CN111848157A - Zirconia ceramic block prepared by gel film-injection process and preparation method thereof - Google Patents
Zirconia ceramic block prepared by gel film-injection process and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a zirconia ceramic block prepared by a gel film-injection process and a preparation method thereof, wherein the preparation method comprises the following steps: adding acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder into a water solvent, and adding a dispersing agent with the mass fraction of 0.2-2% of powder to obtain a premixed solution; adjusting the pH value of the premixed liquid to 9-11, and then adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%; performing slurry viscosity test by using a rotational viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio; adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry in turn and stirring uniformly; injecting the prepared slurry into a prefabricated mold, curing and demolding to obtain a wet blank; drying the wet blank to obtain a blank body; sintering to obtain the zirconia ceramic block. The method has the advantages of simple preparation process, good compactness of the porcelain block, few defects of the porcelain block, low organic matter content of the porcelain block, high hardness and strength, capability of machining, simple instruments required for preparation, low mold cost and the like.
Description
Technical Field
The invention relates to the technical field of zirconia ceramic block preparation, in particular to a zirconia ceramic block prepared by a gel film-injection process and a preparation method thereof.
Background
Dental caries, defective dentition, malformation or loss of dentition are the most common oral diseases, wherein dental caries is one of the three major diseases which endanger human health, and is also the main reason for formation of tooth bodies, defective dentition and loss. The main component of natural tooth is calcium-containing substance with higher hardness and wear resistance, so the false tooth mainly adopts materials with high hardness and good wear resistance such as alloy and zirconia, the problems of black lines in oral cavity, even allergy and the like can be caused after the alloy false tooth is repaired for a long time, and the aesthetic degree is lower than that of the zirconia restoration, so the zirconia material restoration forms the first choice material for the false tooth repair.
The production mode of zirconia in the market at present is dry pressing production, namely, an adhesive or an organic matter is added into zirconia powder, and the zirconia powder is molded by unidirectional extrusion or bidirectional counter pressing, so that the prepared zirconia is often subjected to internal defects of the molded zirconia, such as air holes, cracks and agglomeration, due to uneven extrusion force, poor powder flowability, extrusion exhaust problems and the like, the defects often cause low strength of the zirconia, and the zirconia is broken in later-stage processing or milling to cause production failure; the traditional zirconia manufacturing process is complicated, various large-scale equipment such as a dry press, an isostatic press, a pre-burning furnace, a binder removal furnace and the like needs to be used, the cost and energy consumption investment are large, and the production efficiency is general.
Thus, there is a need for improvements and enhancements in the art.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide the zirconia ceramic block prepared by the gel film-injection process and the preparation method thereof, and aims to solve the problems of complex process, high cost, low production efficiency, low strength, more defects and the like of the produced zirconia ceramic block in the conventional preparation method.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing a zirconia ceramic block prepared by a gel film-casting process comprises the following steps:
a. adding acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder into a water solvent, and adding a dispersing agent with the mass fraction of 0.2-2% of powder to obtain a premixed solution;
b. adjusting the pH value of the premixed liquid to 9-11, and then adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%;
c. performing slurry viscosity test by using a rotational viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio;
d. adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry in turn and stirring uniformly;
e. D, injecting the slurry prepared in the step d into a prefabricated mold, curing in situ for 1-2 hours at room temperature, and demolding to obtain a wet blank;
f. drying the wet blank at a three-stage temperature and humidity to obtain a blank body;
g. and f, sintering the blank prepared in the step f to obtain the zirconia ceramic block.
The preparation method of the zirconia ceramic block prepared by the gel casting process comprises the following steps of a, adding acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder into a water solvent, and adding a dispersing agent with the mass fraction of 0.2-2% of powder into the water solvent to obtain a premixed solution, wherein the water solvent is deionized water.
The preparation method of the zirconia ceramic block prepared by the gel casting process comprises the following steps of a, adding acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder into a water solvent, and then adding a dispersing agent with the mass fraction of 0.2-2% of powder to obtain a premixed solution, wherein the dispersing agent is one of sodium hexametaphosphate, polyvinyl alcohol, ammonium polyacrylate and ammonium citrate.
The preparation method of the zirconia ceramic block prepared by the gel casting process comprises the following steps of b, adjusting the pH value of the premixed solution to 9-11, and adding nano zirconia powder to enable the volume fraction of the solid phase of the slurry to reach more than 50%, wherein the adjustment of the pH value of the premixed solution to 9-11 is realized by adding strong ammonia water.
The preparation method of the zirconia ceramic block prepared by the gel casting process comprises the step d of sequentially adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry and uniformly stirring, wherein the initiator is ammonium persulfate, and the catalyst is tetramethyl ethylene diamine.
