CN114656260A - Preparation method and application of medical high-permeability zirconia ceramic sintered body - Google Patents

Preparation method and application of medical high-permeability zirconia ceramic sintered body Download PDF

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CN114656260A
CN114656260A CN202210429988.8A CN202210429988A CN114656260A CN 114656260 A CN114656260 A CN 114656260A CN 202210429988 A CN202210429988 A CN 202210429988A CN 114656260 A CN114656260 A CN 114656260A
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zirconia
sintered body
powder
zirconium
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唐蜜雪
曹峰
高源�
朱晓东
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Yantai Hejing Ceramic New Materials Co ltd
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Abstract

The invention relates to a preparation method and application of a medical high-oxygen-permeability zirconium ceramic sintered body, wherein the preparation method comprises the following steps: s1, mixing soluble zirconium salt, yttrium salt and magnesium oxide, dissolving in water, and carrying out hydrothermal reaction; s2, carrying out pH adjustment on the solution after the hydrothermal reaction, adjusting the pH to be alkaline, washing, drying, carrying out heat treatment, and cooling to obtain zirconium oxide powder; s3, adding water into the zirconia powder for sanding to obtain zirconia slurry, then adding a binder, a dispersing agent and a softening agent for granulation to obtain zirconia granulated powder; and S4, preparing the granulated powder into a green body, and sintering the green body to obtain the zirconia ceramic sintered body. The role of magnesium oxide is mainly to concentrate at high concentrations at the grain boundaries, thereby preventing too fast crystal growth during sintering and promoting porosity reduction. The zirconia ceramic sintered body obtained by the preparation method has excellent mechanical property, strong light transmission and good jade porcelain feeling, and is close to real teeth of people.

Description

Preparation method and application of medical high-permeability zirconia ceramic sintered body
Technical Field
The invention relates to a preparation method and application of a medical high-oxygen-permeability zirconium ceramic sintered body, belonging to the technical field of ceramic material preparation.
Background
Under the trend of increasingly aging global population, the demand of dentures is rapidly increasing. The zirconia ceramics has the reputation of ceramic steel, has excellent mechanical properties (bending strength and fracture toughness), good biocompatibility and beautiful and natural color, is considered as an ideal all-ceramic repair material, gradually replaces alumina ceramics, and plays an important role in repairing hard tissue damage.
The zirconia ceramics are polycrystalline sintered bodies formed and sintered by powder, and the microstructure of the zirconia ceramics consists of crystal grains, grain boundaries among the crystal grains, impurities and air holes. When light is incident into the ceramic, the ceramic grains, the grain boundary, the impurities and the air holes refract and scatter the light, so that light loss is caused, and the light transmittance of the ceramic is greatly reduced.
The zirconia material commonly used at present is tetragonal zirconia partially stabilized by yttria or cesium oxide, the color of a sintered body of the tetragonal zirconia has no transparency, and the tetragonal zirconia is treated by the following methods in order not to influence the aesthetic property:
firstly, a layer of color-shading porcelain is added on the surface of the material to shade the white color of the material or the zirconium oxide blank is soaked in a coloring liquid to be colored and then sintered, so that the surface of the material presents the color similar to that of a tooth. However, the connection between zirconia and porcelain is weak, so that the porcelain breaking problem is easy to occur, and the repair failure is often caused.
And (II) a coloring method is adopted to replace the traditional method of the color-shading porcelain to solve the problem of false white and opaque teeth, and the coloring method comprises an endogenous coloring method and an exogenous coloring method. The endogenous coloring adopts the rare earth metal oxide with color mixed in the powder, and the method can play a role in enabling the tooth coping to have color. The extrinsic dyeing is to soak the ceramic presintered body in a dyeing solution for 1-30min, dry and sinter to form. Although the coloring method is fast and easy to operate, the problem of tooth pseudo-white and non-transparent is solved, the coloring method has more influence factors and is easy to cause uneven dyeing, and after dyeing, false tooth processing procedures such as porcelain glazing and the like are still needed, so that the possibility of false tooth porcelain collapse still exists, the product application failure is finally caused, and meanwhile, the dip dyeing process can cause the change of some physical and chemical characteristics of a porcelain block blank, and the physical properties such as the strength and the like of a finished porcelain block are influenced.
