CN115959901A - Gradient zirconia tooth prosthesis and preparation method thereof - Google Patents

Gradient zirconia tooth prosthesis and preparation method thereof Download PDF

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CN115959901A
CN115959901A CN202210429535.5A CN202210429535A CN115959901A CN 115959901 A CN115959901 A CN 115959901A CN 202210429535 A CN202210429535 A CN 202210429535A CN 115959901 A CN115959901 A CN 115959901A
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zirconia
gradient
yttrium
prosthesis
dental restoration
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CN115959901B (en
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熊焰
沈未
丁伟明
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Wuxi Yiya Technology Partnership LP
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Abstract

The invention provides a gradient zirconia dental prosthesis and a preparation method thereof, belonging to the technical field of dental prostheses. Mixing yttrium-stabilized zirconia powder, an additive and deionized water until uniform zirconia slurry is formed; injecting the zirconia slurry into a dental restoration body mould, and forming under the condition of supergravity to obtain a restoration body green body with gradient change; and sintering the prosthesis green body at high temperature to obtain the gradient zirconia dental prosthesis. The method can solve the technical problems of complex process, raw material waste, discontinuous gradient and the like in the existing preparation process of the gradient zirconia prosthesis, so as to obtain the zirconia dental prosthesis which is in continuous gradient distribution and does not have warping phenomenon after sintering.

Description

Gradient zirconia tooth prosthesis and preparation method thereof
Technical Field
The invention relates to the technical field of dental restorations, in particular to a gradient zirconia dental restoration and a preparation method thereof.
Background
The zirconia ceramics has reliable biological stability and excellent mechanical property, and is one of the mainstream repair materials in the field of dental repair materials at present. The natural tooth has a unique gradient structure, the color and the transmittance of the natural tooth have the tendency of gradient gradual change from the neck end to the cut end, and the natural tooth has excellent aesthetic property. The gradient zirconia prosthesis has been widely regarded in the field of prosthesis materials because of its ability to simulate the aesthetic properties of natural teeth.
At present, a zirconia restoration body with gradient characteristics can be prepared by means of ceramic layer stacking, a zirconia restoration body with color gradient is prepared by Chinese patent CN201510216534.2 by means of lamination, the restoration body prepared by the method is formed by stacking a plurality of ceramic layers with different colors, and the effect of color gradient gradual change is realized by color change between the ceramic layers. Chinese patent CN201410132765.0 discloses a gradient transparent zirconia dental ceramic and a preparation method thereof, the invention prepares 5-11 ceramic layers with different transparencies by changing the mass fraction of zirconia, and the gradient transparent zirconia dental ceramic is obtained by stacking according to the transparency sequence. However, in the preparation process of the gradient zirconia ceramic, the preparation of the zirconia ceramic layer needs to be considered preferentially, the process parameters such as the proportioning ratio, isostatic pressure and the like of different ceramic layers need to be adjusted in real time in the preparation process, in order to ensure the purity of the color of the ceramic layer, the colored ceramic layer needs to be formed by using a separate tablet press, and the preparation process is complicated in actual production. Secondly, the different ceramic layers have different compositions and different crystal grain sizes, so that the prosthesis has partial warping phenomenon after sintering, and the performance of the finished product is greatly influenced.
The prior art also has another preparation process of the gradient zirconia restoration. Chinese patent CN202010555488.X discloses a zirconia false tooth with gradient mechanical property and a manufacturing method thereof. The denture prosthesis is divided into a basal body and an occlusal surface, the basal body and the occlusal surface with different compositions are prepared, and the integral gradient characteristic of the prosthesis is shown through the performance difference of the occlusal surface and the basal body. In the process of preparing the gradient prosthesis, corresponding performance design needs to be carried out on different parts, the process is complex, the gradient change only exists between different parts such as the occlusal surface and the basal body, the occlusal surface and the basal body have no gradient change characteristic, and the continuous gradient characteristic on the aesthetic property and the mechanical property of the natural tooth cannot be simulated.