The preparation method of the zirconia ceramic block prepared by the gel film-casting process comprises the following steps of (a) drying a wet blank at three-stage temperature and humidity, wherein the blank obtained after drying specifically comprises the following steps:
the low-temperature and high-humidity environment is adopted for slow drying, and then the high-temperature and low-humidity environment is adopted for slow drying.
The preparation method of the zirconia ceramic block prepared by the gel film-casting process comprises the steps of firstly adopting a low-temperature high-humidity environment to carry out slow drying, and then adopting a high-temperature low-humidity environment to carry out slow drying, wherein the whole drying time is not less than 48 hours.
The preparation method of the zirconia ceramic block prepared by the gel film-casting process comprises the following steps of:
when the temperature reaches 1480-1550 ℃, the temperature is maintained for 2H.
A zirconia ceramic block prepared by a gel film-casting process is prepared by the preparation method of the zirconia ceramic block prepared by the gel film-casting process.
The zirconia denture is characterized by being prepared from the zirconia porcelain block prepared by the gel film-injection process.
Compared with the prior art, the invention provides the zirconia ceramic block prepared by the gel casting process and the preparation method thereof, according to the preparation method provided by the invention, acrylamide and methylene bisacrylamide with the powder mass fraction of 1-5% are added into a water solvent, and a dispersing agent with the powder mass fraction of 0.2-2% is added to obtain a premixed solution; adjusting the pH value of the premixed liquid to 9-11, and then adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%; performing slurry viscosity test by using a rotational viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio; adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry in turn and stirring uniformly; injecting the prepared slurry into a prefabricated mold, curing in situ for 1-2 hours at room temperature, and demolding to obtain a wet blank; drying the wet blank at a three-stage temperature and humidity to obtain a blank body; and sintering the green body to obtain the zirconia ceramic block. The preparation method can effectively eliminate the agglomeration defect of the traditional zirconia ceramic block molding particles, has the advantages of simple preparation process, good compactness of the ceramic block, few defects of the ceramic block, low organic matter content of the ceramic block, high hardness and strength, capability of machining, simple instruments required for preparation, low mold cost and the like, and can be used for solving the limitation of the traditional zirconia ceramic block preparation method at present.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
Fig. 1 is a flow chart of a method for preparing a zirconia ceramic block by a gel casting process according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the description of the present invention, the terms "comprising," "including," "having," "containing," and the like, as used herein, are open-ended terms that mean including, but not limited to. Reference to the description of the terms "one embodiment," "a particular embodiment," "some embodiments," "for example," etc., means that a particular feature, structure, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. 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, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. The sequence of steps involved in the embodiments is for illustrative purposes to illustrate the implementation of the present application, and the sequence of steps is not limited and can be adjusted as needed.
Various non-limiting embodiments of the present invention are described in detail below with reference to the accompanying drawings.
Referring to fig. 1, the present invention provides a method for preparing a zirconia ceramic block by a gel casting process, wherein the method comprises the following steps:
s100, adding acrylamide and methylene bisacrylamide, the mass fraction of which is 1-5%, into a water solvent, and adding a dispersing agent, the mass fraction of which is 0.2-2%, into the water solvent to obtain a premixed solution;
specifically, in some embodiments of the present invention, the water solvent is deionized water, the deionized water refers to pure water from which impurities in the form of ions are removed, the deionized water is manufactured through ion exchange and reverse osmosis processes, the process is advanced, the yield is high, the internal energy consumption is low, and the organic macromolecules are removed through ion exchange and reverse osmosis, so that the effect is better. Acrylamide is an organic monomer, and the organic monomer plays a role in crosslinking and polymerizing with a crosslinking agent to form three-dimensional network polymerized gel, and enables zirconium oxide particles to be bonded, cured and formed in situ.
Further, in some embodiments of the present invention, the dispersant is one of sodium hexametaphosphate, polyvinyl alcohol, ammonium polyacrylate, and ammonium citrate.
S200, adjusting the pH value of the premixed liquid to 9-11, and adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%;
Specifically, in some embodiments of the present invention, the adjustment of the pH of the premix to 9-11 is performed by adding concentrated ammonia and adjusting the pH of the premix to 9-11 using pH paper or pH meter.
Further, in some embodiments of the present invention, the pH value of the premixed solution is adjusted to 9 to 11, and then the nano zirconia powder is gradually and slowly added in multiple times, so that the solid phase volume fraction of the slurry reaches more than 50%.
S300, performing a slurry viscosity test by using a rotary viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio;
specifically, a probe of the rotational viscosity tester is extended into the slurry, and a reading is obtained when the rotating speed of the rotor. Rotor selection principle: firstly, roughly estimating the viscosity range of the slurry, and reasonably selecting according to a measuring range table, wherein if the viscosity range cannot be estimated, the high viscosity is selected to be small, and the rotating speed is low; the low viscosity is selected for large rotors and high rotational speeds.