And thirdly, obtaining the zirconium oxide ceramic block with gradation change in color by adopting a multilayer blank making technology of materials with different colors. The color of the ceramic block blank obtained by adopting multilayer blank making is changed and is rigid and uncoordinated. Although theoretically, the more the layers are, the more natural and uniform the color change tends to be, from the aspect of the forming process, the more the layers are not possible to be added, and the processing difficulty and the cost are increased.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the preparation method of the medical high-transparency zirconia ceramic sintered body, and the zirconia ceramic sintered body obtained by the preparation method has excellent mechanical property, strong light transmission and good jade porcelain feeling, and is close to the real teeth of people.
The technical scheme for solving the technical problems is as follows: a preparation method of a medical high-permeability zirconia ceramic sintered body comprises the following steps:
s1, mixing and dissolving soluble zirconium salt, yttrium salt and magnesium oxide in water to obtain a mixed solution, and carrying out hydrothermal reaction;
s2, carrying out pH adjustment on the solution after the hydrothermal reaction, adjusting the pH to be alkaline, and carrying out washing, drying, heat treatment and cooling to obtain zirconium oxide powder;
s3, adding water into the zirconia powder, sanding to obtain zirconia slurry, adding a binder, a dispersing agent and a softening agent into the zirconia slurry, and granulating to obtain zirconia granulated powder;
and S4, preparing the granulated powder into a green body, and sintering the green body to obtain the zirconia ceramic sintered body.
Further, in step S1, the molar ratio of the soluble zirconium salt to the yttrium salt is (95-97): (3-5), wherein the magnesium oxide accounts for 0.3-5% of the mass of the soluble zirconium salt.
The soluble zirconium salt is zirconium oxychloride octahydrate; the yttrium salt is yttrium oxide or yttrium nitrate, but is not limited to the yttrium salt.
Further, in step S1, the hydrothermal reaction conditions are: hydrothermal synthesis is carried out for 6-100h at the temperature of 150 ℃ and 260 ℃, and after hydrothermal reaction, the grain size range of the zirconia crystal in the solution is 40-100 nm.
Further, in step S2, the pH adjustment process includes: and adjusting the pH of the solution after the hydrothermal reaction to 9-11 by using ammonia water.
Further, in step S2, the temperature range of the heat treatment is 700-.
Preferably, in step S2, the temperature range of the heat treatment is 1100-1200 ℃.
Further, in step S3, 50-100 parts by weight of zirconia powder; 50-100 parts of water; 0.1-8.0 parts of binder; 0.1-5.0 parts of a dispersant; 0.1-0.5 part of softening agent.
Further, the dispersant is at least one of acrylic acid, polyacrylic acid, acrylamide and polyurethane;
the binder is at least one of polyvinyl alcohol, polyethylene glycol, acrylic resin and carboxymethyl cellulose.
Further, in step S3, after granulation by a spray method, sieving is performed to obtain zirconia granulated powder having a particle size range of 40 to 100 um.
Further, in step S4, the granulation powder is made into a green body by adopting a dry pressing forming method, the pressure of the dry pressing is 20-30Mpa, and the time of the dry pressing is 1-15 min; the sintering temperature of the green body is 900-1600 ℃, and the sintering time is 1-5 h.
Preferably, the sintering temperature is 1350-.
The invention also discloses application of the medical high-permeability zirconia ceramic sintered body, and the zirconia ceramic sintered body is applied to false teeth.
The invention has the beneficial effects that:
1) the tetragonal zirconia has anisotropy, and the light scattering in the crystal can reduce the light transmittance, and the technical scheme of the invention adds the yttrium oxide and sets the corresponding proportion to ensure that the zirconia is cubic zirconia which is isotropic and has low light scattering and good translucency; 2) the zirconia ceramic sintered body is doped with a proper amount of magnesia, and the magnesia is gathered at the grain boundary in a high concentration, so that the crystal is prevented from excessively fast growing in the sintering process, and the air holes are promoted to be reduced;
3) in the preparation process of the zirconia ceramic sintered body, the obtained zirconia granulation powder has uniform particles, good sphericity, good fluidity and excellent forming performance, and the addition of the softener coats a layer of lubricant on the surfaces of the particles, so that the forming density of a blank is improved, the friction force between the edge of the blank and the inner side of a mold is reduced, the loss of the mold is reduced, and the adhesion between the upper surface and the lower surface of the blank and the mold is prevented;
4) the density of the ceramic block of the zirconia ceramic sintered body measured by Archimedes can reach 6.07-6.09g/cm3The light transmittance of visible light measured under the thickness of 1mm is 35-50%, a three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, the bending resistance strength is 800-;
5) the zirconia ceramic sintered body has excellent mechanical property, strong light transmission and good jade porcelain feeling, and is close to real teeth of people.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the aforementioned objects, features and advantages of the invention more comprehensible. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
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 herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Example 1
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium oxide and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium oxide is 97: 3, the magnesium oxide is 0.3 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 150 ℃ for 80 h;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 11 by using ammonia water, washing the solution by using a membrane until the conductivity of slurry is 100us/cm, performing spray drying, performing heat treatment on the powder at 1000 ℃, keeping the temperature for 2h, cooling the powder to room temperature to obtain zirconia powder, performing ball milling on the zirconia powder again, adding water in the ball milling process to obtain zirconia slurry, wherein the particle size of zirconium beads used in the ball milling process is 0.2-0.3 mm;
s3, adding polyacrylic acid, polyvinyl alcohol and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder, water, polyacrylic acid, polyvinyl alcohol and the softening agent is 70: 50:0.5: 3: 0.1. and uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain 75-95 um zirconia granulated powder.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa, 10 min.
