CN107935623B - Wear-resistant ceramic material and preparation method and application thereof - Google Patents

Wear-resistant ceramic material and preparation method and application thereof Download PDF

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CN107935623B
CN107935623B CN201711334959.9A CN201711334959A CN107935623B CN 107935623 B CN107935623 B CN 107935623B CN 201711334959 A CN201711334959 A CN 201711334959A CN 107935623 B CN107935623 B CN 107935623B
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张松
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Suzhou New Hansheng precision ceramic technology Co.,Ltd.
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Abstract

The invention discloses a wear-resistant ceramic material and a preparation method and application thereof, wherein the ceramic material comprises the following raw materials in parts by weight: 11-19 parts of zirconium oxide, 1-5 parts of simethicone, 15-25 parts of levulinic acid, 22-30 parts of vermiculite, 3-7 parts of propylene carbonate and 3-7 parts of ethyl cellulose. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, adding a levulinic acid solution, heating, sealing and stirring to obtain a mixture A; placing simethicone and propylene carbonate into the mixture A, cooling, sealing, stirring, heating, stirring, performing ultrasonic treatment, centrifuging, collecting precipitate, washing, oven drying, making into blank, firing, and cooling. The invention reduces the porosity, improves the mechanical property of the ceramic material, has good fracture toughness and bending strength, good mechanical property, strong chemical stability and excellent biocompatibility, has almost the same color and luster with the human teeth, and has extremely high simulation degree.

