CN115959923A - Porous ceramic, atomizing core, atomizing device and preparation method of porous ceramic - Google Patents
Porous ceramic, atomizing core, atomizing device and preparation method of porous ceramic Download PDFInfo
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Abstract
The invention provides a porous ceramic, an atomizing core, an atomizing device and a preparation method of the porous ceramic, wherein the structural strength and the porosity of the porous ceramic are improved and enhanced by regulating and controlling the size of an inorganic pore-forming agent and improving the formula of raw materials on the basis of the proportioning of aggregate powder and the inorganic pore-forming agent and the cooperative regulation and control of particle sizes of the aggregate powder and the inorganic pore-forming agent and by the dry pressing and the cooperative regulation and control of sintering process conditions, so that the porous ceramic has higher porosity and stronger compressive strength, and the problems of small liquid storage amount, long sintering time, poorer structural strength caused by high porosity and the like of the porous ceramic for preparing the atomizing core can be effectively solved. In addition, the porous ceramic provided by the embodiment of the invention has the advantages of high porosity, short sintering time, high structural strength, low carbon and environmental protection. In addition, the preparation method of the porous ceramic provided by the embodiment of the invention has the advantages of simple process flow, easiness in operation and low cost.
Description
Technical Field
The invention belongs to the technical field of atomization, and particularly relates to an atomization core, porous ceramic, an atomization core, an atomization device and a preparation method of the porous ceramic.
Background
In the current preparation process of porous ceramics, the mixed particles containing diatomite, pore-forming agent and sintering aid are generally dry-pressed into a dry-pressed green body, and then the formed dry-pressed green body is sintered to form the porous ceramics. In the sintering stage, the porosity and compressive strength of the porous ceramic are greatly reduced, and simultaneously, the added organic phase substances and the residual graphite powder can irreversibly discharge carbon dioxide when being combusted at high temperature. Therefore, the porous ceramic prepared by the existing porous ceramic preparation process has the problems of low porosity, long sintering time, poor structural strength caused by porosity and the like, and also can obviously increase carbon emission, thereby being not beneficial to sustainable development in the field of manufacturing porous ceramic atomizing cores.
Disclosure of Invention
Based on the above problems in the prior art, an object of an embodiment of the present invention is to provide a porous ceramic, so as to solve the problems that after an atomizing core is made of the porous ceramic in the prior art, the porosity is low, the sintering time is long, the structural strength is poor, and carbon dioxide is emitted under high-temperature combustion.
In order to realize the purpose, the invention adopts the technical scheme that: providing an atomization core, wherein the porous ceramic comprises the following raw materials in percentage by mass:
30-45% of aggregate powder;
30-60% of inorganic pore-forming agent;
10 to 25 percent of binder;
wherein, the inorganic pore-forming agent is at least one of ammonium chloride, sodium chloride, potassium sulfate and ammonium sulfate.
Optionally, the aggregate powder is at least one of diatomite, boron nitride and alumina.
Optionally, the binder includes glass frit, and the softening point of the glass frit is 800 to 900 ℃.
Optionally, the particle size of the inorganic pore former is 56 to 145 μm.
Based on the above problems in the prior art, it is another object of the embodiments of the present invention to provide an atomizing core having the porous ceramic provided in any one of the above aspects.
In order to achieve the purpose, the invention adopts the technical scheme that: an atomizing core is provided, which comprises the porous ceramic provided by any scheme.
Based on the above problems in the prior art, it is a further object of the embodiments of the present invention to provide an atomizing device having a porous ceramic or atomizing core provided in any of the above aspects.
In order to achieve the purpose, the invention adopts the technical scheme that: an atomization device is provided, which comprises the porous ceramic or the atomization core provided by any scheme.
Compared with the prior art, one or more technical schemes in the embodiment of the invention have at least one of the following beneficial effects:
according to the atomizing core, the atomizer and the atomizing device in the embodiment of the invention, through regulation and control of the size of the inorganic pore-forming agent and improvement of the formula of the raw materials, on the basis of the ratio of the aggregate powder and the inorganic pore-forming agent and the cooperative regulation and control of the particle sizes of the aggregate powder and the inorganic pore-forming agent, and through dry pressing molding and the cooperative regulation and control of sintering process conditions, the structural strength and porosity of the porous ceramic are improved and improved, the porous ceramic has higher porosity and stronger compressive strength, and the problems of small liquid storage amount, long sintering time, poor structural strength caused by high porosity and the like of the porous ceramic for preparing the atomizing core can be effectively solved. In addition, the porous ceramic provided by the embodiment of the invention has the advantages of high porosity, short sintering time, high structural strength, low carbon, environmental friendliness and low cost, and can reduce carbon dioxide emission under high-temperature combustion.
Based on the above problems in the prior art, it is a fourth object of the embodiments of the present invention to provide a method for preparing an atomizing core.
