CN114455947A - Preparation method of zirconia ceramic material with porous structure - Google Patents
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Abstract
The invention discloses a preparation method of a zirconia ceramic material with a porous structure. The method comprises the following steps: (1) preparing zirconia ceramic slurry; (2) molding; (3) drying at room temperature; (4) and (5) sintering. The preparation method of the invention is directly injection-molded after preparing the water-based ceramic slurry, and the molded ligand can be dried and compact at room temperature, thereby omitting the process of external pressure of the traditional porous ceramic molding, simplifying the process, reducing the preparation cost and simultaneously. The sintering temperature is fixed, the temperature rise in the sintering process is simple, and the pore-forming agent can be completely decomposed to leave a porous structure.
Description
Technical Field
The invention relates to a preparation method of a zirconia ceramic material with a porous structure, belonging to the technical field of biological medicines.
Background
The porous ceramic is an inorganic non-metallic material containing many pores, and the required physical and chemical properties of heat, electricity, magnetism, light and the like are achieved by utilizing the structure and the surface area of the pores in the material and combining the material of the material, so that the porous ceramic can be used as a material for filtering, separating, dispersing, permeating, heat insulating, heat exchanging, sound absorbing, sound insulating, adsorbing, carrying, reacting, sensing and the like. Compared with glass fiber, metal and the like, the porous ceramic has excellent properties such as uniformly distributed pores, high porosity, high specific surface area, low density, low thermal conductivity and unique physical surface characteristics, selective permeability to liquid and gas, and energy absorption characteristics; in addition, the ceramic material has the characteristics of high temperature resistance, corrosion resistance, good stability and excellent thermal shock resistance, so that the porous ceramic is widely applied to the fields of chemical industry, petroleum, smelting, medicine, environmental protection, aerospace, aviation and the like.
The zirconia porous ceramics have a unique structure, so that the zirconia porous ceramics show a plurality of unique physical and chemical properties. (1) The chemical stability is good. Through material selection and process control, the porous ceramic suitable for various environments with corrosive candles can be prepared. (2) The pore passages are distributed uniformly. (3) High temperature resistance and good thermal shock resistance. The ceramic matrix has excellent quick heating and quenching resistance, generally higher melting point and good thermal stability. (4) Porous ceramics have uniform permeability, tortuous flow paths, and energy absorbing properties, and also exhibit selective permeability or pressure barrier properties to liquid and gaseous media. (5) High specific surface area and controllable low resistance fluid fluidity. (6) Low density and low thermal conductivity. (7) Good mechanical properties at room temperature and high temperature.
The preparation method of the zirconia porous ceramic mainly comprises the following steps:
(1) organic foam impregnation method. The porous ceramic with the through hole net structure is prepared by taking sponge with a three-dimensional open hole net structure as a template, uniformly coating ceramic dish materials on the surface of the sponge, removing redundant materials, and then carrying out reduction drying and high-temperature sintering. The method has simple process and lower cost, and is a method for preparing the porous ceramic which is generally used in the industry at present.
(2) Foaming method. The process is to make the prepared ceramic charge generate bubbles by a physical or chemical method, and then to carry out solidification, drying and sintering, thereby preparing the porous material. The physical method is to add a surfactant to introduce bubbles by vigorous stirring. The chemical method is to generate gas by adding organic or inorganic compound substances and carrying out chemical reaction, and the process is not easy to control.
(3) Sol-gel method. The principle of the method is that colloidal particles are mutually stacked to form a porous structure in the gelation process, and then small pores are left in the drying and sintering processes of the gel, so that the porous material with a controllable structure is formed. The price is high.
(4) And (4) freeze drying. The preparation process of the process comprises the steps of freezing the ceramic slurry to change a liquid-phase solvent into solid-phase ice, then reducing the pressure to dry a ligand, sublimating the ice to directly change the ice into vapor to be discharged, and finally sintering at high temperature to obtain the porous ceramic. The price is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a zirconia ceramic material with a porous structure, which has the advantages of no need of external pressure forming, simple process, single sintering temperature, simple temperature rise and cost saving.