Description

Wear-resistant ceramic material and preparation method and application thereof
Technical Field
The invention relates to the technical field of materials, in particular to a wear-resistant ceramic material and a preparation method and application thereof.
Background
The dental ceramics used in clinic at present have various varieties, mainly comprise alumina-based ceramics, glass-based ceramics and zirconia-based ceramics, and because the main components of each kind of ceramics are different, the physical and chemical properties of the ceramics are also different. The zirconia is unique in a plurality of dental all-ceramic materials due to excellent mechanical properties, and the indication of the all-ceramic restoration is greatly widened. However, zirconia is used in a large amount and at a high cost, and other components are added to reduce the amount of zirconia used. The added components comprise vermiculite and the like, but the vermiculite has good heat preservation performance and brittleness due to the structural particularity of the vermiculite, so that the vermiculite expands after being treated at high temperature. Even a product obtained by mixing zirconia with vermiculite cannot solve the above problems, so that the above problems need to be changed for its handling.
Disclosure of Invention
The invention aims to provide a wear-resistant ceramic material, a preparation method and application thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a wear-resistant ceramic material comprises the following raw materials in parts by weight: 11-19 parts of zirconium oxide, 1-5 parts of simethicone, 15-25 parts of levulinic acid, 22-30 parts of vermiculite, 3-7 parts of propylene carbonate and 3-7 parts of ethyl cellulose.
As a further scheme of the invention: the wear-resistant ceramic material comprises the following raw materials in parts by weight: 13-17 parts of zirconium oxide, 2-4 parts of simethicone, 18-22 parts of levulinic acid, 24-28 parts of vermiculite, 4-6 parts of propylene carbonate and 4-6 parts of ethyl cellulose.
As a further scheme of the invention: the wear-resistant ceramic material comprises the following raw materials in parts by weight: 15 parts of zirconium oxide, 3 parts of simethicone, 20 parts of levulinic acid, 26 parts of vermiculite, 5 parts of propylene carbonate and 5 parts of ethyl cellulose.
A preparation method of a wear-resistant ceramic material comprises the following steps:
1) mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution;
2) mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving with a sieve of 150-200 meshes, adding a levulinic acid solution, heating to 120 ℃ at 118-120 ℃, and carrying out sealed stirring treatment for 2.2-2.4h at the temperature to obtain a mixture A;
3) placing the dimeticone and the propylene carbonate into the mixture A, cooling to 82-85 ℃, hermetically stirring for 1.5-1.6h at the temperature, then heating to 140-143 ℃, stirring for 1.1h at the temperature, then stopping heating, performing ultrasonic treatment for 30min, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B;
4) preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
As a further scheme of the invention: in the step 2), the stirring speed is 150 r/min.
As a further scheme of the invention: in the step 3), the stirring speed is 350 r/min.
As a further scheme of the invention: in the step 3), the ultrasonic power is 600W.
As a further scheme of the invention: in the step 3), the centrifugal rotating speed is 14000r/min, and the centrifugal time is 30 min.
The invention also aims to provide application of the ceramic material in preparing a simulated tooth material.
Compared with the prior art, the invention has the beneficial effects that:
the ceramic material prepared by compounding the raw materials of zirconium oxide, vermiculite, propylene carbonate, ethyl cellulose and the like and through the preparation process has a synergistic effect, so that the porosity of the ceramic material is reduced, the mechanical property of the ceramic material is improved, the ceramic material has good fracture toughness and bending strength, good mechanical property, strong chemical stability and excellent biocompatibility, the color of the ceramic material is almost completely consistent with that of a human tooth, the simulation degree is extremely high, the color difference with the human tooth is within a plus-minus 1 color range, and the problems of brittleness, difficulty in molding, large color difference and the like in the prior art are solved. The invention has simple raw materials and easily controlled preparation process parameters, and is suitable for industrial production.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In the embodiment of the invention, the wear-resistant ceramic material comprises the following raw materials: 11kg of zirconium oxide, 1kg of dimeticone, 15kg of levulinic acid, 22kg of vermiculite, 3kg of propylene carbonate and 3kg of ethyl cellulose.
Mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving by a 150-mesh sieve, then adding a levulinic acid solution, heating to 118 ℃, sealing and stirring at the temperature for 2.2 hours at the stirring speed of 150r/min to obtain a mixture A. Placing dimeticone and propylene carbonate into the mixture A, cooling to 82 ℃, hermetically stirring for 1.5h at the temperature, then heating to 140 ℃, stirring for 1.1h at the temperature at the stirring speed of 350r/min, then stopping heating, performing ultrasonic treatment for 30min at the ultrasonic power of 600W, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
Example 2
In the embodiment of the invention, the wear-resistant ceramic material comprises the following raw materials: 19kg of zirconium oxide, 5kg of simethicone, 25kg of levulinic acid, 30kg of vermiculite, 7kg of propylene carbonate and 7kg of ethyl cellulose.
Mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving by a 200-mesh sieve, then adding a levulinic acid solution, heating to 120 ℃, sealing and stirring at the temperature for 2.4 hours at the stirring speed of 150r/min to obtain a mixture A. Placing dimeticone and propylene carbonate into the mixture A, cooling to 85 ℃, hermetically stirring for 1.6h at the temperature, then heating to 143 ℃, stirring for 1.1h at the temperature at the stirring speed of 350r/min, then stopping heating, performing ultrasonic treatment for 30min at the ultrasonic power of 600W, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
Example 3
In the embodiment of the invention, the wear-resistant ceramic material comprises the following raw materials: 13kg of zirconium oxide, 2kg of dimeticone, 18kg of levulinic acid, 24kg of vermiculite, 4kg of propylene carbonate and 4kg of ethyl cellulose.
Mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving by a 200-mesh sieve, then adding a levulinic acid solution, heating to 119 ℃, sealing and stirring at the temperature for 2.3 hours at the stirring speed of 150r/min, and obtaining a mixture A. Placing dimeticone and propylene carbonate into the mixture A, cooling to 85 ℃, hermetically stirring for 1.6h at the temperature, then heating to 143 ℃, stirring for 1.1h at the temperature at the stirring speed of 350r/min, then stopping heating, performing ultrasonic treatment for 30min at the ultrasonic power of 600W, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
Example 4
In the embodiment of the invention, the wear-resistant ceramic material comprises the following raw materials: 17kg of zirconium oxide, 4kg of simethicone, 22kg of levulinic acid, 28kg of vermiculite, 6kg of propylene carbonate and 6kg of ethyl cellulose.
Mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving by a 200-mesh sieve, then adding a levulinic acid solution, heating to 119 ℃, sealing and stirring at the temperature for 2.3 hours at the stirring speed of 150r/min, and obtaining a mixture A. Placing dimeticone and propylene carbonate into the mixture A, cooling to 85 ℃, hermetically stirring for 1.6h at the temperature, then heating to 143 ℃, stirring for 1.1h at the temperature at the stirring speed of 350r/min, then stopping heating, performing ultrasonic treatment for 30min at the ultrasonic power of 600W, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
Example 5
In the embodiment of the invention, the wear-resistant ceramic material comprises the following raw materials: 15kg of zirconium oxide, 3kg of simethicone, 20kg of levulinic acid, 26kg of vermiculite, 5kg of propylene carbonate and 5kg of ethyl cellulose.
Mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution. Mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving by a 200-mesh sieve, then adding a levulinic acid solution, heating to 119 ℃, sealing and stirring at the temperature for 2.3 hours at the stirring speed of 150r/min, and obtaining a mixture A. Placing dimeticone and propylene carbonate into the mixture A, cooling to 85 ℃, hermetically stirring for 1.6h at the temperature, then heating to 143 ℃, stirring for 1.1h at the temperature at the stirring speed of 350r/min, then stopping heating, performing ultrasonic treatment for 30min at the ultrasonic power of 600W, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst.
Comparative example 1
The starting materials and preparation were as in example 5 except that levulinic acid was not present.
Comparative example 2
Only zirconia and vermiculite were used, and the preparation process was identical to that of example 5.
Comparative example 3
Only zirconia, vermiculite, levulinic acid, the preparation process was identical to example 5.
Comparative example 4
Directly mixing the raw materials, adding the other substances added in the example 5, heating to 143 ℃, stirring at the temperature for 1.1h at the stirring speed of 350r/min, stopping heating, centrifugally separating, taking precipitate, washing and drying to obtain a mixture B; the centrifugal speed is 14000r/min, and the centrifugal time is 30 min. Preparing the mixture B into a blank, heating to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5h at the temperature, then heating to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5h at the temperature, stopping heating, and naturally cooling to obtain the catalyst. The amounts of the respective raw materials added were the same as in example 5.
Example 6
The products of examples 1 to 5 and comparative examples 1 to 4 were tested and the results are shown in Table 1.
TABLE 1
Figure BDA0001507211450000051
Figure BDA0001507211450000061
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (4)

