CN114044695A - Porous ceramic material and preparation method thereof - Google Patents

Porous ceramic material and preparation method thereof Download PDF

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CN114044695A
CN114044695A CN202111272911.6A CN202111272911A CN114044695A CN 114044695 A CN114044695 A CN 114044695A CN 202111272911 A CN202111272911 A CN 202111272911A CN 114044695 A CN114044695 A CN 114044695A
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porous ceramic
drying
complex phase
quartz glass
preserving heat
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CN114044695B (en
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宋文正
胡勇齐
李俊辉
齐会龙
丁磊
聂革
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Shenzhen Woody Vapes Technology Co Ltd
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Shenzhen Woody Vapes Technology Co Ltd
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Abstract

The invention relates to the technical field of ceramic product preparation processes, in particular to a porous ceramic material and a preparation method thereof, wherein the porous ceramic material comprises the following raw materials in percentage by mass: 40 to 46 percent of quartz glass powder, 3 to 10 percent of complex phase additive, 0.2 to 2 percent of dispersant, 0.5 to 5 percent of foaming agent, 0.02 to 0.5 percent of green body reinforcing agent and 40 to 53 percent of water; the complex phase additive is a mixture of two or three of zirconia, magnesia and titania. The sintering temperature is reduced by controlling the content of each raw material component and adding a complex phase additive; by adding the green body reinforcing agent, the green body strength is improved, and the automatic production is facilitated; the preparation method combines the advantages of the foaming method and the grouting method, and can prepare the quartz glass porous ceramic with high porosity, good strength, uniform pore diameter, stable performance and easy production by designing the sintering curve.

Description

Porous ceramic material and preparation method thereof
Technical Field
The invention relates to the technical field of ceramic product preparation processes, in particular to a porous ceramic material and a preparation method thereof.
Background
The porous ceramic has the advantages of high mechanical strength, small expansion coefficient, wear resistance, corrosion resistance, high temperature resistance, good thermal stability, lower cost and the like, is successfully applied to the fields of ceramics, metallurgy, building materials, chemical industry, national defense, scientific research and the like, and is a novel ceramic material with the widest application in oxide ceramics.
The common preparation methods of the porous ceramics at present mainly comprise a particle stacking method, a pore-forming agent adding method, a foaming method, a sol-gel method and the like. The particle stacking method is a dry pressing method, cannot prepare ceramics with complex structures, has low porosity, has certain requirements on raw materials due to the addition of a pore-forming agent method, and ensures that the prepared ceramics have uneven pore size distribution. The sol-gel method is expensive in raw materials used at present, contains organic matters, is harmful to health, and has long preparation period and easy shrinkage in the drying process. The porosity range of the sample prepared by the slip casting method is narrow. The pores of the porous ceramics prepared by the foaming method are mostly of closed pore structures. How to prepare quartz glass porous ceramics with high porosity and high strength is a problem which needs to be solved urgently at present.
Disclosure of Invention
Based on the porous ceramic material, the invention provides the porous ceramic material which can be used for preparing the porous ceramic with high porosity and high strength.
A porous ceramic material comprises the following raw materials in percentage by mass:
Figure BDA0003329269580000011
Figure BDA0003329269580000021
the complex phase additive is a mixture of two or three of zirconia, magnesia and titania.
In one embodiment, the mass percentages of zirconia, magnesia and titania in the complex phase additive are respectively: 60-80% of zirconium oxide, 0-30% of magnesium oxide and 0-40% of titanium oxide.
In one embodiment, the particle size of the silica glass frit is one of 150 mesh, 300 mesh, and 600 mesh.
In one embodiment, the dispersant is one or more of tetramethylammonium hydroxide, polyethylene glycol, polyethyleneimine, polyvinylpyrrolidone, and citric acid.
In one embodiment, the foaming agent is one or two of lauryl triethanolamine sulfate and n-propyl gallate.
In one embodiment, the blank reinforcing agent is one or two of sodium carboxymethylcellulose and polyvinyl alcohol.
