WO2025107895A1 - Porous ceramic material and preparation method therefor, ceramic atomizing core and atomizing device - Google Patents
Porous ceramic material and preparation method therefor, ceramic atomizing core and atomizing device Download PDFInfo
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- WO2025107895A1 WO2025107895A1 PCT/CN2024/122706 CN2024122706W WO2025107895A1 WO 2025107895 A1 WO2025107895 A1 WO 2025107895A1 CN 2024122706 W CN2024122706 W CN 2024122706W WO 2025107895 A1 WO2025107895 A1 WO 2025107895A1
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Definitions
- the invention relates to the field of atomization technology, and in particular to a porous ceramic material and a preparation method thereof, a ceramic atomization core and an atomization device.
- the atomizer core is the core component of the atomizer device. It consists of a porous liquid storage medium and a heating element. There are two main types: cotton core and ceramic atomizer core. Ceramic atomizer cores have the advantages of high temperature resistance, strong designability, automated production, and low leakage. In addition, ceramics are rigid materials, which can reduce or eliminate the use of structural parts to achieve structural and functional integration of the atomizer core, thereby reducing costs. Therefore, ceramic atomizer cores have gradually become a hot spot for industry research and development.
- the ceramic atomizer core in the current atomizer equipment has the problems of low liquid storage capacity and slow liquid absorption speed, which reduces the user experience.
- a porous ceramic material in a first aspect of the present application, includes: component A and component B; in terms of mass fractions, component A includes 15-40 parts of aggregate powder, 15-35 parts of glass powder, 15-35 parts of pore formers, and 20-50 parts of porous inorganic non-metallic powder; the average particle size D50 of the porous inorganic non-metallic powder is 20 ⁇ m-50 ⁇ m;
- component B includes 40%-60% paraffin wax, 1.5%-6.5% dispersant and 1.5%-5% binder.
- the above-mentioned porous ceramic material is prepared by using raw materials of component A and component B with specific composition and proportion, especially introducing a porous inorganic non-metallic powder component containing a porous structure and a pore-forming agent to increase the porosity of the main structure of the above-mentioned porous ceramic material, and further using an adhesive as a shape-preserving component to fix and maintain the porosity of the main structure, and by controlling the particle size of the porous inorganic non-metallic powder component, the porous ceramic material can have sufficient strength and improve the permeability of the pores; in this way, the prepared porous ceramic material can not only have higher strength, but also form micro-nano and micron-level pore structures and through pores, so that the porous ceramic material has a larger liquid storage capacity and liquid absorption speed, thereby improving the liquid supply capacity of the porous ceramic material.
- the binder is selected from at least one of a thermoplastic resin and ethyl cellulose.
- thermoplastic resin is selected from at least one of EVA and PE.
- the weight of the binder accounts for 2%-3% of the total weight of component A.
- the porous inorganic non-metallic powder is selected from at least one of zeolite, perlite, medical stone and diatomaceous earth.
- the aggregate powder is selected from at least one of SiC powder, silicon nitride powder, corundum powder, quartz powder, mullite and cordierite; and/or the average particle size D50 of the aggregate powder is 30 ⁇ m-100 ⁇ m.
- the pore-forming agent is selected from at least one of PMMA, PS, PP, wood flour and wheat flour; and/or the average particle size D50 of the pore-forming agent is 20 ⁇ m-80 ⁇ m.
- the average particle size D50 of the glass powder is 1 ⁇ m-10 ⁇ m; and/or the initial melting temperature of the glass powder is 450° C.-550° C.
- the dispersant is selected from at least one of beeswax and oleic acid.
- a method for preparing the porous ceramic material comprising the following steps:
- the mixed slurry is made into an embryo body, and the embryo body is sintered to obtain a porous ceramic material.
- the step of mixing and kneading the prepared raw materials comprises:
- the B component is melted, and then added into the A component for mixing to obtain a mixed slurry.
- the mixing and kneading temperature is 70° C.-100° C.; and/or,
- the rotating speed of the mixing and kneading is 15 r/min-50 r/min; and/or,
- the mixing time is 0.5-1.5h.
- the sintering process includes first keeping the temperature at 200°C-250°C for 1.5h-4h, then keeping the temperature at 380°C-420°C for 0.5h-3h, and then keeping the temperature at 640°C-685°C for 15min-60min.
- the heating step of heating to 200°C-250°C includes: first heating to 50°C-70°C at 0.5°C/min-1.5°C/min, then heating to 80°C-110°C at 0.3°C/min-1°C/min, and then heating to 200°C-250°C at 0.8°C/min ⁇ 1.5°C/min.
- a porous ceramic atomization core comprising the porous ceramic material mentioned above.
- a fourth aspect of the present invention provides an atomization device, wherein the atomization device comprises the porous ceramic atomization core.
- first and second are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as “first” and “second” may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of “plurality” is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.
- a porous ceramic material is provided.
- the raw materials for preparing the porous ceramic material include: component A and component B; component A includes 15-40 parts of aggregate powder, 15-35 parts of glass powder, 15-35 parts of pore-forming agent and 20-50 parts of porous inorganic non-metallic powder by weight; the average particle size D50 of the porous inorganic non-metallic powder is 20 ⁇ m-50 ⁇ m;
- Component B includes 40%-60% paraffin wax, 1.5%-6.5% dispersant and 1.5%-5% binder in terms of the total mass of component A.
- the mass percentage of paraffin wax in component B is 40%-60%
- the mass percentage of dispersant is 1.5%-6.5%
- the mass percentage of binder is 1.5%-5%.
- the above-mentioned porous ceramic material is prepared by using raw materials of component A and component B with specific composition and proportion, especially introducing a porous inorganic non-metallic powder component containing a porous structure and a pore-forming agent to increase the porosity of the main structure of the above-mentioned porous ceramic material, and further using an adhesive as a shape-preserving component to fix and maintain the porosity of the main structure, and by controlling the particle size of the porous inorganic non-metallic powder component, the porous ceramic material can have sufficient strength and improve the permeability of the pores; in this way, the prepared porous ceramic material can not only have higher strength, but also form micro-nano and micron-level pore structures and through pores, so that the porous ceramic material has a larger liquid storage capacity and liquid absorption speed, thereby improving the liquid supply capacity of the porous ceramic material.
- the content of the porous inorganic non-metallic powder in component A is 20-50 parts by weight.
- the content of the porous inorganic non-metallic powder in component A can be 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 48 parts or 50 parts.
- the weight percentage of the porous inorganic non-metallic powder in component A can be a range value composed of any two of the above point values.
- the content of the porous inorganic non-metallic powder in component A is 45-50 parts.
- the average particle size D50 of the porous inorganic non-metallic powder is 20 ⁇ m-50 ⁇ m.
- the average particle size D50 of the porous inorganic non-metallic powder can be 20 ⁇ m, 25 ⁇ m, 30 ⁇ m, 35 ⁇ m, 40 ⁇ m, 45 ⁇ m or 50 ⁇ m.
- the average particle size D50 of the porous inorganic non-metallic powder can be a range consisting of any two of the above point values as end values.
- the average particle size D50 of the porous inorganic non-metallic powder is 30 ⁇ m-50 ⁇ m.
- the average particle size D50 of the porous inorganic non-metallic powder By further controlling the average particle size D50 of the porous inorganic non-metallic powder, it is avoided that the particle size of the porous inorganic non-metallic powder is too large to reduce the mechanical strength of the porous ceramic, and it is also avoided that the particle size of the porous inorganic non-metallic powder is too small, resulting in its distribution in the gaps formed by the accumulation between the aggregate powder and the glass powder, thereby reducing the through porosity of the gaps in the porous ceramic material.
- the porous inorganic non-metallic powder can be selected from at least one of zeolite, perlite, medical stone and diatomaceous earth. Further, the porous inorganic non-metallic powder is diatomaceous earth.
- the binder may be selected from at least one of a thermoplastic resin and ethyl cellulose.
- the thermal decomposition temperature of the thermoplastic resin is 230° C.-400° C.
- the thermoplastic resin may be selected from at least one of ethylene vinyl acetate (EVA) and polyethylene (PE).
- EVA ethylene vinyl acetate
- PE polyethylene
- the above-mentioned "1.5%-5% adhesive” means that the mass of the adhesive may account for 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5% of the total mass of component A. Furthermore, the mass of the above-mentioned adhesive may account for a range of any two of the above-mentioned point values as end values. Preferably, the mass of the adhesive accounts for 2%-3% of the total mass of component A.
- the addition of the adhesive can also make the slurry less prone to particle sedimentation during the preparation process, make the slurry have better stability, and optimize the amount of admixture to make it have rheological properties suitable for hot die casting.
- the aggregate powder may be selected from at least one of SiC powder, silicon nitride powder, corundum powder, quartz powder, mullite and cordierite.
- the aggregate powder may be selected from at least one of corundum and mullite.
- the average particle size D50 of the aggregate powder is 30 ⁇ m-100 ⁇ m.
- the average particle size D50 of the aggregate powder can be 30 ⁇ m, 40 ⁇ m, 50 ⁇ m, 60 ⁇ m, 70 ⁇ m, 80 ⁇ m, 90 ⁇ m or 100 ⁇ m.
- the average particle size D50 of the above-mentioned bone powder can be a range consisting of any two of the above-mentioned point values as end values.
- the average particle size D50 of the above-mentioned aggregate powder is 30 ⁇ m-50 ⁇ m.
- the pore former may be selected from at least one of polymethyl methacrylate (PMMA), polystyrene (PS), polypropylene (PP), wood flour, and wheat flour.
- PMMA polymethyl methacrylate
- PS polystyrene
- PP polypropylene
- wood flour wood flour
- wheat flour wheat flour
- the average particle size D50 of the pore former is 20 ⁇ m-80 ⁇ m.
- the average particle size D50 of the pore former may be 20 ⁇ m, 30 ⁇ m, 40 ⁇ m, 50 ⁇ m, 60 ⁇ m, 70 ⁇ m or 80 ⁇ m.
- the average particle size D50 of the pore former may be a range consisting of any two of the above point values as end values.
- the average particle size D50 of the pore former is 30 ⁇ m-50 ⁇ m.