1. The wear-resistant ceramic material is characterized by comprising the following raw materials in parts by weight: 11-19 parts of zirconium oxide, 1-5 parts of simethicone, 15-25 parts of levulinic acid, 22-30 parts of vermiculite, 3-7 parts of propylene carbonate and 3-7 parts of ethyl cellulose; the preparation method of the wear-resistant ceramic material comprises the following steps: 1) mixing levulinic acid with deionized water with the mass of 8.5 times that of the levulinic acid to prepare a levulinic acid solution; 2) mixing and grinding zirconium oxide, vermiculite and ethyl cellulose, sieving with a sieve of 150-200 meshes, adding a levulinic acid solution, heating to 120 ℃ at 118-120 ℃, and carrying out sealed stirring treatment for 2.2-2.4h at the temperature to obtain a mixture A; 3) placing the dimeticone and the propylene carbonate into the mixture A, cooling to 82-85 ℃, hermetically stirring for 1.5-1.6h at the temperature, then heating to 140-143 ℃, stirring for 1.1h at the temperature, then stopping heating, performing ultrasonic treatment for 30min, performing centrifugal separation, taking precipitate, washing and drying to obtain a mixture B; 4) preparing the mixture B into a blank, heating up to 520 ℃ at the speed of 0.5 ℃/min, preserving heat for 4.5 hours at the temperature, then heating up to 1270 ℃ at the speed of 1 ℃/min, preserving heat for 5 hours at the temperature, stopping heating, and naturally cooling to obtain the material; wherein, in the step 2), the stirring speed is 150r/min, in the step 3), the stirring speed is 350r/min, the ultrasonic power is 600W, the centrifugal rotating speed is 14000r/min, and the centrifugal time is 30 min.
2. The wear-resistant ceramic material of claim 1, comprising the following raw materials in parts by weight: 13-17 parts of zirconium oxide, 2-4 parts of simethicone, 18-22 parts of levulinic acid, 24-28 parts of vermiculite, 4-6 parts of propylene carbonate and 4-6 parts of ethyl cellulose.
3. The wear-resistant ceramic material of claim 1, comprising the following raw materials in parts by weight: 15 parts of zirconium oxide, 3 parts of simethicone, 20 parts of levulinic acid, 26 parts of vermiculite, 5 parts of propylene carbonate and 5 parts of ethyl cellulose.
4. Use of a ceramic material according to any one of claims 1 to 3 for the preparation of a simulated dental material.
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CN108066158A (en) * 2017-12-08 2018-05-25 郑州搜趣信息技术有限公司 High ceramic tooth material of a kind of fracture toughness and its preparation method and application
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CN112250439A (en) * 2020-10-20 2021-01-22 哈工宁伯医疗科技泰州有限公司 Ceramic material for tooth restoration and manufacturing method thereof

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