到混合物，将混合物在1000℃~1400℃下煅烧0.5小时~3小时得到前驱体，将前驱体研磨得到前驱体粉末。
其中，混合物中按质量百分比计，无定型二氧化硅（SiO2）占80%~98%，三氧化二铝（Al2O3）占1%~10%，三氧化二铁（Fe2O3）占1%~10%。
优选的，无定型二氧化硅、三氧化二铝及三氧化二铁均为分析纯。
优选的，将前驱体研磨后过50目标准筛得到前驱体粉末。当然，也可以用其他方法筛选前驱体粉末，只要能保证前驱体粉末的粒度符合要求即可。
优选的，煅烧在高温常压氧化炉中进行。
优选的，将无定型二氧化硅，三氧化二铝及三氧化二铁混合时采用滚筒球磨机或行星球磨机干混0.5小时~8小时。当然，还可以采用其他方式混合，只要保证几种材料混合均匀即可，比如使用搅拌机或捏合机搅拌干混10分钟~2小时。
该步骤中，将混合物预烧结，得到的前驱体具有一定疏松结构。
步骤S120、将前驱体粉末、硅酸钠以及造孔剂混合均匀得到预混料。
其中，预混料中按质量百分比计，前驱体粉末占60%~90%，硅酸钠占0~20%，造孔剂占10%~40%。
本实施方式中，硅酸钠（Na2SiO3）以Na2SiO3、九水合硅酸钠（Na2SiO3•9H2O）或模数为1.5-3.5的硅酸钠的水溶液的形式与前驱体粉末及造孔剂混合，只要保证九水合硅酸钠（Na2SiO3•9H2O ）或模数为1.5-3.5的硅酸钠的水溶液中的Na2SiO3 与其他两种原料（前驱体粉末及造孔剂）的质量比例即可。
本实施方式中，造孔剂选自蔗糖、淀粉、木纤维及短碳纤维中的至少一种。优选的，蔗糖及淀粉的粒径为10μm~150μm，木纤维及短碳纤维的直径为50μm~300μm，长度为300μm~3000μm。
优选的，将前驱体粉末、硅酸钠以及造孔剂混合时采用滚筒球磨机或行星球磨机干混0.5小时~8小时。当然，还可以采用搅拌机或捏合机搅拌干混10分钟~2小时。
该步骤中，采用淀粉、蔗糖、木纤维及短碳纤维这种大粒径的复杂有机物或无机物作为造孔剂，可以根据需求控制最终形成的多孔陶瓷的孔径及孔隙率，得到适于储存、传导液体和产生烟雾的连通孔结构。
步骤S130、将预混料与水混合均匀后压制成型得到压坯。
优选的，预混料与水的质量比为3:1~6:1。
优选的，压制成型在0.5MPa~20MPa下进行。
本实施方式中，将预混料与水混合后得到半湿料，将半湿料装入圆柱形模具中，在0.5MPa~20MPa的压力下压制成圆柱形压坯。当然，压坯的形状取决于最终产品的形状，不限于为圆柱形。
该步骤中，将预混料与水混合后，预混料中的某些种类造孔剂在水的作用下具有一定的粘度，硅酸钠溶液亦具有一定粘度，起到成型剂的作用，简化了原料组成和生产工艺，降低了成本。
步骤S140、将压坯先在200℃~600℃下保温1小时~6小时，再在700℃~1200℃下烧结0.5小时~3小时，得到多孔陶瓷。
优选的，将压坯以1℃/min~10℃/min的升温速率升温烧结，直至升温至200℃~600℃，然后在200℃~600℃下保温1小时~6小时。
本实施方式中，在700℃~1200℃下烧结时在常压下进行。
优选的，保温及烧结均在高温常压氧化炉中进行。
最终得到的多孔陶瓷的孔隙率为40%~80%，孔径为10μm~300μm。
