CN114368966A - Zirconia-based all-ceramic denture and preparation method thereof - Google Patents

Zirconia-based all-ceramic denture and preparation method thereof Download PDF

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CN114368966A
CN114368966A CN202110327610.2A CN202110327610A CN114368966A CN 114368966 A CN114368966 A CN 114368966A CN 202110327610 A CN202110327610 A CN 202110327610A CN 114368966 A CN114368966 A CN 114368966A
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zirconia
ceramic
denture
parts
silicon
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CN114368966B (en
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王焕平
裴魏魏
曹永盛
荣华
李登豪
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Zhejiang Dansden Biomaterials Co ltd
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Zhejiang Dansden Biomaterials Co ltd
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Abstract

The invention relates to a zirconia-based full-ceramic denture and a preparation method thereof, wherein the core layer comprises the following components in parts by mass: ZrO (ZrO)290 to 94 portions of Y2O35-9 parts of Al2O30.1-0.5 part of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20-0.2 part, and the mass parts of the shell layer are as follows: CaCO324.5 to 49.5 portions of SiO245-50 parts of MgO, 0-25 parts of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20 to 0.2 portion. The preparation process comprises the following steps: dry pressing and isostatic pressing the raw material of the nuclear layer, pre-sintering and carving to obtain a zirconia-based denture biscuit; simultaneously, calcining the raw material of the shell layer, adding deionized water, a dispersing agent and an adhesive, and performing ball milling and mixing to obtain calcium-magnesium-silicon-based ceramic slurry; and coating the calcium-magnesium-silicon-based ceramic slurry on the surface of the zirconia-based denture biscuit and sintering to obtain the zirconia-based all-ceramic denture. The zirconia-based fully-ceramic denture has good jade texture and is closer to the natural color of natural teeth.

Description

Zirconia-based all-ceramic denture and preparation method thereof
Technical Field
The invention relates to a dental material and a preparation method thereof, in particular to a zirconia-based fully-ceramic denture and a preparation method thereof, belonging to the technical field of material science.
Background
Since the 90 s of the last century, zirconia ceramics have begun to be used as coping materials for dental fixed restorations. However, pure zirconia ceramics have great brittleness due to weak capability of resisting crack generation and development; in order to solve the brittleness problem of pure zirconia ceramics, oxide modifiers such as yttrium oxide, magnesium oxide, cesium oxide, calcium oxide and the like are mainly added to improve the toughness of the zirconia ceramics at present. Among zirconia ceramics stabilized by various oxide modifiers, tetragonal polycrystalline zirconia stabilized by yttria has become the ceramic material with the widest application range and the highest strength at present, and particularly, the tetragonal polycrystalline zirconia is 3Y-ZrO with the yttria content of about 3 mol percent2Powder (3Y-TZP), alreadyBecomes the preferred material for the current porcelain false tooth repair.
In China, a plurality of patents relating to zirconia ceramics for full-ceramic false teeth exist, for example, a patent with the application number of 2006101176270 discloses 'machinable colored zirconia ceramics and application thereof', wherein a coloring material is added into zirconia powder, and the ceramic block is prepared by presintering at 900-1000 ℃ after isostatic pressing; when the porcelain block is used, firstly, the shape of the false tooth is turned by a lathe according to a three-dimensional digital design, and then the false tooth is sintered into the ceramic at the temperature of 1450-1520 ℃. The invention patent with the application number of 200510134251.X discloses a zirconia all-ceramic dental restoration material and a preparation method thereof, wherein 5-10% of boron-aluminum-silicon glass or hydroxyapatite is added into Y-TZP zirconia powder as a fluxing agent, and 3-4% of a binder are added, and the zirconia all-ceramic dental restoration material with the bending strength of 1000-1300 MPa is obtained by mixing, granulating, isostatic pressing, binder removing and sintering at 1250-1400 ℃.