S5, pre-sintering the green body at 1450 ℃ for 4h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic is obtained.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3And the light transmittance of visible light measured under the thickness of 1mm is 41%, and the three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, wherein the bending resistance strength is 1200 Mpa.
Example 2
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium oxide and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium oxide is 96.5: 3.5, the magnesium oxide is 0.4 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 170 ℃ for 72 h;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 10.8 by using ammonia water, washing the solution by using a membrane until the conductivity of slurry is 100us/cm, carrying out spray drying, carrying out heat treatment on the powder at 1100 ℃, keeping the temperature for 2h, cooling the powder to room temperature to obtain zirconia powder, carrying out ball milling on the zirconia powder again, adding water in the ball milling process to obtain zirconia slurry, wherein the particle size of zirconium beads used in the ball milling process is 0.4-0.5 mm; s3, adding polyacrylic acid, polyvinyl alcohol and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder, water, polyacrylic acid, polyvinyl alcohol and the softening agent is 70: 60: 0.5: 1: 0.1. and uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain zirconia granulated powder of 100-150 um.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa, 10 min.
S5, pre-sintering the green body at 1500 ℃ for 4h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic is obtained.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3And the light transmittance of visible light measured under the thickness of 1mm is 45%, and the three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, wherein the bending resistance strength is 1172 Mpa.
Example 3
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium oxide and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium oxide is 96: 4, the magnesium oxide is 0.3 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 180 ℃ for 30 h;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 10.5 by using ammonia water, washing the solution by a membrane until the conductivity of slurry is 100us/cm, carrying out spray drying, carrying out heat treatment on the powder at 1150 ℃, keeping the temperature for 2h, cooling to room temperature to obtain zirconia powder, carrying out ball milling on the zirconia powder again, adding water in the ball milling process to obtain zirconia slurry, wherein the particle size of zirconium beads used in the ball milling process is 0.5-0.6 mm;
s3, adding polyacrylic acid, polyvinyl alcohol and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder, water, polyacrylic acid, polyvinyl alcohol and a softening agent is 50:50: 1: 2: 0.1. and uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain 75-95 um zirconia granulated powder.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa for 10 min.
And S5, pre-sintering the green body at 1530 ℃ for 4h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3And the light transmittance of visible light measured under the thickness of 1mm is 48%, and the obtained ceramic block is subjected to three-point bending resistance test by a three-point bending resistance method, wherein the bending resistance strength is 1100 Mpa.
Example 4
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium nitrate and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium nitrate is 97: 3, the magnesium oxide is 3 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 230 ℃ for 70 h;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 10 by using ammonia water, washing the solution by using a membrane until the conductivity of slurry is 100us/cm, performing spray drying, performing thermal treatment on the powder at 900 ℃, keeping the temperature for 2h, cooling the powder to room temperature to obtain zirconia powder, performing ball milling on the zirconia powder again, adding water in the ball milling process to obtain zirconia slurry, wherein the particle size of zirconium beads used in the ball milling process is 0.1-0.2 mm;
s3, adding acrylamide, acrylic resin and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder, water, acrylamide, acrylic resin and a softening agent is 50: 100: 0.2: 3: 0.5. and uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain zirconia granulated powder of 45-80 um.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa for 10 min.
S5, pre-sintering the green body at 1550 ℃ for 3h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic is obtained.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3Transmittance of visible light measured at a thickness of 1mmThe light rate is 42%, and the three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, and the bending strength is 1190 Mpa.