- the glass powder has an initial melting temperature of 450°C-550°C.
- the average particle size D50 of the glass powder is 1 ⁇ m-10 ⁇ m.
- the average particle size D50 of the glass powder can be 1 ⁇ m, 2 ⁇ m, 3 ⁇ m, 4 ⁇ m, 5 ⁇ m, 6 ⁇ m, 7 ⁇ m, 8 ⁇ m, 9 ⁇ m or 10 ⁇ m.
- the average particle size D50 of the glass powder can be a range consisting of any two of the above point values as end values.
- the average particle size D50 of the glass powder is 2 ⁇ m-5 ⁇ m.
- the dispersant may be selected from at least one of beeswax and oleic acid.
- the dispersant may be selected from beeswax and oleic acid.
- the mass of the beeswax accounts for 1%-5% of the total mass of component A.
- the mass of beeswax accounts for 1%, 2%, 3%, 4% or 5% of the total mass of component A.
- the mass of beeswax accounts for a percentage of the total mass of component A that can be a range consisting of any two of the above point values as end values.
- the mass of beeswax accounts for 2%-3.5% of the total mass of component A.
- the mass of the oleic acid accounts for 0.5%-1.5% of the total mass of component A.
- the mass of the oleic acid accounts for 0.5%, 1% or 1.5% of the total mass of component A.
- the mass of the oleic acid accounts for a range of any two of the above point values as end values.
- a method for preparing the porous ceramic material comprising the following steps S10-S20.
- step S10 preparing a green body from the mixed slurry in step S10, and sintering the green body to obtain a porous ceramic material.
- the mixing and kneading of the raw materials can be performed in an internal mixer.
- the temperature of the internal mixer can be set to 70°C-100°C.
- the rotation speed of the internal mixer can be set to 15r/min-50r/min.
- the mixing and kneading time is 0.5 h-1.5 h.
- the step of mixing and kneading the raw materials includes: melting component B, then adding component A to mix, to obtain a mixed slurry. Melting component B first and then adding component A is beneficial to improving the uniformity and efficiency of the mixing.
- the raw materials of component A are mixed to obtain a first mixed material. Furthermore, the first mixed material is preheated.
- the preheating step includes baking the first mixed material at 80° C.-120° C. for 0.5 h-1.5 h.
- the step of mixing and kneading the prepared raw materials includes: adding component A and component B together into an internal mixer for mixing and kneading.
- the method of preparing an embryo body from the mixed slurry comprises steps S21 - S23 .
- the temperature of the hot die casting machine can be set to 60°C-80°C.
- the pressure of the hot die casting machine can be set to 0.5 MPa-0.8 MPa.
- the sintering step includes first keeping the temperature at 200°C-250°C for 1.5h-4h, then keeping the temperature at 380°C-420°C for 0.5h-3h, and then keeping the temperature at 640°C-685°C for 15min-60min.
- the heating step of heating to 200°C-250°C includes: first heating to 50°C-70°C at 0.5°C/min-1.5°C/min, then heating to 80°C-110°C at 0.3°C/min-1°C/min, and then heating to 200°C-250°C at 0.8°C/min ⁇ 1.5°C/min.
- the sintering process includes first keeping the temperature at 220°C-230°C for 1.5h-4h, then heating to 400°C-420°C at 0.8 ⁇ 1.5°C/min and keeping the temperature for 0.5h-3h, then heating to 640°C-685°C at 2°C/min-6°C/min and keeping the temperature for 15min-60min; then cooling with the furnace.
- the organic matter is discharged slowly step by step, so that the ceramic particles do not rearrange violently, and the collapse of the voids in the ceramic is prevented.
- the sintered product is ultrasonically cleaned and dried to obtain a porous ceramic material.
- the porous ceramic material can be applied to a carrier for adsorbing liquid, and its application products include but are not limited to atomizer cores.
- a porous ceramic atomization core is provided, and the porous ceramic atomization core includes the above-mentioned porous ceramic material.
- an atomization device which includes the above-mentioned porous ceramic atomization core.
- the atomizing device includes but is not limited to an electronic cigarette.
- the raw materials for preparation of Example 1 include component A and component B, wherein:
- Component A by mass, comprising 27.5 parts of quartz powder with a D50 of about 50 ⁇ m, 28 parts of glass powder with a D50 of 5.5 ⁇ m and a melting point of 465°C, 20 parts of wheat flour with a D50 of 32 ⁇ m, and 24.5 parts of diatomaceous earth with a D50 of 28.5 ⁇ m;
- component B Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% EVA.
- the first mixed material is placed in an oven and baked at 100° C. for 1 h to obtain a second mixed material.
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.7 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain the green billet after cooling.
- step (5) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 230°C at a rate of 1°C/min and kept at this temperature for 3 h, then heated to 400°C at a rate of 1°C/min and kept at this temperature for 1.5 h, then heated to 670°C at a rate of 5°C/min and kept at this temperature for 30 min, and then cooled in the furnace.
- step (6) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- the raw materials for preparing Example 2 include component A and component B, wherein:
- Component A by mass, comprising 15 parts of quartz powder with a D50 of about 32 ⁇ m, 34 parts of glass powder with a D50 of 2.1 ⁇ m and a melting point of 465°C, 16 parts of wheat flour with a D50 of 20 ⁇ m, and 35 parts of diatomaceous earth with a D50 of 20 ⁇ m;
- component B Based on the total mass of component A, component B includes 60% paraffin, 1.5% oleic acid, 4.5% beeswax and 5.0% EVA.
- the first mixed material is placed in an oven and baked at 100° C. for 0.5 h to obtain a second mixed material.
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 0.5 h to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 60°C, and adjust the pressure to 0.8 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
- step (6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 0.5°C/min, then heated to 100°C at a rate of 0.3°C/min, then heated to 230°C at a rate of 0.8°C/min and kept at this temperature for 1.5 h, then heated to 400°C at a rate of 0.8°C/min and kept at this temperature for 1 h, then heated to 640°C at a rate of 2°C/min and kept at this temperature for 60 min, and then cooled in the furnace.
- step (6) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- the raw materials for preparation of Example 3 include component A and component B, wherein:
- Component A by mass, including 39 parts of quartz powder with a D50 of about 98 ⁇ m, 15 parts of glass powder with a D50 of 5.5 ⁇ m and a melting point of 465°C, 31 parts of PMMA with a D50 of 76 ⁇ m, and 20 parts of medical stone with a D50 of 48.5 ⁇ m;
- component B Based on the total mass of component A, component B includes 40% paraffin, 1% oleic acid, 1% beeswax and 2% EVA.
- the raw materials of component A are weighed and mixed to obtain a first mixed material.
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1.5 hours to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 80°C, and adjust the pressure to 0.5 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
- step (5) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 230°C at a rate of 1°C/min and kept at this temperature for 2.5 h, then heated to 400°C at a rate of 1°C/min and kept at this temperature for 1.5 h, then heated to 685°C at a rate of 5°C/min and kept at this temperature for 15 min, and then cooled in the furnace.
- step (6) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- the raw materials for preparing Example 4 include component A and component B, wherein:
- Component A 15 parts of SiC powder with a D50 of about 70 ⁇ m, 15 parts of glass powder with a D50 of 10 ⁇ m and a melting point of 465°C, 25 parts of PS with a D50 of 50 ⁇ m, and 45 parts of zeolite with a D50 of 40 ⁇ m;
- component B Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% ethyl cellulose.
- the raw materials of component A are weighed and mixed to obtain a first mixed material.
- the first mixed material is placed in an oven and baked at 100° C. for 1 h to obtain a second mixed material.
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1.5 h to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 70°C, and adjust the pressure to 0.8 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
- step (5) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 250°C at a rate of 1°C/min and kept at this temperature for 1 h, then heated to 420°C at a rate of 1°C/min and kept at this temperature for 2 h, then heated to 670°C at a rate of 5°C/min and kept at this temperature for 30 min, and then cooled in the furnace.
- step (6) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- the raw materials for preparing Example 5 include component A and component B, wherein:
- Component A by mass, comprising 30 parts of silicon nitride powder with a D50 of about 60 ⁇ m, 20 parts of glass powder with a D50 of 10 ⁇ m and a melting point of 465°C, 35 parts of PP with a D50 of 50 ⁇ m, and 15 parts of perlite with a D50 of 35 ⁇ m;
- component B Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% EVA.
- the raw materials of component A are weighed and mixed to obtain a first mixed material.
- the first mixture is placed in an oven and baked at 100°C for 0.5 h to obtain a second mixture.
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.6 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
- step (6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 0.5°C/min, then heated to 100°C at a rate of 0.3°C/min, then heated to 230°C at a rate of 0.8°C/min and kept at this temperature for 1.5 h, then heated to 400°C at a rate of 0.8°C/min and kept at this temperature for 1 h, then heated to 650°C at a rate of 2°C/min and kept at this temperature for 60 min, and then cooled in the furnace.
- step (6) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- the preparation methods of Examples 6-8 are basically the same as those of Example 1, with the only difference being that the average particle size D50 of diatomaceous earth in the preparation raw materials is different. Specifically, the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 6 is 20 ⁇ m, the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 7 is 40 ⁇ m, and the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 8 is 50 ⁇ m.
- Example 9-11 The preparation methods of Examples 9-11 are basically the same as those of Example 1, with the only difference being that the mass fraction of diatomaceous earth in component A is different. Specifically, the mass fraction of diatomaceous earth in component A of Example 9 is 50 parts, the mass fraction of diatomaceous earth in component A of Example 10 is 40 parts, and the mass fraction of diatomaceous earth in component A of Example 11 is 30 parts.
- Example 12-14 The preparation methods of Examples 12-14 are basically the same as those of Example 1, with the only difference being that the mass of EVA in component B is different. Specifically, the mass of EVA in component B of Example 12 is 5% of the total mass of component A, the mass of EVA in component B of Example 13 is 4% of the total mass of component A, and the mass of EVA in component B of Example 14 is 1.5% of the total mass of component A.
- Example 15 The preparation method of Example 15 is basically the same as that of Example 1, with the only difference being that EVA in component B of Example 15 is replaced by PE of equal mass.
- Example 16 The raw material formula of Example 16 is the same as that of Example 1, and the only difference is that the preparation method is different.