Due to the above-mentioned drawbacks of the related art, it is necessary to provide a zirconia dental prosthesis and a method for manufacturing the same, which are simple in process and can realize gradient change characteristics.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides a gradient zirconia dental prosthesis and a preparation method thereof, aiming at solving the technical problems of complex process, raw material waste, discontinuous gradient and the like in the existing preparation process of the gradient zirconia dental prosthesis, so as to obtain the zirconia dental prosthesis which is in continuous gradient distribution and does not have warping after sintering.
The specific technical scheme provided by the invention is as follows:
on one hand, the preparation method of the gradient zirconia dental prosthesis comprises the following steps:
the method comprises the following steps: mixing yttrium-stabilized zirconia powder, an additive and deionized water until uniform zirconia slurry is formed;
step two: injecting the zirconia slurry into a dental restoration body mould, and forming under the condition of supergravity to obtain a restoration body green body with gradient change;
step three: and sintering the prosthesis green body at high temperature to obtain the gradient zirconia dental prosthesis.
Optionally, the yttrium-stabilized zirconia powder comprises an yttrium oxide stabilizer and zirconia powder; the molar percentage of the dosage of the yttrium oxide stabilizer in the dosage of the yttrium stabilized zirconia powder is 2.5-5.5mol%.
Optionally, the additive is a compound of at least three of ammonium polyacrylate, polyacrylic acid, polyethylene glycol, polyglycerol and polyvinyl alcohol.
Optionally, the additive comprises a dispersant, a lubricant and a binder, wherein the dispersant comprises at least one of ammonium polyacrylate and polyacrylic acid, the lubricant comprises at least one of polyethylene glycol and polyglycerol, and the binder is polyvinyl alcohol.
Optionally, the volume ratio of the yttrium-stabilized zirconia powder to the deionized water is 1 (1-3), and the additive accounts for 0.5-3.5wt% of the yttrium-stabilized zirconia powder.
Optionally, the supergravity condition in step two is: the hypergravity coefficient range is 10000-30000g, wherein g is the gravity acceleration.
Optionally, the high-temperature sintering temperature in the third step is 1450-1600 ℃, and the sintering time is 20-60min.
On the other hand, the gradient zirconia dental prosthesis is prepared by any one of the methods.
Compared with the prior art, the invention has the advantages and beneficial effects that:
1. the preparation method of the invention does not need to consider the difference of preparation processes among different gradient components, can realize the gradient characteristic of the restoration by using the yttrium-stabilized zirconia powder with single stabilizer content, simplifies the process flow and is suitable for large-scale production.
2. The gradient zirconia dental prosthesis is in continuous gradient distribution, has aesthetic property similar to that of natural teeth, and can not generate warping after being sintered.
3. The zirconia slurry is subjected to supergravity forming in a restoration body die, and a porcelain cake is not required to be cut, so that the restoration body raw materials are saved, and the production process cost is reduced.
4. The prosthesis prepared by the invention does not need a cutting process, and the surface of the obtained prosthesis finished product does not contain the grains of a cutting tool, so that the gloss of the surface of the prosthesis is further improved, and the prosthesis is suitable for being used as a dental prosthesis.
Drawings
Fig. 1 (a) is a diagram of a gradient effect of a single crown prosthesis provided in embodiment 1 of the present invention, and fig. 1 (b) is a corresponding black and white picture.
Fig. 2 (c) is a graph of the gradient effect of the triple-bridged prosthesis provided in example 2 of the present invention, and fig. 2 (d) is a corresponding black-and-white picture.
Detailed Description
The technical solutions in the embodiments will be clearly and completely described below, and all other embodiments that can be obtained by a person skilled in the art without making creative efforts based on the embodiments of the present invention belong to the protection scope of the present invention.
The preparation method of the gradient zirconia dental prosthesis comprises the following steps:
the method comprises the following steps: mixing yttrium-stabilized zirconia powder, an additive and deionized water until uniform zirconia slurry is formed;
step two: injecting the zirconia slurry into a dental restoration body mould, and forming under the condition of supergravity to obtain a restoration body green body;
step three: and sintering the prosthesis green body at high temperature to obtain the gradient zirconia dental prosthesis.
