CN112979309A - Ceramic material for oral restoration and preparation method thereof - Google Patents
Ceramic material for oral restoration and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a ceramic material for oral restoration and a preparation method thereof, relating to the technical field of oral restoration. The ceramic material comprises, by weight, 45-65 parts of zirconium oxide, 30-40 parts of aluminum oxide, 10-20 parts of zinc oxide, 5-10 parts of aluminum borate, 10-20 parts of borax, 10-15 parts of rare earth oxide, 5-10 parts of silicon dioxide, 10-20 parts of sodium fluoride, 5-10 parts of resorcinol monobenzoate, 4-8 parts of a thickening agent and 4-8 parts of a flocculating agent. According to the invention, the zirconia is taken as a main material, the alumina is taken as an auxiliary material, and the zinc oxide and the silicon dioxide are added, so that the strength and the toughness of the prepared ceramic material are ensured, the defect that the traditional ceramic material is brittle and easy to break is overcome, the clinical success rate is improved, a certain sterilization effect is achieved through the sodium fluoride, the light stability of the ceramic material is improved through the resorcinol monobenzoate, the attractiveness of the ceramic material is improved, gaps generated in the ceramic filling and sintering process are filled through the thickening agent and the flocculating agent, the defects of the dental prosthesis are reduced, and the product strength is improved.
Description
Technical Field
The invention belongs to the technical field of oral restoration, and particularly relates to an oral restoration ceramic material and a preparation method thereof.
Background
The oral cavity restoration refers to the treatment work of adopting the artificially manufactured restoration body aiming at the defects of soft and hard tissues of the oral cavity and the maxillofacial part, and also comprises the treatment of periodontal disease and temporomandibular joint disease by a restoration means. With the improvement of living standard and the diversified development of diet, the number of patients with tooth loss caused by decayed teeth, periodontitis and tooth injury in China is increasing. Ceramic materials are considered the best material to match the appearance of human teeth, their excellent aesthetics, wear resistance, and color stability, making them the most common oral restorative material. At present, the ceramic is mainly applied to oral restoration in a mode of fusing and adhering a metal crown by porcelain, the ceramic is widely applied to dental clinic due to the combination of the strength, the edge tightness and the porcelain attractiveness of a metal inner crown, and the biological ceramic is a ceramic material with a specific biological or physiological function. Because the biological ceramic material has the advantages of good biocompatibility, affinity with biological tissues, corrosion resistance, sterilization property, physical and chemical stability and the like, the biological ceramic material occupies an increasingly important position in the oral cavity field.
The mechanical property and the processing property of the existing ceramic material are often not compatible, which limits the clinical application range, the oral cavity repairing material should have good biological property and mechanical property, and at the same time, the oral cavity repairing material should also have better processing formability, although the existing cast ceramic, glass permeable alumina ceramic, compact polycrystalline alumina ceramic and zirconia ceramic products are available and used clinically, the mechanical property and the processing property of the obtained ceramic material are often not compatible, which limits the clinical application range, and in addition, in the clinical use, the requirement of patients on the aesthetic property is higher and higher.
Disclosure of Invention
The invention aims to provide a ceramic material for oral restoration and a preparation method thereof, wherein the ceramic material is mainly prepared from zirconium oxide and auxiliary aluminum oxide, and is added with zinc oxide and silicon dioxide, so that the strength and toughness of the prepared ceramic material are ensured, the defect that the traditional ceramic material is brittle and easy to break is overcome, the clinical success rate is improved, a certain sterilization effect is achieved through sodium fluoride, the light stability of the ceramic material is improved through resorcinol monobenzoate, the attractiveness of the ceramic material is improved, gaps generated in the sintering process of filling the ceramic material are filled through a thickening agent and a flocculating agent, the defects of an oral restoration body are reduced, the product strength is improved, and the problems of insufficient strength and insufficient attractiveness in the prior art are solved.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to an oral repair ceramic material which comprises, by weight, 45-65 parts of zirconium oxide, 30-40 parts of aluminum oxide, 10-20 parts of zinc oxide, 5-10 parts of aluminum borate, 10-20 parts of borax, 10-15 parts of rare earth oxide, 5-10 parts of silicon dioxide, 10-20 parts of sodium fluoride, 5-10 parts of resorcinol monobenzoate, 4-8 parts of a thickening agent and 4-8 parts of a flocculating agent.