- the preparation method of Example 16 is:
- step (3) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
- step (4) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.7 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine.
- the mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain the green billet after cooling.
- step (6) The green embryo obtained in step (5) was placed in a box-type air sintering furnace, first heated to 400°C at 1°C/min and kept at that temperature for 1.5 h, then heated to 670°C at 5°C/min and kept at that temperature for 30 min, and then cooled in the furnace.
- step (6) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
- Example 17 uses corundum powder to replace the quartz powder in Example 1
- Example 18 uses mullite powder to replace the quartz powder in Example 1.
- Other conditions and process steps are the same as those of Example 1.
- Comparative Example 1 The preparation methods of Comparative Example 1 and Example 1 are basically the same, the only difference is that the formula of component A is different. Specifically, the formula of component A in Comparative Example 1 is 52 parts of quartz powder with a D50 of about 50 ⁇ m, 28 parts of glass powder with a D50 of 5.5 ⁇ m and a melting point of 465°C, and 20 parts of wheat flour with a D50 of 32 ⁇ m.
- Comparative Example 2 The preparation method of Comparative Example 2 is consistent with that of Example 1, and the only difference is that the formula of component B is different. Specifically, the formula of component B of Comparative Example 2 is: based on the total mass of component A, it includes 50% paraffin, 1% oleic acid and 2% beeswax.
- Comparative Example 3 The preparation method of Comparative Example 3 is consistent with that of Example 1, except that the formula of component B is different. Specifically, the formula of component B of Comparative Example 3 is: based on the total mass of component A, it includes 50% paraffin, 1% oleic acid, 2% beeswax and 8% EVA.
- Comparative Example 4 The preparation method of Comparative Example 4 is consistent with that of Example 1, except that the average particle size D50 of the diatomaceous earth in component A is different. Specifically, the average particle size D50 of the diatomaceous earth in component A of Comparative Example 4 is 10 ⁇ m, and the mass, particle size and material of other raw material components are consistent with those of Example 1.
- Comparative Example 5 The preparation method of Comparative Example 5 is consistent with that of Example 1, except that the average particle size D50 of the diatomaceous earth in component A is different. Specifically, the average particle size D50 of the diatomaceous earth in component A of Comparative Example 5 is 70 ⁇ m. The mass, particle size and material of other raw material components are consistent with those of Example 1.
- the mass of each raw material component in component A in Table 1 is calculated by mass fraction, and the mass of component B is calculated by the percentage of the total mass of component A.
- Test method for liquid storage capacity and liquid absorption speed of porous ceramic atomizer core Test according to the following method:
- Bending strength test method Test according to the three-point bending strength test method specified in GB/T 4741-1999.
- the ceramic green body prepared in Examples 1-18 has higher strength after sintering, and at the same time forms micro-nanoscale liquid storage pores and micron-scale through-void structures, so that the porous ceramic atomization core has a larger liquid storage capacity and suction speed, thereby improving the liquid supply capacity of the porous ceramic atomization core and improving the taste experience of the atomization equipment.
- Example 1 when preparing the porous ceramic atomizer core, the diatomaceous earth component and the adhesive EVA component were removed respectively in Comparative Examples 1 and 2.
- the porous ceramic atomizer cores prepared in Comparative Examples 1 and 2 had lower liquid storage capacities of only 0.089 g and 0.093 g, and liquid absorption speeds of only 1.32 mg/s and 1.42 mg/s, respectively, which were far less than the liquid storage capacity and liquid absorption speed of Example 1.
- the oral sense evaluation results of the porous ceramic atomizer cores prepared in Comparative Examples 1 and 2 were also unqualified.
- the particle size of the diatomite in Comparative Example 4 is only 10 ⁇ m, and the liquid absorption rate of the ceramic atomizer core prepared therefrom is 1.21 mg/s, and the liquid storage capacity is 0.085 g; its particle size is small, and it is easy to be distributed in the gap formed by the accumulation of aggregate powder and glass powder, etc., which affects the permeability of the pores, thereby reducing the liquid absorption rate.
- the average particle size of the diatomite in Comparative Example 5 is 70 ⁇ m, and the bending strength of the ceramic atomizer core prepared therefrom is only 4.5 MPa, which is less than the bending strength of the ceramic atomizer core prepared in Example 1.
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Abstract
Description
相关申请Related Applications
本申请要求2023年11月23日提交中国专利局,申请号为202311589040X,名称为“多孔陶瓷材料及其制备方法、陶瓷雾化芯和雾化设备”的中国专利申请的优先权,在此将其全文引入作为参考。This application claims priority to the Chinese patent application filed with the China Patent Office on November 23, 2023, with application number 202311589040X, entitled “Porous ceramic materials and preparation methods thereof, ceramic atomization core and atomization equipment”, the entire text of which is hereby incorporated by reference.
本发明涉及雾化技术领域,特别是涉及一种多孔陶瓷材料及其制备方法、陶瓷雾化芯和雾化设备。The invention relates to the field of atomization technology, and in particular to a porous ceramic material and a preparation method thereof, a ceramic atomization core and an atomization device.
雾化芯是雾化设备的核心部件,由多孔储液介质及发热体两部分构成,主要有棉芯和陶瓷雾化芯两类。陶瓷雾化芯具有耐高温、可设计性强、可自动化生产及不易漏液等优点。此外,陶瓷为刚性材料,可减少或不使用结构件,以实现雾化芯的结构功能一体化,进而降低成本。因此,陶瓷雾化芯逐渐成为行业研究开发的热点。The atomizer core is the core component of the atomizer device. It consists of a porous liquid storage medium and a heating element. There are two main types: cotton core and ceramic atomizer core. Ceramic atomizer cores have the advantages of high temperature resistance, strong designability, automated production, and low leakage. In addition, ceramics are rigid materials, which can reduce or eliminate the use of structural parts to achieve structural and functional integration of the atomizer core, thereby reducing costs. Therefore, ceramic atomizer cores have gradually become a hot spot for industry research and development.
然而,目前的雾化设备中的陶瓷雾化芯存在储液量低和吸液速度慢的问题,降低用户的体验感。However, the ceramic atomizer core in the current atomizer equipment has the problems of low liquid storage capacity and slow liquid absorption speed, which reduces the user experience.
基于此,有必要提供一种储液量高、吸液速度快的多孔陶瓷材料及其制备方法、陶瓷雾化芯和雾化设备。Based on this, it is necessary to provide a porous ceramic material with high liquid storage capacity and fast liquid absorption speed and a preparation method thereof, a ceramic atomization core and an atomization device.
本申请第一方面,提供了一种多孔陶瓷材料,所述多孔陶瓷材料的制备原料包括:A组分和B组分;按质量份数计,所述A组分包括15份-40份的骨料粉、15份-35份的玻璃粉、15份-35份的造孔剂以及20份-50份的多孔无机非金属粉体;所述多孔无机非金属粉体的平均粒径D50为20μm-50μm;In a first aspect of the present application, a porous ceramic material is provided. The raw materials for preparing the porous ceramic material include: component A and component B; in terms of mass fractions, component A includes 15-40 parts of aggregate powder, 15-35 parts of glass powder, 15-35 parts of pore formers, and 20-50 parts of porous inorganic non-metallic powder; the average particle size D50 of the porous inorganic non-metallic powder is 20 μm-50 μm;
按A组分总质量的百分含量计,所述B组分包括40%-60%的石蜡、1.5%-6.5%的分散剂以及1.5%-5%的粘合剂。Calculated by percentage of the total mass of component A, component B includes 40%-60% paraffin wax, 1.5%-6.5% dispersant and 1.5%-5% binder.
上述多孔陶瓷材料通过采用特定组成及比例的A组分和B组分的制备原料,特别是引入本身含有孔隙结构的多孔无机非金属粉体组分以及造孔剂以提升上述多孔陶瓷材料的主体结构的孔隙,并进一步通过粘合剂作为保型组分起到固定和保持主体结构的孔隙的作用,并通过控制多孔无机非金属粉体组分的粒径可使多孔陶瓷材料具有足够的强度和提高孔隙的贯通性;如此可使制备出的多孔陶瓷材料不仅具有较高强度,还能形成微纳米级和微米级的孔隙结构及贯通孔隙,使得多孔陶瓷材料具有更大储液量和吸液速度,提高了多孔陶瓷材料的供液能力。The above-mentioned porous ceramic material is prepared by using raw materials of component A and component B with specific composition and proportion, especially introducing a porous inorganic non-metallic powder component containing a porous structure and a pore-forming agent to increase the porosity of the main structure of the above-mentioned porous ceramic material, and further using an adhesive as a shape-preserving component to fix and maintain the porosity of the main structure, and by controlling the particle size of the porous inorganic non-metallic powder component, the porous ceramic material can have sufficient strength and improve the permeability of the pores; in this way, the prepared porous ceramic material can not only have higher strength, but also form micro-nano and micron-level pore structures and through pores, so that the porous ceramic material has a larger liquid storage capacity and liquid absorption speed, thereby improving the liquid supply capacity of the porous ceramic material.
在一些实施例中,所述粘合剂选自热塑性树脂及乙基纤维素中的至少一种。In some embodiments, the binder is selected from at least one of a thermoplastic resin and ethyl cellulose.
在一些实施例中,所述热塑性树脂选自EVA及PE中的至少一种。In some embodiments, the thermoplastic resin is selected from at least one of EVA and PE.
在一些实施例中,所述粘合剂的质量占A组分总质量的2%-3%。In some embodiments, the weight of the binder accounts for 2%-3% of the total weight of component A.
在一些实施例中,所述多孔无机非金属粉体选自沸石、珍珠岩、麦饭石及硅藻土中的至少一种。In some embodiments, the porous inorganic non-metallic powder is selected from at least one of zeolite, perlite, medical stone and diatomaceous earth.
在一些实施例中,所述骨料粉选自SiC粉、氮化硅粉、刚玉粉、石英粉、莫来石及堇青石中的至少一种;和/或,所述骨料粉的平均粒径D50为30μm-100μm。In some embodiments, the aggregate powder is selected from at least one of SiC powder, silicon nitride powder, corundum powder, quartz powder, mullite and cordierite; and/or the average particle size D50 of the aggregate powder is 30 μm-100 μm.