In order to realize the purpose, the invention adopts the technical scheme that: provided is a preparation method of an atomizing core, which comprises the following steps:
step S01: respectively weighing aggregate powder, an inorganic pore-forming agent and a binder according to the components contained in the porous ceramic, and mixing the raw materials to obtain a premix;
step S02: dry-pressing the premix to obtain a dry-pressed green body;
step S03: and sintering the dry-pressed green body, and cooling to obtain a porous ceramic finished product.
Optionally, the step S01 further includes the following steps: grinding the inorganic pore-forming agent, wherein the particle size of the ground inorganic pore-forming agent is 56-145 mu m; and then putting the binder and the ground inorganic pore-forming agent into a tank mill for mixing, then adding the aggregate powder into the tank mill, and uniformly mixing to obtain the premix.
Optionally, in the step S02, the pressure for dry pressing the premix is 10 to 30MPa.
Optionally, in the step S03, sintering the dry-pressed green body includes at least one of a temperature programmed sintering method, a rapid temperature-programmed sintering method, and a multi-stage rapid temperature-programmed sintering method;
the temperature programmed sintering mode comprises the following steps: placing the dry pressing blank body on a high temperature resistant ceramic flat plate, placing the dry pressing blank body in a central heating area of a sintering furnace, heating to 900-1200 ℃ at a heating rate of 5-10 ℃/min in an air atmosphere, and preserving heat for 4-40 min;
the rapid heating sintering mode comprises the following steps: firstly, heating a sintering furnace in an air atmosphere at a heating rate of 5-10 ℃/min to enable the sintering furnace to reach a preset temperature of 900-1200 ℃; then placing the dry pressing green body on a high-temperature resistant ceramic flat plate, quickly pushing the dry pressing green body into the sintering furnace, and preserving heat for 4-40 min to carry out quick high-temperature sintering treatment on the dry pressing green body;
the multi-stage rapid temperature rise sintering mode comprises the following steps: respectively presetting a low-temperature area and a high-temperature area in a double-temperature-area tube furnace, heating the low-temperature area to a preset temperature of 600-700 ℃ at a heating rate of 5-10 ℃/min, and heating the high-temperature area to a preset temperature of 900-1200 ℃ at a heating rate of 5-10 ℃/min; and placing the dry pressing blank on a high-temperature resistant ceramic flat plate, pushing the dry pressing blank into a low-temperature area from a room-temperature area for sintering and heat preservation for 4-10 min, then pushing the dry pressing blank into the high-temperature area from the low-temperature area for sintering and heat preservation for 4-10 min, and then pulling the dry pressing blank back to the low-temperature area from the high-temperature area for sintering and heat preservation for 4-10 min.
Compared with the prior art, one or more technical schemes in the embodiment of the invention have at least one of the following beneficial effects:
according to the preparation method of the atomizing core, the size of the inorganic pore-forming agent is regulated and controlled, the cooperative regulation and control of the particle sizes of the aggregate powder and the inorganic pore-forming agent are combined, the structural strength and the porosity of the porous ceramic are improved and improved through dry pressing and the cooperative regulation and control of sintering process conditions on the basis of the ratio of the aggregate powder to the inorganic pore-forming agent and the cooperative regulation and control of the particle sizes of the aggregate powder and the inorganic pore-forming agent, the porous ceramic has high porosity and high compressive strength, and the problems that the porous ceramic for preparing the atomizing core is small in liquid storage amount, long in sintering time, poor in structural strength and the like caused by high porosity can be effectively solved. In addition, the porous ceramic provided by the embodiment of the invention has the advantages of high porosity, short sintering time, high structural strength, capability of reducing carbon dioxide emission under high-temperature combustion, low carbon and environmental protection. In addition, the preparation method of the porous ceramic provided by the embodiment of the invention has the advantages of simple process flow, easiness in operation and low cost.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 is a photograph of a dry pressed blank before it is unsintered in example 4 of the present invention;
FIG. 2 is a photograph of a dry-pressed blank before being unsintered in comparative example 1 of the present invention;
FIG. 3 is a side photograph of a porous ceramic after sintering for molding in example 4 of the present invention;
FIG. 4 is a side photograph of the porous ceramic of comparative example 1 of the present invention after sintering for molding;
FIG. 5 is a photograph of the surface of the porous ceramic after sintering and forming in example 4 of the present invention;
FIG. 6 is a photograph of the surface of the porous ceramic in comparative example 1 of the present invention after sintering for molding.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides the porous ceramic which has high porosity, short sintering time and high structural strength and reduces the emission of carbon dioxide under high-temperature combustion. The porous ceramic provided by the embodiment of the invention comprises the following raw materials in percentage by mass:
30-45% of aggregate powder;
30-60% of inorganic pore-forming agent;
10 to 25 percent of binder;
