CN110627496A - Low-temperature preparation method of titanium oxide porous ceramic - Google Patents
Low-temperature preparation method of titanium oxide porous ceramic Download PDFInfo
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Abstract
The invention relates to a low-temperature preparation method of titanium oxide porous ceramic, and relates to the field of porous ceramic forming. The preparation method comprises the following steps: preparing ceramic slurry, namely adding titanium powder, adding a small amount of dispersing agent and gelatin, and putting the mixture into a ball milling tank for ball milling for a plurality of hours; freeze-drying the prepared ceramic slurry in a freeze dryer to obtain a blank; and then carrying out powder embedding sintering to obtain the porous ceramic. The invention has the advantages that the problems that the existing prepared porous ceramic material is generally closed-cell, the sintering temperature of the ceramic is too high, and the energy consumption is large are solved, and the prepared porous ceramic material has excellent performance and wide application prospect in the field of environment-friendly instruments. Meanwhile, the preparation method is simple and easy to operate, high in manufacturing efficiency and low in energy consumption, and is worthy of large-scale popularization and application.
Description
Technical Field
The invention belongs to the technical field of porous ceramic forming, and particularly relates to a low-temperature preparation method of titanium oxide porous ceramic.
Background
The porous ceramic has been widely used in various fields due to its excellent properties, and has good mechanical bearing and corrosion resistance, so that it is widely used in the field of environmental protection. But the production cost is always high due to the high sintering temperature of the oxide ceramics; on the other hand, the porous ceramic material prepared by the existing preparation method has a pore structure which is generally a closed pore structure, so that the application of the porous ceramic material in the field of filtration is influenced. And cracks are distributed on the surface of a product obtained by adopting reactive sintering, so that the service performance is seriously influenced.
Disclosure of Invention
The invention aims to solve the problems, provides a low-temperature preparation method of titanium oxide porous ceramic, solves the problems that the existing titanium oxide ceramic is too high in sintering temperature and cracks are easy to generate in a conventional porous material sintering blank, and reduces the high-temperature sintering cost of the oxide ceramic.
In order to achieve the purpose, the invention provides the following technical scheme:
a low-temperature preparation method of titanium oxide porous ceramic comprises the following steps:
s1: sequentially adding titanium powder, gelatin, a dispersing agent, deionized water and zirconia balls into a ball milling tank;
s2: placing the mixture into an oven, standing for 1-24 hours at the temperature of 30-100 ℃, and performing ball milling for 24-72 hours;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 12-72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃ to-60 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: and (3) putting the crucible into a muffle furnace, and preserving the heat for 1-24 hours at the temperature of below 900 ℃.
Further, in the step S1, the granularity of the titanium powder is 200-1000 meshes, and the mass fraction of the titanium powder is as follows: 5-50%, and the mass fraction of gelatin is as follows: 0-5 percent of dispersant, and the mass fraction of the dispersant is: 0 to 5 percent of the total weight of the solution, and the balance of deionized water.
Further, in the S1, the granularity of the titanium powder is 400-700 meshes, the mass fraction of the titanium powder in the slurry is 15-30%, the mass fraction of the gelatin is 2-3%, the mass fraction of the dispersing agent is 2-3%, and the balance is deionized water.
Further, in the step S2, the placing time in the oven is 4-20 hours, the ball milling time is 36-70 hours, and the volume ratio of the zirconia balls to the slurry is 2: 1.
further, in the step S2, the placing time in the oven is 12-18 hours, the ball milling time is 40-60 hours, and the volume ratio of the zirconia balls to the slurry is 2: 1.
further, in the S3, the freeze-drying time is 20-70 hours, and the temperature of the freeze dryer is-20 ℃ to-50 ℃.
Further, in the S3, the freeze-drying time is 30-60 hours, and the temperature of the freeze dryer is controlled to be-30 ℃ to-45 ℃.
Further, in the S4, the ceramic slurry contains 10-40% by mass of titanium powder, 1-4% by mass of gelatin and 1-4% by mass of a dispersing agent, and is sintered at a constant temperature in 500-900 ℃ air.
Further, in the S5, the temperature of the muffle furnace is controlled to be below 800 ℃, and the temperature is kept for 4-20 hours; and in the S5, controlling the temperature of the muffle furnace to be below 700 ℃, and preserving the heat for 5-18 hours.