在一些实施例中,所述造孔剂选自PMMA、PS、PP、木粉及小麦粉中的至少一种;和/或,所述造孔剂的平均粒径D50为20μm-80μm。In some embodiments, the pore-forming agent is selected from at least one of PMMA, PS, PP, wood flour and wheat flour; and/or the average particle size D50 of the pore-forming agent is 20 μm-80 μm.
在一些实施例中,所述玻璃粉的平均粒径D50为1μm-10μm;和/或,所述玻璃粉的始熔温度为450℃-550℃。In some embodiments, the average particle size D50 of the glass powder is 1 μm-10 μm; and/or the initial melting temperature of the glass powder is 450° C.-550° C.
在一些实施例中,所述分散剂选自蜂蜡和油酸中的至少一种。In some embodiments, the dispersant is selected from at least one of beeswax and oleic acid.
本发明第二方面,提供了上述多孔陶瓷材料的制备方法,所述制备方法包括如下步骤:In a second aspect of the present invention, a method for preparing the porous ceramic material is provided, the method comprising the following steps:
将所述制备原料混合密炼,得到混合浆料;Mixing and kneading the prepared raw materials to obtain a mixed slurry;
将所述混合浆料制成胚体,对胚体进行烧结处理,得到多孔陶瓷材料。The mixed slurry is made into an embryo body, and the embryo body is sintered to obtain a porous ceramic material.
在一些实施例中,将所述制备原料混合密炼的步骤包括:In some embodiments, the step of mixing and kneading the prepared raw materials comprises:
将B组分进行熔融,然后加入A组份进行混合,得到混合浆料。The B component is melted, and then added into the A component for mixing to obtain a mixed slurry.
在一些实施例中,所述混合密炼的温度为70℃-100℃;和/或,In some embodiments, the mixing and kneading temperature is 70° C.-100° C.; and/or,
所述混合密炼的转速为15r/min-50r/min;和/或,The rotating speed of the mixing and kneading is 15 r/min-50 r/min; and/or,
所述密炼时间为0.5-1.5h。The mixing time is 0.5-1.5h.
在一些实施例中,所述烧结处理包括先于200℃-250℃下保温1.5h-4h,然后于380℃-420℃下保温0.5h-3h,再于640℃-685℃下保温15min-60min。In some embodiments, the sintering process includes first keeping the temperature at 200°C-250°C for 1.5h-4h, then keeping the temperature at 380°C-420°C for 0.5h-3h, and then keeping the temperature at 640°C-685°C for 15min-60min.
在一些实施例中,升温至200℃-250℃的升温步骤包括:先以0.5℃/min-1.5℃/min升温至50℃-70℃,而后以0.3℃/min-1℃/min升温至80℃-110℃,再以0.8℃/min~1.5℃/min升温至200℃-250℃。In some embodiments, the heating step of heating to 200°C-250°C includes: first heating to 50°C-70°C at 0.5°C/min-1.5°C/min, then heating to 80°C-110°C at 0.3°C/min-1°C/min, and then heating to 200°C-250°C at 0.8°C/min~1.5°C/min.
本发明第三方面,提供了一种多孔陶瓷雾化芯,所述多孔陶瓷雾化芯包括上述多孔陶瓷材料。According to a third aspect of the present invention, a porous ceramic atomization core is provided, wherein the porous ceramic atomization core comprises the porous ceramic material mentioned above.
本发明第四方面,提供了一种雾化设备,所述雾化设备包括上述多孔陶瓷雾化芯。A fourth aspect of the present invention provides an atomization device, wherein the atomization device comprises the porous ceramic atomization core.
下面将结合本申请实施例,对本申请实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本申请一部分实施例,而不是全部的实施例。基于本申请中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本申请保护的范围。The following will be combined with the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used herein in the specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention. The term "and/or" used herein includes any and all combinations of one or more of the related listed items.
此外,术语“第一”、“第二”仅用于描述目的,而不能理解为指示或暗示相对重要性或者隐含指明所指示的技术特征的数量。由此,限定有“第一”、“第二”的特征可以明示或者隐含地包括至少一个该特征。在本发明的描述中,“多个”的含义是至少两个,例如两个,三个等,除非另有明确具体的限定。In addition, the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance or implicitly indicating the number of the indicated technical features. Therefore, the features defined as "first" and "second" may explicitly or implicitly include at least one of the features. In the description of the present invention, the meaning of "plurality" is at least two, such as two, three, etc., unless otherwise clearly and specifically defined.
在本发明一实施方式中,提供了一种多孔陶瓷材料,该多孔陶瓷材料的制备原料包括:A组分和B组分;按质量份数计,A组分包括15份-40份的骨料粉、15份-35份的玻璃粉、15份-35份的造孔剂以及20份-50份的多孔无机非金属粉体;多孔无机非金属粉体的平均粒径D50为20μm-50μm;In one embodiment of the present invention, a porous ceramic material is provided. The raw materials for preparing the porous ceramic material include: component A and component B; component A includes 15-40 parts of aggregate powder, 15-35 parts of glass powder, 15-35 parts of pore-forming agent and 20-50 parts of porous inorganic non-metallic powder by weight; the average particle size D50 of the porous inorganic non-metallic powder is 20 μm-50 μm;
按A组分总质量的百分含量计,B组分包括40%-60%的石蜡、1.5%-6.5%的分散剂以及1.5%-5%的粘合剂。换言之,在多孔陶瓷材料的制备原料中,以A组分总质量为基准,B组分中石蜡的质量百分含量为40%-60%,分散剂的质量百分含量为1.5%-6.5%,粘合剂的质量百分含量为1.5%-5%。Component B includes 40%-60% paraffin wax, 1.5%-6.5% dispersant and 1.5%-5% binder in terms of the total mass of component A. In other words, in the raw materials for preparing the porous ceramic material, based on the total mass of component A, the mass percentage of paraffin wax in component B is 40%-60%, the mass percentage of dispersant is 1.5%-6.5%, and the mass percentage of binder is 1.5%-5%.
上述多孔陶瓷材料通过采用特定组成及比例的A组分和B组分的制备原料,特别是引入本身含有孔隙结构的多孔无机非金属粉体组分以及造孔剂以提升上述多孔陶瓷材料的主体结构的孔隙,并进一步通过粘合剂作为保型组分起到固定和保持主体结构的孔隙的作用,并通过控制多孔无机非金属粉体组分的粒径可使多孔陶瓷材料具有足够的强度和提高孔隙的贯通性;如此可使制备出的多孔陶瓷材料不仅具有较高强度,还能形成微纳米级和微米级的孔隙结构及贯通孔隙,使得多孔陶瓷材料具有更大储液量和吸液速度,提高了多孔陶瓷材料的供液能力。The above-mentioned porous ceramic material is prepared by using raw materials of component A and component B with specific composition and proportion, especially introducing a porous inorganic non-metallic powder component containing a porous structure and a pore-forming agent to increase the porosity of the main structure of the above-mentioned porous ceramic material, and further using an adhesive as a shape-preserving component to fix and maintain the porosity of the main structure, and by controlling the particle size of the porous inorganic non-metallic powder component, the porous ceramic material can have sufficient strength and improve the permeability of the pores; in this way, the prepared porous ceramic material can not only have higher strength, but also form micro-nano and micron-level pore structures and through pores, so that the porous ceramic material has a larger liquid storage capacity and liquid absorption speed, thereby improving the liquid supply capacity of the porous ceramic material.
在一些实施例中,按重量份数计,A组分中上述多孔无机非金属粉体的含量为20份-50份。作为示例,A组分中上述多孔无机非金属粉体的含量可以为20份、25份、30份、35份、40份、45份、48份或50份。进一步地,A组分中上述多孔无机非金属粉体的重量份数可以为上述任意两个点值作为构成的范围值。优选地,A组分中上述多孔无机非金属粉体的含量为45份-50份。In some embodiments, the content of the porous inorganic non-metallic powder in component A is 20-50 parts by weight. As an example, the content of the porous inorganic non-metallic powder in component A can be 20 parts, 25 parts, 30 parts, 35 parts, 40 parts, 45 parts, 48 parts or 50 parts. Further, the weight percentage of the porous inorganic non-metallic powder in component A can be a range value composed of any two of the above point values. Preferably, the content of the porous inorganic non-metallic powder in component A is 45-50 parts.
在一些实施例中,上述多孔无机非金属粉体的平均粒径D50为20μm-50μm。作为示例,上述多孔无机非金属粉体的平均粒径D50可以为20μm、25μm、30μm、35μm、40μm、45μm或50μm。进一步地,上述多孔无机非金属粉体的平均粒径D50可为上述任意两个点值作为端值构成的范围。优选地,多孔无机非金属粉体的平均粒径D50为30μm-50μm。通过进一步控制多孔无机非金属粉体的平均粒径D50,避免多孔无机非金属粉体的粒径过大而降低多孔陶瓷的力学强度,同时也避免多孔无机非金属粉体的粒径过小导致其分布在上述骨料粉及玻璃粉之间堆积形成的空隙内,进而降低多孔陶瓷材料中的空隙的贯通孔性。In some embodiments, the average particle size D50 of the porous inorganic non-metallic powder is 20μm-50μm. As an example, the average particle size D50 of the porous inorganic non-metallic powder can be 20μm, 25μm, 30μm, 35μm, 40μm, 45μm or 50μm. Furthermore, the average particle size D50 of the porous inorganic non-metallic powder can be a range consisting of any two of the above point values as end values. Preferably, the average particle size D50 of the porous inorganic non-metallic powder is 30μm-50μm. By further controlling the average particle size D50 of the porous inorganic non-metallic powder, it is avoided that the particle size of the porous inorganic non-metallic powder is too large to reduce the mechanical strength of the porous ceramic, and it is also avoided that the particle size of the porous inorganic non-metallic powder is too small, resulting in its distribution in the gaps formed by the accumulation between the aggregate powder and the glass powder, thereby reducing the through porosity of the gaps in the porous ceramic material.