The invention is realized by the following technical scheme:
a preparation method of a porous zirconia ceramic material comprises the following steps:
(1) preparing zirconia ceramic slurry: mixing a ceramic dispersant and water, adding a ceramic sintering aid after mixing, adding water glass and a ceramic adhesive after mixing, adding zirconia ceramic powder after stirring and mixing, adding a polymer microsphere pore-forming agent after stirring and mixing, and mixing to obtain slurry;
(2) molding: injecting the slurry into a mold, placing the mold at room temperature, solidifying the slurry, and demolding to obtain a water-containing ceramic blank;
(3) drying at room temperature: continuously drying at room temperature to obtain a ceramic blank;
(4) and (3) sintering: and sintering the ceramic blank body in a sintering furnace at the temperature of 1700-1900 ℃ to obtain the zirconia ceramic material.
The preparation method of the porous zirconia ceramic material comprises the following steps of, by weight, 80-100 parts of zirconia ceramic powder: 0.5-1 part of ceramic dispersant, 30-50 parts of water, 1-2.5 parts of ceramic sintering aid, 4-8 parts of water glass, 4-8 parts of ceramic sintering adhesive and 40-60 parts of polymer microsphere pore-forming agent.
In the preparation method of the zirconia ceramic material with the porous structure, the particle size of the zirconia ceramic powder is 700-900 nm.
According to the preparation method of the porous zirconia ceramic material, the ceramic dispersing agent is polyethylene glycol, sodium carboxymethyl cellulose and sodium polymethacrylate which are prepared according to the proportion of 2:3: 2.
The preparation method of the porous zirconia ceramic material comprises the following steps: low molecular weight polymethacrylate/protein collagen complexes.
The preparation method of the porous zirconia ceramic material comprises the following steps: the polypropylene microspheres are 20-100 mu m in size.
According to the preparation method of the porous zirconia ceramic material, the ceramic sintering aid is nano magnesia.
The preparation method of the porous zirconia ceramic material comprises the step of drying the mold at 60-85 ℃ and then using the mold, wherein the mold is a gypsum mold or a silica gel mold.
The preparation method of the porous zirconia ceramic material comprises the following specific steps of molding and sintering: injecting the ceramic slurry into a mold, standing for 10-14h, drying at 45-55 ℃ for 3.5-4.5h, demolding to obtain a complete ceramic blank, standing the ceramic blank at room temperature for 24-48h, using a high-temperature ceramic sintering furnace, raising the temperature from room temperature to 1800 ℃, and keeping the temperature at 1800 ℃ for sintering for 2-3 h. Obtaining the zirconia porous ceramic material.
According to the preparation method of the porous zirconia ceramic material, the temperature rise rate of the sintering furnace is 15 ℃/min.
The invention achieves the following beneficial effects:
the preparation method of the invention is directly injection-molded after preparing the ceramic slurry, and the molded ligand can be dried and compact in room temperature environment, thus saving the process of external pressure of the traditional porous ceramic molding, greatly simplifying the process, reducing the cost, simultaneously having single sintering temperature and simple temperature rise, and the polymer pore-forming agent can be completely decomposed to leave a porous structure.
The invention adopts the polypropylene microspheres as the polymer pore-forming agent, the polymer pore-forming agent can be completely decomposed to leave a porous structure, the porous structure is regular into spheres, the cavities are communicated with each other, and the porous structure has good water permeability and is beneficial to the attachment of other tissues or media.
Drawings
FIG. 1 is an SEM representation of a porous ceramic material of zirconia.
Fig. 2 is a three-dimensional modeling image of a zirconia porous ceramic material.
Detailed Description
The invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
A preparation method of a porous zirconia ceramic material comprises the following steps:
1. drying the gypsum mould at 60-85 deg.C
2. Grinding the zirconia ceramic powder in a ball mill, and sieving to obtain the zirconia ceramic powder with the particle size of 700-900 nm;
3. preparing injection zirconia ceramic slurry:
3.1 adding 0.5 part of ceramic dispersant and 30 parts of water, and mechanically stirring for 20-40 min;
3.2 adding 2.5 parts of nano magnesium oxide, and mechanically stirring for 20-40 min;
3.3 adding 4 parts of water glass and 4 parts of ceramic adhesive, and stirring for 10-30 min;
3.4 adding 80 parts of the ground zirconia ceramic powder, and stirring for 10-30 min;
3.5 adding 50 parts of polymer microsphere pore-forming agent, and stirring for 60-80 min; obtaining zirconia ceramic slurry;
4. injecting the ceramic slurry into a mold, standing for 12h, drying at 50 ℃ for 4h, and demolding to obtain a complete ceramic blank;
5. placing the ceramic blank body at room temperature for 24h to evaporate water in the blank body to form a compact structure;
6. sintering of zirconia ceramic: and (3) using a high-temperature ceramic sintering furnace, raising the temperature from room temperature to 1800 ℃ at the rate of 15 ℃/min, and sintering for 2h while keeping the temperature at 1800 ℃ to obtain the zirconia porous ceramic material.
