CN111423247A - Porous ceramic, preparation method and heating element thereof - Google Patents
Porous ceramic, preparation method and heating element thereof Download PDFInfo
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- 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
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Abstract
The invention relates to a porous ceramic, a preparation method and a heating body thereof, wherein the preparation method of the porous ceramic comprises the following steps: mixing the raw materials and a pore-forming agent and then forming to obtain a blank body; according to the mass percentage, the raw material comprises 15-50% of Si3N4Powder and 50 to 85 percent of Si powder; and sintering the green body in a nitrogen atmosphere to obtain the porous ceramic. The prepared porous ceramic has a fibrous tissue structure and a structure similar to that of the cotton core, and can improve the taste; meanwhile, the porous ceramic with the fiber structure has the strength of ceramic and is easy to prepareThe fixed shape is convenient for assembly and automatic production.
Description
Technical Field
The invention relates to the technical field of electronic cigarettes, in particular to porous ceramic, a preparation method and a heating body thereof.
Background
The electronic cigarette is also known as a virtual cigarette and an electronic atomizer. The electronic cigarette is used as a substitute for cigarette products and is mainly used for quitting smoking. Electronic cigarettes have an appearance and taste similar to cigarettes, but generally do not contain other harmful components such as tar, aerosols, etc. in cigarettes.
The electronic cigarette mainly comprises an atomizer and a power supply assembly. The atomizer is used as a core device for generating atomizing gas by the electronic cigarette, and the atomizing effect of the atomizer determines the quality and the taste of the smoke. At present, an atomizer of an electronic cigarette is generally formed by embedding a heating body and an atomizing core. The heating body is connected with the power supply and is conducted to generate heat during suction. The atomizing core mainly comprises a cotton core and a porous ceramic core which both belong to porous structures and play roles in guiding oil and dispersing tobacco tar. After the tobacco tar is absorbed by the atomizing core, the tobacco tar is heated by the heating body to generate smoke sol, and the atomization effect is realized.
The cotton core is adopted as the atomization core of the electronic cigarette, and atomized smoke has good mouthfeel and is also the atomization core which is widely used initially. So far, the design of a novel electronic cigarette heating element still pursues the taste similar to that brought by cotton core atomization. However, when the atomization temperature is too high, the cotton core is liable to develop a scorched smell during use. In addition, the size of the atomization core manufactured by adopting the cotton core is difficult to accurately control, and the product performance and the taste of the same batch of products are easy to be different; meanwhile, the atomizer is difficult to realize automation in manufacturing or assembling, and the labor cost is high. The porous ceramic atomizing core is an atomizing core which is rapidly developed and widely applied in recent years, and ceramic has certain strength and the function of a supporting structure, so that the ceramic atomizing core has the function of a structural element during assembly; and the consistency of the ceramics is better, the performance is stable, the ceramic is suitable for large-scale batch production, and the automation is easy to realize. In addition, the ceramic also has multiple functions of sound, light, electricity, magnetism and the like, and can endow the atomizing core with multiple optimized functions through reasonable design. However, the mouthfeel brought by the ceramic atomizing core at present still cannot be compared with that of a cotton core.
Disclosure of Invention
Based on the above, there is a need for a method for preparing porous ceramic, which has a fiber structure and a certain strength, and can be used in an electronic cigarette atomizer to atomize electronic cigarette smoke by being inlaid or combined with a heating wire/heating net.
A preparation method of porous ceramics comprises the following steps:
mixing the raw materials and a pore-forming agent and then forming to obtain a blank body; according to the mass percentage, the raw material comprises 15-50% of Si3N4Powder and 50 to 85 percent of Si powder;
and sintering the green body to obtain the porous ceramic.