wherein the inorganic pore-forming agent is at least one of ammonium chloride, sodium chloride, potassium sulfate and ammonium sulfate. In the embodiment of the invention, the inorganic pore-forming agent is preferably ammonium chloride. Ammonium chloride is preferably selected as an inorganic pore-forming agent, on one hand, the ammonium chloride does not contain toxic elements and carbon elements, carbon emission can be effectively avoided, and the use safety of the porous ceramic is improved, on the other hand, the ammonium chloride can be fully decomposed into ammonia gas and hydrogen chloride gas at 340 ℃, and powdery ammonium chloride is regenerated on the inner wall of the cold end of a quartz tube of a sintering furnace, so that the direct recycling of the inorganic pore-forming agent is facilitated. In addition, the particle size range of the inorganic pore-forming agent is controlled to be 56-145 mu m, so that the porous ceramic has higher porosity and the surface of the porous ceramic is ensured to be smooth. When the particle size of the inorganic pore-forming agent is less than 56 μm, it is advantageous to enhance the structural strength of the porous ceramic, but not advantageous to form pores in the porous ceramic, resulting in a decrease in the porosity of the porous ceramic. When the particle size of the inorganic pore-forming agent is larger than 145 μm, although pore-forming is favorably performed on the porous ceramic and the porosity of the porous ceramic is improved, the defects of unevenness, cracks and the like of the prepared porous surface and adverse effect on the structural strength of the porous ceramic are caused by the overlarge particle size of the inorganic pore-forming agent. The aggregate powder is at least one of diatomite, boron nitride and alumina, the raw material purity of the aggregate powder is more than 99.9%, and the particle size of the aggregate powder is 30-60 mu m. When the particle size of the aggregate powder is less than 30 μm, the packing density among particles is increased, so that the compressive strength of the porous ceramic is enhanced, but the porosity and the pore diameter of the porous ceramic are seriously reduced, so that the particle size of the aggregate powder is not less than 30 μm. When the particle size of the aggregate powder is larger than 60 micrometers, the particle packing density is reduced, so that the pore diameter of the porous ceramic is increased, the porosity of the porous ceramic is improved, and along with the reduction of the particle packing density, a ceramic green body is easy to shrink and deform in a later sintering process, so that the pore shrinkage of the porous ceramic is reduced and even closed, the porosity of the porous ceramic is reduced, the pore diameter of the porous ceramic is reduced, the compressive strength of the porous ceramic is reduced, and the particle size of the aggregate powder is not larger than 60 micrometers. The binder may include, but is not limited to, glass frit having a softening point of 800 to 900 c, a particle size of 5 to 10 μm, and a softening temperature range of 800 to 900 c, mainly because the sintering temperature of the ceramic after printing the electrode is 900 c, and the actual sintering temperature is above 900 c in order to match the sintering temperature of the electrode and prevent secondary shrinkage, which is advantageous for the glass frit to form a mobile phase, so that the softening temperature of the selected glass frit is less than 900 c, and on the other hand, if the softening temperature is too low, a liquid phase is formed prematurely, which is disadvantageous for sintering, so that a glass frit having a narrower softening range, for example, 800 to 900 c, is selected.
According to the porous ceramic provided by the embodiment of the invention, by regulating and controlling the size of the inorganic pore-forming agent and improving the formula of the raw materials, on the basis of the proportioning of the aggregate powder and the inorganic pore-forming agent and the cooperative regulation and control of the particle sizes of the aggregate powder and the inorganic pore-forming agent, the structural strength and the porosity of the porous ceramic are improved and increased by dry pressing and combining with the cooperative regulation and control of sintering process conditions, the porous ceramic has higher porosity and stronger compressive strength, and the problems of small liquid storage amount, long sintering time, poorer structural strength caused by high porosity and the like of the porous ceramic for preparing the atomizing core can be effectively solved. In addition, the porous ceramic provided by the embodiment of the invention has the advantages of high porosity, short sintering time, high structural strength, low carbon, environmental friendliness and low cost, and can reduce carbon dioxide emission under high-temperature combustion.
The embodiment of the invention also provides an atomizing core, which comprises the porous ceramic provided by any one of the embodiments. Since the atomizing core has all the technical features of the porous ceramic provided in any one of the above embodiments, it has the same technical effects as the porous ceramic described above.
The embodiment of the invention also provides an atomization device which comprises the porous ceramic or the atomization core provided by any one of the embodiments. Since the atomization device has all the technical characteristics of the porous ceramic or the atomization core provided in any one of the above embodiments, the atomization device has the same technical effects as the porous ceramic or the atomization core.
The embodiment of the invention also provides a preparation method of the porous ceramic.
In some embodiments, the preparation method of the porous ceramic provided by the embodiments of the present invention includes the following steps:
step S01: respectively weighing aggregate powder, an inorganic pore-forming agent and a binder according to the components contained in the porous ceramic in any embodiment, and mixing the raw materials to obtain a premix;
step S02: dry pressing the premix to obtain a dry pressed green body;
step S03: and sintering the dry-pressed green body, and cooling to obtain a porous ceramic finished product.
