CN116003124A - Gradient zirconia ceramic block and preparation method thereof - Google Patents
Gradient zirconia ceramic block and preparation method thereof Download PDFInfo
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- CN116003124A CN116003124A CN202210279388.8A CN202210279388A CN116003124A CN 116003124 A CN116003124 A CN 116003124A CN 202210279388 A CN202210279388 A CN 202210279388A CN 116003124 A CN116003124 A CN 116003124A
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 title claims abstract description 300
- 239000000919 ceramic Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000002002 slurry Substances 0.000 claims abstract description 61
- 239000000843 powder Substances 0.000 claims abstract description 52
- 229910002076 stabilized zirconia Inorganic materials 0.000 claims abstract description 40
- 239000003381 stabilizer Substances 0.000 claims abstract description 20
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 20
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000004519 manufacturing process Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 26
- 239000000654 additive Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 25
- 239000007790 solid phase Substances 0.000 claims description 25
- 230000000996 additive effect Effects 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 230000003321 amplification Effects 0.000 claims description 10
- 238000003199 nucleic acid amplification method Methods 0.000 claims description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 230000005484 gravity Effects 0.000 claims description 9
- DLRVVLDZNNYCBX-UHFFFAOYSA-N Polydextrose Polymers OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(O)O1 DLRVVLDZNNYCBX-UHFFFAOYSA-N 0.000 claims description 6
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 3
- 229920001100 Polydextrose Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 3
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 3
- 229930006000 Sucrose Natural products 0.000 claims description 3
- 230000001133 acceleration Effects 0.000 claims description 3
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 3
- 239000008103 glucose Substances 0.000 claims description 3
- 239000001259 polydextrose Substances 0.000 claims description 3
- 229940035035 polydextrose Drugs 0.000 claims description 3
- 235000013856 polydextrose Nutrition 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 239000005720 sucrose Substances 0.000 claims description 3
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- 230000003287 optical effect Effects 0.000 abstract description 12
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 4
- 230000008025 crystallization Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000012071 phase Substances 0.000 description 9
- 238000003754 machining Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 238000000635 electron micrograph Methods 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000010987 cubic zirconia Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 description 1
- 238000002490 spark plasma sintering Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 1
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Abstract
The invention discloses a gradient zirconia ceramic block for dentistry and a preparation method thereof, belonging to the field of materials for dental restorations. The zirconia ceramic block provided by the invention adopts yttrium stabilized zirconia powder taking yttrium oxide as a stabilizer as an initial raw material, the optical transparency of the zirconia ceramic obtained after crystallization and sintering is changed in a gradient way in at least one space dimension, and meanwhile, the content of yttrium oxide is not changed in the dimension in which the optical transparency is changed in a gradient way; the preparation method of the zirconia ceramic block comprises the steps of firstly preparing zirconia slurry, and then obtaining the zirconia ceramic block with the gradient distribution of the particle size of the powder by utilizing the difference of the sedimentation speeds of the powder with different particle sizes in the zirconia slurry in a hypergravity environment. The zirconia ceramic block for dentistry has stable quality, simple preparation method and high efficiency, and is suitable for mass production.
Description
Technical Field
The invention relates to the field of ceramic materials for dental restorations, in particular to a gradient zirconia ceramic block and a preparation method thereof.
Background
Zirconia ceramics have reliable biostability and excellent mechanical properties, and the machining of zirconia ceramics by cutting is one of the main methods currently in the field of dental restorative materials. Pure zirconia ceramics cannot be used directly and stabilizers must be added. The commonly used stabilizer comprises rare earth metal oxides such as yttrium oxide, alkaline earth metal oxides such as magnesium oxide and calcium oxide, and the stabilizer in the zirconia ceramic for the denture is mainly yttrium oxide.
In the related art Transparent Nanometric Cubic and Tetragonal Zirconia Obtained by High-Pressure Pulsed Electric Current Sintering, adv.funct.mate, 17 (2007), 3267, three crystal structures of a main monoclinic phase, a tetragonal phase and a cubic phase of zirconia ceramics are described, wherein the tetragonal phase and the cubic phase are two main crystal structures of zirconia ceramics for denture. The content of yttrium oxide affects the crystal structure of zirconium oxide, and further affects the optical transparency and mechanical strength of the zirconium oxide porcelain block for the denture. When the mole percentage of the yttrium oxide in the yttrium stabilized zirconia powder is about 3%, the zirconia is in a tetragonal crystal form; when the mole percentage of the yttrium oxide in the yttrium stabilized zirconia powder is more than 8 percent, the zirconium oxide is in a cubic crystal form; the optical transparency of cubic phase zirconia ceramics is better than tetragonal phase zirconia ceramics, but the mechanical strength of cubic phase zirconia is inferior to tetragonal phase zirconia ceramics.