By the preparation method, the technical processes of ceramic layer stacking and ceramic block cutting are omitted, namely, the mass fraction (or mole percentage) of yttrium stabilized zirconia powder does not need to be changed, multilayer powder paving is carried out, the zirconia ceramic block with gradient transparency is obtained, and then cutting is carried out to form the gradient tooth restoration, so that the preparation process is simplified, and raw materials are saved. Through a supergravity process, yttrium-stabilized zirconia powder with the same mass fraction (or molar percentage) is adopted, the principle that the zirconia powder has a certain particle size difference is utilized, the difference of mass transfer rates of zirconia particles with different particle sizes is amplified, the zirconia particles with different particle sizes are separated from each other, and the characteristic of gradient is shown.
The preparation method of the gradient zirconia dental restoration of the specific embodiment of the invention comprises the steps of preparing yttrium stabilized zirconia powder by using a yttrium oxide stabilizer and zirconium oxide powder; the molar percentage of the dosage of the yttrium oxide stabilizer in the dosage of the yttrium stabilized zirconia powder is 2.5-5.5mol%.
Yttrium and zirconia form a solid solution in zirconia, yttrium ions can maintain a tetragonal crystal phase of the zirconia within a certain content range, the performance of the zirconia is improved, but the tetragonal crystal phase structure of the zirconia is reduced and the strength of the zirconia is reduced after a certain content of yttrium is exceeded, so that yttrium is selected as a stabilizing agent in the invention, and the molar mass percentage of yttrium in zirconia powder with yttrium as the stabilizing agent is 2.5-5.5mol%.
The preparation method of the gradient zirconia dental prosthesis of the specific embodiment of the invention comprises the steps of compounding at least three of ammonium polyacrylate, polyacrylic acid, polyethylene glycol, polyglycerol and polyvinyl alcohol as additives; in some embodiments, the additive may be a combination of three of polyacrylic acid, and polyethylene glycol, or a combination of three of polyacrylic acid, polyethylene glycol, and polyglycerol, or a combination of three of polyacrylic acid, polyglycerol, and polyvinyl alcohol.
Wherein, ammonium polyacrylate and polyacrylic acid are used as dispersing agent, polyethylene glycol and polyglycerol are used as lubricant, and polyvinyl alcohol is used as binder, and as a preferred embodiment, the additive at least comprises one dispersing agent, one lubricant and one binder.
According to the preparation method of the gradient zirconia dental restoration, the volume ratio of the yttrium-stabilized zirconia powder to the deionized water is 1 (1-3).
The performance of the preparation method of the gradient zirconia dental restoration provided by the embodiment of the invention is influenced by the powder content in the zirconia slurry, the volume fraction ratio of zirconia is too low, which can cause the strength of the zirconia restoration to be insufficient, and the volume fraction ratio of zirconia is too high, which can cause the slurry to be difficult to disperse, and influence the uniformity of the restoration. Therefore, the volume ratio of the zirconium oxide powder to the deionized water is 1 (1-3).
In the preparation method of the gradient zirconia dental restoration of the specific embodiment of the invention, the amount of the additive accounts for 0.5 to 3.5 weight percent of the amount of the yttrium stabilized zirconia powder.
The performance of the gradient zirconia dental restoration obtained by the method is influenced by the composition and the dosage of the additive, the added dispersant is less, the dispersing effect is not strong, the zirconia powder is easy to agglomerate to influence the uniformity of the slurry, the added dispersant can cause the molecules of the dispersant to be mutually wound in the slurry, and the viscosity of the slurry is increased to cause the poor dispersibility of the slurry. The lubricant can improve the fluidity of zirconia slurry, but the lubricant is a high molecular substance, and the addition of the lubricant is excessive, so that the binder removal is difficult, namely the binder can be cracked for a long time, and the sintering effect is influenced. The adhesive can increase the strength of the powder, but too much addition can cause difficult glue discharging and affect the sintering effect, so that the content of the additive is 0.5-3.5wt% of the mass percent of the yttrium-stabilized zirconia powder, and specifically, the dosage of the dispersant, the lubricant and the adhesive respectively accounts for 0.15-1.5wt%,0.2-1.5wt% and 0.15-0.5wt% of the mass percent of the yttrium-stabilized zirconia powder.