Specifically, in step S01, the components contained in the porous material of the embodiment of the present invention are as above, and the porous material contains the following components in parts by mass:
30-45% of aggregate powder;
30-60% of inorganic pore-forming agent;
10 to 25 percent of binder;
wherein the inorganic pore-forming agent is at least one of ammonium chloride, sodium chloride, potassium sulfate and ammonium sulfate. In the step S01, the step S01 further includes the following steps: the inorganic pore-forming agent is firstly ground, a grinding device can be but is not limited to a planetary ball mill, the size range of grinding beads of the planetary ball mill can be 10-20 mm, the number of the grinding beads of the planetary ball mill can be 10-100, the rotating speed of the planetary ball mill can be 300-400rpm, the grinding time can be 30-100min, and the particle size of the ground inorganic pore-forming agent is 250-300 mu m. Referring to table 1, in some embodiments, after grinding, the inorganic pore-forming agent may be further sieved, and after grinding and sieving, the particle size of the inorganic pore-forming agent ranges from 56 μm to 145 μm, so that the porous ceramic has a high porosity and the surface of the porous ceramic is smooth. And then the binder and the inorganic pore-forming agent after grinding and screening are put into a tank mill for mixing, the mixing time is 30-60 min, and the mixing rotating speed is 350-450 rpm. And then adding the aggregate powder into the tank mill, continuously mixing for 60-100 min at the mixing speed of 250-400 rpm, and uniformly mixing to obtain the premix. The inorganic pore-forming agent such as ammonium chloride or ammonium sulfate can be directly recovered by recrystallization upon cooling after thermal decomposition. The pore-forming agent of inorganic salts such as sodium chloride and potassium sulfate is recovered by water washing and recrystallization. The water washing recrystallization can adopt multiple times of water washing, and the water washing can adopt ultrasonic water washing. It should be noted that, the size range of the inorganic pore-forming agent needs to be strictly controlled, and too large size of the inorganic pore-forming agent easily causes the problems of cracks or rough and uneven appearance of a prepared ceramic sample, which further causes the defects of product slag falling, uneven and discontinuous subsequent coating, resistance stability influence and the like. Therefore, on the basis of strictly controlling the size range of the inorganic pore-forming agent, the aggregate powder, the binder and the inorganic pore-forming agent in a preset proportion are mixed, so that the contact among the three materials is favorably improved, the subsequent sintering effect is further improved, and the uniformity of pores of the prepared porous ceramic is improved.
TABLE 1 ball milling method for controlling ammonium chloride particle size
100g of ammonium chloride is added into a ball milling tank, a certain amount of ball milling beads are added, and the rotating speed and the time are set. And collecting ammonium chloride after ball milling, and obtaining the D50 particle size by a dry test by using a laser particle sizer. As can be seen from Table 1, when the particle size D50 of the ammonium chloride particles is in the range of 56 to 145. Mu.m, a porous ceramic having a flat surface can be obtained.
In the step S02, the dry pressing equipment is a Shanghai Xinnuo instrument digital display protective tablet press (SYP-30 TFS). Because the dry pressing pressure is too small, the dry pressing blank is not easy to form, and the prepared dry pressing blank is easy to crack and other defects because of too large dry pressing pressure. Therefore, the pressure for dry pressing the premix is controlled to be 10-30 MPa, which is beneficial to forming a dry pressing blank and can avoid the influence on the structural strength caused by the defects of easy generation of cracks and the like of the dry pressing blank.
The particle size in the invention is D50 particle size, D50 represents the diameter of powder particles, D50 represents the diameter of cumulative 50% point (or 50% passing particle size), and the physical meaning of the invention is that the particle size is more than 50% of the particles and less than 50% of the particles.
In the step S03, sintering the dry-pressed green body includes at least one of a programmed temperature sintering method, a rapid temperature sintering method, and a multi-stage rapid temperature sintering method;
the temperature programming sintering mode comprises the following steps: putting the dry pressing blank body on a high temperature resistant ceramic flat plate, putting the dry pressing blank body in a central heating area of a sintering furnace, heating to 900-1200 ℃ at a heating rate of 5-10 ℃/min in an air atmosphere, and keeping the temperature for 4-40 min;
the rapid heating sintering mode comprises the following steps: firstly, heating a sintering furnace in an air atmosphere at a heating rate of 5-10 ℃/min to enable the sintering furnace to reach a preset temperature of 900-1200 ℃; then placing the dry pressing green body on a high temperature resistant ceramic flat plate, quickly pushing the dry pressing green body into a sintering furnace, and preserving heat for 4-40 min to carry out quick high temperature sintering treatment on the dry pressing green body;
the multi-stage rapid heating sintering mode comprises the following steps: respectively presetting a low-temperature area and a high-temperature area in a double-temperature-area tube furnace, heating the low-temperature area to the preset temperature of 600-700 ℃ at the heating rate of 5-10 ℃/min, and heating the high-temperature area to the preset temperature of 900-1200 ℃ at the heating rate of 5-10 ℃/min; and placing the dry-pressed green body on a high-temperature-resistant ceramic flat plate, pushing the dry-pressed green body to a low-temperature area from a room-temperature area for sintering and heat preservation for 4-10 min, then pushing the dry-pressed green body to a high-temperature area from the low-temperature area for sintering and heat preservation for 4-10 min, and pulling the dry-pressed green body back to the low-temperature area from the high-temperature area for sintering and heat preservation for 4-10 min.