Wherein the ceramic dispersant is polyethylene glycol, sodium carboxymethylcellulose and sodium polymethacrylate which are prepared according to the proportion of 2:3: 2; the ceramic adhesive is a low molecular weight poly methacrylate/protein collagen compound; the polymer microsphere pore-forming agent is polypropylene microspheres.
SEM characterization was performed on the zirconia porous ceramic material, and the ceramic cross section is shown in FIG. 1. The zirconia ceramics also has obvious porous structure inside. The diameter of the holes is 5-10 μm. A three-dimensional modeled image of the zirconia porous ceramic material is shown in figure 2.
Example 2
A preparation method of a porous zirconia ceramic material comprises the following steps:
(1) preparing zirconia ceramic slurry: mechanically stirring ceramic dispersant and water for 20-40min, adding nano magnesium oxide after mixing, and mechanically stirring for 20-40 min; after mixing, adding water glass and ceramic adhesive, and mechanically stirring for 10-30 min; adding zirconia ceramic powder after mixing, stirring for 10-30min, adding a polymer microsphere pore-forming agent after mixing, stirring for 60-80min, and mixing to obtain slurry;
(2) and (3) sintering: injecting the ceramic slurry into a mold, standing for 10-14h, drying at 45-55 ℃ for 3.5-4.5h, demolding to obtain a complete ceramic blank, standing the ceramic blank at room temperature for 24-48h, using a high-temperature ceramic sintering furnace, heating at the rate of 15 ℃/min to 1800 ℃ from the room temperature, and keeping the temperature of 1800 ℃ for sintering for 2-3 h. Obtaining the zirconia porous ceramic material.
Wherein, the zirconia ceramic powder is 100 parts by weight, and the rest raw materials are respectively: 1 part of ceramic dispersant, 50 parts of water, 1 part of nano magnesium oxide, 8 parts of water glass, 8 parts of ceramic sintering agent and 40 parts of polymer microsphere pore-forming agent.
The mold is a silica gel mold, and the mold is dried at the temperature of 60-85 ℃ and then used. The ceramic dispersant is polyethylene glycol, sodium carboxymethylcellulose and sodium polymethacrylate are prepared according to the proportion of 2:3: 2; the ceramic adhesive is a low molecular weight poly methacrylate/protein collagen compound; the polymer microsphere pore-forming agent is polypropylene microspheres.
Example 3
A preparation method of a porous zirconia ceramic material comprises the following steps:
(1) preparing zirconia ceramic slurry: mechanically stirring ceramic dispersant and water for 20-40min, adding nano magnesium oxide after mixing, and mechanically stirring for 20-40 min; after mixing, adding water glass and ceramic adhesive, and mechanically stirring for 10-30 min; adding zirconia ceramic powder after mixing, stirring for 10-30min, adding a polymer microsphere pore-forming agent after mixing, stirring for 60-80min, and mixing to obtain slurry;
(2) and (3) sintering: injecting the ceramic slurry into a mold, standing for 10-14h, drying at 45-55 ℃ for 3.5-4.5h, demolding to obtain a complete ceramic blank, standing the ceramic blank at room temperature for 24-48h, using a high-temperature ceramic sintering furnace, heating at the rate of 15 ℃/min to 1800 ℃ from the room temperature, and keeping the temperature of 1800 ℃ for sintering for 2-3 h. Obtaining the zirconia porous ceramic material.
Wherein, the zirconia ceramic powder is calculated by 90 parts by weight, and the rest raw materials are respectively in parts by weight: 0.8 part of ceramic dispersant, 40 parts of water, 2 parts of nano magnesium oxide, 5 parts of water glass, 5 parts of ceramic sintering agent and 60 parts of polymer microsphere pore-forming agent.