At present, porous ceramic pores used by the atomizing core are distributed in a compact ceramic framework. The reason that the cotton core has better taste is that the cotton core is formed by mutually intersecting cotton fibers, has a very rich pore structure, and the contact between the cotton fibers and tobacco tar is very sufficient, so that the oil guiding and atomizing effects are better. The prepared porous ceramic has a fiber tissue structure and a structure similar to that of the cotton core, so that the oil guiding capacity and the atomizing capacity of the porous ceramic are improved, and the mouthfeel is improved; meanwhile, the porous ceramic with the fiber structure has the strength of ceramic, is easy to prepare into a specific shape, and is convenient for assembly and automatic production. Inlay or combine with heater/heating network and be applied to electron smog spinning disk atomiser.
In one embodiment, the mass ratio of the pore-forming agent to the raw material is 1: 7-1: 3.
In one embodiment, the pore-forming agent is at least one of carbon powder, graphite powder, starch, polymethyl methacrylate and polystyrene spheres.
In one embodiment, the step of press-forming the raw material and the pore-forming agent further includes adding at least one of a catalyst and a sintering aid to the raw material and the pore-forming agent, and press-forming.
In one embodiment, the catalyst is at least one of a metal, a metal oxide, an intermetallic compound, a rare earth element, and a rare earth compound.
In one embodiment, the catalyst is Fe2O3At least one of Fe, Fe-Si and Ni.
In one embodiment, the sintering aid is MgO and Y2O3At least one of (1).
In one embodiment, the mass ratio of the catalyst to the raw material is 0.1-3%, and the mass ratio of the sintering aid to the raw material is 1-5%.
In one embodiment, the compression molding method is one of compression molding, injection molding and casting molding.
In one embodiment, the green body sintering process is performed in a flowing nitrogen atmosphere with a purity higher than 99.99%.
In one embodiment, the sintering treatment temperature is 1300-1800 ℃ and the time is 0.5-3 hours.
The invention provides a porous ceramic prepared by the preparation method of the porous ceramic.
Further, a heating element is provided, which comprises the porous ceramic and a heating line arranged on the porous ceramic.
Experiments prove that the preparation method of the porous ceramic comprises the steps of mixing Si powder and Si3N4The powder is used as a raw material and is formed into a specific shape under the conditions, the raw material powder is reacted under the specific reaction conditions, then the glue is discharged, and the porous ceramic obtained by sintering has high porosity, can meet the requirement of preparing the atomizing core from the porous ceramic and also has high compressive strength. The prepared porous ceramic has a fiber tissue structure and a structure similar to that of the cotton core, so that the oil guiding capacity and the atomizing capacity of the porous ceramic are improved, and the mouthfeel is improved; meanwhile, the porous ceramic of the fiber structure has the strength of ceramicAnd the material is easy to prepare into a specific shape, and is convenient to assemble and automatically produce. Inlay or combine with heater/heating network and be applied to electron smog spinning disk atomiser. The fiber diameter of the prepared porous ceramic is 0-50 microns; the porosity of the ceramic is 30-90%, the pore diameter is 0-100 microns, and the strength is not less than 20 MPa.
Drawings
FIG. 1 is an electron microscope image of a porous ceramic having a porous fiber structure prepared in example 1;
FIG. 2 is an electron microscope image of a porous ceramic having a porous fiber structure prepared in example 2;
FIG. 3 is an electron microscope image of a porous ceramic having a porous fiber structure prepared in example 3;
FIG. 4 is a schematic view of a structure of a heat generating body according to an embodiment.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
A method of preparing a porous ceramic according to an embodiment includes the steps of:
s11: mixing the raw materials and a pore-forming agent and then forming to obtain a blank body;
wherein the raw material comprises 15-50% of Si by mass percentage3N4Powder, 50-85% of Si powder;
Si3N4is a high-temperature ceramic material, has high hardness and melting point, and can be used in a wide temperature rangeThe silicon nitride in the enclosure is a high-strength hard ceramic with certain thermal conductivity, low thermal expansion coefficient and higher elastic modulus. Unlike general ceramics, it has high fracture toughness. These properties combine to provide excellent thermal shock resistance, ability to withstand high structural loads at high temperatures and excellent wear resistance. The raw material containing Si in the form of particles3N4Is beneficial to the nitridation of Si powder to form Si3N4。
The porous fiber ceramic adopts Si as a raw material, and Si easily forms gaseous Si (g) and SiO (g) in the reaction process of the Si in a nitrogen atmosphere, and the residual Si(s), Si (g) and SiO (g) in the system and N2(g) In the reaction process, a gas-gas reaction process or a gas-solid reaction process exists, and whisker-shaped or fibrous Si is easily formed3N4Substance of Si3N4The material has high porosity, small pore diameter and high strength.