上述多孔陶瓷的制备方法，采用无定型二氧化硅、三氧化二铝及氧化铁作为多孔陶瓷骨料，可以在较低温度、空气气氛及常压下烧结，烧结的条件较为温和；将骨料混合后进行预烧，得到的前驱体具有一定疏松结构，在后续的烧结过程中不会产生阻塞液相的孔隙，同时产生一定孔隙率，在压制成型过程中这部分孔隙难以被压力破坏，保证了多孔陶瓷的孔隙率；预烧得到的前驱体物理结构稳定，有利于提高多孔陶瓷的强度，从而制备的多孔陶瓷具有较高孔隙率且强度较好，将多孔陶瓷应用于电子烟的雾化器时，能简化雾化器的结构，减低成本，多孔陶瓷能储存较多烟液并发挥较好的雾化效果。同时，上述多孔陶瓷的制备方法生产工艺简单，烧结温度低，安全无毒。
请同时参阅图2及图3，一实施方式的电子烟200包括壳体220、烟嘴盖240、雾化组件260及电源组件280。雾化组件260包括储液器262、吸液元件264、吸液元件264的形状大致为与壳体220相配合的圆管。吸液元件264为上述多孔陶瓷的制备方法制备的多孔陶瓷。吸液元件264收容于壳体220内，并位于储液器262的一端。来自储液器262的烟液通过毛细作用能够均匀地分散到吸液元件264的内部和表面。吸液元件264的内部开设有与电子烟200的烟道相通的雾化通道265。发热元件266为收容在雾化通道265内的螺旋管状的发热丝。
需要说明的是，应用上述多孔陶瓷的制备方法制备的多孔陶瓷作为电子烟的吸液元件时，电子烟的结构及吸液元件的结构不限于上面描述的电子烟200的结构，其他类型的电子烟中均可使用该多孔陶瓷作为吸液元件，对应的根据电子烟的结构改变多孔陶瓷的形状即可。按照上述方法制备得到的多孔陶瓷的孔径、孔隙率及强度较好，能够储存较多的烟液并发挥良好的雾化效果，一方面可以降低电子烟成本，另一方面可以取得良好的使用效果及较长的使用寿命。
以下结合具体实施例对上述多孔陶瓷的制备方法做进一步阐述。
本发明实施例制备的多孔陶瓷材料进行性能测试的方法为：阿基米德排水法测定多孔陶瓷块体的孔隙率；用电子万能试验机对样品的抗弯强度（GB/T 4741-1999）进行测试；使用孔径分布测量仪测定多孔陶瓷平均孔径。
实施例1
按照重量取SiO2 80克，Al2O3 10克，Fe2O3 10克行星球磨2h，在高温炉中进行煅烧，煅烧温度1200℃，煅烧时间1h，煅烧后经研磨过50目标准筛得到前驱体粉末。按照前驱体粉末90克 ，造孔剂木纤维10克称取原料并搅拌混合30min，得到混合好的预混料，其中木纤维的直径300μm，长度1-3mm；按照预混料：水=3:1的比例（质量比）加入水混合搅拌5min，得到湿料，装入圆柱形模具中，在0.5MPa压力下压制成所需压坯；将压坯放入高温常压电阻炉中，以2℃/min速率升温至600℃保温1h，脱除造孔剂和水分；将样品再以2℃/min的速率升温至1000℃烧结1h，随炉冷却后得到所需多孔陶瓷。将陶瓷块体进行孔隙率、抗弯强度、平均孔径测量。多孔陶瓷显孔隙率36.1%，抗弯强度15.60MPa，平均孔径200μm。
实施例2：
按照重量取无定型SiO2 98克，Al2O3 1克，Fe2O3 1克，行星球磨1h，在高温炉中进行煅烧，煅烧温度1000℃，煅烧时间3h，煅烧后经研磨过50目标准筛得到前驱体粉末；按照前驱体粉末60克，造孔剂淀粉40克称取原料并行星球磨混合0.5h，得到混合好的预混料，其中淀粉的粒径为20μm；按照预混料：水=6:1的比例（质量比）加入水混合搅拌5min，得到湿料，装入圆柱形模具中，在20Mpa压力下压制成所需压坯；将压坯放入高温常压电阻炉中，以1℃/min速率升温至200℃保温2h，再以同样速率升温至600℃保温4h，脱除造孔剂和水分；将样品再以1℃/min的速率升温至700℃烧结3h，随炉冷却后得到所需多孔陶瓷。将陶瓷块体进行孔隙率、抗弯强度、平均孔径测量。多孔陶瓷显孔隙率65.3%，抗弯强度10.53Mpa，平均孔径20μm。