The optical clarity of natural teeth exhibits a gradual change of gradient from root to tip. The preparation of the gradient zirconia ceramic block for the false tooth is one of important directions in the field of the ceramic false tooth at present, and can simulate the gradual change effect of the optical transparency of the natural tooth. At present, the preparation of gradient zirconia can be realized by stacking yttrium stabilized zirconia powder with different stabilizer contents for a plurality of times in the related art, but the transparency change among the obtained ceramic layers is discontinuous, the zirconia sintering power of different stabilizer contents among different ceramic layers is different, the warping phenomenon caused by different material shrinkage easily occurs during lamination sintering, the whole technological process is required to be adjusted according to the properties of the ceramic layers, the procedure is complicated, and the actual production is not facilitated. The transparency of zirconia ceramics is affected by the grain size in the zirconia ceramics in addition to the yttria content of the stabilizer. However, the classification of the powder with different sizes cannot be realized by a simple powder paving technology.
Disclosure of Invention
In order to solve the defects existing in the related art, the invention aims to provide a gradient zirconia ceramic block and a preparation method thereof. Different from the prior method for paving the yttria-stabilized zirconia powder with different contents layer by layer, the invention adopts zirconia with single yttria content as a raw material, and realizes gradient distribution of the particle size of the powder in the porcelain block by utilizing different deposition speeds of particles with different sizes under a hypergravity environment; after the prepared zirconia ceramic block is crystallized and sintered, the zirconia ceramic with optical transparency changing in a gradient way in at least one space dimension is obtained, and meanwhile, the content of yttrium oxide does not change in the dimension with optical transparency changing in a gradient way.
The aim of the invention is achieved by the following specific technical scheme:
in one aspect, the invention provides a dental gradient zirconia ceramic block, which is formed by a zirconia slurry through a supergravity method, wherein the zirconia slurry comprises yttrium-stabilized zirconia powder, an additive and water, the yttrium-stabilized zirconia powder accounts for 10-55% of the volume of the zirconia slurry, the additive accounts for 0.05-10% of the volume of the zirconia slurry, and the balance is water.
As previously described: if the stabilizer is used too much, the tetragonal zirconia content is reduced, and the mechanical properties of the porcelain blocks are insufficient; if the stabilizer is used too little, the content of cubic zirconia is too low, and the light transmittance of the porcelain block is reduced. For this reason, the yttrium-stabilized zirconia powder is used by adopting yttrium oxide as a stabilizer, and the content of yttrium oxide in the yttrium-stabilized zirconia powder is 2.5-5.5 mol percent.
In another aspect, the zirconia ceramic block is used for making dental restorations.
In yet another aspect, a method for preparing the zirconia ceramic block is provided, wherein the zirconia slurry is molded by a hypergravity method, and the method specifically comprises the following steps:
1) Yttrium stabilized zirconia powder taking yttrium oxide as a stabilizer is taken as a main raw material, and is mixed with an additive and deionized water to prepare zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry under the condition of supergravity;
3) Drying the solid phase substance to obtain a zirconia ceramic block primary blank;
4) And carrying out appearance processing on the zirconia ceramic block primary blank to obtain the zirconia ceramic block.
Optionally, in step 1), the content of the yttrium-stabilized zirconia powder in the zirconia slurry is 10-55% by volume. The volume fraction of the yttrium stabilized zirconia powder is too low, and the thickness of the zirconia ceramic block prepared after gravity acceleration sedimentation cannot meet the requirement of actual processing size; when the volume fraction is too high, the yttrium-stabilized zirconia powder in the slurry is difficult to disperse, and sedimentation is easy to occur. For this reason, the yttrium-stabilized zirconia powder of the present invention is present in the formulated zirconia slurry in a volume percentage ranging from 10 to 55%, more preferably from 25 to 50%.
