CN114044683A - Oral cavity repairing ceramic material and preparation method thereof - Google Patents
Oral cavity repairing ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an oral repair ceramic material and a preparation method thereof. The cryogenic treatment is a new technology developed on the basis of a common cold treatment process, but most of research objects of the cryogenic treatment at the present stage are limited to steel materials. In order to prolong the service life of the traditional silicon nitride ceramic material as an oral cavity repairing material, the sintered silicon nitride ceramic is put into liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for the first time. Experiments show that the cryogenic treatment for 20-60min can obviously improve the fracture toughness of the silicon nitride ceramic material and can be improved to 8.91 MPa.m1/2. Such treatment is reducingThe preparation difficulty of the silicon nitride ceramic is improved, and the application scene of the silicon nitride ceramic as a medical material is widened.
Description
Technical Field
The invention relates to the field of medical materials, in particular to an oral repair ceramic material and a preparation method thereof.
Background
Silicon nitride (Si)3N4) The ceramic has higher room temperature strength and fracture toughness, the room temperature bending strength of the hot-pressed sintered compact silicon nitride is usually 800-1050MPa, the fracture toughness is 6-7 MPa-m 1/2, and the mechanical properties of the silicon nitride ceramic sintered without pressure and sintered by air pressure are slightly lower. At the same timeThe silicon nitride ceramic has high hardness, HV of about 18-21GPa, HRA of about 91-93 and friction coefficient of about 0.02-0.35. Because the silicon nitride ceramics have excellent mechanical properties, thermal properties, chemical stability and dielectric properties, the silicon nitride ceramics are widely applied to a plurality of aspects such as electronics, electric power, biomedicine and the like.
However, the lack of fracture toughness of silicon nitride ceramics limits their useful life as restorative materials for the oral cavity. In order to solve the problem, the Chinese patent CN202110994853.1 finds that the sintering aid Al is mixed according to a specific proportion2O3Can generate synergistic interaction with MgO to improve the fracture toughness of the silicon nitride ceramic material to 8.5 MPa.m1/2The above. However, this method requires accurate weighing of each raw material and is harsh in terms of process conditions, which undoubtedly increases the difficulty of industrial production. In view of the above, the present invention is expected to obtain a process for producing silicon nitride ceramic materials with less operational difficulty.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of an oral repair ceramic material, which can obtain a silicon nitride ceramic material with high fracture toughness.
The preparation method of the oral cavity repairing ceramic material is characterized by comprising the following steps:
A. mixing Si3N4Weighing the powder and the sintering aid according to the proportion;
B. putting the raw material powder into a ball milling tank, taking absolute ethyl alcohol as a dispersion medium, and ball milling the mixed raw material for 6-10h at the rotating speed of 300-350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying box, and drying at the temperature of 100-120 ℃ for 20-24 h;
D. sieving the dried mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 30-32MPa, then carrying out isostatic pressing, the pressure is 100-110MPa, and the pressure maintaining time is 8-10 s;
E. putting the product after the pressing forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5-5.0MPa, the sintering temperature is 1650-1700 ℃, and the sintering time is 2.5-3.0 h;
F. and soaking the sintered ceramic material in liquid nitrogen for cryogenic treatment.
Preferably, the sintering aid is Al2O3Or MgO.
Preferably, the sintering aid is Al2O3And MgO.
Preferably, the temperature of the liquid nitrogen is-196 ℃.
Preferably, the time of the cryogenic treatment is 20-120 min.
Preferably, the time of the cryogenic treatment is 60 min.
Furthermore, the invention also provides an oral cavity repairing ceramic material which is prepared by any one of the methods.
The cryogenic treatment is a new technology developed on the basis of a common cold treatment process, but most of research objects of the cryogenic treatment at the present stage are limited to steel materials. In order to prolong the service life of the traditional silicon nitride ceramic material as an oral cavity repairing material, the sintered silicon nitride ceramic is put into liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for the first time. Experiments show that the cryogenic treatment for 20-60min can obviously improve the fracture toughness of the silicon nitride ceramic material and can be improved to 8.91 MPa.m1/2. The treatment reduces the manufacturing difficulty of the silicon nitride ceramic and widens the application scene of the silicon nitride ceramic as a medical material.
Detailed Description
The technical effects of the present invention are demonstrated below by specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 20 min.
Example 2
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 40 min.
Example 3
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 60 min.
Example 4
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 120 min.
Example 5
A. Mixing Si3N4And MgO are weighed according to the mixture ratio, wherein the mass of the two substances is 89.2g and 8.7g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 60 min.
Example 6
A. Mixing Si3N4And Al2O3Weighing according to the mixture ratio, wherein the mass of the two substances is 89.2g and 8.7g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 60 min.
Example 7
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h;
F. and soaking the sintered ceramic material in liquid nitrogen at the temperature of-196 ℃ for cryogenic treatment for 20min, taking out, standing for 30min at room temperature, and repeating the operation twice (the total duration of the cryogenic treatment is 60 min).