In the step S03, after the sintering heat preservation time is over, the porous ceramic formed by sintering is cooled to room temperature by using a programmed cooling method or a rapid cooling method.
In the procedure cooling mode, after the sintering heat preservation is finished, the cooling rate of the procedure cooling is 4-6 ℃/min until the porous ceramic formed by sintering is cooled to the room temperature.
In the rapid cooling mode, after sintering and heat preservation are finished, the sample is pulled or pushed to a room temperature area from a heating area of the tube furnace at the speed of 0.02-1 m/s.
According to the preparation method of the porous ceramic provided by the embodiment of the invention, by regulating and controlling the size of the inorganic pore-forming agent and improving the formula of the raw materials, on the basis of the proportioning of the aggregate powder and the inorganic pore-forming agent and the cooperative regulation and control of the particle sizes of the aggregate powder and the inorganic pore-forming agent, the structural strength and the porosity of the porous ceramic are improved and increased by dry pressing and the cooperative regulation and control of sintering process conditions, the porous ceramic has higher porosity and stronger compressive strength, and the problems of small liquid storage amount, long sintering time, poorer structural strength caused by high porosity and the like of the porous ceramic for preparing the atomizing core can be effectively solved. In addition, the porous ceramic provided by the embodiment of the invention has the advantages of high porosity, short sintering time, high structural strength, capability of reducing carbon dioxide emission under high-temperature combustion, low carbon and environmental friendliness. In addition, the preparation method of the porous ceramic provided by the embodiment of the invention has the advantages of simple process flow, easiness in operation and low cost.
In the embodiment of the present invention, the solid-phase diatomite, the glass powder, and the ammonium chloride essentially function as the ceramic aggregate, the binder, and the pore-forming agent, respectively. The rapid sintering method is characterized in that under the condition of solid phase powder sintering, due to the fact that the temperature rising speed is high, a ceramic material can not go through a preheating stage in the temperature rising process and directly enters a high-temperature stage, the curvature radius of a neck part between crystal grains is small, a large driving force can be provided to promote a mass transfer process, the mass transfer process can be further accelerated due to the high sintering temperature, accordingly, ultra-rapid densification of the ceramic powder material is achieved, and the mechanical strength of the material is improved. Meanwhile, the pore-forming agent can be rapidly decomposed in a rapid high-temperature sintering stage, a large number of cavities are left, the consideration of the mechanical property and the porous structure of the material is realized in a short sintering time, and the production efficiency is further improved. The rapid sintering method has the advantages of simple equipment, unlimited shape and size and the like, can obtain a ceramic atomizing core porous substrate which is comparable to (even superior to) that obtained by the traditional process by continuously pushing and pulling the sample in different temperature intervals, reduces the raw material cost and the time cost of process preparation due to a simplified formula and a unique sintering mode, and is easy to realize industrial production.
In order that the details of the above-described practice and operation of the invention will be readily understood by those skilled in the art, and the advanced nature of the porous ceramics of the invention and the method of making the same will be apparent, the practice of the invention will now be illustrated by way of example.
Example 1
The embodiment 1 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 45% of diatomite, 25% of glass powder and 30% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 30% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 145 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 25% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 45% of diatomite into a tank mill, and mixing the materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) Putting the premix obtained in the step 3) into a round cake-shaped grinding tool for dry pressing, wherein the dry pressing pressure is controlled to be 19MPa, and the pressure maintaining time is 30s, so as to obtain a ceramic blank body with a specific shape.
5) And (5) placing the ceramic blank in the step 4) on a ceramic flat plate, then placing the ceramic flat plate on a tube furnace for sintering, heating to 1000 ℃ at a heating rate of 5 ℃/min, sintering and preserving heat for 20min, after heat preservation is finished, performing programmed cooling at a cooling rate of 5 ℃/min, and taking out the ceramic flat plate after cooling to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 2
The embodiment 2 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 42% alumina, 18% glass frit and 40% ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 40% ammonium chloride in a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 56 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 18% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 42% of alumina into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) And (3) placing the ceramic blank in the step 4) on a ceramic flat plate, then placing the ceramic flat plate in a tube furnace for sintering, heating to 1000 ℃ at a heating rate of 5 ℃/min, sintering and preserving heat for 4min, after preserving heat, performing programmed cooling at a cooling rate of 5 ℃/min, and taking out after cooling to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 3
The embodiment 3 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 32% boron nitride, 23% glass frit and 45% ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 45% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 145 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 23% of glass powder in a tank mill at the rotating speed of 300rpm for 60min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 32% of boron nitride into a tank mill, and mixing by using the tank mill at the rotating speed of 300rpm for 60min to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) And (3) placing the ceramic blank in the step 4) on a ceramic flat plate, then placing the ceramic flat plate in a tube furnace for sintering, heating to 1000 ℃ at the heating rate of 5 ℃/min, sintering and preserving heat for 10min, after the heat preservation is finished, pushing the sintered ceramic blank out of the tube furnace at the speed of 0.02-1 m/s for rapidly cooling at room temperature, and taking out the ceramic blank after cooling to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 4
The embodiment 4 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) Heating the tube furnace to 1000 ℃, placing the ceramic blank in the step 4) on a ceramic flat plate, placing the ceramic flat plate on the tube furnace at the speed of 0.02-1 m/s for sintering, sintering and preserving heat for 20min, performing programmed cooling at the cooling rate of 5 ℃/min after heat preservation is finished, and taking out the ceramic flat plate after cooling to obtain a finished product of the porous ceramic.