In one embodiment, the mass ratio of the pore-forming agent to the raw material is 1: 7-1: 3; the pore-forming agent with the proportion can ensure that the porous ceramic has proper strength and controllable porosity. It will be appreciated that the amount of pore former may be controlled depending on the amount of tobacco tar required to be stored in the atomizing core and the amount of smoke required during use.
The pore-forming agent may be a pore-forming agent commonly used in the art, such as carbon, organic polymers, starch, and the like.
Further, the pore-forming agent is at least one of carbon powder, graphite powder, starch, polymethyl methacrylate and polystyrene spheres. The pore-forming agent adopts organic polymer, the particle size distribution of the organic polymer is better controlled, and the particle size distribution of the starch is larger.
Specifically, the step of press forming the raw material and the pore-forming agent comprises the step of press forming at least one of the catalyst and the sintering aid with the raw material and the pore-forming agent. The reaction can be promoted by adding a catalyst or a sintering aid.
Further, the catalyst is at least one of metal, metal oxide, intermetallic compound, rare earth element and rare earth compound; in a specific example, the catalystCan be Fe2O3At least one of Fe, Fe-Si and Ni.
The sintering aid can enable the porous ceramic obtained after sintering to have higher compressive strength and reduce the sintering temperature. The sintering aid can be, but is not limited to, MgO, Y2O3At least one of (1).
The mass ratio of the catalyst to the raw material is 0.1-3%; the mass ratio of the sintering aid to the raw material is 1-5%. The catalyst and the sintering aid in the proportion can ensure that the obtained porous ceramic has proper strength and controllable porosity. It can be understood that the contents of the catalyst and the sintering aid can be controlled according to actual requirements.
The above-mentioned forming method can adopt the forming method commonly used in the art, including but not limited to compression forming, injection forming, casting forming and other forming methods, to design the product shape according to the structure requirement of the electronic cigarette.
S120: and sintering the green body in a nitrogen atmosphere to obtain the porous ceramic.
Specifically, the step of sintering the green body in the nitrogen atmosphere comprises sintering the green body for 0.5 to 3 hours at the temperature of 1300 to 1800 ℃ in the flowing nitrogen atmosphere with the purity higher than 99.99 percent.
In a specific example, the sintering temperature may be 1300 ℃, 1400 ℃, 1500 ℃, 1600 ℃, 1700 ℃ or 1800 ℃.
The preparation method of the porous ceramic has at least the following advantages:
experiments prove that the preparation method of the porous ceramic comprises the steps of mixing Si powder and Si3N4The powder is used as a raw material and is formed into a specific shape under the conditions, the raw material powder is reacted under the specific reaction conditions, then the glue is discharged, and the porous ceramic obtained by sintering has high porosity, can meet the requirement of preparing the atomizing core from the porous ceramic and also has high compressive strength. The prepared porous ceramic has a fiber tissue structure and a structure similar to that of a cotton core, and the oil guiding capacity of the porous ceramic is improvedThe atomization capability is realized, so that the mouthfeel is improved; meanwhile, the porous ceramic with the fiber structure has the strength of ceramic, is easy to prepare into a specific shape, and is convenient for assembly and automatic production. Inlay or combine with heater/heating network and be applied to electron smog spinning disk atomiser.