Preferably, the used mold is a metal mold, a polytetrafluoroethylene mold or an alumina ceramic mold; the powder used for embedding the powder comprises the following components: alumina powder, silica powder, iron oxide powder, and other metal oxide powders.
Compared with the prior art, the invention has the beneficial effects that:
the invention effectively reduces the sintering temperature by 500-700 ℃ through reactive sintering, thereby greatly saving the cost. In addition, the porous structure of the titanium oxide porous ceramic prepared by the invention is a through hole structure, the problems that the porous ceramic material is generally closed hole, the sintering temperature of the ceramic is too high and the energy consumption is large in the prior art are solved, and the prepared porous ceramic has excellent performance, can be applied to filtering pollutants and has wide application prospect in the field of environment-friendly instruments. Meanwhile, the preparation method is simple and easy to operate, high in manufacturing efficiency and low in energy consumption, and is worthy of large-scale popularization and application.
Drawings
In order to more clearly illustrate the technical solution of the embodiment of the present invention, the drawings needed to be used in the description of the embodiment will be briefly introduced below, and it is obvious that the drawings in the following description are only for more clearly illustrating the embodiment of the present invention or the technical solution in the prior art, and for those skilled in the art, other drawings can be obtained according to the drawings without any creative effort.
FIG. 1 is a cross-sectional view of a porous ceramic of the present invention;
FIG. 2 is an SEM topography of the porous ceramic of the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described with reference to the following specific examples, which are provided for illustration only and are not intended to limit the present invention.
The low-temperature preparation method of the titanium oxide porous ceramic shown in the figure 1-2 is implemented according to the following steps:
s1: sequentially adding titanium powder, gelatin, a dispersing agent, deionized water and zirconia balls into a ball milling tank;
s2: placing the mixture into an oven, standing for 1-24 hours at the temperature of 30-100 ℃, and performing ball milling for 24-72 hours;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 12-72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃ to-60 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: and (3) putting the crucible into a muffle furnace, and preserving the heat for 1-24 hours at the temperature of below 900 ℃.
Preferably, the volume ratio of the zirconia balls to the slurry is 2: 1, the used mould is a metal mould, a polytetrafluoroethylene mould or an alumina ceramic mould; the powder used for embedding the powder comprises the following components: alumina powder, silica powder, iron oxide powder, and other metal oxide powders.
Embodiment 1:
the ball milling process comprises the following steps: adding 200-1000-mesh titanium powder (mass fraction is 5-50%), gelatin (mass fraction is 0-5%), dispersing agent (mass fraction is 0-5%), deionized water (40-95%) and zirconia balls into a ball milling tank in sequence, putting the ball milling tank into an oven for 1-24 hours, controlling the temperature at 30-100 ℃, and then carrying out ball milling for 24-72 hours.
And (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared container, putting the container into a freeze dryer, and freeze-drying for 12-72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃ to-60 ℃.
The sintering process comprises the following steps: and (3) putting the freeze-dried blank into a crucible, burying and sintering the powder, putting the crucible into a muffle furnace, and then preserving the heat for 1-24 hours at the temperature of below 900 ℃.
Embodiment 2:
the ball milling process comprises the following steps: adding titanium powder (15-40% by mass) of 300-800 meshes, gelatin (1-4% by mass), dispersing agent (1-4% by mass), deionized water (58-93%) and zirconia balls into a ball milling tank in sequence, placing the ball milling tank into an oven for 4-20 hours, controlling the temperature at 30-100 ℃, and then carrying out ball milling for 36-70 hours.
And (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared container, and then putting the container into a freeze dryer for freeze drying for 20-70 hours, wherein the temperature of the freeze dryer is controlled to be-20 ℃ to-50 ℃.
The sintering process comprises the following steps: and (3) putting the freeze-dried blank into a crucible, burying and sintering the powder, putting the crucible into a muffle furnace, and then preserving the heat for 4-20 hours at the temperature of below 800 ℃.
Embodiment 3:
the ball milling process comprises the following steps: adding titanium powder of 400-700 meshes (the mass fraction is 25-30%), gelatin (the mass fraction is 2-3%), dispersing agent (the mass fraction is 2-3%), deionized water (64-71%) and zirconia balls into a ball milling tank in sequence, putting the mixture into an oven for 12-18 hours, controlling the temperature at 30-100 ℃, and then carrying out ball milling for 40-60 hours.
