CN106747434B - Wear-resistant zirconia ceramic and preparation method thereof - Google Patents
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Abstract
The invention provides a wear-resistant zirconia ceramic and a preparation method thereof, wherein the wear-resistant zirconia ceramic comprises the following raw materials in parts by weight: 60-70 parts of zirconium oxide, 1-3 parts of graphene oxide, 10-14 parts of hydroxyapatite, 12-16 parts of surfactant, 9-12 parts of cross-linking agent and 4-8 parts of additive. The preparation method comprises the following steps: uniformly mixing zirconium oxide, mixed liquid of graphene oxide and polysilazane, hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 500-600 ℃, melting the raw material mixture subjected to degumming in a platinum crucible at 1150-1300 ℃ for 2-3 h, transferring to an annealing furnace for heat treatment for 4-5 h, and slowly cooling to room temperature. The ceramic has good wear resistance and reduces the liquid phase sintering temperature.
Description
Technical Field
The invention belongs to the technical field of ceramics, and particularly relates to wear-resistant zirconia ceramics and a preparation method thereof.
Background
Zirconia ceramics have higher strength, toughness and corrosion and abrasion resistance than alumina, are widely applied to the fields of metallurgy, chemical industry, machinery, electronics, petroleum and the like, and are also called as tough ceramics due to the unique stress-induced martensite phase transformation toughening property. The zirconium oxide has extremely high chemical stability and thermal stability (Tm is 2953K), is inert in physiological environment and has good biocompatibility. Pure zirconia has three allotypes and can undergo crystal transformation (phase transition) under certain conditions. When the steel plate is subjected to external force, the process of t-phase-to-m-phase transformation needs to absorb higher energy, so that the stress at the tip of a crack is relaxed, and the crack diffusion resistance is increased to toughen the steel plate, thereby having very high fracture toughness.
The production of zirconia ceramics requires the preparation of powder with high purity, good dispersion property, superfine particles and narrow particle size distribution, the preparation methods of zirconia superfine powder are many, and the purification of zirconia mainly comprises chlorination and thermal decomposition method, alkali metal oxidation decomposition method, lime melting method, plasma arc method, precipitation method, colloid method, hydrolysis method, spray pyrolysis method and the like. The powder processing method includes coprecipitation method, sol-gel method, evaporation method, supercritical synthesis method, microemulsion method, hydrothermal synthesis method, vapor deposition method, etc.
At normal temperature, zirconia only appears in monoclinic phase, and is converted into tetragonal phase when heated to about 1100 ℃, and is converted into cubic phase when heated to higher temperature. Because the monoclinic phase can generate larger volume change when being converted to the tetragonal phase, and the monoclinic phase can generate larger volume change in the opposite direction when being cooled, the product is easy to crack, the application of pure zirconium oxide in the high-temperature field is limited, and the wear-resisting property of the pure zirconium oxide is general.
Disclosure of Invention
The invention provides a wear-resistant zirconia ceramic which has good wear resistance and reduces the liquid phase sintering temperature.
The technical scheme of the invention is realized as follows:
the wear-resistant zirconia ceramic comprises the following raw materials in parts by weight:
60-70 parts of zirconium oxide, 1-3 parts of graphene oxide, 10-14 parts of hydroxyapatite, 12-16 parts of surfactant, 9-12 parts of cross-linking agent and 4-8 parts of additive;
adding the graphene oxide into an N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, and then stirring and ultrasonically treating the mixture to obtain a mixed solution; in the mixed solution, the ratio of the polysilazane content to the graphene oxide content is 1: 0.1-1 by mass.
In some preferred embodiments of the invention, the ratio of Ca to P in the hydroxyapatite is 1: 1.98.
In some preferred embodiments of the present invention, the surfactant is one or more of glyceryl monostearate, sorbitan sesquioleate, propylene glycol fatty acid ester, or dioctyl sodium sulfosuccinate.
In some preferred embodiments of the present invention, the crosslinking agent is one or more of N, N' -methylenebisacrylamide, diethylenetriamine, or divinylbenzene.
In some preferred embodiments of the present invention, the additive is one or more of zinc oxide, barium carbonate and calcium fluoride.
The invention also aims to provide a preparation method of the wear-resistant zirconia ceramic, which comprises the following steps:
1) adding graphene oxide into an N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, stirring and performing ultrasonic treatment to obtain a mixed solution, wherein the ratio of the content of the polysilazane to the content of the graphene oxide in the mixed solution is 1: 0.1-1 by mass;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 500-600 ℃, melting the degummed raw material mixture in a platinum crucible at 1150-1300 ℃ for 2-3 h, transferring to an annealing furnace for heat treatment for 4-5 h, and slowly cooling to room temperature.