The fiber diameter of the prepared porous ceramic is 0-50 microns; the porosity of the ceramic is 30-90%, the pore diameter is 0-100 microns, and the strength is not less than 20 MPa.
The porous ceramic of an embodiment is prepared by the preparation method of the porous ceramic, so that the porous ceramic has high porosity, can meet the requirement of preparing the atomizing core from the porous ceramic, and has high compressive strength.
As shown in fig. 4, a heat generating body 100 according to an embodiment generates heat and atomizes a target liquid in the heat generating body 100. In the present embodiment, the heating element 100 is applied to an electronic cigarette, and is used to atomize tobacco tar of the electronic cigarette. In other embodiments, the heating element 100 may be applied to atomizing other target liquids, including, but not limited to, nicotine-containing electronic cigarette tar, nicotine-free electronic cigarette tar, daily use aroma type atomized liquid, vehicle-mounted aroma type atomized liquid, medical atomized liquid, and the like.
Specifically, the heating element 100 includes the porous ceramic 110 of the above embodiment and the heating line 120 provided on the porous ceramic 110.
The following are specific examples (the following examples, unless otherwise specified, contain no other components not specifically indicated except for unavoidable impurities):
example 1
The preparation process of the porous ceramic of the present example is as follows:
1) weighing raw materials, a catalyst and a pore-forming agent according to the table 1, wherein in the table 1, the content of each substance in the raw materials is the mass percentage;
2) pressing under 10MPa to obtain flat plate, embedding heating element during molding, and sintering the molded blank at 1400 deg.C in nitrogen atmosphere to obtain porous ceramic. An electron microscope image of the porous ceramic obtained in example 1 is shown in FIG. 1, and it can be seen from FIG. 1 that this example obtained a porous ceramic having a fine fiber structure with a large aspect ratio. The fiber diameter is less than 1 micron.
TABLE 1
Example 2
The preparation process of the porous ceramic of the present example is as follows:
1) weighing raw materials, a catalyst and a pore-forming agent according to the table 1;
2) pressing under 20MPa to obtain flat plate, embedding heating net, and sintering at 1300 deg.C in nitrogen atmosphere to obtain porous ceramic. An electron microscope image of the sintered porous ceramic is shown in fig. 2, and it can be seen from fig. 2 that the fiber with large bending degree is taken as a main structure, and the diameter of the fiber is 2-5 microns.
Example 3
The preparation process of the porous ceramic of the present example is as follows:
1) weighing raw materials, a catalyst and a pore-forming agent according to the table 1;
2) pressing under 15MPa to obtain flat plate, embedding heating net during pressing, and sintering the formed blank at 1700 deg.C in nitrogen atmosphere to obtain porous ceramic. An electron microscope image of the sintered porous ceramic is shown in fig. 3, and as can be seen from fig. 3, the sintered material takes fibers as a main structure, and spherical particles of 0-1 micron are distributed on the edges of the fibers. And the fiber diameter is 2-5 microns.
Example 4
The preparation process of the porous ceramic of the present example is as follows:
1) weighing raw materials, a catalyst and a pore-forming agent according to the table 1;
2) pressing under 15MPa to obtain flat plate, embedding heating net during pressing, and sintering the formed blank at 1800 deg.C in flowing nitrogen atmosphere to obtain porous ceramic.
The porous ceramics of examples 5 to 6 were prepared in the same manner as in example 1 except for the difference in the catalyst, pore-forming agent and sintering aid.
Example 7
The porous ceramic of this example was prepared by substantially the same procedure as in example 1 except that the sintering temperature was 1200 ℃.
Example 8
The porous ceramic of this example was prepared by substantially the same procedure as in example 1 except that the sintering temperature was 1900 ℃.