在一些实施例中,上述多孔无机非金属粉体可选自沸石、珍珠岩、麦饭石及硅藻土中的至少一种。进一步地,多孔无机非金属粉体为硅藻土。In some embodiments, the porous inorganic non-metallic powder can be selected from at least one of zeolite, perlite, medical stone and diatomaceous earth. Further, the porous inorganic non-metallic powder is diatomaceous earth.
在一些实施例中,粘合剂可选自热塑性树脂及乙基纤维素中的至少一种。In some embodiments, the binder may be selected from at least one of a thermoplastic resin and ethyl cellulose.
在一些实施例中,热塑性树脂的热分解温度为230℃-400℃。通过选择具有特定分解温度的热塑性树脂作为粘合剂,其分解温度高于石蜡,在烧结处理过程中的石蜡排出阶段,石蜡受热分解被排出而粘合剂未分解,使烧成后的瓷体不会发生因颗粒剧烈重排而导致的孔隙塌陷现象,从而起到保型的作用。In some embodiments, the thermal decomposition temperature of the thermoplastic resin is 230° C.-400° C. By selecting a thermoplastic resin with a specific decomposition temperature as a binder, whose decomposition temperature is higher than that of paraffin wax, during the paraffin discharge stage during the sintering process, the paraffin wax is decomposed by heat and discharged while the binder is not decomposed, so that the pore collapse phenomenon caused by the drastic rearrangement of particles will not occur in the fired porcelain body, thereby playing a role in maintaining the shape.
在一些实施例中,热塑性树脂可选自乙烯-醋酸乙烯共聚物(EVA)及聚乙烯(PE)中的至少一种。In some embodiments, the thermoplastic resin may be selected from at least one of ethylene vinyl acetate (EVA) and polyethylene (PE).
在一些实施例中,上述“1.5%-5%的粘合剂”是指粘合剂的质量占A组分总质量的百分比可以为1.5%、2%、2.5%、3%、3.5%、4%、4.5%或5%。进一步地,上述粘合剂的质量占A组分总质量的百分比可以为上述任意两个点值作为端值构成的范围。优选地,粘合剂的质量占A组分总质量的2%-3%。粘合剂的加入,还能在制备过程中使浆料不易发生颗粒沉降,使浆料具有更好的稳定性,通过优化掺入量使其具有适合热压铸成型的流变性能。In some embodiments, the above-mentioned "1.5%-5% adhesive" means that the mass of the adhesive may account for 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5% or 5% of the total mass of component A. Furthermore, the mass of the above-mentioned adhesive may account for a range of any two of the above-mentioned point values as end values. Preferably, the mass of the adhesive accounts for 2%-3% of the total mass of component A. The addition of the adhesive can also make the slurry less prone to particle sedimentation during the preparation process, make the slurry have better stability, and optimize the amount of admixture to make it have rheological properties suitable for hot die casting.
在一些实施例中,上述骨料粉可选自SiC粉、氮化硅粉、刚玉粉、石英粉、莫来石及堇青石中的至少一种。优选地,骨料粉可选自刚玉及莫来石中的至少一种。In some embodiments, the aggregate powder may be selected from at least one of SiC powder, silicon nitride powder, corundum powder, quartz powder, mullite and cordierite. Preferably, the aggregate powder may be selected from at least one of corundum and mullite.
在一些实施例中,骨料粉的平均粒径D50为30μm-100μm。作为示例,骨料粉的平均粒径D50可以为30μm、40μm、50μm、60μm、70μm、80μm、90μm或100μm。进一步地,上述骨粉的平均粒径D50可以为上述任意两个点值作为端值构成的范围。优选地,上述骨料粉的平均粒径D50为30μm-50μm。In some embodiments, the average particle size D50 of the aggregate powder is 30 μm-100 μm. As an example, the average particle size D50 of the aggregate powder can be 30 μm, 40 μm, 50 μm, 60 μm, 70 μm, 80 μm, 90 μm or 100 μm. Further, the average particle size D50 of the above-mentioned bone powder can be a range consisting of any two of the above-mentioned point values as end values. Preferably, the average particle size D50 of the above-mentioned aggregate powder is 30 μm-50 μm.
在一些实施例中,造孔剂可选自聚甲基丙烯酸甲酯(PMMA)、聚苯乙烯(PS)、聚丙烯(PP)、木粉及小麦粉中的至少一种。In some embodiments, the pore former may be selected from at least one of polymethyl methacrylate (PMMA), polystyrene (PS), polypropylene (PP), wood flour, and wheat flour.
在一些实施例中,造孔剂的平均粒径D50为20μm-80μm。作为示例,造孔剂的平均粒径D50可以为20μm、30μm、40μm、50μm、60μm、70μm或80μm。进一步地,上述造孔剂的平均粒径D50可以为上述任意两个点值作为端值构成的范围。优选地,造孔剂的平均粒径D50为30μm-50μm。In some embodiments, the average particle size D50 of the pore former is 20 μm-80 μm. As an example, the average particle size D50 of the pore former may be 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 70 μm or 80 μm. Further, the average particle size D50 of the pore former may be a range consisting of any two of the above point values as end values. Preferably, the average particle size D50 of the pore former is 30 μm-50 μm.
在一些实施例中,玻璃粉的始熔温度为450℃-550℃。In some embodiments, the glass powder has an initial melting temperature of 450°C-550°C.
在一些实施例中,玻璃粉的平均粒径D50为1μm-10μm。作为示例,玻璃粉的平均粒径D50可以为1μm、2μm、3μm、4μm、5μm、6μm、7μm、8μm、9μm或10μm。进一步地,上述玻璃粉的平均粒径D50可以为上述任意两个点值作为端值构成的范围。优选地,玻璃粉的平均粒径D50为2μm-5μm。In some embodiments, the average particle size D50 of the glass powder is 1 μm-10 μm. As an example, the average particle size D50 of the glass powder can be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm or 10 μm. Further, the average particle size D50 of the glass powder can be a range consisting of any two of the above point values as end values. Preferably, the average particle size D50 of the glass powder is 2 μm-5 μm.
在一些实施例中,分散剂可选自蜂蜡和油酸中的至少一种。In some embodiments, the dispersant may be selected from at least one of beeswax and oleic acid.
在一些实施例中,分散剂可选自蜂蜡和油酸。In some embodiments, the dispersant may be selected from beeswax and oleic acid.
在一些实施例中,上述蜂蜡的质量占A组分总质量的百分比为1%-5%。作为示例,蜂蜡的质量占A组分总质量的百分比可以为1%、2%、3%、4%或5%。进一步地,上述蜂蜡的质量占A组分总质量的百分比为可以为上述任意两个点值作为端值构成的范围。优选地,蜂蜡的质量占A组分总质量的百分比为2%-3.5%。In some embodiments, the mass of the beeswax accounts for 1%-5% of the total mass of component A. As an example, the mass of beeswax accounts for 1%, 2%, 3%, 4% or 5% of the total mass of component A. Further, the mass of beeswax accounts for a percentage of the total mass of component A that can be a range consisting of any two of the above point values as end values. Preferably, the mass of beeswax accounts for 2%-3.5% of the total mass of component A.
在一些实施例中,上述油酸的质量占A组分总质量的百分比为0.5%-1.5%。作为示例,油酸的质量占A组分总质量的百分比可以为0.5%、1%或1.5%。进一步地,上述油酸的质量占A组分总质量的百分比为可以为上述任意两个点值作为端值构成的范围。In some embodiments, the mass of the oleic acid accounts for 0.5%-1.5% of the total mass of component A. As an example, the mass of the oleic acid accounts for 0.5%, 1% or 1.5% of the total mass of component A. Further, the mass of the oleic acid accounts for a range of any two of the above point values as end values.
在本发明一实施方式中,提供了上述多孔陶瓷材料的制备方法,包括如下步骤S10-S20。In one embodiment of the present invention, a method for preparing the porous ceramic material is provided, comprising the following steps S10-S20.
S10、将上述制备原料混合密炼,得到混合浆料;S10, mixing and kneading the above-prepared raw materials to obtain a mixed slurry;
S10、将S10步骤中的混合浆料制成胚体,对胚体进行烧结处理,得到多孔陶瓷材料。S10, preparing a green body from the mixed slurry in step S10, and sintering the green body to obtain a porous ceramic material.
在一些实施例中,上述将制备原料混合密炼可以在密炼机中进行。In some embodiments, the mixing and kneading of the raw materials can be performed in an internal mixer.
在一些实施例中,上述密炼机的温度可以设置为70℃-100℃。In some embodiments, the temperature of the internal mixer can be set to 70°C-100°C.
在一些实施例中,上述密炼机的转速可以设置为15r/min-50r/min。In some embodiments, the rotation speed of the internal mixer can be set to 15r/min-50r/min.
在一些实施例中,混合密炼的时间为0.5h-1.5h。In some embodiments, the mixing and kneading time is 0.5 h-1.5 h.
在一些实施例中,上述将制备原料混合密炼的步骤包括:将B组分进行熔融,然后加入A组份进行混合,得到混合浆料。先将B组分进行熔融然后再加入A组分,有利于提高混料的均匀性以及效率。In some embodiments, the step of mixing and kneading the raw materials includes: melting component B, then adding component A to mix, to obtain a mixed slurry. Melting component B first and then adding component A is beneficial to improving the uniformity and efficiency of the mixing.
在一些实施例中,加入A组分进行混合之前,还包括对A组分原料进行混合,得到第一混合料。进一步地,还包括对第一混合料进行预热处理。In some embodiments, before adding component A for mixing, the raw materials of component A are mixed to obtain a first mixed material. Furthermore, the first mixed material is preheated.
在一些实施例中,上述预热处理步骤包括将第一混合料在80℃-120℃条件下烘烤0.5h-1.5h。In some embodiments, the preheating step includes baking the first mixed material at 80° C.-120° C. for 0.5 h-1.5 h.
在一些实施例中,上述将制备原料混合密炼的步骤包括:将A组分和B组分一同添加到密炼机中进行混合密炼。In some embodiments, the step of mixing and kneading the prepared raw materials includes: adding component A and component B together into an internal mixer for mixing and kneading.
在一些实施例中,将混合浆料制成胚体的方法包括步骤S21-S23。In some embodiments, the method of preparing an embryo body from the mixed slurry comprises steps S21 - S23 .