A preparation method of porous ceramics comprises the following steps:
preparing a complex phase additive: weighing two or three of zirconia, magnesia and titania, fully mixing, storing at high temperature, cooling, crushing, ball-milling by a wet method, and drying to obtain a complex phase additive;
mixing materials: weighing quartz glass powder, and mixing the quartz glass powder with a complex phase additive to obtain a mixed material;
preparing ceramic slurry: mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH to 7-9 by using inorganic base, and stirring uniformly to obtain ceramic slurry;
preparing a blank body: injecting the ceramic slurry into a preheated gypsum mold, drying, and demolding after drying to obtain a ceramic blank;
and (3) sintering: and sintering the ceramic blank in a sintering furnace, and cooling to room temperature to obtain the quartz glass porous ceramic.
In one embodiment, the inorganic base is aqueous ammonia.
In one embodiment, the step of preparing the green body comprises: preheating the gypsum mould at 30 ℃/h; and/or the presence of a gas in the gas,
after the ceramic slurry is injected into a preheated gypsum mold, the drying conditions are as follows: drying at 32-40 ℃ for 5-8 hours, drying at 45-53 ℃ for 3-6 hours, drying at 65-73 ℃ for 1-3 hours, and drying at 95-110 ℃ for 0.5-1 hour.
In one embodiment, in the sintering step, the ceramic green body is placed into a sintering furnace for sintering, and the sintering conditions are as follows: heating to 150 ℃ at a speed of 20-50 ℃/h, preserving heat for 1-2 h, heating to 300 ℃ at a speed of 45-60 ℃/h, preserving heat for 1-2 h, heating to 500 ℃ at a speed of 60-80 ℃/h, preserving heat for 2-4 h, heating to 900 ℃ at a speed of 180-200 ℃/h, preserving heat for 1-2 h, heating to 1100 ℃ at a speed of 90-120 ℃/h, and preserving heat for 1-2 h.
The porous ceramic material and the preparation method thereof have the beneficial effects that:
1. the sintering temperature is reduced by controlling the content of each raw material component and adding a complex phase additive; by adding the green body reinforcing agent, the green body strength is improved, and the automatic production is facilitated;
2. the preparation method combines the advantages of the foaming method and the grouting method, and can prepare the quartz glass porous ceramic with high porosity, good strength, uniform pore diameter, stable performance and easy production by designing the sintering curve.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. 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.
The invention provides a porous ceramic material which comprises the following raw materials in percentage by mass:
Figure BDA0003329269580000041
the complex phase additive is a mixture of two or three of zirconia, magnesia and titania.
In one embodiment, the mass percentages of zirconia, magnesia and titania in the complex phase additive are respectively: 60-80% of zirconium oxide, 0-30% of magnesium oxide and 0-40% of titanium oxide.
In one embodiment, the quartz glass powder has a particle size of one of 150 mesh, 300 mesh and 600 mesh, which is advantageous for stable molding.
The dispersant is mainly used for increasing the dispersion degree of each component in the slurry, so that the compactness and the porosity of each part of the ceramic are uniform, and the dispersant can be one or more of tetramethylammonium hydroxide, polyethylene glycol, polyethyleneimine, polyvinylpyrrolidone and citric acid.
The foaming agent is mainly used for eliminating foams generated in the preparation process and preventing the foams in the slurry from damaging ceramic forming, and can be one or two of lauryl triethanolamine sulfate and n-propyl gallate.
By adding the green body reinforcing agent, the green body strength is improved, and the automatic production is facilitated. The blank reinforcing agent can be one or two of sodium carboxymethylcellulose and polyvinyl alcohol.
A preparation method of porous ceramic is prepared by adopting the porous ceramic material, and comprises the following steps:
s100, preparing a complex phase additive: weighing two or three of zirconia, magnesia and titania, fully mixing, storing at high temperature, cooling, crushing, ball milling by a wet method, and drying to obtain the complex phase additive.
Mechanically mixing zirconia, magnesia and titania, placing the mixture into a sagger, preserving the heat at 1200-1300 ℃ for about 2 hours, then cooling and crushing the mixture, carrying out wet ball milling, and drying the mixture to obtain the complex phase additive with the particle size of 15-30 mu m.
S200, mixing materials: weighing quartz glass powder, and mixing the quartz glass powder with a complex phase additive to obtain a mixed material.
The quartz glass powder and the complex phase additive can be mixed by adopting a three-dimensional mixer, for example, the quartz glass powder, the zirconia, the magnesia and the titania are added into the three-dimensional mixer, the rotating speed is 100-150 r/min, and the mixture is mixed for 3-6 hours.