Example 5
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium nitrate and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium nitrate is 96: 4, the magnesium oxide is 5 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 200 ℃ for 90 hours;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 11 by using ammonia water, washing the solution by using a membrane until the conductivity of slurry is 100us/cm, performing spray drying, performing heat treatment on the powder at 1100 ℃, keeping the temperature for 2h, cooling the powder to room temperature to obtain zirconia powder, performing ball milling on the zirconia powder again, adding water in the ball milling process to obtain zirconia slurry, wherein the particle size of zirconium beads used in the ball milling process is 0.4-0.5 mm; (ii) a
S3, adding polyurethane, carboxymethyl cellulose and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder to the water to the polyurethane to the carboxymethyl cellulose to the softening agent is 50:50:0.5:2: 0.2. And uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain zirconia granulated powder of 60-90 um.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa, 10 min.
S5, pre-sintering the green body at 1350 ℃ for 5h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3And the light transmittance of visible light measured under the thickness of 1mm is 45%, and the obtained ceramic block is subjected to three-point bending resistance test by a three-point bending resistance method, wherein the bending resistance strength is 1120 MPa.
Example 6
S1, mixing and dissolving zirconium oxychloride octahydrate, yttrium nitrate and magnesium oxide in water to prepare a mixed solution, wherein the molar ratio of the zirconium oxychloride octahydrate to the yttrium nitrate is 95: 5, the magnesium oxide is 0.8 percent of the mass fraction of the zirconium oxychloride octahydrate; carrying out hydrothermal reaction on the mixed solution at 180 ℃ for 20 h;
s2, adjusting the pH value of the solution after the hydrothermal reaction to 11 by using ammonia water, performing heat treatment at 1100 ℃ after membrane washing, drying and grinding, keeping the temperature for 4 hours, cooling to room temperature to obtain zirconium oxide powder, performing ball milling on the zirconium oxide powder again, adding water in the ball milling process to obtain the zirconium oxide powder, wherein the particle size of zirconium beads used in the ball milling process is 0.05-0.06 mm;
s3, adding acrylic acid, polyethylene glycol and a softener into the zirconia slurry; wherein the mass ratio of the zirconia powder, the water, the acrylic acid, the polyethylene glycol and the softening agent is 90:100:2:8: 0.5. And uniformly mixing, granulating to obtain the powder for the high-permeability zirconia sintered body, and performing spray granulation to obtain 50-75 um zirconia granulated powder.
S4, carrying out dry pressing on the zirconia granulation powder to prepare a green body, wherein the dry pressing conditions are as follows: 23MPa for 10 min.
S5, pre-sintering the green body at 1500 ℃ for 2h, wherein the heating rate is 40 ℃/h, and sintering the zirconia ceramic is obtained.
The density of the sintered zirconia ceramic body obtained in this example was 6.08g/cm3The visible light transmittance measured at a thickness of 1mm was 48%, and the obtained ceramic block was subjected to a three-point bending test by a three-point bending method, the bending strength being 1170 Mpa.
Comparative example 1
The same procedure as in example 1 was used, with the difference that: no magnesium oxide was added.
The density of the sintered zirconia ceramic compact obtained in this comparative example was 6.08g/cm3And the light transmittance of visible light measured under the thickness of 1mm is 37%, and the obtained ceramic block is subjected to a three-point bending resistance test by a three-point bending resistance method, wherein the bending resistance strength is 960 Mpa.
Through the performance conditions of the zirconia ceramic sintered bodies in the embodiment 1 and the comparative example 1, it is obvious that the addition of the magnesia can effectively improve the light transmission condition of the zirconia ceramic sintered bodies, and is more beneficial to the application of the ceramic sintered bodies in false teeth.
Comparative example 2
The same procedure as in example 1 was followed, except that: no softener was added: after spray granulation, the obtained zirconia granulated powder has high crushing strength and is not beneficial to molding
The density of the sintered zirconia ceramic compact obtained in this comparative example was 6.08g/cm3The visible light transmittance measured under the thickness of 1mm is 41%, and the three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, wherein the bending strength is 1120Mpa
According to the performance conditions of the zirconia ceramic sintered body products of the embodiment 1 and the comparative example 2, it can be obviously seen that in the preparation process, the addition of the softener does not influence the light transmittance and the strength of the final sintered body product, but can improve the forming performance.