The performance of the gradient zirconia dental prosthesis obtained by the method is influenced by a supergravity molding process, the supergravity coefficient is too large, the gradient change of the prosthesis is too large, and the strength of the cut end is too low; the supergravity coefficient is too low, the gradient distribution of the prosthesis is not obvious, and the application requirement cannot be met. Therefore, the overweight coefficient in the hypergravity forming process in the step two is 10000-30000g, the hypergravity forming time is 10-30min, and g is the gravity acceleration.
The performance of the gradient zirconia dental restoration obtained by the method of the present invention is affected by the sintering temperature. The sintering temperature is too low, and the sintering time is too short, so that the compactness of a sintered body is low; if the sintering temperature is too high and the sintering time is too long, the crystal grain growth is too large, the strength of the prosthesis is reduced, and the heat energy consumption is high. Therefore, the sintering temperature in the third step is 1450-1600 ℃, and the sintering time is 20-60min.
Example 1 preparation of a uni-crown prosthesis
The method comprises the following steps: yttrium-stabilized zirconia powder, an additive and deionized water are mixed to form uniform zirconia slurry, the additive is dispersant ammonium polyacrylate, lubricant polyethylene glycol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material refers to table 1 and table 2.
Step two: and injecting the prepared zirconia slurry into a single-crown mold, setting the overweight coefficient to 26000g, and maintaining for 13min to mold the slurry to obtain a prosthesis green body with gradient characteristics.
Step three: and sintering the obtained prosthesis green body at the temperature of 1550 ℃ for 35min to obtain the single-crown prosthesis.
EXAMPLE 2 preparation of triple bridge prosthesis
The method comprises the following steps: yttrium-stabilized zirconia powder, an additive and deionized water are mixed to form uniform zirconia slurry, the additive is dispersant ammonium polyacrylate, lubricant polyethylene glycol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material refers to table 1 and table 2.
Step two: and injecting the prepared zirconia slurry into a triple-bridge mold, setting the overweight coefficient to be 20000g, and maintaining for 20min to mold the slurry to obtain the prosthesis green body with the gradient characteristic.
Step three: and sintering the obtained prosthesis green body at 1600 ℃ for 20min to obtain the triple-bridged prosthesis.
Example 3 preparation of veneers
The method comprises the following steps: the yttrium-stabilized zirconia powder, the additive and the deionized water are mixed to form uniform zirconia slurry, the used additive is dispersant polyacrylic acid, lubricant polyethylene glycol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material is shown in table 1 and table 2.
Step two: and injecting the prepared zirconia slurry into a veneering die, setting the overweight coefficient to be 30000g, and maintaining for 10min to form the slurry so as to obtain the prosthesis green body with the gradient characteristic.
Step three: sintering the obtained prosthesis green body at 1450 ℃ for 60min to obtain the veneering prosthesis.
EXAMPLE 4 preparation of the inlay
The method comprises the following steps: yttrium-stabilized zirconia powder, an additive and deionized water are mixed to form uniform zirconia slurry, the additive is dispersant ammonium polyacrylate, lubricant polyglycerol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material refers to table 1 and table 2.
Step two: and injecting the prepared zirconia slurry into an inlay mold, setting the overweight coefficient to 15000g, and maintaining for 25min to form the slurry to obtain a prosthesis green body with gradient characteristics.
Step three: and sintering the obtained prosthesis green body at the temperature of 1530 ℃ for 40min to obtain the inlay prosthesis.
Example 5 preparation of the coping
The method comprises the following steps: yttrium-stabilized zirconia powder, an additive and deionized water are mixed to form uniform zirconia slurry, the used additive is dispersant polyacrylic acid, lubricant polyglycerol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material is shown in tables 1 and 2.