S21、将混合浆料置于热压铸机内;S21, placing the mixed slurry in a hot die casting machine;
S22、将装好发热片的模具放在压铸机出浆位置;S22, placing the mold with the heating plate installed at the slurry discharge position of the die-casting machine;
S23、将热压铸机内的混合浆料压入模具内,冷却后得到胚体。S23, pressing the mixed slurry in the hot die casting machine into a mold, and obtaining a blank after cooling.
在一些实施例中,上述热压铸机的温度可以设置为60℃-80℃。In some embodiments, the temperature of the hot die casting machine can be set to 60°C-80°C.
在一些实施例中,上述热压铸机的压力可以设置为0.5MPa-0.8MPa。In some embodiments, the pressure of the hot die casting machine can be set to 0.5 MPa-0.8 MPa.
在一些实施例中,烧结处理的步骤包括先于200℃-250℃下保温1.5h-4h,然后于380℃-420℃下保温0.5h-3h,再于640℃-685℃下保温15min-60min。In some embodiments, the sintering step includes first keeping the temperature at 200°C-250°C for 1.5h-4h, then keeping the temperature at 380°C-420°C for 0.5h-3h, and then keeping the temperature at 640°C-685°C for 15min-60min.
在一些实施例中,升温至200℃-250℃的升温步骤包括:先以0.5℃/min-1.5℃/min升温至50℃-70℃,而后以0.3℃/min-1℃/min升温至80℃-110℃,再以0.8℃/min~1.5℃/min升温至200℃-250℃。In some embodiments, the heating step of heating to 200°C-250°C includes: first heating to 50°C-70°C at 0.5°C/min-1.5°C/min, then heating to 80°C-110°C at 0.3°C/min-1°C/min, and then heating to 200°C-250°C at 0.8°C/min~1.5°C/min.
在一些实施例中,烧结处理的步骤包括先于220℃-230℃下保温1.5h-4h,然后以0.8~1.5℃/min升温至400℃-420℃并保温0.5h-3h,再以2℃/min-6℃/min升温至640℃-685℃并保温15min-60min;然后随炉冷却。通过烧结制度的优化使得有机物逐级缓慢排出,从而使陶瓷颗粒不发生剧烈重排,防止陶瓷中空隙的塌陷。In some embodiments, the sintering process includes first keeping the temperature at 220℃-230℃ for 1.5h-4h, then heating to 400℃-420℃ at 0.8~1.5℃/min and keeping the temperature for 0.5h-3h, then heating to 640℃-685℃ at 2℃/min-6℃/min and keeping the temperature for 15min-60min; then cooling with the furnace. By optimizing the sintering system, the organic matter is discharged slowly step by step, so that the ceramic particles do not rearrange violently, and the collapse of the voids in the ceramic is prevented.
在一些实施例中,对胚体进行烧结处理后,还包括对烧结产物进行超声清洗并烘干,得到多孔陶瓷材料。In some embodiments, after the embryo body is sintered, the sintered product is ultrasonically cleaned and dried to obtain a porous ceramic material.
在一些实施例中,上述多孔陶瓷材料可应用于吸附液体的载体,其应用产品包括但不限于雾化芯。In some embodiments, the porous ceramic material can be applied to a carrier for adsorbing liquid, and its application products include but are not limited to atomizer cores.
在本申请一实施方式中,提供了一种多孔陶瓷雾化芯,该多孔陶瓷雾化芯包括上述多孔陶瓷材料。In one embodiment of the present application, a porous ceramic atomization core is provided, and the porous ceramic atomization core includes the above-mentioned porous ceramic material.
在本申请一实施方式中,提供了一种雾化设备,该雾化设备包括上述多孔陶瓷雾化芯。In one embodiment of the present application, an atomization device is provided, which includes the above-mentioned porous ceramic atomization core.
在一些实施例中,雾化设备包括但不限于电子烟。In some embodiments, the atomizing device includes but is not limited to an electronic cigarette.
为了使本申请的目的、技术方案及优点更加简洁明了,本申请用以下具体实施例进行说明,但本申请绝非仅限于这些实施例。以下所描述的实施例仅为本申请较好的实施例,可用于描述本申请,不能理解为对本申请的范围的限制。应当指出的是,凡在本申请的精神和原则之内所做的任何修改、等同替换和改进等,均应包含在本申请的保护范围之内。In order to make the purpose, technical solutions and advantages of the present application more concise and clear, the present application is described with the following specific embodiments, but the present application is by no means limited to these embodiments. The embodiments described below are only preferred embodiments of the present application and can be used to describe the present application, and cannot be understood as limiting the scope of the present application. It should be pointed out that any modifications, equivalent substitutions and improvements made within the spirit and principles of the present application should be included in the protection scope of the present application.
为了更好地说明本申请,下面结合实施例对本申请内容作进一步说明。以下为具体实施例。In order to better illustrate the present application, the present application is further described below in conjunction with the embodiments. The following are specific embodiments.
实施例1Example 1
实施例1的制备原料包括A组分和B组分,其中,The raw materials for preparation of Example 1 include component A and component B, wherein:
A组分:按质量份数计,包括27.5份的D50约为50μm的石英粉、28份的D50为5.5μm且始熔温度为465℃的玻璃粉、20份的D50为32μm的小麦粉以及24.5份的D50为28.5μm的硅藻土;Component A: by mass, comprising 27.5 parts of quartz powder with a D50 of about 50 μm, 28 parts of glass powder with a D50 of 5.5 μm and a melting point of 465°C, 20 parts of wheat flour with a D50 of 32 μm, and 24.5 parts of diatomaceous earth with a D50 of 28.5 μm;
以A组分总质量为基准,B组分包括50%的石蜡、1%的油酸、2%的蜂蜡和2.5%的EVA。Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% EVA.
(1)按上述配方称量A组分原料,并进行混合,得到第一混合料。(1) The raw materials of component A are weighed according to the above formula and mixed to obtain a first mixed material.
(2)将第一混合料放入烘箱内,在100℃条件下烘烤1h后,得到第二混合料。(2) The first mixed material is placed in an oven and baked at 100° C. for 1 h to obtain a second mixed material.
(3)按上述配方称量B组分原料,并将B组分原料倒入密炼机内进行融化。将密炼机的温度设定为90℃,搅拌转速设为30r/min。(3) Weigh the raw materials of component B according to the above formula, and pour the raw materials of component B into an internal mixer to melt. Set the temperature of the internal mixer to 90°C and the stirring speed to 30 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼1h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至75℃,压力调至0.7MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.7 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain the green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以1℃/min的速率升温至60℃,而后以0.5℃/min的速率升温至100℃,再以1℃/min升温至230℃,并保温3h,而后以1℃/min升温至400℃并保温1.5h,再以5℃/min升温至670℃并保温30min,而后随炉冷却。(6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 230°C at a rate of 1°C/min and kept at this temperature for 3 h, then heated to 400°C at a rate of 1°C/min and kept at this temperature for 1.5 h, then heated to 670°C at a rate of 5°C/min and kept at this temperature for 30 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例2Example 2
实施例2的制备原料包括A组分和B组分,其中,The raw materials for preparing Example 2 include component A and component B, wherein:
A组分:按质量份数计,包括15份的D50约为32μm的石英粉、34份的D50为2.1μm且始熔温度为465℃的玻璃粉、16份的D50为20μm的小麦粉以及35份的D50为20μm的硅藻土;Component A: by mass, comprising 15 parts of quartz powder with a D50 of about 32 μm, 34 parts of glass powder with a D50 of 2.1 μm and a melting point of 465°C, 16 parts of wheat flour with a D50 of 20 μm, and 35 parts of diatomaceous earth with a D50 of 20 μm;
以A组分总质量为基准,B组分包括60%的石蜡,1.5%的油酸,4.5%的蜂蜡和5.0%的EVA。Based on the total mass of component A, component B includes 60% paraffin, 1.5% oleic acid, 4.5% beeswax and 5.0% EVA.
(1)按上述配方称量A组分原料,进行混合,得到第一混合料。(1) The raw materials of component A are weighed according to the above formula and mixed to obtain a first mixed material.
(2)将第一混合料放入烘箱内,在100℃条件下烘烤0.5h后,得到第二混合料。(2) The first mixed material is placed in an oven and baked at 100° C. for 0.5 h to obtain a second mixed material.
(3)按上述配方称量B组分原料,并将B组分原料倒入密炼机内进行融化。将密炼机的温度设定为75℃,搅拌转速设为45r/min。(3) Weigh the raw materials of component B according to the above formula, and pour the raw materials of component B into an internal mixer to melt. Set the temperature of the internal mixer to 75°C and the stirring speed to 45 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼0.5h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 0.5 h to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至60℃,压力调至0.8MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 60°C, and adjust the pressure to 0.8 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以0.5℃/min的速率升温至60℃,而后以0.3℃/min的速率升温至100℃,再以0.8℃/min升温至230℃,并保温1.5h,而后以0.8℃/min升温至400℃并保温1h,再以2℃/min升温至640℃并保温60min,而后随炉冷却。(6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 0.5°C/min, then heated to 100°C at a rate of 0.3°C/min, then heated to 230°C at a rate of 0.8°C/min and kept at this temperature for 1.5 h, then heated to 400°C at a rate of 0.8°C/min and kept at this temperature for 1 h, then heated to 640°C at a rate of 2°C/min and kept at this temperature for 60 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例3Example 3
实施例3的制备原料包括A组分和B组分,其中,The raw materials for preparation of Example 3 include component A and component B, wherein:
A组分:按质量份数计,包括39份的D50约为98μm的石英粉、15份的D50为5.5μm且始熔温度为465℃的玻璃粉、31份的D50为76μm的PMMA以及20份的D50为48.5μm的麦饭石;Component A: by mass, including 39 parts of quartz powder with a D50 of about 98 μm, 15 parts of glass powder with a D50 of 5.5 μm and a melting point of 465°C, 31 parts of PMMA with a D50 of 76 μm, and 20 parts of medical stone with a D50 of 48.5 μm;
以A组分总质量为基准,B组分包括40%的石蜡,1%的油酸和1%的蜂蜡和2%的EVA。Based on the total mass of component A, component B includes 40% paraffin, 1% oleic acid, 1% beeswax and 2% EVA.