Optionally, in step 1), the content of the additive in the zirconia slurry is 0.05-10% by volume.
Optionally, the additive is at least one of ethylene glycol, polyethylene glycol, glycerol, glucose, polydextrose, sucrose, ethylene oxide, citric acid and polyvinyl alcohol.
Optionally, in step 2), the hypergravity condition is: the range of the hypergravity coefficient is 1000-10000 g, wherein g is gravity acceleration. The hypergravity coefficient is too high, the cost of required preparation equipment is increased, the hypergravity coefficient is too low, and solid phase components in the slurry cannot be completely settled. For this purpose, the hypergravity conditions in step 2) of the present invention are in the range of 1000 to 10000g, more preferably 2000 to 7000g.
Optionally, in step 3), the drying conditions are: the humidity range is 40-90% and the temperature range is 15-80 ℃. Too high a drying temperature can cause the moisture inside the porcelain block to evaporate too quickly to crack; and when the temperature is too low, the drying time is long, and the process time is prolonged. Therefore, the humidity range of the drying in the step 3) is 40-90%, and the temperature range is 15-80 ℃; the humidity range is 60-80% and the temperature range is 20-70 ℃.
Optionally, in step 3), the amplification factor of the zirconia ceramic block blank ranges from 1.195 to 1.255.
The invention has the following beneficial effects:
1. according to the invention, the zirconia ceramic blocks for false teeth with large particles under and small particles above and distributed in natural continuous gradient are obtained by utilizing the difference of sedimentation speeds of powder with different particle sizes in a hypergravity environment; the optical transparency gradient of the zirconia ceramic obtained after crystallization and sintering has continuity, and the performance of the zirconia ceramic is more consistent with that of natural teeth.
2. According to the invention, in the process of raw material selection, each zirconia ceramic block only uses one content of yttrium oxide as the yttrium stable zirconia powder of the stabilizer, the raw material composition is simple, and multiple raw material components are not needed.
3. The invention omits the powder laying process of the multi-layer raw materials, and the warping phenomenon caused by different shrinkage due to different stabilizer contents can not occur during sintering.
4. Compared with the traditional preparation method of the gradient zirconia ceramic block, the preparation method of the invention has simple preparation process and low cost, and is suitable for large-scale production.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate the invention and together with the description serve to explain, without limitation, the invention.
FIG. 1 is a photograph of a sample of the dental gradient zirconia ceramic block prepared in example 1 after crystallization and sintering;
FIG. 2 is an electron micrograph of the microstructure of the top surface of the zirconia ceramic block obtained in step 4) of example 1;
FIG. 3 is an electron micrograph of the microstructure of the lower surface of the bottom end of the tile obtained in step 4) of example 1.
Detailed Description
The sources of reagents used in the embodiments of the invention are commercially available unless otherwise specified.
Name interpretation referred to in this invention:
the yttrium-stabilized zirconia powder according to the present invention is a zirconia powder in which yttrium oxide is used as a stabilizer.
The zirconia ceramic block of the specific embodiment of the invention is formed by a hypergravity method from zirconia slurry, wherein the zirconia slurry comprises yttrium-stabilized zirconia powder, an additive and water, and the volume percentage of the yttrium-stabilized zirconia powder in the zirconia slurry is 10-55%, and can be 10%,20%,30%,40%,50%,55% and the like by way of illustration; below 10% or above 55% the solid phase material is prone to delamination cracking during drying; the content of the additive in the zirconia slurry is 0.05 to 10% by volume, and may be, for example, 0.05%,1%,2%,3%. 10%, etc.; less than 0.05% or more than 10%, the solid phase substance is easy to crack in the drying process, and the permeability of the obtained zirconia ceramic block is reduced after sintering; the other balance is water, namely the total volume fraction of the yttrium stabilized zirconia powder, the additive and the water is 100 percent.
The zirconia ceramic block of the specific embodiment of the invention is characterized in that the yttrium stabilized zirconia powder takes yttrium oxide as a stabilizer; the total content of the stabilizer is 2.5-5.5 mol percent of the yttrium-stabilized zirconia powder.