Comparative example 1
The porous ceramic of comparative example 1 was prepared in substantially the same manner as in example 1 except that the composition of the raw material was different, and in comparative example 1, the raw material was composed of 10% by mass of Si3N4Powder and 90% Si powder.
Comparative example 2
The porous ceramic of comparative example 2 was prepared in substantially the same manner as in example 1 except that the composition of the raw material was different from that of example 1, and in comparative example 1, the raw material was composed of 55% by mass of Si3N4Powder and 45% Si powder.
Comparative example 3
The porous ceramic of comparative example 3 was prepared by substantially the same procedure as in example 1, except that the composition of the raw material was different, and in comparative example 1, only Si powder was used as the raw material in terms of mass percentage content.
And (3) testing:
the compressive strength of the porous ceramics of examples 1-6 and comparative examples 1-3 was tested according to the GB1964-1980 test method for compressive strength of porous ceramics; respectively testing the porosity of the porous ceramics of the examples 1-5 and the comparative examples 1-3 according to GB/T1966-1996 porous ceramic apparent porosity and capacity test methods; the pore sizes of the porous ceramics of examples 1 to 5 and comparative examples 1 to 3 were respectively tested according to the GB/T32361-2015 bubble point method, and the smaller the pore size distribution interval, the more uniform the pore structure. The compressive strength, porosity and pore size of the porous ceramics of examples 1 to 5 and comparative examples 1 to 3 are shown in table 2.
TABLE 2
As can be seen from Table 2, the fiber porous ceramic cores (examples 1-3) prepared by the method have appropriate strength, are convenient to assemble as structural members, and are more convenient to assemble than cotton cores; the micro-pore channel structure is similar to that of a cotton core, and the smoke quantity generated during suction is larger. Compared with cotton fiber, the porous ceramic material has stable performance in a high-temperature working state, is not easy to generate scorched flavor and burnt flavor, has good taste, and has better reduction degree of aroma and sweet taste than a non-fiber structure.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (13)
1. The preparation method of the porous ceramic is characterized by comprising the following steps:
mixing the raw materials and a pore-forming agent and then forming to obtain a blank body; according to the mass percentage, the raw material comprises 15-50% of Si3N4Powder and 50 to 85 percent of Si powder;
and sintering the green body in a nitrogen atmosphere to obtain the porous ceramic.
2. The preparation method according to claim 1, wherein the mass ratio of the pore-forming agent to the raw material is 1:7 to 1: 3.
3. The preparation method of claim 2, wherein the pore-forming agent is at least one of carbon powder, graphite powder, starch, polymethyl methacrylate and polystyrene spheres.
4. The method of claim 1, wherein the step of press-forming the raw material and the pore-forming agent comprises press-forming at least one of the catalyst and the sintering aid with the raw material and the pore-forming agent.
5. The method according to claim 4, wherein the catalyst is at least one of a metal, a metal oxide, an intermetallic compound, a rare earth element, and a rare earth compound.
6. The method of claim 5, wherein the catalyst is Fe2O3At least one of Fe, Fe-Si and Ni.
7. The method according to claim 4, wherein the sintering aid is MgO or Y2O3At least one of (1).
8. The production method according to claim 4, wherein the mass ratio of the catalyst to the raw material is 0.1 to 3%, and the mass ratio of the sintering aid to the raw material is 1 to 5%.
9. The production method according to claim 1, wherein the molding method employs one of press molding, injection molding, and tape casting.
10. The method according to claim 1, wherein the green body sintering process is performed under a flowing nitrogen atmosphere having a purity of more than 99.99%.
11. The method according to claim 10, wherein the sintering treatment is carried out at a temperature of 1300 ℃ to 1800 ℃ for 0.5 hour to 3 hours.
12. A porous ceramic produced by the method for producing a porous ceramic according to any one of claims 1 to 11.
13. A heat-generating body characterized by comprising the porous ceramic according to claim 12 and a heat-generating line provided on the porous ceramic.
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