In some preferred embodiments of the invention, the concentration of the N, N-dimethylformamide solution is 2-5 mol/L.
In some preferred embodiments of the present invention, the soaking time is 0.5 to 1.5 hours.
In some preferred embodiments of the present invention, the heat treatment temperature is 200 to 300 ℃.
The invention has the advantages that:
1. according to the invention, graphene oxide is used as a sintering aid instead of traditional magnesium oxide and silicon oxide, and the graphene oxide is found to promote sintering, so that the hardness and wear resistance of the ceramic are improved.
2. The inventor surprisingly finds that the graphene oxide is mixed, then is added into an N, N-dimethylformamide solution for soaking pretreatment, and then is mixed with a polysilazane solution, so that the high-temperature resistance of the graphene oxide at a high temperature is improved, the subsequent high-temperature sintering is facilitated, the porosity of the material is rapidly reduced, the density of the material is increased, and the sintering temperature of a tetragonal polycrystalline zirconia (TZP) material is greatly reduced.
Detailed Description
Example 1
The wear-resistant zirconia ceramic comprises the following raw materials in parts by weight:
65 parts of zirconium oxide, 2 parts of graphene oxide, 12 parts of hydroxyapatite, 14 parts of surfactant, 10 parts of cross-linking agent and 6 parts of additive.
The ratio of Ca to P in the hydroxyapatite is 1: 1.98.
The surfactant is a mixture of glyceryl monostearate and sorbitan sesquioleate.
The cross-linking agent is N, N' -methylene bisacrylamide.
The additives are zinc oxide and calcium fluoride.
The preparation method comprises the following steps:
1) adding graphene oxide into 4mol/L N, N-dimethylformamide solution to prepare graphene oxide dispersion liquid, mixing with polysilazane solution, stirring, and performing ultrasonic treatment to obtain mixed liquid, wherein the ratio of the polysilazane content to the graphene oxide content in the mixed solution is 1: 0.6 according to the mass ratio;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 500 ℃, melting the degummed raw material mixture in a platinum crucible at 1200 ℃ for 3h, transferring to an annealing furnace for heat treatment for 4h, wherein the heat treatment temperature is 260 ℃, and slowly cooling to room temperature.
Example 2
The wear-resistant zirconia ceramic comprises the following raw materials in parts by weight:
60 parts of zirconium oxide, 1 part of graphene oxide, 10 parts of hydroxyapatite, 16 parts of surfactant, 12 parts of cross-linking agent and 8 parts of additive.
The ratio of Ca to P in the hydroxyapatite is 1: 1.98.
The surfactant is a mixture of propylene glycol fatty acid ester and dioctyl sodium sulfosuccinate.
The crosslinking agent is divinylbenzene.
The additive is calcium fluoride.
The preparation method comprises the following steps:
1) adding graphene oxide into 2mol/L N, N-dimethylformamide solution to prepare graphene oxide dispersion liquid, mixing with polysilazane solution, stirring, and performing ultrasonic treatment to obtain mixed liquid, wherein the ratio of the polysilazane content to the graphene oxide content in the mixed solution is 1: 0.9 according to the mass ratio;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 550 ℃, melting the degummed raw material mixture in a platinum crucible at 1150 ℃ for 2h, transferring to an annealing furnace for heat treatment for 4.5h, wherein the heat treatment temperature is 200 ℃, and slowly cooling to room temperature.
Example 3
The wear-resistant zirconia ceramic comprises the following raw materials in parts by weight:
70 parts of zirconium oxide, 3 parts of graphene oxide, 10 parts of hydroxyapatite, 16 parts of surfactant, 9 parts of cross-linking agent and 4 parts of additive.
The ratio of Ca to P in the hydroxyapatite is 1: 1.98.
The surfactant is a mixture of glyceryl monostearate and dioctyl sodium sulfosuccinate.
The cross-linking agent is N, N' -methylene bisacrylamide.
The preparation method comprises the following steps:
1) adding graphene oxide into a 5mol/L N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, stirring and performing ultrasonic treatment to obtain a mixed solution, wherein the ratio of the content of the polysilazane to the content of the graphene oxide is 1: 0.1 in the mixed solution according to the mass ratio;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 600 ℃, melting the degummed raw material mixture in a platinum crucible at 1250 ℃ for 2h, transferring to an annealing furnace for heat treatment for 5h, wherein the heat treatment temperature is 300 ℃, and slowly cooling to room temperature.