Although the Y-TZP zirconia ceramic has excellent mechanical properties, the ceramic is in a dead white color after being sintered, has poor permeability under natural light, has no luster under the condition of not being polished into a mirror surface, and has larger difference with the natural jade texture of human teeth, so that the aesthetic requirements of people are difficult to meet in the era of increasingly pursuing beauty and vividness at present. In order to improve the jade texture and the aesthetic property of the Y-TZP zirconia ceramic false tooth, the zirconia ceramic false tooth is often sintered into porcelain at about 1500 ℃, then a layer of porcelain powder is coated on the surface of the porcelain, and then the porcelain is baked at 850-960 ℃, so that the prepared zirconia ceramic false tooth has better jade texture and aesthetic property, but the porcelain is very easy to break due to the fact that the strength of the porcelain powder is less than 100 MPa.
Disclosure of Invention
The invention aims to provide a zirconia-based all-ceramic denture with good jade texture and higher strength and a preparation method thereof.
The zirconia-based full-ceramic false tooth has a core-shell structure; the core layer comprises the following raw materials in parts by mass: ZrO (ZrO)290 to 94 portions of Y2O35-9 parts of Al2O30.1-0.5 part of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20-0.2 parts of the total; the shell layer comprises the following raw materials in parts by mass: CaCO324.5 to 49.5 portions of SiO245-50 parts of MgO, 0-25 parts of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20 to 0.2 portion.
The preparation of the zirconia-based fully-ceramic denture comprises the following steps:
(1) ZrO is weighed according to a certain mass ratio2、Y2O3、Al2O3、Fe2O3、Er2O3、MnO2Mixing the powder, and then putting the mixture into a mould to be dry-pressed and molded at 3-20 MPa; vacuum packaging the molded product by using a plastic bag, and then performing isostatic pressing under 150-300 MPa; putting the product subjected to isostatic pressing into a sintering furnace, heating to 950-1100 ℃ from room temperature, and preserving heat for 2-4 hours for pre-sintering to obtain a zirconia-based ceramic block;
(2) weighing CaCO according to a certain mass ratio3、SiO2、MgO、Fe2O3、Er2O3、MnO2Adding deionized water into the powder, ball-milling and mixing for 4-24 hours by using a zirconia mill, drying for 4-24 hours at 80-120 ℃, and calcining for 2-4 hours at 1100-1250 ℃ to obtain calcium-magnesium-silicon ceramic powder;
(3) adding a dispersing agent according to 0-0.2% of the total mass of the calcium-magnesium-silicon ceramic powder, adding an adhesive according to 0.1-0.5% of the total mass of the powder, adding deionized water according to 0.5-5 times of the total mass of the powder, and then carrying out ball milling and mixing for 4-24 hours by using a zirconia grinding medium to obtain calcium-magnesium-silicon-based ceramic slurry;
(4) carving a zirconia-based denture biscuit on a zirconia-based ceramic block by using a carving machine, soaking the zirconia-based denture biscuit in calcium-magnesium-silicon-based ceramic slurry, taking out and draining, or coating the calcium-magnesium-silicon-based ceramic slurry on the surface of the zirconia-based denture biscuit by using a writing brush, then drying in an oven at 90-120 ℃, and then sintering in a sintering furnace at 1400-1550 ℃ for 2-4 hours to obtain the zirconia-based ceramic denture.
In the preparation process, the dispersing agent is one or more of fatty alcohol-polyoxyethylene ether, sodium alkyl benzene sulfonate and organic silicon resin, and the adhesive is one or more of polyvinyl alcohol, methyl cellulose and acrylic resin.