S300, preparing ceramic slurry: mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using inorganic base, and stirring uniformly to obtain the ceramic slurry.
The inorganic alkali is preferably ammonia water, the ammonia water does not influence the molding of the quartz glass porous ceramic, and the formed gas is completely volatilized during the preparation of the blank and sintering to generate certain pores, which is beneficial to improving the porosity of the quartz glass porous ceramic.
S400, preparing a blank: and (3) injecting the ceramic slurry into a preheated gypsum mold, drying, and demolding after drying to obtain a ceramic blank.
The preheating condition of the gypsum mold is 30 ℃/h, after the gypsum is preheated, the ceramic slurry is injected into the gypsum mold, and then the ceramic slurry is dried for 5-8 hours at the temperature of 32-40 ℃, dried for 3-6 hours at the temperature of 45-53 ℃, dried for 1-3 hours at the temperature of 65-73 ℃ and dried for 0.5-1 hour at the temperature of 95-110 ℃. Through the temperature rise curve, the ceramic slurry is gradually dried and formed, the component particles are tightly combined, a prototype pore is formed, ammonia gas for adjusting the PH value is gradually volatilized, and the porosity is increased.
S500, sintering: and sintering the ceramic blank in a sintering furnace, and cooling to room temperature to obtain the quartz glass porous ceramic.
In one embodiment, the ceramic body is placed into a sintering furnace for sintering, and the sintering conditions are as follows: heating to 150 ℃ at a speed of 20-50 ℃/h, preserving heat for 1-2 h, heating to 300 ℃ at a speed of 45-60 ℃/h, preserving heat for 1-2 h, heating to 500 ℃ at a speed of 60-80 ℃/h, preserving heat for 2-4 h, heating to 900 ℃ at a speed of 180-200 ℃/h, preserving heat for 1-2 h, heating to 1100 ℃ at a speed of 90-120 ℃/h, and preserving heat for 1-2 h.
The preparation method of the porous ceramic combines the advantages of a foaming method and a grouting method according to the performance characteristics of all raw materials, and can prepare the quartz glass porous ceramic which has high porosity, good strength, uniform pore diameter and stable performance and is easy to produce by designing a sintering curve.
The following is an example description.
Example 1
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 45% of quartz glass powder, 7% of complex phase additive, 0.7% of dispersing agent, 2% of foaming agent, 0.2% of green body reinforcing agent and 45.1% of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 65% of zirconium oxide, 23% of magnesium oxide and 12% of titanium oxide.
The particle size of the quartz glass powder is 150 meshes.
The dispersant is 5: 2 and citric acid.
The foaming agent is lauryl sulfate triethanolamine.
The green body reinforcing agent is prepared from the following components in percentage by mass: 1 sodium carboxymethylcellulose and polyvinyl alcohol.
The preparation method of the quartz glass porous ceramic prepared by the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, keeping the temperature at 1200 ℃ for 2 hours, then cooling and crushing, carrying out wet ball milling, and drying to obtain the complex phase additive with the particle size of 15-20 microns.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 120r/min, and mixing for 4 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould for 1 hour at the temperature of 30 ℃, injecting ceramic slurry into the preheated gypsum mould, then drying for 8 hours at the temperature of 35 ℃, drying for 4 hours at the temperature of 50 ℃, drying for 2 hours at the temperature of 70 ℃, drying for 0.5 hour at the temperature of 100 ℃, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 30 ℃/h, preserving heat for 1h, heating to 300 ℃ at a speed of 50 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 65 ℃/h, preserving heat for 3h, heating to 900 ℃ at a speed of 200 ℃/h, preserving heat for 1h, heating to 1100 ℃ at a speed of 100 ℃/h, preserving heat for 2h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 2
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 42 percent of quartz glass powder, 8 percent of complex phase additive, 0.9 percent of dispersant, 1.5 percent of foaming agent, 0.4 percent of green body reinforcing agent and 47.2 percent of water.
The mass percent of zirconia and magnesia in the complex phase additive are respectively as follows: 80% of zirconium oxide and 20% of magnesium oxide.
The particle size of the quartz glass powder is 300 meshes.