Preferably, the coating comprises, by weight, 48-62 parts of zirconium oxide, 32-38 parts of aluminum oxide, 11-18 parts of zinc oxide, 6-8 parts of aluminum borate, 7-9 parts of borax, 11-14 parts of rare earth oxide, 6-9 parts of silicon dioxide, 12-17 parts of sodium fluoride, 6-9 parts of resorcinol monobenzoate, 5-7 parts of a thickening agent and 5-7 parts of a flocculating agent.
A preparation method of an oral cavity repairing ceramic material comprises the following steps:
the method comprises the following steps: putting zirconia into an ethanol solution, and fully dissolving the zirconia by a stirring dispersion machine;
step two: heating the solution obtained in the step one to 60-80 ℃, then respectively adding alumina, zinc oxide and silicon dioxide at 60-80 ℃, and standing for reaction;
step three: cooling the reactant obtained in the step two, and then adding a polyethylene glycol solution;
step four: adding a thickening agent and a coagulant into the solution obtained in the third step at normal temperature, and preparing the solution into colloid by a three-roll grinder;
step five: putting the colloid obtained in the fourth step into a high-pressure reaction kettle for reaction, and obtaining first powder after the reaction is finished;
step six: mixing the first powder obtained in the fifth step with aluminum borate, borax, rare earth oxide, sodium fluoride and resorcinol monobenzoate;
step seven: adding the mixed material obtained in the sixth step into a ball milling tank for wet ball milling for 8-20 hours, drying, sieving with a 150-mesh sieve, and then putting into a graphite mold for compression molding under the pressure of 15-40MPa to obtain a blank;
step eight: and sintering the green body obtained in the seventh step with nitrogen at the sintering temperature of 1250-1350 ℃, and naturally cooling to room temperature to obtain the ceramic material.
Preferably, the rare earth oxide in the sixth step comprises Ta2O5, Sm2O3 and Nd2O3, and the weight ratio of Ta2O5, Sm2O3 and Nd2O3 is 1:2: 4.
Preferably, the weight ratio of the alumina, the zinc oxide and the silicon dioxide in the second step is 3:2: 1.
Preferably, the weight ratio of the first powder, the aluminum borate, the borax, the rare earth oxide, the sodium fluoride and the resorcinol monobenzoate in the sixth step is 6:1:2:1.5:1: 1.
Preferably, the sintering pressure in the step eight is 35MPa, and the heat preservation and pressure maintaining time is 80 minutes.
Preferably, the thickener in the fourth step is composed of carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, polyoxyethylene and other components, and the coagulant is composed of a high-molecular coagulant and a coagulant aid.
The invention has the following beneficial effects:
1. according to the invention, the zirconia is taken as a main material, the alumina is taken as an auxiliary material, and the zinc oxide and the silicon dioxide are added, so that the strength and the toughness of the prepared ceramic material are ensured, the defect that the traditional ceramic material is brittle and easy to break is overcome, and the clinical success rate is improved.
2. The invention has certain bactericidal effect through sodium fluoride, improves the light stability of the ceramic material through resorcinol monobenzoate and increases the aesthetic property of the ceramic material.
3. The invention fills the gap generated in the ceramic sintering process by the thickening agent and the coagulant, reduces the defect of the dental prosthesis and increases the product strength.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
Detailed Description
In the description of the present invention, it is to be understood that the terms "upper", "middle", "outer", "inner", and the like, indicate orientations or positional relationships, are used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referenced components or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention.