The invention has the following beneficial characteristics: by calcining CaCO3、MgO、SiO2The mixture of the calcium, magnesium and silicon ceramic powder is synthesized, the melting temperature of the calcium, magnesium and silicon ceramic powder is about 1350 ℃, the difference between the melting temperature and the sintering temperature (1400-1550 ℃) of zirconia ceramic is only 50-200 ℃, and the calcium, magnesium and silicon ceramic powder has good sintering matching property. When the calcium-magnesium-silicon ceramic slurry is coated on the surface of the zirconia-based denture biscuit, the calcium-magnesium-silicon ceramic slurry can penetrate into the gap of the zirconia-based denture biscuit, then the zirconia-based denture biscuit can be sintered into ceramic in the co-sintering process at 1400-1550 ℃, and the calcium-magnesium-silicon ceramic slurry can be melted, penetrated and coated on the surface of the zirconia-based denture to form perfect combination, so that a core-shell structure is obtained. Because the expansion coefficient of the calcium-magnesium-silicon ceramic is slightly lower than that of the zirconia-based ceramic, the sintered calcium-magnesium-silicon ceramic forms good matching with the zirconia-based denture, and the higher bending strength of the calcium-magnesium-silicon ceramic is utilized to improve the overall mechanical property of the zirconia-based denture. The calcium-magnesium-silicon ceramic is a white substance with jade texture, so that the zirconia false tooth has the appearance similar to a real tooth; meanwhile, the calcium-magnesium-silicon ceramic has good biocompatibility. Furthermore, by adding Fe2O3、Er2O3、MnO2The color of the zirconia-based denture is adjusted, so that the product of the invention is closer to the natural color of natural teeth.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1:
90 parts of ZrO are weighed according to the mass ratio29 parts of Y2O30.5 part of Al2O30.01 part of Fe2O30.49 parts of Er2O3Mixing is carried outMixing, and then putting into a mould for dry pressing and forming at 20 MPa; vacuum packaging the formed product by using a plastic bag, and then performing isostatic pressing under 300 MPa; and putting the product subjected to isostatic pressing into a sintering furnace, heating to 1100 ℃ from room temperature, and preserving heat for 2 hours for pre-sintering to obtain the zirconia-based ceramic block.
24.5 parts of CaCO by mass ratio350 parts of SiO225 parts of MgO and 0.49 part of Fe2O30.01 part of Er2O3Adding deionized water into the powder, ball-milling and mixing the mixture for 24 hours by using a zirconia mill, drying the mixture for 4 hours at 120 ℃, and calcining the dried mixture for 4 hours at 1100 ℃ to obtain the calcium-magnesium-silicon ceramic powder. And adding 0.2 part of fatty alcohol-polyoxyethylene ether serving as a dispersing agent, 0.5 part of polyvinyl alcohol serving as an adhesive and 500 parts of deionized water into the calcium-magnesium-silicon ceramic powder, and then carrying out ball milling and mixing for 4 hours by using a zirconia mill to obtain the calcium-magnesium-silicon-based ceramic slurry.
Carving a zirconia-based denture biscuit on a zirconia-based ceramic block by using a carving machine, soaking the zirconia-based denture biscuit in calcium-magnesium-silicon-based ceramic slurry, taking out and draining, then drying in a drying oven at 90 ℃, and then sintering in a sintering furnace at 1550 ℃ for 2 hours to obtain the zirconia-based ceramic.
In order to test the strength of the zirconia-based full-ceramic false tooth, 10 zirconia-based biscuit with the length of 35mm, the width of 5mm and the height of 4mm are carved on a zirconia-based ceramic block by a carving machine, then the strip zirconia-based biscuit is soaked in calcium-magnesium-silicon-based ceramic slurry and taken out for draining, then the strip zirconia-based biscuit is put into an oven for drying at 90 ℃, and then the strip zirconia-based ceramic is put into a sintering furnace for sintering at 1550 ℃ for 2 hours to obtain the strip zirconia-based ceramic. The zirconia-based ceramic was subjected to a three-point bending strength test using an electronic universal tester, and it was found that the zirconia-based ceramic had no significant ceramic chipping on the surface and had an average bending strength of 1127 MPa.