The dispersant is 8: 1, a mixture of polyvinylpyrrolidone and citric acid.
The foaming agent is lauryl sulfate triethanolamine.
The blank reinforcing agent is sodium carboxymethyl cellulose.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconia and magnesia, fully mixing, putting into a sagger, preserving heat for about 2 hours at 1200-1300 ℃, then cooling and crushing, and mixing the materials according to the weight ratio of M (material) M (ball) M (water) to 1: 2: 1.5, performing wet ball milling for 3 hours, and drying to obtain the complex phase additive with the particle size of 30 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 120r/min, and mixing for 6 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould for 1 hour at the temperature of 30 ℃, injecting the ceramic slurry into the preheated gypsum mould, then drying for 8 hours at the temperature of 35 ℃, drying for 4 hours at the temperature of 50 ℃, drying for 2 hours at the temperature of 70 ℃, drying for 0.5 hour at the temperature of 100 ℃, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 20 ℃/h, preserving heat for 2h, heating to 300 ℃ at a speed of 45 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 60 ℃/h, preserving heat for 4h, heating to 900 ℃ at a speed of 180 ℃/h, preserving heat for 2h, heating to 1100 ℃ at a speed of 90 ℃/h, preserving heat for 2h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 3
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 40% of quartz glass powder, 15% of complex phase additive, 0.7% of dispersing agent, 0.8% of foaming agent, 0.31% of blank reinforcing agent and 43.19% of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 60% of zirconium oxide, 15% of magnesium oxide and 25% of titanium oxide.
The particle size of the quartz glass powder is 150 meshes.
The dispersant is 5: 2 and citric acid.
The foaming agent is n-propyl gallate.
The green body reinforcing agent is prepared from the following components in percentage by mass of 30: 1 sodium carboxymethylcellulose and polyvinyl alcohol.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, heating to 1280 ℃ at the speed of 220 ℃/h, preserving heat for 2 hours, cooling to break the zirconium oxide, the magnesium oxide and the titanium oxide into small particles of 1-3cm, heating to 1280 ℃ at the speed of 220 ℃/h, preserving heat for 2 hours, and drying to obtain the complex phase additive with the particle size of 16-25 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 150r/min, and mixing for 3 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at 30 ℃ for 1h, injecting ceramic slurry into the preheated gypsum mould, then drying for 8 hours at 35 ℃, drying for 4 hours at 50 ℃, drying for 2 hours at 70 ℃, drying for 0.5 hour at 100 ℃, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 35 ℃/h, preserving heat for 2h, heating to 300 ℃ at a speed of 60 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 70 ℃/h, preserving heat for 2h, heating to 900 ℃ at a speed of 180 ℃/h, preserving heat for 1h, heating to 1100 ℃ at a speed of 110 ℃/h, preserving heat for 2h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 4
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 43 percent of quartz glass powder, 5 percent of complex phase additive, 0.2 percent of dispersant, 0.6 percent of foaming agent, 0.5 percent of green body reinforcing agent and 48.9 percent of water.
The mass percentage of the zirconia and the titanium oxide in the complex phase additive are respectively as follows: 70% of zirconium oxide and 30% of titanium oxide.
The particle size of the quartz glass powder is 600 meshes.
The dispersant is prepared from the following components in a mass ratio of 1: 1 of polyethylene glycol and polyethyleneimine.
The foaming agent is prepared from the following raw materials in a mass ratio of 1: 1 triethanolamine lauryl sulfate and n-propyl gallate.
The blank reinforcing agent is sodium carboxymethyl cellulose.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconia and magnesia, fully mixing, putting into a sagger, preserving heat for 1.5 hours at 1300 ℃, then cooling and crushing, and mixing according to the weight ratio of M (material), M (ball), M (water) to 1: 2: and (3) performing wet ball milling for 3 hours according to the proportion of 1.5, and drying to obtain the complex phase additive with the particle size of 20-30 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 100r/min, and mixing for 5 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at the temperature of 30 ℃/h, injecting ceramic slurry into the preheated gypsum mould, then drying at the temperature of 40 ℃ for 5 hours, drying at the temperature of 53 ℃ for 3.5 hours, drying at the temperature of 65 ℃ for 2 hours, drying at the temperature of 110 ℃ for 0.5 hour, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 40 ℃/h, preserving heat for 1h, heating to 300 ℃ at a speed of 50 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 80 ℃/h, preserving heat for 4h, heating to 900 ℃ at a speed of 200 ℃/h, preserving heat for 1h, heating to 1100 ℃ at a speed of 90 ℃/h, preserving heat for 1h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 5
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 41% of quartz glass powder, 12% of complex phase additive, 1.5% of dispersing agent, 4% of foaming agent, 0.1% of green body reinforcing agent and 41.4% of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 72% of zirconium oxide, 8% of magnesium oxide and 20% of titanium oxide.