The first embodiment is as follows:
an oral cavity repairing ceramic material comprises, by weight, 45-65 parts of zirconium oxide, 30-40 parts of aluminum oxide, 10-20 parts of zinc oxide, 5-10 parts of aluminum borate, 10-20 parts of borax, 10-15 parts of rare earth oxide, 5-10 parts of silicon dioxide, 10-20 parts of sodium fluoride, 5-10 parts of resorcinol monobenzoate, 4-8 parts of a thickening agent and 4-8 parts of a flocculating agent.
Further, the coating comprises, by weight, 48-62 parts of zirconium oxide, 32-38 parts of aluminum oxide, 11-18 parts of zinc oxide, 6-8 parts of aluminum borate, 7-9 parts of borax, 11-14 parts of rare earth oxide, 6-9 parts of silicon dioxide, 12-17 parts of sodium fluoride, 6-9 parts of resorcinol monobenzoate, 5-7 parts of a thickening agent and 5-7 parts of a flocculating agent.
Example two:
a preparation method of an oral cavity repairing ceramic material comprises the following steps:
the method comprises the following steps: putting zirconia into an ethanol solution, and fully dissolving the zirconia by a stirring dispersion machine;
step two: heating the solution obtained in the step one to 60-80 ℃, then respectively adding alumina, zinc oxide and silicon dioxide at 60-80 ℃, and standing for reaction;
step three: cooling the reactant obtained in the step two, and then adding a polyethylene glycol solution;
step four: adding a thickening agent and a coagulant into the solution obtained in the third step at normal temperature, and preparing the solution into colloid by a three-roll grinder;
step five: putting the colloid obtained in the fourth step into a high-pressure reaction kettle for reaction, and obtaining first powder after the reaction is finished;
step six: mixing the first powder obtained in the fifth step with aluminum borate, borax, rare earth oxide, sodium fluoride and resorcinol monobenzoate;
step seven: adding the mixed material obtained in the sixth step into a ball milling tank for wet ball milling for 8-20 hours, drying, sieving with a 150-mesh sieve, and then putting into a graphite mold for compression molding under the pressure of 15-40MPa to obtain a blank;
step eight: and sintering the green body obtained in the seventh step with nitrogen at the sintering temperature of 1250-1350 ℃, and naturally cooling to room temperature to obtain the ceramic material.
The rare earth oxide in the sixth step comprises Ta2O5, Sm2O3 and Nd2O3, wherein the weight ratio of Ta2O5, Sm2O3 and Nd2O3 is 1:2: 4.
In the second step, the weight ratio of the aluminum oxide to the zinc oxide to the silicon dioxide is 3:2: 1.
In the sixth step, the weight ratio of the first powder, the aluminum borate, the borax, the rare earth oxide, the sodium fluoride and the resorcinol monobenzoate is 6:1:2:1.5:1: 1.
And step eight, sintering pressure is 35MPa, and heat preservation and pressure maintaining time is 80 minutes.
The thickener in the fourth step consists of carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, polyoxyethylene and other components, and the coagulant consists of polymer coagulant and coagulant aid.
Example three:
aiming at the quality detection of the ceramic material for oral restoration prepared by the method, the ceramic material prepared by the method is selected, preferably, the ceramic material comprises 45 parts of zirconium oxide, 30 parts of aluminum oxide, 10 parts of zinc oxide, 5 parts of aluminum borate, 10 parts of borax, 10 parts of rare earth oxide, 5 parts of silicon dioxide, 10 parts of sodium fluoride, 5 parts of resorcinol monobenzoate, 4 parts of thickening agent and 4 parts of flocculating agent, a group of common ceramics sold on the market is selected for detection comparison, two comparison groups A and B are set up, wherein the group A is a common group sold on the market, the group B is the ceramic material prepared by the method, the detection standards are the density/(g.cm-3), the average grain diameter/mm-3, the surface roughness Ra/mm-3, the bending strength/MPa and the fracture toughness K/(MPa.m 1/2) of the ceramic material of each group, the test conditions are shown in the following table:
table one is the comparative case of the detection of 2 groups of ceramic materials:
group of | Group A | Group B |
Density/(g cm-3) | 3.93 | 6.05 |
Average particle diameter/mm-3 | 3 | 0.2 |
Surface roughness Ra/mm-3 | 0.02 | 0.008 |
Flexural strength/MPa | 595 | 1000 |
Fracture toughness K/(MPa. m1/2) | 5 | 15 |
As can be seen from Table 1, the ceramic material prepared by the method has better quality in density than similar products sold in the market, and generally has higher material properties such as average particle size, surface roughness, bending strength, fracture toughness and the like than similar products, so that the strength and toughness of the ceramic material are improved, the defect that the traditional ceramic material is brittle and fragile per se is overcome, and the clinical success rate is improved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. An oral repair ceramic material, comprising: the coating comprises, by weight, 45-65 parts of zirconium oxide, 30-40 parts of aluminum oxide, 10-20 parts of zinc oxide, 5-10 parts of aluminum borate, 10-20 parts of borax, 10-15 parts of rare earth oxide, 5-10 parts of silicon dioxide, 10-20 parts of sodium fluoride, 5-10 parts of resorcinol monobenzoate, 4-8 parts of a thickening agent and 4-8 parts of a flocculating agent.