Example 2:
weighing 94 parts of ZrO according to the mass ratio25 parts of Y2O30.29 part of Al2O30.5 part of Fe2O30.01 part by weightEr2O30.2 part of MnO2Mixing, and then putting the mixture into a mould to be dry-pressed and molded at 3 MPa; vacuum packaging the formed product by using a plastic bag, and then performing isostatic pressing under 150 MPa; and putting the product subjected to isostatic pressing into a sintering furnace, heating to 950 ℃ from room temperature, and preserving heat for 4 hours for pre-sintering to obtain the zirconia-based ceramic block.
49.5 parts of CaCO by mass ratio349.3 parts of SiO20.5 part of Fe2O30.5 parts of Er2O30.2 part of MnO2Adding deionized water into the powder, ball-milling and mixing for 4 hours by using a zirconia mill, drying for 24 hours at 80 ℃, and calcining for 2 hours at 1250 ℃ to obtain the calcium-magnesium-silicon ceramic powder. And adding 0.1 part of methylcellulose serving as a bonding agent into the calcium-magnesium-silicon ceramic powder, adding 50 parts of deionized water, and then carrying out ball milling and mixing for 24 hours by using a zirconia milling medium to obtain the calcium-magnesium-silicon-based ceramic slurry.
Carving a zirconia-based denture biscuit on a zirconia-based ceramic block by using a carving machine, then coating calcium-magnesium-silicon-based ceramic slurry on the surface of the zirconia-based denture biscuit by using a writing brush, then drying the zirconia-based denture biscuit in an oven at 120 ℃, and then sintering the zirconia-based denture biscuit in a sintering furnace at 1400 ℃ for 4 hours to obtain the zirconia-based ceramic denture.
In order to test the strength of the zirconia-based full-ceramic false tooth, 10 zirconia-based blanks with the length of 35mm, the width of 5mm and the height of 4mm are carved on a zirconia-based ceramic block by a carving machine, then calcium-magnesium-silicon-based ceramic slurry is coated on the surface of the strip-shaped zirconia-based blank by a writing brush, then the strip-shaped zirconia-based blank is placed into an oven to be dried at the temperature of 120 ℃, and then the strip-shaped zirconia-based ceramic is placed into a sintering furnace to be sintered for 4 hours at the temperature of 1400 ℃ to obtain the strip-shaped zirconia-based ceramic. The zirconia-based ceramic is subjected to a three-point bending strength test by using an electronic universal testing machine, and the zirconia-based ceramic is found to have no obvious ceramic collapse on the surface and the average bending strength of 985 MPa.
Example 3:
93.1 parts of ZrO were weighed in a mass ratio26 parts of Y2O30.1 part of Al2O30.2 part of Fe2O30.5 parts of Er2O30.1 part of MnO2Mixing, and then putting the mixture into a mould to be dry-pressed and molded at 10 MPa; vacuum packaging the formed product by using a plastic bag, and then performing isostatic pressing under 250 MPa; and putting the product subjected to isostatic pressing into a sintering furnace, heating to 1050 ℃ from room temperature, and preserving heat for 3 hours for pre-sintering to obtain the zirconia-based ceramic block.
44.7 parts of CaCO by mass ratio345 parts of SiO210 parts of MgO and 0.01 part of Fe2O30.19 parts of Er2O30.1 part of MnO2The powder is added with deionized water and ball-milled and mixed for 12 hours by a zirconia mill, then dried for 8 hours at 100 ℃, and then calcined for 2 hours at 1200 ℃, so as to obtain the calcium-magnesium-silicon ceramic powder. Adding 0.1 part of organic silicon resin serving as a dispersing agent, 0.1 part of acrylic resin and 0.1 part of polyvinyl alcohol serving as an adhesive into the calcium-magnesium-silicon ceramic powder, adding 200 parts of deionized water, and performing ball milling and mixing for 8 hours by using a zirconia milling medium to obtain the calcium-magnesium-silicon-based ceramic slurry.