The mould is a gypsum mould, and the mould is dried at the temperature of 60-85 ℃ and then used. The ceramic dispersant is polyethylene glycol, sodium carboxymethylcellulose and sodium polymethacrylate are prepared according to the proportion of 2:3: 2; the ceramic adhesive is a low molecular weight poly methacrylate/protein collagen compound; the polymer microsphere pore-forming agent is polypropylene microspheres.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various improvements and modifications without departing from the technical principle of the present invention, and those improvements and modifications should be considered as the protection scope of the present invention.
Claims (10)
1. A preparation method of a zirconia ceramic material with a porous structure is characterized by comprising the following steps:
(1) preparing zirconia ceramic slurry: mixing a ceramic dispersant and water, adding a ceramic sintering aid after mixing, adding water glass and a ceramic adhesive after mixing, adding zirconia ceramic powder after stirring and mixing, adding a polymer microsphere pore-forming agent after stirring and mixing, and mixing to obtain slurry;
(2) molding: injecting the slurry into a mold, placing the mold at room temperature, and demolding after the slurry is solidified to obtain a water-containing ceramic blank;
(3) drying at room temperature: continuously drying at room temperature to obtain a ceramic blank;
(4) and (3) sintering: and sintering the ceramic blank body in a sintering furnace at the temperature of 1700-1900 ℃ to obtain the zirconia ceramic material.
2. The preparation method of the porous zirconia ceramic material as claimed in claim 1, wherein the weight parts of the zirconia ceramic powder are 80-100 parts, and the weight parts of the rest raw materials are respectively: 0.5-1 part of ceramic dispersant, 30-50 parts of water, 1-2.5 parts of ceramic sintering aid, 4-8 parts of water glass, 4-8 parts of ceramic sintering adhesive and 40-60 parts of polymer microsphere pore-forming agent.
3. The method for preparing a zirconia ceramic material with a porous structure as claimed in claim 1 or 2, wherein the particle size of the zirconia ceramic powder is 700-900 nm.
4. The preparation method of the porous zirconia ceramic material according to claim 1 or 2, wherein the ceramic dispersant is polyethylene glycol, sodium carboxymethylcellulose and sodium polymethacrylate, and the ratio of the polyethylene glycol to the sodium carboxymethylcellulose to the sodium polymethacrylate is 2:3: 2.
5. The method for preparing a porous zirconia ceramic material according to claim 1 or 2, wherein the ceramic binder is: low molecular weight polymethacrylate/protein collagen complexes.
6. The method for preparing the zirconia ceramic material with the porous structure as claimed in claim 1 or 2, wherein the polymer microsphere pore-forming agent is: the polypropylene microspheres are 20-100 mu m in size.
7. The method for preparing a zirconia ceramic material with a porous structure as claimed in claim 1 or 2, wherein the ceramic sintering aid is nano magnesia.
8. The method for preparing the porous zirconia ceramic material according to claim 1 or 2, wherein the mold is a plaster mold or a silica gel mold, and the mold is dried at 60-85 ℃ and then used.
9. The preparation method of the porous zirconia ceramic material as claimed in claim 8, wherein the specific steps of forming and sintering are as follows: injecting the ceramic slurry into a mold, standing for 10-14h, drying at 45-55 ℃ for 3.5-4.5h, demolding to obtain a complete ceramic blank, standing the ceramic blank at room temperature for 24-48h, using a high-temperature ceramic sintering furnace, raising the temperature from room temperature to 1800 ℃, and keeping the temperature at 1800 ℃ for sintering for 2-3 h. Obtaining the zirconia porous ceramic material.
10. The method for preparing a porous zirconia ceramic material according to claim 9, wherein the temperature rise rate of the sintering furnace is 15 ℃/min.
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| CN115947597A (en) * | 2022-09-30 | 2023-04-11 | 武汉科技大学 | Micro-closed-pore light-weight zirconia refractory material and preparation method thereof |
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| CN115947597B (en) * | 2022-09-30 | 2023-08-04 | 武汉科技大学 | Micro-closed-cell lightweight zirconia refractory material and preparation method thereof |
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