6) And recovering ammonium chloride from the quartz tube wall, and reusing the ammonium chloride as a pore-forming agent.
Example 5
This example 5 provides a porous ceramic applied to preparing an atomizing core and a preparation method thereof, and includes the following raw materials by mass percent: 40% of diatomite, 10% of glass powder and 48% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 48% ammonium chloride in a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 10% of glass powder in a tank mill at the rotation speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 40% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) Heating the tubular furnace to 1000 ℃, placing the ceramic blank in the step 4) on a ceramic flat plate, placing the ceramic flat plate in the tubular furnace at the speed of 0.02-1 m/s for sintering, sintering and preserving heat for 20min, pushing the sintered ceramic blank out of the tubular furnace at the speed of 0.02-1 m/s after heat preservation, rapidly cooling at room temperature, cooling and taking out to obtain a finished product of the porous ceramic.
6) And recovering ammonium chloride from the quartz tube wall, and reusing the ammonium chloride as a pore-forming agent.
Example 6
The embodiment 6 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 40% of diatomite, 20% of glass powder and 40% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 40% ammonium chloride in a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 20% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 40% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) Respectively heating 650 ℃ and 1050 ℃ by using a tube furnace in a heating area, then placing the ceramic blank in the step 4) into a quartz boat, pushing the ceramic blank from the room temperature to a low-temperature area of 650 ℃ at a pushing speed of 0.02-1 m/s for heating for 4min, then pushing the ceramic blank to a high-temperature area of 1050 ℃ at a pushing speed of 0.02-1 m/s for heating for 4min, then pushing the ceramic blank to a low-temperature area of 650 ℃ at a pushing speed of 0.02-1 m/s for heating for 4min, finally pushing the sintered ceramic blank out of the tube furnace at a speed of 0.02-1 m/s for rapidly cooling at the room temperature, and taking out the ceramic blank after cooling to obtain a finished product of the porous ceramic.
6) And recovering ammonium chloride from the quartz tube wall, and reusing the ammonium chloride as a pore-forming agent.
Example 7
This embodiment 7 provides a porous ceramic applied to preparing an atomizing core and a preparation method thereof, and the porous ceramic comprises the following raw materials by mass: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotation speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) And (5) placing the ceramic blank in the step 4) on a ceramic flat plate, then placing the ceramic flat plate on a tube furnace for sintering, heating to 1000 ℃ at a heating rate of 5 ℃/min, sintering and preserving heat for 20min, after heat preservation is finished, performing programmed cooling at a cooling rate of 5 ℃/min, and taking out the ceramic flat plate after cooling to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 8
This embodiment 8 provides a porous ceramic used for preparing an atomization core and a preparation method thereof, which includes the following raw materials by mass percent: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) And (3) placing the ceramic blank in the step 4) on a ceramic flat plate, then placing the ceramic flat plate in a tube furnace for sintering, heating to 1000 ℃ at the heating rate of 5 ℃/min, sintering and preserving heat for 20min, after the heat preservation is finished, pushing the sintered ceramic blank out of the tube furnace at the speed of 0.02-1 m/s for rapidly cooling at room temperature, and taking out the ceramic blank after cooling to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 9
This example 9 provides a porous ceramic applied to preparing an atomizing core and a preparation method thereof, and includes the following raw materials by mass percent: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) Heating the tube furnace to 1000 ℃, placing the ceramic blank in the step 4) on a ceramic flat plate, pushing the sample into the tube furnace at a pushing speed of 0.02-1 m/s, sintering for 20min, pushing the sintered ceramic blank out of the tube furnace at a speed of 0.02-1 m/s after heat preservation, rapidly cooling at room temperature, cooling, and taking out to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Example 10
The embodiment 10 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 90 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Putting the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing materials by using the tank mill, wherein the rotating speed of the tank mill is 300rpm, and the mixing time is 60min, so as to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) Heating the tubular furnace to 1000 ℃, placing the ceramic blank in the step 4) on a ceramic flat plate, pushing the sample into the tubular furnace at a pushing speed of 0.02-1 m/s, sintering for 4min, carrying out programmed cooling at a cooling rate of 5 ℃/min after heat preservation is finished, and taking out the cooled ceramic blank to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Comparative example 1
The comparative example 1 provides a porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 30% of diatomite, 14% of glass powder and 60% of ammonium chloride.