Comparative example
A. Mixing Si3N4、Al2O3And MgO are weighed according to the mixture ratio, wherein the mass of the three substances is 89.2g, 5.1g and 3.6g respectively;
B. putting the raw material powder into a polyurethane ball milling tank, using absolute ethyl alcohol as a dispersion medium and boron nitride as ball milling balls, and ball milling the mixed raw material for 6 hours at the rotating speed of 350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying oven, and drying for 20h at 120 ℃;
D. sieving the dried mixed powder with a 80-mesh sieve, weighing 40g of the mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 32MPa, then carrying out isostatic pressing, the pressure is 105MPa, and the pressure maintaining time is 8 s;
E. and putting the product after the press forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5MPa, the sintering temperature is 1650 ℃, and the sintering time is 2.5 h.
Next, we evaluate the fracture toughness of each sample, and determine the fracture toughness of each sample by using a single-edge notched beam method, which specifically comprises: the samples were machined to a size of 3 x 4 x 40mm, a sharp crack having a width of 0.2mm and a depth of 1.5mm was prepared in the center of the sample using a diamond cutting blade, and then the sample was fractured at the crack by a pressure from the top to the bottom, the span in the test was 20mm, the loading rate was 0.5mm/min, and 5 parallel tests were performed for each sample, and the average value thereof was calculated. The test data for each experimental sample is shown in table 1.
TABLE 1 fracture toughness of the samples
| Numbering | Fracture toughness/MPa.m1/2 |
| Example 1 | 8.01 |
| Example 2 | 8.34 |
| Example 3 | 8.55 |
| Example 4 | 8.39 |
| Example 5 | 7.53 |
| Example 6 | 7.04 |
| Example 7 | 8.91 |
| Comparative example | 7.33 |
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. The preparation method of the oral cavity repairing ceramic material is characterized by comprising the following steps:
A. mixing Si3N4Weighing the powder and the sintering aid according to the proportion;
B. putting the raw material powder into a ball milling tank, taking absolute ethyl alcohol as a dispersion medium, and ball milling the mixed raw material for 6-10h at the rotating speed of 300-350rad/s by using a planetary ball mill;
C. placing the mixed slurry after ball milling in a drying box, and drying at the temperature of 100-120 ℃ for 20-24 h;
D. sieving the dried mixed powder, putting the mixed powder into a mould for compression molding, wherein the pressure is 30-32MPa, then carrying out isostatic pressing, the pressure is 100-110MPa, and the pressure maintaining time is 8-10 s;
E. putting the product after the pressing forming into an atmosphere pressure sintering furnace, and sintering in a nitrogen atmosphere, wherein the sintering pressure is 4.5-5.0MPa, the sintering temperature is 1650-1700 ℃, and the sintering time is 2.5-3.0 h;
F. and soaking the sintered ceramic material in liquid nitrogen for cryogenic treatment.
2. A method of preparing a ceramic restorative material according to claim 1, wherein the sintering aid is Al2O3Or MgO.
3. A process for the preparation of a ceramic restorative material according to claim 1 or 2, wherein the sintering aid is Al2O3And MgO.
4. A method of preparing an oral cavity restoration ceramic material according to claims 1-3 wherein the temperature of the liquid nitrogen is-196 ℃.
5. A method of preparing an oral cavity restoration ceramic material according to claim 1, wherein the time of said cryogenic treatment is 20-120 min.
6. A method of preparing an oral cavity restoration ceramic material according to claim 1, wherein the time of said cryogenic treatment is 60 min.
7. An ceramic restorative oral material produced by the method of any of claims 1-6.
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- 2021-12-16 CN CN202111544099.8A patent/CN114044683B/en active Active
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| CN101695808A (en) * | 2009-10-27 | 2010-04-21 | 重庆泰蒙科技有限公司 | Preparation method of high-performance pored ceramic blade |
| CN102329151A (en) * | 2011-09-23 | 2012-01-25 | 重庆文理学院 | Cryogenic treatment method for ceramic/metal ceramic cutting tool |
| CN108585909A (en) * | 2018-07-09 | 2018-09-28 | 七七七电气科技有限公司 | For the high-strength tenacity of vacuum interrupter and the ceramic preparation process of high insulation resistance |
| US20210032165A1 (en) * | 2019-07-30 | 2021-02-04 | Chongqing Institute Of East China Normal University | Method for preparing carbon-reinforced metal-ceramic composite material |
| CN113429211A (en) * | 2021-08-27 | 2021-09-24 | 中南大学湘雅医院 | Silicon nitride ceramic material and preparation method thereof |
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| Title |
|---|
| 穆柏春: "SiCp/Si_3N_4复合材料的低温冷处理与强韧化", 《硅酸盐学报》 * |
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