Comparative example 3
The same procedure as in example 1 was followed, except that: the conditions of the hydrothermal reaction are as follows: hydrothermal synthesis is carried out for 5h at 130 ℃, and after hydrothermal reaction, the zirconia powder in the solution is 230-375nm nano powder; and after spray granulation, obtaining 320um-386um zirconia granulation powder.
The density of the sintered zirconia ceramic compact obtained in this comparative example was 6.08g/cm3The light transmittance of visible light measured under the thickness of 1mm is 32%, the three-point bending resistance test is carried out on the prepared porcelain block by adopting a three-point bending resistance method, and the bending strength is 740Mpa
According to the performance conditions of the zirconia ceramic sintered body products of the embodiment 1 and the comparative example 3, it is obvious that the zirconia ceramic sintered body products obtained under the hydrothermal synthesis condition have better light transmission condition and strength in the preparation process, and are more beneficial to application in false teeth.
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 should be subject to the appended claims.

Claims (10)

1. The preparation method of the medical high-permeability zirconia ceramic sintered body is characterized by comprising the following steps:
s1, mixing and dissolving soluble zirconium salt, yttrium salt and magnesium oxide in water to obtain a mixed solution, and carrying out hydrothermal reaction;
s2, carrying out pH adjustment on the solution after the hydrothermal reaction, adjusting the pH to be alkaline, washing, drying, carrying out heat treatment, and cooling to obtain zirconium oxide powder;
s3, adding water into the zirconia powder, sanding to obtain zirconia slurry, adding a binder, a dispersing agent and a softening agent into the zirconia slurry, and granulating to obtain zirconia granulated powder;
and S4, preparing the granulated powder into a green body, and sintering the green body to obtain the zirconia ceramic sintered body.
2. The preparation method of the medical high oxygen permeability zirconium ceramic sintered body according to claim 1, characterized in that, in the step S1, the molar ratio of the soluble zirconium salt and yttrium salt is (95-97): (3-5), wherein the magnesium oxide accounts for 0.3-5% of the mass of the soluble zirconium salt.
3. The method for preparing the medical zirconium ceramic sintered body with high oxygen permeability according to claim 1, wherein in step S1, the hydrothermal reaction conditions are as follows: hydrothermal synthesis is carried out for 6-100h at the temperature of 150 ℃ and 260 ℃; after hydrothermal reaction, the grain diameter of the zirconia crystal in the solution is in the range of 40-100 nm.
4. The method for preparing the medical high oxygen permeability zirconium ceramic sintered body according to claim 1, wherein in step S2, the process of pH adjustment is as follows: and adjusting the pH of the solution after the hydrothermal reaction to 9-11 by using ammonia water.
5. The method for preparing the medical zirconium oxide ceramic sintered body with high oxygen permeability as claimed in claim 1, wherein in step S2, the temperature of the heat treatment is 700-1200 ℃, the temperature is kept for 1-5h, and the temperature is reduced to room temperature, so as to obtain zirconium oxide powder.
6. The method for preparing the medical high oxygen permeability zirconium ceramic sintered body according to claim 1, wherein in step S3, 50-100 parts by weight of zirconium oxide powder; 50-100 parts of water; 0.1-8.0 parts of binder; 0.1-2.0 parts of a dispersant; 0.1-0.5 part of softening agent.
7. The method for preparing the medical zirconium ceramic sintered body with high oxygen permeability according to claim 6, wherein the dispersant is at least one of acrylic acid, polyacrylic acid, acrylamide and polyurethane;
the binder is at least one of polyvinyl alcohol, polyethylene glycol, acrylic resin and carboxymethyl cellulose.
8. The method for preparing a sintered zirconia ceramic body for medical use according to claim 1, wherein in step S3, the powder is granulated by spraying and then sieved to obtain zirconia granulated powder having a particle size range of 40 to 100 μm.
9. The method for preparing the medical zirconium oxide ceramic sintered body with high oxygen permeability as claimed in claim 1, wherein in step S4, the green body made of the granulated powder is prepared by a dry pressing method, the pressure of the dry pressing is 20-30Mpa, and the time of the dry pressing is 1-15 min; the sintering temperature of the green body is 900-1600 ℃, and the sintering time is 1-5 h.
10. Use of a sintered body of medical high-permeability zirconia ceramic according to any one of claims 1 to 9, wherein the sintered body of zirconia ceramic is used for a denture.
CN202210429988.8A 2022-04-22 2022-04-22 Preparation method and application of medical high-permeability zirconia ceramic sintered body Pending CN114656260A (en)

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