The particle size of the quartz glass powder is 150 meshes.
The dispersant is prepared from the following components in a mass ratio of 1: 2: 1 of tetramethylammonium hydroxide, polyethylene glycol and polyethyleneimine.
The foaming agent is prepared from the following raw materials in a mass ratio of 2: 3 triethanolamine lauryl sulfate, n-propyl gallate.
The green body reinforcing agent is polyvinyl alcohol.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, preserving heat for 2 hours at 1200 ℃, then cooling and crushing, and mixing according to the weight ratio of M (material) M (ball) M (water) 1: 2: and (3) performing wet ball milling for 3 hours according to the proportion of 1.5, and drying to obtain the complex phase additive with the particle size of 15-30 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 130r/min, and mixing for 4 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at the temperature of 30 ℃/h, injecting ceramic slurry into the preheated gypsum mould, then drying at the temperature of 32 ℃ for 7 hours, drying at the temperature of 53 ℃ for 3 hours, drying at the temperature of 73 ℃ for 2 hours, drying at the temperature of 110 ℃ for 0.5 hour, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 20 ℃/h, preserving heat for 2h, heating to 300 ℃ at a speed of 45 ℃/h, preserving heat for 1h, heating to 500 ℃ at a speed of 80 ℃/h, preserving heat for 3h, heating to 900 ℃ at a speed of 200 ℃/h, preserving heat for 2h, heating to 1100 ℃ at a speed of 100 ℃/h, preserving heat for 1h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 6
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 42% of quartz glass powder, 4% of complex phase additive, 0.2% of dispersing agent, 1% of foaming agent, 0.02% of green body reinforcing agent and 52.78% of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 80% of zirconium oxide, 10% of magnesium oxide and 10% of titanium oxide.
The particle size of the quartz glass powder is 300 meshes.
The mass ratio of the dispersing agent is 2: 2: 5 polyethylene glycol, polyethyleneimine and citric acid.
The foaming agent is n-propyl gallate.
The blank reinforcing agent is sodium carboxymethyl cellulose.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, preserving heat at 1300 ℃ for about 2 hours, then cooling and crushing, and mixing according to the weight ratio of M (material) M (ball) M (water) 1: 2: 2, performing wet ball milling for 4 hours, and drying to obtain the complex phase additive with the particle size of 15-20 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 130r/min, and mixing for 5 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at 30 ℃ for 1h, injecting ceramic slurry into the preheated gypsum mould, then drying at 40 ℃ for 5 hours, drying at 53 ℃ for 4 hours, drying at 65 ℃ for 1 hour, drying at 100 ℃ for 1 hour, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 40 ℃/h, preserving heat for 2h, heating to 300 ℃ at a speed of 45 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 60 ℃/h, preserving heat for 2h, heating to 900 ℃ at a speed of 200 ℃/h, preserving heat for 2h, heating to 1100 ℃ at a speed of 120 ℃/h, preserving heat for 2h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 7
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 46 percent of quartz glass powder, 5 percent of complex phase additive, 1.3 percent of dispersant, 3 percent of foaming agent, 0.08 percent of green body reinforcing agent and 44.62 percent of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 75% of zirconium oxide, 20% of magnesium oxide and 5% of titanium oxide.
The particle size of the quartz glass powder is 600 meshes.
The dispersant is tetramethyl ammonium hydroxide.
The foaming agent is lauryl sulfate triethanolamine.