The preparation method of the zirconia ceramic block in the specific embodiment of the invention specifically comprises the following steps:
1) Yttrium stabilized zirconia powder taking yttrium oxide as a stabilizer is taken as a main raw material, and is mixed with an additive and deionized water to prepare zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry under the condition of supergravity;
3) Drying the solid phase substance to obtain a zirconia ceramic block primary blank;
4) And carrying out appearance processing on the zirconia ceramic block primary blank to obtain the dental gradient zirconia ceramic block.
In some embodiments, the method for preparing the zirconia ceramic block may be:
1) Yttrium-stabilized zirconia powder with the content of 2.5-5.5 mol% of stabilizer is taken as a main raw material, the volume percentage of the yttrium-stabilized zirconia powder in the zirconia slurry is 10-55%, the volume percentage of the additive in the zirconia slurry is 0.05-10%, and the balance is deionized water, and the zirconium oxide slurry is prepared by mixing;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of supergravity with the supergravity coefficient of 1000-10000 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity range of the drying is 40-90%, and the temperature range is 15-80 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient zirconia ceramic block, wherein the amplification factor of the zirconia ceramic block ranges from 1.195 to 1.255.
Taking example 1 as an example, the invention provides a sample photograph of a dental gradient zirconia ceramic block subjected to crystallization sintering, and an electron microscope photograph of the microstructure of the upper surface of the top end of the zirconia ceramic block and the electron microscope photograph of the microstructure of the lower surface of the bottom end of the ceramic block, which are obtained by a supergravity molding method, and the contents of other embodiments of the invention can be directly and unambiguously determined by a person skilled in the art through the same method.
Example 1
1) Yttrium-stabilized zirconia powder with the yttrium content of 2.5mol percent is taken as a main raw material, and according to the volume percentage of the yttrium-stabilized zirconia powder in the zirconia slurry being 40 percent, the volume percentage of the additive in the zirconia slurry being 0.05 percent, and the balance being deionized water, the zirconium slurry is prepared by mixing;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of hypergravity with the hypergravity coefficient of 10000 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 80% and the temperature is 20 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient zirconia ceramic block with the amplification factor of 1.195.
As can be seen from fig. 1, the optical transparency of the sample in the form of a cylinder exhibits a macroscopic gradient change from top to bottom, and the gradient change is continuous and natural.
As can be seen from fig. 2 and 3, the grain size of the upper surface with better optical transparency is significantly smaller than the grain size of the lower surface with lower optical transparency.
Example 2
1) Yttrium-stabilized zirconia powder with the yttrium content of 2.5mol percent is taken as a main raw material, and according to the volume percent of the yttrium-stabilized zirconia powder in the zirconia slurry being 55 percent, the volume percent of the additive in the zirconia slurry being 3.23 percent, and the balance being deionized water, the zirconium slurry is prepared by mixing;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of high gravity with a high gravity coefficient of 8500 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 80% and the temperature is 35 ℃;
4) For the dried zirconia ceramics obtained in step 3)
And carrying out appearance processing on the block blank to obtain the gradient machinable zirconia ceramic block for dentistry, wherein the amplification factor is 1.207.
Example 3
1) Mixing yttrium-stabilized zirconia powder containing 3.5mol% of yttrium as a main raw material, wherein the content of the yttrium-stabilized zirconia powder in the zirconia slurry is 35% by volume, the content of the additive in the zirconia slurry is 4.95% by volume, and the balance is deionized water to prepare the zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of the hypergravity with the hypergravity coefficient of 7200 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 65% and the temperature is 30 ℃;
4) And (3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step (3) to obtain the dental gradient machinable zirconia ceramic block with the amplification factor of 1.211.
Example 4
1) Mixing yttrium-stabilized zirconia powder containing 4.0mol% of yttrium as a main raw material, wherein the volume percentage of the yttrium-stabilized zirconia powder in the zirconia slurry is 25%, the volume percentage of the additive in the zirconia slurry is 6.72%, and the balance is deionized water to prepare the zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of supergravity with the supergravity coefficient of 5500 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 60% and the temperature is 30 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient machinable zirconia ceramic block with the amplification factor of 1.226.