And (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared container, putting the container into a freeze dryer, and freeze-drying for 30-60 hours, wherein the temperature of the freeze dryer is controlled to be-30-45 ℃.
The sintering process comprises the following steps: and (3) putting the freeze-dried blank into a crucible, burying and sintering the powder, putting the crucible into a muffle furnace, and then preserving the heat for 12-18 hours at the temperature below 700 ℃.
The beneficial effects of the present invention are demonstrated by the following examples:
example 1:
a low-temperature preparation method of titanium oxide porous ceramic is specifically carried out according to the following steps:
s1: ball milling: adding 500-mesh titanium powder (with the mass fraction of 25%), gelatin (with the mass fraction of 5%), a dispersing agent (with the mass fraction of 5%), deionized water and zirconia balls into a ball milling tank in sequence;
s2: and (3) after 12 hours of putting the mixture into an oven, controlling the temperature at 50 ℃, and carrying out ball milling for 72 hours, wherein the volume ratio of the zirconia balls to the slurry is 2: 1;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: the crucible was placed in a muffle furnace and held at 900 ℃ for 24 hours.
The porosity of the titanium oxide porous ceramic obtained in the embodiment is 55-70%, and the compressive strength is 30-40 MPa.
Example 2:
a low-temperature preparation method of titanium oxide porous ceramic is specifically carried out according to the following steps:
s1: ball milling: sequentially adding 800-mesh titanium powder (mass fraction is 20%), gelatin (mass fraction is 5%), dispersing agent (mass fraction is 5%), deionized water 70% and zirconia balls into a ball milling tank;
s2: and (3) after 12 hours of putting the mixture into an oven, controlling the temperature at 50 ℃, and carrying out ball milling for 72 hours, wherein the volume ratio of the zirconia balls to the slurry is 2: 1;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: the crucible was placed in a muffle furnace and held at 900 ℃ for 24 hours.
The porosity of the titanium oxide porous ceramic obtained in the embodiment is 65-80%, and the compressive strength is 25-40 MPa.
Example 3:
a low-temperature preparation method of titanium oxide porous ceramic is specifically carried out according to the following steps:
s1: ball milling: sequentially adding 1000-mesh titanium powder (mass fraction is 15%), gelatin (mass fraction is 1%), dispersing agent (mass fraction is 4%), deionized water 80% and zirconia balls into a ball milling tank;
s2: and (3) after 12 hours of putting the mixture into an oven, controlling the temperature at 50 ℃, and carrying out ball milling for 72 hours, wherein the volume ratio of the zirconia balls to the slurry is 2: 1;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: the crucible was placed in a muffle furnace and held at 800 ℃ for 24 hours.
The porosity of the titanium oxide porous ceramic obtained in the embodiment is 15% -30%, and the compressive strength is 20-35 MPa.
Example 4:
a low-temperature preparation method of titanium oxide porous ceramic is specifically carried out according to the following steps:
s1: ball milling: sequentially adding 1000-mesh titanium powder (mass fraction is 5%), gelatin (mass fraction is 2%), dispersing agent (mass fraction is 3%), deionized water 90% and zirconia balls into a ball milling tank;
s2: and (3) after 12 hours of putting the mixture into an oven, controlling the temperature at 50 ℃, and carrying out ball milling for 72 hours, wherein the volume ratio of the zirconia balls to the slurry is 2: 1;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: the crucible was placed in a muffle furnace and held at 900 ℃ for 24 hours.
The porosity of the titanium oxide porous ceramic obtained in the embodiment is 70-85%, and the compressive strength is 30-50 MPa.
Example 5:
a low-temperature preparation method of titanium oxide porous ceramic is specifically carried out according to the following steps:
s1: ball milling: sequentially adding 800-mesh titanium powder (mass fraction is 50%), gelatin (mass fraction is 4%), dispersing agent (mass fraction is 1%), deionized water 45% and zirconia balls into a ball milling tank;
s2: after being put into an oven for 12 hours, the temperature is controlled at 50 ℃, and ball milling is carried out for 72 hours;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: the crucible was placed in a muffle furnace and held at 700 ℃ for 24 hours.
The porosity of the titanium oxide porous ceramic obtained in the embodiment is 65-80%, and the compressive strength is 20-30 MPa.