The preparation method of the porous ceramic comprises the following steps:
1) And (3) placing the 60% ammonium chloride into a planetary ball mill for ball milling to obtain ammonium chloride particles with the particle size of 260 mu m.
2) Mixing the ammonium chloride obtained in the step 1) and 14% of glass powder in a tank mill at the rotating speed of 400rpm for 40min to obtain mixture powder.
3) Placing the mixture powder obtained in the step 2) and 30% of diatomite into a tank mill, and mixing the materials by using the tank mill at the rotating speed of 300rpm for 60min to obtain the premix.
4) And (3) putting the premix in the step 3) into a round cake-shaped grinding tool for dry pressing, controlling the dry pressing pressure to be 19MPa, and keeping the pressure for 30s to obtain a ceramic blank with a specific shape.
5) And (3) placing the ceramic blank in the step 4) on a ceramic flat plate, pushing the sample into a tube furnace at a pushing speed, sintering for 4min, and after heat preservation is finished, cooling and taking out to obtain a finished product of the porous ceramic.
6) And recovering the ammonium chloride on the wall of the quartz tube, and reusing the ammonium chloride as a pore-forming agent.
Comparative example 2
The comparative example 2 provides porous ceramic applied to preparing an atomization core and a preparation method thereof, and the porous ceramic comprises the following raw materials in percentage by mass: 30% of diatomite, 14% of glass powder and 60% of organic pore-forming agent PMMA.
The preparation method of the porous ceramic comprises the following steps:
the porous ceramic is prepared by adopting the conventional process in the comparative example 2: the hot-pressing injection molding process is a preparation process commonly applied to the current porous ceramics, and comprises the steps of material mixing, heating and stirring, hot-pressing injection molding, dewaxing, high-temperature sintering and the like, wherein an organic pore-forming agent is added in the material mixing stage, paraffin and organic acid are further added in the heating and stirring process, hot-pressing molding is carried out after 4 hours, then demoulding and graphite powder embedding are carried out, dewaxing is carried out at 200 ℃ for 4 hours, and finally sintering is carried out at 1000 ℃ for 4 hours. The process relates to the use of more organic matters, and not only can discharge carbon dioxide and consume time in the sintering process, but also the organic pore-forming agent cannot be recovered.
Testing the relevant performance of the porous ceramics:
the porous ceramics prepared in the above examples 1 to 10 and comparative examples 1 to 2 were subjected to the tests of the relevant items of parameters such as liquid storage amount, pore-forming agent recovery rate, compressive strength, porosity, and the like, respectively.
1. Stock solution amount testing method
Putting the porous ceramic into a drying oven for pretreatment for 15min at 120 ℃, and weighing the mass as m 0 . Then the tobacco leaves are put into a special vessel containing a fixed amount of tobacco juice, and the height of the tobacco juice is about 1.27mm. After the adsorption saturation, taking out the porous ceramic to erase the smoke liquid on the surface, weighing the mass of the porous ceramic after adsorbing the smoke liquid as m 1 And calculating to obtain the mass (C, unit mg/g) of the porous ceramic adsorption smoke liquid per unit mass.
2. Test for compressive Strength
Compressive strength = P/a, wherein: p and A are respectively pressure (unit N) and stress area (unit square meter). And (3) testing equipment: shimadzu Universal testing machine (AGX-X-50 KN). And (3) placing the sample on a universal testing machine, continuously and slowly applying pressure to obtain a spectrogram, and analyzing the spectrogram to obtain the maximum compressive strength of the sample under a certain stroke.
3. Porosity test
Porosity is the percentage (%) of the volume of open pores (pores open to the atmosphere) in the sample to the total volume of the sample. The apparatus was a porous ceramic porosity/water absorption analyzer (second quasi-MAY-Entries 120). The specific method comprises the following steps: and (3) placing the sample in an electrothermal drying box, and drying at 110 +/-5 ℃ to constant weight. Weighing the dry weight mass of the sample, and recording the dry weight mass as m 1 After the dry weights of all the samples were measured, the samples were sequentially placed in a sample tank, and deionized water was injected. And transferring the sample groove into a transparent vacuum chamber and vacuumizing. Pumping at-100 kpa for 5min. Taking out the sample, adsorbing the water on the surface by using the nano sponge, and measuring the mass m of the saturated sample in the air 2 . Finally, the mass m3 of the saturated sample in water was measured and the porosity was calculated by the following formula:
the results of the relevant tests are shown in Table 2 below.