Carving a zirconia-based denture biscuit on a zirconia-based ceramic block by using a carving machine, soaking the zirconia-based denture biscuit in calcium-magnesium-silicon-based ceramic slurry, taking out, draining, drying in an oven at 100 ℃, and sintering in a sintering furnace at 1500 ℃ for 3 hours to obtain the zirconia-based denture.
In order to test the strength of the zirconia-based full-ceramic false tooth, 10 zirconia-based biscuit with the length of 35mm, the width of 5mm and the height of 4mm are carved on a zirconia-based ceramic block by a carving machine, then the strip zirconia-based biscuit is soaked in calcium-magnesium-silicon-based ceramic slurry and taken out for draining, then the strip zirconia-based biscuit is put into an oven for drying at 100 ℃, and then the strip zirconia-based ceramic is put into a sintering furnace for sintering at 1500 ℃ for 3 hours to obtain the strip zirconia-based ceramic. The zirconia-based ceramic is subjected to a three-point bending strength test by using an electronic universal testing machine, and the zirconia-based ceramic is found to have no obvious ceramic collapse on the surface and the average bending strength of 1274 MPa.

Claims (3)

1. Zirconia baseAn all-ceramic denture, characterized by having a core-shell structure; the core layer comprises the following raw materials in parts by mass: ZrO (ZrO)290 to 94 portions of Y2O35-9 parts of Al2O30.1-0.5 part of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20-0.2 parts of the total; the shell layer comprises the following raw materials in parts by mass: CaCO324.5 to 49.5 portions of SiO245-50 parts of MgO, 0-25 parts of Fe2O30.01-0.5 part of Er2O30.01 to 0.5 part by weight of MnO20 to 0.2 portion.
2. The zirconia-based fully ceramic denture of claim 1, wherein the preparation process comprises the steps of:
(1) ZrO is weighed according to a certain mass ratio2、Y2O3、Al2O3、Fe2O3、Er2O3、MnO2Mixing the powder, and then putting the mixture into a mould to be dry-pressed and molded at 3-20 MPa; vacuum packaging the molded product by using a plastic bag, and then performing isostatic pressing under 150-300 MPa; putting the product subjected to isostatic pressing into a sintering furnace, heating to 950-1100 ℃ from room temperature, and preserving heat for 2-4 hours for pre-sintering to obtain a zirconia-based ceramic block;
(2) weighing CaCO according to a certain mass ratio3、SiO2、MgO、Fe2O3、Er2O3、MnO2Adding deionized water into the powder, ball-milling and mixing for 4-24 hours by using a zirconia mill, drying for 4-24 hours at 80-120 ℃, and calcining for 2-4 hours at 1100-1250 ℃ to obtain calcium-magnesium-silicon ceramic powder;
(3) adding a dispersing agent according to 0-0.2% of the total mass of the calcium-magnesium-silicon ceramic powder, adding an adhesive according to 0.1-0.5% of the total mass of the powder, adding deionized water according to 0.5-5 times of the total mass of the powder, and then carrying out ball milling and mixing for 4-24 hours by using a zirconia grinding medium to obtain calcium-magnesium-silicon-based ceramic slurry;
(4) carving a zirconia-based denture biscuit on a zirconia-based ceramic block by using a carving machine, soaking the zirconia-based denture biscuit in calcium-magnesium-silicon-based ceramic slurry, taking out and draining, or coating the calcium-magnesium-silicon-based ceramic slurry on the surface of the zirconia-based denture biscuit by using a writing brush, then drying in an oven at 90-120 ℃, and then sintering in a sintering furnace at 1400-1550 ℃ for 2-4 hours to obtain the zirconia-based ceramic denture.
3. The method for preparing a zirconia-based all-ceramic denture according to claim 2, wherein the dispersant is one or more of fatty alcohol-polyoxyethylene ether, sodium alkyl benzene sulfonate and organic silicon resin, and the adhesive is one or more of polyvinyl alcohol, methyl cellulose and acrylic resin.
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