(1)按上述配方城称量A组分原料,并进行混合,得到第一混合料。(1) According to the above formula, the raw materials of component A are weighed and mixed to obtain a first mixed material.
(2)将第一混合料放入烘箱内,在100℃条件下烘烤1.5h后,得到第二混合料;(2) placing the first mixed material into an oven and baking it at 100° C. for 1.5 h to obtain a second mixed material;
(3)按上述配方称量B组分原料,并将B组分原料倒入密炼机内进行融化。将密炼机的温度设定为90℃,搅拌转速设为15r/min。(3) Weigh the raw materials of component B according to the above formula, and pour the raw materials of component B into an internal mixer to melt. Set the temperature of the internal mixer to 90°C and the stirring speed to 15 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼1.5h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1.5 hours to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至80℃,压力调至0.5MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 80°C, and adjust the pressure to 0.5 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以1℃/min的速率升温至60℃,而后以0.5℃/min的速率升温至100℃,再以1℃/min升温至230℃,并保温2.5h,而后以1℃/min升温至400℃并保温1.5h,再以5℃/min升温至685℃并保温15min,而后随炉冷却。(6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 230°C at a rate of 1°C/min and kept at this temperature for 2.5 h, then heated to 400°C at a rate of 1°C/min and kept at this temperature for 1.5 h, then heated to 685°C at a rate of 5°C/min and kept at this temperature for 15 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例4Example 4
实施例4的制备原料包括A组分和B组分,其中,The raw materials for preparing Example 4 include component A and component B, wherein:
A组分:包括15份的D50约为70μm的SiC粉、15份的D50为10μm且始熔温度为465℃的玻璃粉、25份的D50为50μm的PS以及45份的D50为40μm的沸石;Component A: 15 parts of SiC powder with a D50 of about 70 μm, 15 parts of glass powder with a D50 of 10 μm and a melting point of 465°C, 25 parts of PS with a D50 of 50 μm, and 45 parts of zeolite with a D50 of 40 μm;
以A组分总质量为基准,B组分包括50%的石蜡、1%的油酸、2%的蜂蜡和2.5%的乙基纤维素。Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% ethyl cellulose.
(1)按上述配方城称量A组分原料,进行混合,得到第一混合料。(1) According to the above formula, the raw materials of component A are weighed and mixed to obtain a first mixed material.
(2)将第一混合料放入烘箱内,在100℃条件下烘烤1h后,得到第二混合料。(2) The first mixed material is placed in an oven and baked at 100° C. for 1 h to obtain a second mixed material.
(3)按上述配方城称量B组分原料,并将B组分原料倒入密炼机内进行融化。将密炼机的温度设定为85℃,搅拌转速设为30 r/min。(3) Weigh the raw materials of component B according to the above formula, and pour the raw materials of component B into an internal mixer to melt. Set the temperature of the internal mixer to 85°C and the stirring speed to 30 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼1.5 h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1.5 h to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至70℃,压力调至0.8MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 70°C, and adjust the pressure to 0.8 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以1℃/min的速率升温至60℃,而后以0.5℃/min的速率升温至100℃,再以1℃/min升温至250℃,并保温1h,而后以1℃/min升温至420℃并保温2h,再以5℃/min升温至670℃并保温30min,而后随炉冷却。(6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 1°C/min, then heated to 100°C at a rate of 0.5°C/min, then heated to 250°C at a rate of 1°C/min and kept at this temperature for 1 h, then heated to 420°C at a rate of 1°C/min and kept at this temperature for 2 h, then heated to 670°C at a rate of 5°C/min and kept at this temperature for 30 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body cooled in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例5Example 5
实施例5的制备原料包括A组分和B组分,其中,The raw materials for preparing Example 5 include component A and component B, wherein:
A组分:按质量份数计,包括30份的D50约为60μm的氮化硅粉、20份的D50为10μm且始熔温度为465℃的玻璃粉、35份的D50为50μm的PP以及15份的D50为35μm的珍珠岩;Component A: by mass, comprising 30 parts of silicon nitride powder with a D50 of about 60 μm, 20 parts of glass powder with a D50 of 10 μm and a melting point of 465°C, 35 parts of PP with a D50 of 50 μm, and 15 parts of perlite with a D50 of 35 μm;
以A组分总质量为基准,B组分包括50%的石蜡、1%的油酸、2%的蜂蜡和2.5%的EVA。Based on the total mass of component A, component B includes 50% paraffin, 1% oleic acid, 2% beeswax and 2.5% EVA.
(1)按上述配方城称量A组分原料,并进行混合,得到第一混合料。(1) According to the above formula, the raw materials of component A are weighed and mixed to obtain a first mixed material.
(2)将第一混合料放入烘箱内,在100℃条件下烘烤0.5 h后,得到第二混合料。(2) The first mixture is placed in an oven and baked at 100°C for 0.5 h to obtain a second mixture.
(3)按上述配方称量B组分原料,并将B组分原料倒入密炼机内进行融化。将密炼机的温度设定为85℃,搅拌转速设为20 r/min。(3) Weigh the raw materials of component B according to the above formula, and pour the raw materials of component B into an internal mixer to melt. Set the temperature of the internal mixer to 85°C and the stirring speed to 20 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼1h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至75℃,压力调至0.6MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.6 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain a green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以0.5℃/min的速率升温至60℃,而后以0.3℃/min的速率升温至100℃,再以0.8℃/min升温至230℃,并保温1.5h,而后以0.8℃/min升温至400℃并保温1h,再以2℃/min升温至650℃并保温60min,而后随炉冷却。(6) The green embryo obtained in step (5) is placed in a box-type air sintering furnace and first heated to 60°C at a rate of 0.5°C/min, then heated to 100°C at a rate of 0.3°C/min, then heated to 230°C at a rate of 0.8°C/min and kept at this temperature for 1.5 h, then heated to 400°C at a rate of 0.8°C/min and kept at this temperature for 1 h, then heated to 650°C at a rate of 2°C/min and kept at this temperature for 60 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例6-8与实施例1的制备方法基本一致,区别仅在于,制备原料中硅藻土的平均粒径D50的值不同,具体地,实施例6的制备原料中硅藻土的平均粒径D50为20μm,实施例7的制备原料中硅藻土的平均粒径D50为40μm,实施例8的制备原料中硅藻土的平均平均粒径D50为50μm。The preparation methods of Examples 6-8 are basically the same as those of Example 1, with the only difference being that the average particle size D50 of diatomaceous earth in the preparation raw materials is different. Specifically, the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 6 is 20 μm, the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 7 is 40 μm, and the average particle size D50 of diatomaceous earth in the preparation raw materials of Example 8 is 50 μm.
实施例9-11与实施例1的制备方法基本一致,区别仅在于,A组分中硅藻土的质量份数不同,具体地,实施例9的A组分硅藻土的质量份数为50份,实施例10的A组分中硅藻土的质量份数为40份,实施例11的A组分中硅藻土的质量份数为30份。The preparation methods of Examples 9-11 are basically the same as those of Example 1, with the only difference being that the mass fraction of diatomaceous earth in component A is different. Specifically, the mass fraction of diatomaceous earth in component A of Example 9 is 50 parts, the mass fraction of diatomaceous earth in component A of Example 10 is 40 parts, and the mass fraction of diatomaceous earth in component A of Example 11 is 30 parts.
实施例12-14与实施例1的制备方法基本一致,区别仅在于,B组分中EVA的质量不同,具体地,实施例12的B组分中EVA的质量为A组分总质量的5%,实施例13的B组分中EVA的质量为A组分总质量的4%,实施例14的B组分中EVA的质量为A组分总质量的1.5%。The preparation methods of Examples 12-14 are basically the same as those of Example 1, with the only difference being that the mass of EVA in component B is different. Specifically, the mass of EVA in component B of Example 12 is 5% of the total mass of component A, the mass of EVA in component B of Example 13 is 4% of the total mass of component A, and the mass of EVA in component B of Example 14 is 1.5% of the total mass of component A.
实施例15与实施例1的制备方法基本一致,区别仅在于,实施例15的B组分中将EVA替换成了等质量的PE。The preparation method of Example 15 is basically the same as that of Example 1, with the only difference being that EVA in component B of Example 15 is replaced by PE of equal mass.
实施例16Example 16
实施例16与实施例1的原料配方一致,区别仅在于制备方法有所不同。实施例16的制备方法为:The raw material formula of Example 16 is the same as that of Example 1, and the only difference is that the preparation method is different. The preparation method of Example 16 is:
(1)按上述配方称量A组分、B组分原料,并将A、B组分原料均倒入密炼机内进行熔化。将密炼机的温度设定为90℃,搅拌转速设为30r/min。(1) Weigh the raw materials of component A and component B according to the above formula, and pour the raw materials of component A and component B into an internal mixer for melting. Set the temperature of the internal mixer to 90°C and the stirring speed to 30 r/min.
(4)待步骤(3)中的物料全部熔化后,将步骤(2)中的第二混合料缓慢倒入密炼机内,密炼1h后得到混合浆料。(4) After all the materials in step (3) are melted, slowly pour the second mixed material in step (2) into an internal mixer and mix for 1 hour to obtain a mixed slurry.
(5)将步骤(4)中的混合浆料倒入热压铸机内,热压铸机温度调至75℃,压力调至0.7MPa。将装好发热片的模具倒放在压铸机出浆位置,模具呈外径4.8mm、内径1.5mm、高度12mm的环形圆柱,启动开关,将浆料压入模具内,冷却后得到生坯。(5) Pour the mixed slurry in step (4) into a hot die casting machine, adjust the temperature of the hot die casting machine to 75°C, and adjust the pressure to 0.7 MPa. Place the mold with the heating plate installed upside down at the slurry outlet position of the die casting machine. The mold is an annular cylinder with an outer diameter of 4.8 mm, an inner diameter of 1.5 mm, and a height of 12 mm. Start the switch to press the slurry into the mold, and obtain the green billet after cooling.