2. The ceramic material for oral cavity restoration according to claim 1, wherein the ceramic material comprises, by weight, 48-62 parts of zirconia, 32-38 parts of alumina, 11-18 parts of zinc oxide, 6-8 parts of aluminum borate, 7-9 parts of borax, 11-14 parts of rare earth oxide, 6-9 parts of silicon dioxide, 12-17 parts of sodium fluoride, 6-9 parts of resorcinol monobenzoate, 5-7 parts of thickener and 5-7 parts of coagulant.
3. A preparation method of an oral cavity repairing ceramic material is characterized by comprising the following steps:
the method comprises the following steps: putting zirconia into an ethanol solution, and fully dissolving the zirconia by a stirring dispersion machine;
step two: heating the solution obtained in the step one to 60-80 ℃, then respectively adding alumina, zinc oxide and silicon dioxide at 60-80 ℃, and standing for reaction;
step three: cooling the reactant obtained in the step two, and then adding a polyethylene glycol solution;
step four: adding a thickening agent and a coagulant into the solution obtained in the third step at normal temperature, and preparing the solution into colloid by a three-roll grinder;
step five: putting the colloid obtained in the fourth step into a high-pressure reaction kettle for reaction, and obtaining first powder after the reaction is finished;
step six: mixing the first powder obtained in the fifth step with aluminum borate, borax, rare earth oxide, sodium fluoride and resorcinol monobenzoate;
step seven: adding the mixed material obtained in the sixth step into a ball milling tank for wet ball milling for 8-20 hours, drying, sieving with a 150-mesh sieve, and then putting into a graphite mold for compression molding under the pressure of 15-40MPa to obtain a blank;
step eight: and sintering the green body obtained in the seventh step with nitrogen at the sintering temperature of 1250-1350 ℃, and naturally cooling to room temperature to obtain the ceramic material.
4. The method for preparing an oral cavity repairing ceramic material according to claim 3, wherein the rare earth oxide in the sixth step comprises Ta2O5, Sm2O3 and Nd2O3, and the weight ratio of Ta2O5, Sm2O3 and Nd2O3 is 1:2: 4.
5. The method for preparing ceramic material for oral cavity restoration according to claim 3, wherein the weight ratio of alumina, zinc oxide and silicon dioxide in the second step is 3:2: 1.
6. The method for preparing an oral cavity repairing ceramic material according to claim 3, wherein the weight ratio of the first powder, the aluminum borate, the borax, the rare earth oxide, the sodium fluoride and the resorcinol monobenzoate in the sixth step is 6:1:2:1.5:1: 1.
7. The method for preparing an oral cavity repairing ceramic material according to claim 3, wherein the sintering pressure in step eight is 35MPa, and the holding time is 80 minutes.
8. The method for preparing ceramic material for oral cavity restoration according to claim 3, wherein said thickener in step four comprises carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, and polyoxyethylene, and said coagulant comprises polymeric coagulant and coagulant aid.
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