S400, sequentially adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry, and uniformly stirring;
specifically, the gel cure time of the stable suspension slurry varies with the amount of initiator and catalyst added. In order to control the time for the slurry to start to carry out gel reaction and avoid too short time for pouring and too long time for preparation period, the gel reaction time is controlled to be 20-40 min; in some embodiments of the invention, the initiator is ammonium persulfate at a concentration of 5-10 wt% and the catalyst is tetramethylethylenediamine at a concentration of 20-60% by volume.
S500, injecting the slurry prepared in the step S400 into a prefabricated mold, curing in situ for 1-2 hours at room temperature, and demolding to obtain a wet blank;
specifically, the prefabricated mold has no special requirements on the material, and can be made of glass, silica gel, plastic and the like.
S600, drying the wet blank at a three-stage temperature and humidity to obtain a blank body;
specifically, in some embodiments of the present invention, the step S600 specifically includes:
the low-temperature and high-humidity environment is adopted for slow drying, and then the high-temperature and low-humidity environment is adopted for slow drying.
Specifically, it will be understood by those skilled in the art that the low temperature and high humidity is a relative comparison with the high temperature and low humidity, and in some embodiments, no particular numerical requirement is made, so long as the difference between low and high is highlighted.
Further, in some embodiments of the present invention, the slow drying is performed in a low-temperature and high-humidity environment, and then the slow drying is performed in a high-temperature and low-humidity environment, wherein the total drying time is not less than 48 hours.
S700, sintering the blank prepared in the step S600 to obtain the zirconia ceramic block.
Specifically, the green body contains a small amount of organic matters, the organic matters can be released at the temperature of 200-600 ℃, and the temperature rise rate has no great influence on the sintering of the green body after the temperature exceeds 600 ℃; further, in some embodiments of the present invention, 2H is incubated after reaching 1480-1550 ℃. The density of the zirconia ceramic block obtained after sintering is 6.05g/cm 3And the appearance of the crystal grains is complete through microscopic observation, the size of the crystal grains is uniform, and the structure is compact.
In order to further understand the above steps S100-S700 of the present invention, the principle of gel forming and curing will now be described.
Principle of gel forming and curing: the method is characterized in that the prepared nano zirconia slurry with low viscosity, high solid content, good stability and good dispersibility is taken as a basis, an organic monomer and a cross-linking agent in the slurry are still in a solution dispersion state, an initiator is added firstly, then a catalyst is added, the initiator can rapidly initiate monomer polymerization and cross-linking by the catalyst to form a three-dimensional reticular polymer, water molecules and ceramic block particles are fixed and formed in a reticular structure in situ to form a gel zirconia ceramic block with certain strength, the zirconia ceramic block is slowly dried by controlling temperature and humidity, and the zirconia ceramic block can be obtained after sintering.
Based on the embodiment, the invention also provides a zirconia ceramic block prepared by the gel film-casting process, wherein the zirconia ceramic block is prepared by adopting the preparation method of the zirconia ceramic block prepared by the gel film-casting process, and the preparation method is specifically as described above.
Based on the above embodiment, the invention also provides a zirconia denture, wherein the zirconia porcelain block prepared by the gel film-casting process is prepared, and the preparation method is specifically as described above.
In summary, the invention provides a zirconia ceramic block prepared by a gel film-casting process and a preparation method thereof, according to the preparation method provided by the invention, acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder are added into a water solvent, and a dispersant with the mass fraction of 0.2-2% of powder is added to obtain a premixed solution; adjusting the pH value of the premixed liquid to 9-11, and then adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%; performing slurry viscosity test by using a rotational viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio; adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry in turn and stirring uniformly; injecting the prepared slurry into a prefabricated mold, curing in situ for 1-2 hours at room temperature, and demolding to obtain a wet blank; drying the wet blank at a three-stage temperature and humidity to obtain a blank body; and sintering the green body to obtain the zirconia ceramic block. The preparation method can effectively eliminate the agglomeration defect of the traditional zirconia ceramic block molding particles, has the advantages of simple preparation process, good compactness of the ceramic block, few defects of the ceramic block, low organic matter content of the ceramic block, high hardness and strength, capability of machining, simple instruments required for preparation, low mold cost and the like, and can be used for solving the limitation of the traditional zirconia ceramic block preparation method at present.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A method for preparing zirconia ceramic blocks by a gel film-casting process is characterized by comprising the following steps:
a. adding acrylamide and methylene bisacrylamide with the mass fraction of 1-5% of powder into a water solvent, and adding a dispersing agent with the mass fraction of 0.2-2% of powder to obtain a premixed solution;
b. adjusting the pH value of the premixed liquid to 9-11, and then adding nano zirconia powder to enable the solid phase volume fraction of the slurry to reach more than 50%;
c. Performing slurry viscosity test by using a rotational viscosity tester to obtain the zirconia stable suspension slurry with low viscosity and high solid phase ratio;
d. adding 0.2-1 vol% of initiator and 0.4-1 vol% of catalyst into the stable suspension slurry in turn and stirring uniformly;
e. d, injecting the slurry prepared in the step d into a prefabricated mold, curing in situ for 1-2 hours at room temperature, and demolding to obtain a wet blank;
f. drying the wet blank at a three-stage temperature and humidity to obtain a blank body;
g. and f, sintering the blank prepared in the step f to obtain the zirconia ceramic block.