The additive is zinc oxide.
Example 4
The wear-resistant zirconia ceramic comprises the following raw materials in parts by weight:
66 parts of zirconium oxide, 2 parts of graphene oxide, 13 parts of hydroxyapatite, 15 parts of surfactant, 12 parts of cross-linking agent and 8 parts of additive.
The ratio of Ca to P in the hydroxyapatite is 1: 1.98.
The surfactant is a mixture of glyceryl monostearate, sorbitan sesquioleate and dioctyl sodium sulfosuccinate.
The cross-linking agent is diethylenetriamine.
The additive is a mixture of zinc oxide and calcium fluoride.
The preparation method comprises the following steps:
1) adding graphene oxide into a 5mol/L N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, stirring and performing ultrasonic treatment to obtain a mixed solution, wherein the ratio of the content of the polysilazane to the content of the graphene oxide is 1:1 in the mixed solution according to the mass ratio;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 540 ℃, melting the degummed raw material mixture in a platinum crucible at 1300 ℃ for 2h, transferring to an annealing furnace for heat treatment for 5h, wherein the heat treatment temperature is 300 ℃, and slowly cooling to room temperature.
Comparative example 1
Same as example 1, except that: the graphene oxide was replaced with barium oxide.
Performance testing
The ceramics of examples 1 to 4 and comparative example 1 were subjected to performance tests, and the results are shown in Table 1.
TABLE 1 results of ceramic Performance test of examples 1-4 and comparative example 1
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The wear-resistant zirconia ceramic is characterized by comprising the following raw materials in parts by weight: 60-70 parts of zirconium oxide, 1-3 parts of graphene oxide, 10-14 parts of hydroxyapatite, 12-16 parts of surfactant, 9-12 parts of cross-linking agent and 4-8 parts of additive;
adding the graphene oxide into an N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, and then stirring and ultrasonically treating the mixture to obtain a mixed solution; in the mixed solution, the ratio of the polysilazane content to the graphene oxide content is 1: 0.1-1 by mass;
the additive is one or more of zinc oxide, barium carbonate and calcium fluoride.
2. The wear-resistant zirconia ceramic of claim 1 wherein the ratio of Ca to P in the hydroxyapatite is 1: 1.98.
3. The wear-resistant zirconia ceramic of claim 1 wherein the surfactant is one or more of glyceryl monostearate, sorbitan sesquioleate, propylene glycol fatty acid ester or dioctyl sodium sulfosuccinate.
4. The wear-resistant zirconia ceramic of claim 1 wherein the cross-linking agent is one or more of N, N' -methylenebisacrylamide, diethylenetriamine or divinylbenzene.
5. A method for preparing the wear-resistant zirconia ceramic according to any one of claims 1 to 4, comprising the steps of:
1) adding graphene oxide into an N, N-dimethylformamide solution to prepare a graphene oxide dispersion solution, mixing the graphene oxide dispersion solution with a polysilazane solution, stirring and performing ultrasonic treatment to obtain a mixed solution, wherein the ratio of the content of the polysilazane to the content of the graphene oxide in the mixed solution is 1: 0.1-1 by mass;
2) uniformly mixing zirconium oxide, the mixed solution obtained in the step 1), hydroxyapatite, a surfactant, a cross-linking agent and an additive to obtain a raw material mixture, then carrying out degumming treatment at 500-600 ℃, melting the degummed raw material mixture in a platinum crucible at 1150-1300 ℃ for 2-3 h, transferring to an annealing furnace for heat treatment for 4-5 h, and slowly cooling to room temperature.
6. The method for preparing the wear-resistant zirconia ceramic according to claim 5, wherein the concentration of the N, N-dimethylformamide solution is 2-5 mol/L.
7. The preparation method of the wear-resistant zirconia ceramic according to claim 6, wherein the soaking time is 0.5-1.5 h.
8. The method for preparing the wear-resistant zirconia ceramic according to claim 6, wherein the heat treatment temperature is 200-300 ℃.
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| CN104744037A (en) * | 2015-03-31 | 2015-07-01 | 苏州维泰生物技术有限公司 | Wear-resisting zirconium oxide ceramics and preparation method thereof |
| CN105503145A (en) * | 2015-12-10 | 2016-04-20 | 上海高诚创意科技集团有限公司 | Preparation method of ceramic containing graphene oxide |
| CN105732064A (en) * | 2016-02-24 | 2016-07-06 | 厦门大学 | Method for preparing cylindrical graphene reinforced SiCN ceramic temperature sensor |
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