The invention effectively reduces the sintering temperature by 500-700 ℃ through reactive sintering, thereby greatly saving the cost. In addition, the porous structure of the titanium oxide porous ceramic prepared by the invention is a through hole structure, the problems that the porous ceramic material is generally closed hole, the sintering temperature of the ceramic is too high and the energy consumption is large in the prior art are solved, and the prepared porous ceramic has excellent performance, can be applied to filtering pollutants and has wide application prospect in the field of environment-friendly instruments. Meanwhile, the preparation method is simple and easy to operate, high in manufacturing efficiency and low in energy consumption, and is worthy of large-scale popularization and application.
The details of the present invention not described in detail are prior art.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The low-temperature preparation method of the titanium oxide porous ceramic is characterized by comprising the following steps of:
s1: sequentially adding titanium powder, gelatin, a dispersing agent, deionized water and zirconia balls into a ball milling tank;
s2: placing the mixture into an oven, standing for 1-24 hours at the temperature of 30-100 ℃, and performing ball milling for 24-72 hours;
s3: and (3) forming of a blank body: pouring the prepared ceramic slurry into a prepared mould, putting the mould into a freeze dryer, and freeze-drying for 12-72 hours, wherein the temperature of the freeze dryer is controlled at-10 ℃ to-60 ℃;
s4: the sintering process comprises the following steps: putting the freeze-dried green body into a crucible, and burying and sintering the powder;
s5: and (3) putting the crucible into a muffle furnace, and preserving the heat for 1-24 hours at the temperature of below 900 ℃.
2. The low-temperature preparation method of titanium oxide porous ceramic according to claim 1, wherein in S1, the titanium powder has a particle size of 200-1000 meshes, and the mass fraction of the titanium powder is as follows: 5-50%, and the mass fraction of gelatin is as follows: 0-5 percent of dispersant, and the mass fraction of the dispersant is: 0 to 5 percent of the total weight of the solution, and the balance of deionized water.
3. The method for preparing the titanium oxide porous ceramic at the low temperature according to claim 1, wherein in S1, the titanium powder has a particle size of 400-700 meshes, the titanium powder in the slurry has a mass fraction of 15-30%, the gelatin has a mass fraction of 2-3%, the dispersant has a mass fraction of 2-3%, and the balance is deionized water.
4. The low-temperature preparation method of the titanium oxide porous ceramic according to claim 1, wherein in S2, the placing time in an oven is 4-20 hours, the ball milling time is 36-70 hours, and the volume ratio of the zirconia balls to the slurry is 2: 1.
5. the low-temperature preparation method of the titanium oxide porous ceramic according to claim 1, wherein in S2, the placing time in an oven is 12-18 hours, the ball milling time is 40-60 hours, and the volume ratio of the zirconia balls to the slurry is 2: 1.
6. the method for preparing titanium oxide porous ceramic at low temperature according to claim 1, wherein in S3, the freeze-drying time is 20-70 hours, and the temperature of the freeze dryer is controlled to-20 ℃ to-50 ℃.
7. The method for preparing titanium oxide porous ceramic at low temperature according to claim 1, wherein in S3, the freeze-drying time is 30-60 hours, and the temperature of the freeze dryer is controlled to-30 ℃ to-45 ℃.
8. The method for preparing the titanium oxide porous ceramic at the low temperature according to claim 1, wherein in S4, the ceramic slurry contains 10-40% by mass of titanium powder, 1-4% by mass of gelatin and 1-4% by mass of dispersing agent, and is sintered at a constant temperature in air at 500-900 ℃.
9. The method for preparing the titanium oxide porous ceramic at the low temperature according to claim 1, wherein in S5, the temperature of a muffle furnace is controlled to be below 800 ℃, and the temperature is kept for 4-20 hours; and in the S5, controlling the temperature of the muffle furnace to be below 700 ℃, and preserving the heat for 5-18 hours.
10. The low-temperature preparation method of titanium oxide porous ceramic according to any one of claims 1 to 9, wherein the mold is a metal mold, a polytetrafluoroethylene mold or an alumina ceramic mold; the powder used for embedding the powder comprises the following components: alumina powder, silica powder, iron oxide powder, and other metal oxide powders.
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| CN111675533A (en) * | 2020-05-29 | 2020-09-18 | 北方民族大学 | High conductivity β' -Al2O3Method for preparing ceramic electrolyte |
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Application publication date: 20191231 |