Step two: and injecting the prepared zirconia slurry into a base crown mold, setting the overweight coefficient to 10000g, and maintaining for 30min to form the slurry so as to obtain a prosthesis green body with gradient characteristics.
Step three: and sintering the obtained restoration body green body at the temperature of 1550 ℃ for 35min to obtain the base crown restoration body.
EXAMPLE 6 preparation of abutment
The method comprises the following steps: yttrium-stabilized zirconia powder, an additive and deionized water are mixed to form uniform zirconia slurry, the used additive is dispersant polyacrylic acid, lubricant polyglycerol and binder polyvinyl alcohol, the mixture is uniformly stirred to obtain the zirconia slurry, and the specific dosage of each raw material is shown in tables 1 and 2.
Step two: and injecting the prepared zirconia slurry into a base mould, setting the gravity coefficient to be 17000g, and maintaining for 22min to form the slurry so as to obtain a prosthesis green body with gradient characteristics.
Step three: and sintering the obtained restoration green body at 1520 ℃ for 30min to obtain the abutment restoration.
Table 1 amounts of raw materials and process parameters for examples 1 to 6
Figure BDA0003609541600000071
The additive in each embodiment of the invention consists of a dispersant, a lubricant and a binder, wherein the dispersant is ammonium polyacrylate and polyacrylic acid, the lubricant is polyethylene glycol and polyglycerol, and the binder is polyvinyl alcohol. The concrete mass fractions are 0.15-1.5wt% of dispersant, 0.2-1.5wt% of lubricant and 0.15-0.5wt% of binder. The composition and mass ratios of the additives of the examples are shown in table 2.
TABLE 2 compositions and amounts of additives of examples 1-6
Figure BDA0003609541600000081
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Claims (10)

1. A preparation method of a gradient zirconia dental prosthesis is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: mixing yttrium-stabilized zirconia powder, an additive and deionized water until uniform zirconia slurry is formed;
step two: injecting the zirconia slurry into a dental restoration body mould, and forming under the condition of supergravity to obtain a restoration body green body with gradient change;
step three: and sintering the prosthesis green body at high temperature to obtain the gradient zirconia dental prosthesis.
2. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the yttrium-stabilized zirconia powder comprises an yttrium oxide stabilizer and zirconia powder; the molar percentage of the dosage of the yttrium oxide stabilizer in the dosage of the yttrium stabilized zirconia powder is 2.5-5.5mol%.
3. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the additive is a compound of at least three of ammonium polyacrylate, polyacrylic acid, polyethylene glycol, polyglycerol and polyvinyl alcohol.
4. The method for manufacturing a gradient zirconia dental restoration according to claim 3, wherein: the additive at least comprises a dispersant, a lubricant and a binder, wherein the dispersant comprises at least one of ammonium polyacrylate and polyacrylic acid, the lubricant comprises at least one of polyethylene glycol and polyglycerol, and the binder is polyvinyl alcohol.
5. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the volume ratio of the yttrium-stabilized zirconia powder to the deionized water is 1 (1-3).
6. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the mass percentage of the additive accounting for the yttrium stabilized zirconia powder is 0.5-3.5wt%.
7. The method for manufacturing a gradient zirconia dental restoration according to claim 4, wherein:
the mass percentage of the dispersant accounting for the yttrium stable zirconia powder is 0.15-1.5wt%,
the mass percentage of the lubricant accounting for the yttrium stabilized zirconia powder is 0.2-1.5wt%,
the mass percentage of the binder accounting for the yttrium-stabilized zirconia powder is 0.15-0.5wt%.
8. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the supergravity condition in the second step is as follows: the hypergravity coefficient range is 10000-30000g, wherein g is the gravity acceleration.
9. The method for manufacturing a gradient zirconia dental restoration according to claim 1, wherein: the high-temperature sintering temperature in the third step is 1450-1600 ℃, and the sintering time is 20-60min.
10. A gradient zirconia dental restoration obtained by the production method according to any one of claims 1 to 8.
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