TABLE 2 tables for testing relevant properties of porous ceramics in examples 1 to 10 and comparative examples 1 to 2
As can be seen from the analysis in Table 2, the porous ceramics in examples 1 to 10 are significantly improved in the liquid storage amount, the porosity, the compressive strength, and other related properties as compared with those in comparative examples 1 to 2, which indicates that the porous ceramics in examples 1 to 10 of the present invention have both higher porosity and stronger compressive strength. In addition, the inorganic pore-forming agent adopted in embodiments 1 to 10 of the present invention can be recycled, and after the porous ceramic is used for manufacturing the atomizing core, carbon dioxide emission can be reduced under high temperature combustion, so that the present invention has characteristics of low carbon, environmental protection, and low cost. In addition, in combination with table 2 and fig. 1 to 6, the appearance of the dry-pressed blank before the sintering and the sintered porous ceramic product of example 4 and comparative example 1 of the present invention were compared, and it was found that, in comparative example 1, compared with example 4, there were problems that the blank was incomplete before the sintering and the side of the porous ceramic product after the sintering had cracked surface roughness, whereas example 4 of the present invention had the blank intact before the sintering and the side of the porous ceramic product after the sintering had no cracks and had smooth and flat surface.
The above description is intended to be illustrative of the preferred embodiment of the present invention and should not be taken as limiting the invention, but rather, the intention is to cover all modifications, equivalents, and alternatives falling within the spirit and scope of the invention.
Claims (10)
1. The porous ceramic is characterized by being prepared from the following raw materials in percentage by mass:
30-45% of aggregate powder;
30-60% of inorganic pore-forming agent;
10 to 25 percent of binder;
wherein, the inorganic pore-forming agent is at least one of ammonium chloride, sodium chloride, potassium sulfate and ammonium sulfate.
2. The porous ceramic of claim 1, wherein the aggregate powder is at least one of diatomaceous earth, boron nitride, and alumina.
3. The porous ceramic of claim 1, wherein the binder comprises a glass frit having a softening point of 800 to 900 ℃.
4. The porous ceramic of any one of claims 1 to 3, wherein the inorganic pore former has a particle size of 56 to 145 μm.
5. An atomizing core, comprising the porous ceramic of any one of claims 1 to 4.
6. An atomizing device comprising the porous ceramic according to any one of claims 1 to 4 or the atomizing core according to claim 5.
7. The preparation method of the porous ceramic is characterized by comprising the following steps:
step S01: respectively weighing aggregate powder, an inorganic pore-forming agent and a binder according to the components contained in the porous ceramic of any one of claims 1 to 4, and mixing the raw materials to obtain a premix;
step S02: dry-pressing the premix to obtain a dry-pressed green body;
step S03: and sintering the dry pressing blank, and cooling to obtain a porous ceramic finished product.
8. The method for preparing a porous ceramic according to claim 7, wherein the step S01 further comprises the steps of: grinding the inorganic pore-forming agent, wherein the particle size of the ground inorganic pore-forming agent is 56-145 mu m; and then putting the binder and the ground inorganic pore-forming agent into a tank mill for mixing, then adding the aggregate powder into the tank mill, and uniformly mixing to obtain the premix.
9. The method for preparing porous ceramic according to claim 7, wherein the pressure for dry-pressing the premix in the step S02 is 10 to 30MPa.
10. The method for preparing a porous ceramic according to claim 7, wherein the sintering of the dry-pressed green body in step S03 includes at least one of a temperature-programmed sintering method, a rapid-temperature-rise sintering method, and a multi-stage rapid-temperature-rise sintering method;
the temperature programmed sintering mode comprises the following steps: placing the dry pressing blank body on a high temperature resistant ceramic flat plate, placing the dry pressing blank body in a central heating area of a sintering furnace, heating to 900-1200 ℃ at a heating rate of 5-10 ℃/min in an air atmosphere, and preserving heat for 4-40 min;
the rapid heating sintering mode comprises the following steps: firstly, heating a sintering furnace in an air atmosphere at a heating rate of 5-10 ℃/min to enable the sintering furnace to reach a preset temperature of 900-1200 ℃; then placing the dry pressing blank body on a high temperature resistant ceramic flat plate, quickly pushing the dry pressing blank body into the sintering furnace, and preserving heat for 4-40 min to carry out quick high temperature sintering treatment on the dry pressing blank body;
the multi-stage rapid heating sintering mode comprises the following steps: respectively presetting a low-temperature area and a high-temperature area in a double-temperature-area tube furnace, heating the low-temperature area to a preset temperature of 600-700 ℃ at a heating rate of 5-10 ℃/min, and heating the high-temperature area to a preset temperature of 900-1200 ℃ at a heating rate of 5-10 ℃/min; and placing the dry pressing blank on a high-temperature resistant ceramic flat plate, pushing the dry pressing blank into a low-temperature area from a room-temperature area for sintering and heat preservation for 4-10 min, then pushing the dry pressing blank into the high-temperature area from the low-temperature area for sintering and heat preservation for 4-10 min, and then pulling the dry pressing blank back to the low-temperature area from the high-temperature area for sintering and heat preservation for 4-10 min.
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