(6)步骤(5)得到的生胚置于箱式空气烧结炉中,先以1℃/min升温至400℃并保温1.5h,再以5℃/min升温至670℃并保温30min,而后随炉冷却。(6) The green embryo obtained in step (5) was placed in a box-type air sintering furnace, first heated to 400°C at 1°C/min and kept at that temperature for 1.5 h, then heated to 670°C at 5°C/min and kept at that temperature for 30 min, and then cooled in the furnace.
(7)步骤(6)中冷却后的陶瓷体置于超声清洗机内清洗并烘干,得到多孔陶瓷雾化芯。(7) The ceramic body after cooling in step (6) is placed in an ultrasonic cleaning machine for cleaning and drying to obtain a porous ceramic atomizing core.
实施例17-18与实施例1的制备方法基本一致,区别仅在于,骨料粉的材质不同,具体地,实施例17采用刚玉粉替代实施例1中的石英粉,实施例18采用莫来石粉替代实施例1中的石英粉,其他条件及工艺步骤与实施例1一致。The preparation methods of Examples 17-18 are basically the same as those of Example 1, with the only difference being that the materials of the aggregate powder are different. Specifically, Example 17 uses corundum powder to replace the quartz powder in Example 1, and Example 18 uses mullite powder to replace the quartz powder in Example 1. Other conditions and process steps are the same as those of Example 1.
对比例1Comparative Example 1
对比例1与实施例1的制备方法基本一致,区别仅在于,A组分的配方不同,具体地,对比例1中A组分的配方为52份的D50约为50μm的石英粉、28份的D50为5.5μm且始熔温度为465℃的玻璃粉和20份的D50为32μm的小麦粉。The preparation methods of Comparative Example 1 and Example 1 are basically the same, the only difference is that the formula of component A is different. Specifically, the formula of component A in Comparative Example 1 is 52 parts of quartz powder with a D50 of about 50 μm, 28 parts of glass powder with a D50 of 5.5 μm and a melting point of 465°C, and 20 parts of wheat flour with a D50 of 32 μm.
对比例2Comparative Example 2
对比例2与实施例1的制备方法一致,区别仅在于,B组分的配方不同,具体地,对比例2的B组分的配方为:以A组分总质量为基准,包括50%的石蜡、1%的油酸和2%的蜂蜡。The preparation method of Comparative Example 2 is consistent with that of Example 1, and the only difference is that the formula of component B is different. Specifically, the formula of component B of Comparative Example 2 is: based on the total mass of component A, it includes 50% paraffin, 1% oleic acid and 2% beeswax.
对比例3Comparative Example 3
对比例3与实施例1的制备方法一致,区别仅在于,B组分的配方不同,具体地,对比例3的B组分的配方为:以A组分总质量为基准,包括50%的石蜡、1%的油酸、2%的蜂蜡和8%的EVA。The preparation method of Comparative Example 3 is consistent with that of Example 1, except that the formula of component B is different. Specifically, the formula of component B of Comparative Example 3 is: based on the total mass of component A, it includes 50% paraffin, 1% oleic acid, 2% beeswax and 8% EVA.
对比例4Comparative Example 4
对比例4与实施例1的制备方法一致,区别仅在于,A组分中硅藻土的平均粒径D50的值不同,具体地,对比例4的A组分中硅藻土的平均粒径D50为10μm,其他原料组分的质量、粒径及材质与实施例1一致。The preparation method of Comparative Example 4 is consistent with that of Example 1, except that the average particle size D50 of the diatomaceous earth in component A is different. Specifically, the average particle size D50 of the diatomaceous earth in component A of Comparative Example 4 is 10 μm, and the mass, particle size and material of other raw material components are consistent with those of Example 1.
对比例5Comparative Example 5
对比例5与实施例1的制备方法一致,区别仅在于,A组分中硅藻土的平均粒径D50的值不同,具体地,对比例5的A组分中的硅藻土的平均粒径D50为70μm。其他原料组分的质量、粒径及材质与实施例1一致。The preparation method of Comparative Example 5 is consistent with that of Example 1, except that the average particle size D50 of the diatomaceous earth in component A is different. Specifically, the average particle size D50 of the diatomaceous earth in component A of Comparative Example 5 is 70 μm. The mass, particle size and material of other raw material components are consistent with those of Example 1.
各实施例及对比例中的原料组分配方如表1所示。The raw material component formulas in each embodiment and comparative example are shown in Table 1.
表1Table 1
续表1Table 1
注:表1中A组分中各原料组分的质量按质量份数计,B组分中的质量按A组分总质量的百分含量计。Note: The mass of each raw material component in component A in Table 1 is calculated by mass fraction, and the mass of component B is calculated by the percentage of the total mass of component A.
性能测试方法Performance Testing Methods
多孔陶瓷雾化芯的储液量及吸液速度测试方法:按照如下方法测试:Test method for liquid storage capacity and liquid absorption speed of porous ceramic atomizer core: Test according to the following method:
1、将上述标准规格的陶瓷雾化芯称重,质量为m 1; 1. Weigh the ceramic atomizer core of the above standard specifications, the mass is m 1 ;
2、将称重后的陶瓷雾化芯放入浸满丙三醇/丙二醇质量比为5/5的混合液的海绵上,当陶瓷刚接触海绵时开始计时为t 1,陶瓷在吸液过程中颜色会发生变化,当整个陶瓷都变颜色后,即为吸满液体的状态,当完全吸满液体时计时为t 2,并将完全吸满液体的陶瓷雾化芯取出称重为m 2; 2. Place the weighed ceramic atomizer core on a sponge soaked in a mixture of propylene glycol and propylene glycol in a mass ratio of 5/5. When the ceramic just touches the sponge, the time is t 1 . The color of the ceramic will change during the liquid absorption process. When the entire ceramic changes color, it is fully absorbed by the liquid. When it is completely absorbed by the liquid, the time is t 2 . Take out the ceramic atomizer core that is fully absorbed by the liquid and weigh it as m 2 .
3、根据公式计算陶瓷雾化芯的储液量及吸液速度,储液量的计算公式为为δm=m 2-m 1;吸液速度为:v=(m 2-m 1)/(t 2-t 1)。 3. Calculate the liquid storage capacity and liquid absorption speed of the ceramic atomizer core according to the formula. The calculation formula for the liquid storage capacity is δm=m 2 -m 1 ; the liquid absorption speed is: v=(m 2 -m 1 )/(t 2 -t 1 ).
抗弯强度测试方法:按照GB/T 4741-1999规定的三点抗弯强度测试方法进行测试。Bending strength test method: Test according to the three-point bending strength test method specified in GB/T 4741-1999.
各实施例及对比例的性能测试结果如表2所示:The performance test results of each embodiment and comparative example are shown in Table 2:
表2Table 2
从表2数据可以看出,实施例1-18通过引入多孔结构的无机非金属粉体组分以及粘合剂保型,并与其他组分之间通过合理搭配,制备出的陶瓷生胚经烧结后具有较高的强度,同时形成了微纳米级储液孔和微米级贯通的空隙结构,使得多孔陶瓷雾化芯具有更大储液量和吸也速度,提高了多孔陶瓷雾化芯的供液能力,改善了雾化设备的口感体验。It can be seen from the data in Table 2 that, by introducing porous inorganic non-metallic powder components and adhesives to maintain the shape, and by reasonably matching with other components, the ceramic green body prepared in Examples 1-18 has higher strength after sintering, and at the same time forms micro-nanoscale liquid storage pores and micron-scale through-void structures, so that the porous ceramic atomization core has a larger liquid storage capacity and suction speed, thereby improving the liquid supply capacity of the porous ceramic atomization core and improving the taste experience of the atomization equipment.
相比于实施例1,对比例1和对比例2在制备多孔陶瓷雾化芯时,分别去掉了硅藻土组分和粘合剂EVA组分,对比例1和对比例2制备的多孔陶瓷雾化芯储液量较低仅有0.089g和0.093g,吸液速度也分别只达到1.32mg/s和1.42mg/s,远不及实施例1的储液量和吸液速度;对比例1和对比例2制备的多孔陶瓷雾化芯的口感测评结果也不合格。Compared with Example 1, when preparing the porous ceramic atomizer core, the diatomaceous earth component and the adhesive EVA component were removed respectively in Comparative Examples 1 and 2. The porous ceramic atomizer cores prepared in Comparative Examples 1 and 2 had lower liquid storage capacities of only 0.089 g and 0.093 g, and liquid absorption speeds of only 1.32 mg/s and 1.42 mg/s, respectively, which were far less than the liquid storage capacity and liquid absorption speed of Example 1. The oral sense evaluation results of the porous ceramic atomizer cores prepared in Comparative Examples 1 and 2 were also unqualified.
对比例3中添加大粘合剂EVA组分含量过多,导致浆料粘度过大,成型困难。对比例4中的硅藻土的粒径仅有10μm,其制备的陶瓷雾化芯的吸液速度为1.21mg/s,储液量0.085g;其粒径较小,容易分布在骨料粉及玻璃粉等堆积形成的间隙内,影响孔的贯通性,进而使得吸液速度下降。对比例5中的硅藻土的平均粒径为70μm,其制备的陶瓷雾化芯的抗弯强度仅有4.5MPa,不及实施例1制备的陶瓷雾化芯的抗弯强度。In Comparative Example 3, too much EVA component of the large binder is added, resulting in excessive viscosity of the slurry and difficulty in molding. The particle size of the diatomite in Comparative Example 4 is only 10 μm, and the liquid absorption rate of the ceramic atomizer core prepared therefrom is 1.21 mg/s, and the liquid storage capacity is 0.085 g; its particle size is small, and it is easy to be distributed in the gap formed by the accumulation of aggregate powder and glass powder, etc., which affects the permeability of the pores, thereby reducing the liquid absorption rate. The average particle size of the diatomite in Comparative Example 5 is 70 μm, and the bending strength of the ceramic atomizer core prepared therefrom is only 4.5 MPa, which is less than the bending strength of the ceramic atomizer core prepared in Example 1.
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
以上所述实施例仅表达了本申请的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对申请专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本申请构思的前提下,还可以做出若干变形和改进,这些都属于本申请的保护范围。因此,本申请专利的保护范围应以所附权利要求为准。The above-described embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be construed as limiting the scope of the patent application. It should be pointed out that, for a person of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the patent application shall be subject to the attached claims.
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