The blank reinforcing agent is sodium carboxymethyl cellulose.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, preserving heat for 2 hours at 1200 ℃, then cooling and crushing, and mixing according to the weight ratio of M (material) M (ball) M (water) 1: 2: and (3) performing wet ball milling for 3 hours according to the proportion of 1.5, and drying to obtain the complex phase additive with the particle size of 15-30 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 150r/min, and mixing for 3 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at 30 ℃ for 1h, injecting ceramic slurry into the preheated gypsum mould, then drying at 40 ℃ for 6 hours, drying at 45 ℃ for 6 hours, drying at 70 ℃ for 3 hours, drying at 110 ℃ for 0.5 hour, and demoulding to obtain a ceramic blank after drying.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 45 ℃/h, preserving heat for 2h, heating to 300 ℃ at a speed of 45 ℃/h, preserving heat for 1h, heating to 500 ℃ at a speed of 70 ℃/h, preserving heat for 4h, heating to 900 ℃ at a speed of 180 ℃/h, preserving heat for 2h, heating to 1100 ℃ at a speed of 90 ℃/h, preserving heat for 2h, and cooling to room temperature to obtain the quartz glass porous ceramic.
Example 8
The porous ceramic material of the embodiment comprises the following raw materials in percentage by mass: 44% of quartz glass powder, 9% of complex phase additive, 1% of dispersant, 5% of foaming agent, 0.2% of blank reinforcing agent and 40.8% of water.
The mass percentage of the zirconia, the magnesia and the titania in the complex phase additive is respectively as follows: 62% of zirconium oxide, 23% of magnesium oxide and 15% of titanium oxide.
The particle size of the quartz glass powder is 300 meshes.
The mass ratio of the dispersing agent is 2: 1 and polyvinylpyrrolidone.
The foaming agent is lauryl sulfate triethanolamine.
The green body reinforcing agent is prepared from the following components in percentage by mass of 1: 1 sodium carboxymethylcellulose and polyvinyl alcohol.
The preparation method of the quartz glass porous ceramic by adopting the porous ceramic material comprises the following steps:
s100, preparing a complex phase additive: weighing zirconium oxide, magnesium oxide and titanium oxide, fully mixing, putting into a sagger, preserving heat for 2 hours at 1200 ℃, then cooling and crushing, and mixing according to the weight ratio of M (material) M (ball) M (water) 1: 2: and (3) performing wet ball milling for 3 hours according to the proportion of 1.5, and drying to obtain the complex phase additive with the particle size of 18-25 mu m.
S200, mixing materials: weighing quartz glass powder, mixing the quartz glass powder and the complex phase additive, adding the mixture into a three-dimensional mixer at the rotating speed of 150r/min, and mixing for 5 hours to obtain a mixed material.
S300, preparing ceramic slurry: and mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH value to 7-9 by using ammonia water, and stirring uniformly to obtain the ceramic slurry.
S400, preparing a blank: preheating a gypsum mould at 30 ℃ for 1h, injecting ceramic slurry into the preheated gypsum mould, then drying at 35 ℃ for 8 hours, drying at 50 ℃ for 3 hours, drying at 70 ℃ for 3 hours, drying at 110 ℃ for 1 hour, and demoulding after drying to obtain a ceramic blank.
S500, sintering: putting the ceramic blank into a sintering furnace for sintering, wherein the sintering conditions are as follows: heating to 150 ℃ at a speed of 40 ℃/h, preserving heat for 1.5h, heating to 300 ℃ at a speed of 50 ℃/h, preserving heat for 2h, heating to 500 ℃ at a speed of 70 ℃/h, preserving heat for 4h, heating to 900 ℃ at a speed of 180 ℃/h, preserving heat for 1h, heating to 1100 ℃ at a speed of 90 ℃/h, preserving heat for 1h, and cooling to room temperature to obtain the quartz glass porous ceramic.
The quartz glass porous ceramics obtained in examples 1 to 8 were subjected to the performance test, and the test results are shown in Table 1.
TABLE 1
Figure BDA0003329269580000151
Figure BDA0003329269580000161
According to the test results, the quartz glass porous ceramic with high porosity, uniform pore diameter and high strength can be obtained by adopting the porous ceramic material and matching with the preparation method of the quartz glass porous ceramic, and the preparation method is easy to operate and suitable for industrial popularization.
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 (10)

1. The porous ceramic material is characterized by comprising the following raw materials in percentage by mass:
Figure FDA0003329269570000011
the complex phase additive is a mixture of two or three of zirconia, magnesia and titania.