2. The method for preparing zirconia ceramic blocks by the gel casting process according to claim 1, wherein in the step a, acrylamide and methylene bisacrylamide are added into an aqueous solvent with the powder mass fraction of 1-5%, and a dispersing agent with the powder mass fraction of 0.2-2% is added to obtain a premixed solution, wherein the aqueous solvent is deionized water.
3. The method for preparing zirconia ceramic blocks by the gel casting process according to claim 1 or 2, wherein in the step a, acrylamide and methylene bisacrylamide are added into the aqueous solvent in an amount of 1-5% by mass of the powder, and a dispersant in an amount of 0.2-2% by mass of the powder is added to obtain a premixed solution, wherein the dispersant is one of sodium hexametaphosphate, polyvinyl alcohol, ammonium polyacrylate and ammonium citrate.
4. The method for preparing zirconia porcelain block by gel casting process according to claim 1, wherein the pH value of the premixed solution is adjusted to 9-11 in the step b, and then nano zirconia powder is added to make the volume fraction of solid phase of the slurry reach more than 50%, wherein the adjustment of the pH value of the premixed solution to 9-11 is realized by adding concentrated ammonia water.
5. The method for preparing zirconia ceramic blocks by gel casting process according to claim 1, wherein step d comprises adding 0.2 vol% -1 vol% of initiator and 0.4 vol% -1 vol% of catalyst into the stable suspension slurry in sequence and stirring uniformly, wherein the initiator is ammonium persulfate and the catalyst is tetramethylethylenediamine.
6. The method for preparing the zirconia ceramic block prepared by the gel film-casting process according to claim 1, wherein the step f is to dry the wet blank at a three-stage temperature and humidity, and the drying to obtain the blank specifically comprises the following steps:
the low-temperature and high-humidity environment is adopted for slow drying, and then the high-temperature and low-humidity environment is adopted for slow drying.
7. The method for preparing zirconia ceramic block by gel casting process according to claim 6, wherein the slow drying is carried out in low temperature and high humidity environment, and then in high temperature and low humidity environment, wherein the whole drying time is not less than 48 hours.
8. The method for preparing the zirconia ceramic block prepared by the gel casting process according to claim 1, wherein the step g of sintering the green body prepared in the step f to obtain the zirconia ceramic block specifically comprises the following steps:
when the temperature reaches 1480-1550 ℃, the temperature is maintained for 2H.
9. A zirconia ceramic block prepared by a gel casting process, which is characterized by being prepared by the preparation method of the zirconia ceramic block prepared by the gel casting process according to any one of claims 1 to 8.
10. A zirconia denture, prepared using the zirconia porcelain block prepared by the gel casting process according to claim 9.
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| CN103373848A (en) * | 2012-04-24 | 2013-10-30 | 天津城市建设学院 | Preparation and curing process of ZrO2 gel-casting slurry |
| CN105272223A (en) * | 2015-09-29 | 2016-01-27 | 北京中材人工晶体研究院有限公司 | Preparation method of large-size zirconia-based heat insulation material |
| CN109485415A (en) * | 2018-09-13 | 2019-03-19 | 南京理工宇龙新材料科技股份有限公司 | A kind of zirconia ceramics and preparation method thereof |
| CN110511021A (en) * | 2019-09-10 | 2019-11-29 | 河南工业大学 | A kind of novel zirconia ceramics forming method |
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| CN103373848A (en) * | 2012-04-24 | 2013-10-30 | 天津城市建设学院 | Preparation and curing process of ZrO2 gel-casting slurry |
| CN105272223A (en) * | 2015-09-29 | 2016-01-27 | 北京中材人工晶体研究院有限公司 | Preparation method of large-size zirconia-based heat insulation material |
| CN109485415A (en) * | 2018-09-13 | 2019-03-19 | 南京理工宇龙新材料科技股份有限公司 | A kind of zirconia ceramics and preparation method thereof |
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