实施例3：
按照重量取无定型SiO2 90克，Al2O3 5克，Fe2O3 5克，滚筒球磨3h，在高温炉中进行煅烧，煅烧温度1400℃，煅烧时间0.5h，煅烧后经研磨过50目标准筛得到前驱体粉末；按照前驱体粉末70克，Na2SiO320克，造孔剂短碳纤维10克称取原料并滚筒球磨混料8h，得到混合好的预混料，其中碳纤维直径50μm，长度300μm；按照预混料：水=3:1（质量比）的比例加入水混合搅拌5min，得到湿料，装入圆柱形模具中，在10Mpa压力下压制成所需压坯；将压坯放入高温常压电阻炉中，以10℃/min速率升温至300℃保温4h，再以同样速率升温至500℃保温2h，脱除造孔剂和水分；将样品再以10℃/min的速率升温至1200℃烧结0.5h，随炉冷却后得到所需多孔陶瓷。将陶瓷块体进行孔隙率、抗弯强度、平均孔径测量。在此条件下，多孔陶瓷显孔隙率54.3%，抗弯强度15.27Mpa，平均孔径50μm。
从实施例1-3可以看出本发明的多孔陶瓷制备方法制备的多孔陶瓷的孔隙率较高，且强度较好。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

  1. 一种多孔陶瓷的制备方法，其特征在于，包括以下步骤：
    将无定型二氧化硅，三氧化二铝及三氧化二铁混合均匀得到混合物，其中，所述混合物中按质量百分比计，所述无定型二氧化硅占80%~98%，所述三氧化二铝占1%~10%，所述三氧化二铁占1%~10%；
    将所述混合物在1000℃~1400℃下煅烧0.5小时~3小时得到前驱体，将所述前驱体研磨得到前驱体粉末，
    将所述前驱体粉末、硅酸钠以及造孔剂混合均匀得到预混料，其中，所述预混料中按质量百分比计，所述前驱体粉末占60%~90%，所述硅酸钠占0~20%，所述造孔剂占10%~40%；
    将所述预混料与水混合均匀后压制成型得到压坯；及
    将所述压坯先在200℃~600℃下保温1小时~6小时，再在700℃~1200℃下烧结0.5小时~3小时，得到所述多孔陶瓷。
  2. 根据权利要求1所述的多孔陶瓷的制备方法，其特征在于，将所述前驱体研磨后过50目标准筛得到所述前驱体粉末。
  3. 根据权利要求1所述的多孔陶瓷的制备方法，其特征在于，所述造孔剂选自蔗糖、淀粉、木纤维及短碳纤维中的至少一种。
  4. 根据权利要求3所述的多孔陶瓷的制备方法，其特征在于，所述蔗糖及所述淀粉的粒径为10μm~150μm，所述木纤维及所述短碳纤维的直径为50μm~300μm，长度为300μm~3000μm。
  5. 根据权利要求1所述的多孔陶瓷的制备方法，其特征在于，所述预混料与所述水的质量比为3:1~6:1。
  6. 根据权利要求1所述的多孔陶瓷的制备方法，其特征在于，所述压制成型在0.5MPa~20MPa下进行。
  7. 根据权利要求6所述的多孔陶瓷的制备方法，其特征在于，所述压坯在200℃~600℃下保温时，将所述压坯以1℃/min~10℃/min的升温速率升温至200℃~600℃。
  8. 一种采用权利要求1~7任一项所述的多孔陶瓷的制备方法制备的多孔陶瓷。
  9. 根据权利要求8所述的多孔陶瓷，其特征在于，所述多孔陶瓷的孔隙率为40%~80%，孔径为10μm~300μm。
  10. 一种电子烟，包括吸液元件，所述吸液元件的材料为采用权利要求1~7任一项所述的多孔陶瓷的制备方法制备的多孔陶瓷。
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