2. The porous ceramic material of claim 1, wherein the mass percentages of the zirconia, the magnesia and the titania in the complex phase additive are respectively as follows: 60-80% of zirconium oxide, 0-30% of magnesium oxide and 0-40% of titanium oxide.
3. The porous ceramic material according to claim 1, wherein the silica glass frit has a particle size of one of 150 mesh, 300 mesh, and 600 mesh.
4. The porous ceramic material of claim 1, wherein the dispersant is one or more of tetramethylammonium hydroxide, polyethylene glycol, polyethyleneimine, polyvinylpyrrolidone, and citric acid.
5. The porous ceramic material of claim 1, wherein the foaming agent is one or both of triethanolamine lauryl sulfate and n-propyl gallate.
6. The porous ceramic material of claim 1, wherein the green body strengthening agent is one or both of sodium carboxymethylcellulose and polyvinyl alcohol.
7. The preparation method of the porous ceramic is characterized by comprising the following steps:
preparing a complex phase additive: weighing two or three of zirconia, magnesia and titania, fully mixing, storing at high temperature, cooling, crushing, ball-milling by a wet method, and drying to obtain a complex phase additive;
mixing materials: weighing quartz glass powder, and mixing the quartz glass powder with the complex phase additive to obtain a mixed material;
preparing ceramic slurry: mixing the mixed material with water, stirring uniformly to form water-based slurry, adding a dispersing agent, a foaming agent and a blank reinforcing agent, adjusting the pH to 7-9 by using inorganic base, and stirring uniformly to obtain ceramic slurry;
preparing a blank body: injecting the ceramic slurry into a preheated gypsum mold for drying, and demolding after drying to obtain a ceramic blank;
and (3) sintering: and sintering the ceramic blank in a sintering furnace, and cooling to room temperature to obtain the quartz glass porous ceramic.
8. The method for producing a porous ceramic according to claim 7, wherein the inorganic base is ammonia water.
9. The method for preparing a porous ceramic according to claim 7, wherein the step of preparing a green body comprises: the preheating condition of the gypsum mould is 30 ℃/h; and/or the presence of a gas in the gas,
after the ceramic slurry is injected into a preheated gypsum mold, the drying conditions are as follows: drying at 32-40 ℃ for 5-8 hours, drying at 45-53 ℃ for 3-6 hours, drying at 65-73 ℃ for 1-3 hours, and drying at 95-110 ℃ for 0.5-1 hour.
10. The method for preparing a porous ceramic according to claim 7, wherein in the sintering step, the ceramic green body is placed in a sintering furnace for sintering under the following conditions: heating to 150 ℃ at a speed of 20-50 ℃/h, preserving heat for 1-2 h, heating to 300 ℃ at a speed of 45-60 ℃/h, preserving heat for 1-2 h, heating to 500 ℃ at a speed of 60-80 ℃/h, preserving heat for 2-4 h, heating to 900 ℃ at a speed of 180-200 ℃/h, preserving heat for 1-2 h, heating to 1100 ℃ at a speed of 90-120 ℃/h, and preserving heat for 1-2 h.
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Publication number Priority date Publication date Assignee Title
CN107098717A (en) * 2017-04-07 2017-08-29 武汉理工大学 A kind of 3 D-printing molding method for preparing of filtering porous ceramics
WO2019223196A1 (en) * 2018-05-23 2019-11-28 苏州神鼎陶瓷科技有限公司 Oil-permeable porous ceramic, preparation method therefor, and application thereof in electronic cigarette
CN113480327A (en) * 2021-07-16 2021-10-08 深圳市吉迩科技有限公司 Atomizing core, porous ceramic and preparation method of porous ceramic

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107098717A (en) * 2017-04-07 2017-08-29 武汉理工大学 A kind of 3 D-printing molding method for preparing of filtering porous ceramics
WO2019223196A1 (en) * 2018-05-23 2019-11-28 苏州神鼎陶瓷科技有限公司 Oil-permeable porous ceramic, preparation method therefor, and application thereof in electronic cigarette
CN113480327A (en) * 2021-07-16 2021-10-08 深圳市吉迩科技有限公司 Atomizing core, porous ceramic and preparation method of porous ceramic

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