Example 5
1) Mixing yttrium-stabilized zirconia powder containing 4.5mol% of yttrium as a main raw material, wherein the content of the yttrium-stabilized zirconia powder is 20% by volume in the zirconia slurry, the content of the additive is 8.45% by volume in the zirconia slurry, and the balance is deionized water to prepare the zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of hypergravity with the hypergravity coefficient of 4300 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 45% and the temperature is 40 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient machinable zirconia ceramic block with the amplification factor of 1.235.
Example 6
1) Taking yttrium-stabilized zirconia powder containing 5.0mol% of yttrium as a main raw material, mixing according to the volume percentage of the yttrium-stabilized zirconia powder in the zirconia slurry being 25%, the volume percentage of the additive in the zirconia slurry being 9.27%, and the balance being deionized water, and preparing the zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of high gravity with a high gravity coefficient of 2900 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 40% and the temperature is 30 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient machinable zirconia ceramic block with the amplification factor of 1.248.
Example 7
1) Mixing yttrium-stabilized zirconia powder containing 5.5mol% of yttrium serving as a main raw material, wherein the content of the zirconia powder is 10% by volume in the zirconia slurry, the content of the additive is 10% by volume in the zirconia slurry, and the balance is deionized water to prepare the zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry prepared in the step 1) under the condition of high gravity with the high gravity coefficient of 1000 g;
3) Drying the solid phase substance obtained in the step 2) to obtain a zirconia ceramic block primary blank; the humidity of the drying is 40% and the temperature is 80 ℃;
4) And 3) carrying out contour machining on the dried zirconia ceramic block blank obtained in the step 3) to obtain the dental gradient machinable zirconia ceramic block with the amplification factor of 1.255.
The amounts of raw materials and process parameters for each example are shown in Table 1.
Table 1 examples 1 to 7 amounts of raw materials and process parameters
The additive in each embodiment of the invention is at least 1 or a combination of more than 1 of polyethylene glycol, ethylene glycol, glycerol, glucose, polydextrose, sucrose, citric acid, ethylene oxide and polyvinyl alcohol. The compositions and amounts of the additives of each example are shown in Table 2.
TABLE 2 composition and content of additives of examples 1 to 7
Claims (10)
1. The gradient zirconia ceramic block for dentistry is characterized in that the zirconia ceramic block is formed by zirconia slurry through a supergravity method, the zirconia slurry comprises yttrium stabilized zirconia powder, an additive and water, the volume percentage of the zirconia powder in the zirconia slurry is 10-55%, the volume percentage of the additive in the zirconia slurry is 0.05-10%, and the balance is water.
2. The zirconia ceramic block of claim 1 wherein the yttrium stabilized zirconia powder is yttria as a stabilizer; the content of the yttrium oxide in the yttrium-stabilized zirconia powder is 2.5-5.5 mol percent.
3. A zirconia ceramic block according to any one of claims 1 to 2 for use in the manufacture of dental restorations.
4. A method for preparing a dental gradient zirconia ceramic block according to any one of claims 1 to 2, characterized in that it is formed from the zirconia slurry by means of supergravity, comprising in particular the following steps:
1) Yttrium stabilized zirconia powder taking yttrium oxide as a stabilizer is taken as a main raw material, and is mixed with an additive and deionized water to prepare zirconia slurry;
2) Separating out solid phase substances in the zirconia slurry under the condition of supergravity;
3) Drying the solid phase substance to obtain a zirconia ceramic block primary blank;
4) And carrying out appearance processing on the zirconia ceramic block primary blank to obtain the zirconia ceramic block.
5. The method according to claim 4, wherein in step 1), the content of the yttrium-stabilized zirconia powder is 10 to 55% by volume in the zirconia slurry.
6. The method according to claim 4, wherein in step 1), the content of the additive in the zirconia slurry is 0.05 to 10% by volume.
7. The method of claim 4, wherein in step 1), the additive is at least one of ethylene glycol, polyethylene glycol, glycerol, glucose, polydextrose, sucrose, ethylene oxide, citric acid, and polyvinyl alcohol.
8. The method according to claim 4, wherein in step 2), the supergravity condition is: the range of the hypergravity coefficient is 1000-10000 g, wherein g is gravity acceleration.
9. The method according to claim 4, wherein in step 3), the drying conditions are: the humidity range is 40-90% and the temperature range is 15-80 ℃.
10. The method of claim 4 wherein in step 3) the zirconia ceramic block has an amplification factor in the range of 1.195 to 1.255.
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