CN115819079A - Material for artificial teeth and preparation method thereof - Google Patents
Material for artificial teeth and preparation method thereof Download PDFInfo
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- CN115819079A CN115819079A CN202211541412.7A CN202211541412A CN115819079A CN 115819079 A CN115819079 A CN 115819079A CN 202211541412 A CN202211541412 A CN 202211541412A CN 115819079 A CN115819079 A CN 115819079A
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- 239000000463 material Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052709 silver Inorganic materials 0.000 claims abstract description 12
- 239000004332 silver Substances 0.000 claims abstract description 12
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 10
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims description 74
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 40
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 36
- 238000010438 heat treatment Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 33
- 239000000843 powder Substances 0.000 claims description 27
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 235000019253 formic acid Nutrition 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- 239000002253 acid Substances 0.000 claims description 19
- 238000000498 ball milling Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 16
- 239000012535 impurity Substances 0.000 claims description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000012188 paraffin wax Substances 0.000 claims description 11
- 238000007873 sieving Methods 0.000 claims description 11
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 9
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical group CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 9
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 claims description 8
- HDYRYUINDGQKMC-UHFFFAOYSA-M acetyloxyaluminum;dihydrate Chemical compound O.O.CC(=O)O[Al] HDYRYUINDGQKMC-UHFFFAOYSA-M 0.000 claims description 8
- 229940009827 aluminum acetate Drugs 0.000 claims description 8
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 8
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 7
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 4
- RBWNDBNSJFCLBZ-UHFFFAOYSA-N 7-methyl-5,6,7,8-tetrahydro-3h-[1]benzothiolo[2,3-d]pyrimidine-4-thione Chemical compound N1=CNC(=S)C2=C1SC1=C2CCC(C)C1 RBWNDBNSJFCLBZ-UHFFFAOYSA-N 0.000 claims description 2
- 235000011054 acetic acid Nutrition 0.000 claims description 2
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 7
- 238000003980 solgel method Methods 0.000 abstract description 4
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 210000000214 mouth Anatomy 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920002845 Poly(methacrylic acid) Polymers 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a material for artificial teeth and a preparation method thereof, wherein a sol-gel method is combined with a cold isostatic pressing and vacuum sintering process to realize the mixing of zirconium, yttrium, aluminum and silver in an atomic scale, and the prepared material has the advantages of high purity, few defects, good uniformity, stable property, good biocompatibility, good antibacterial and bactericidal properties, excellent mechanical properties and capability of completely meeting the requirements of an oral use environment and daily occlusion of a user.
Description
Technical Field
The invention belongs to the technical field of medical engineering materials, and particularly relates to a material for artificial teeth and a preparation method thereof.
Background
The currently widely used artificial tooth materials mainly include three major types, namely metal materials, ceramic materials and polymer resin materials. At present, the most common artificial tooth materials in clinic are polymethyl methacrylate, polymethacrylic acid and other materials (CN 103284889A, CN 113304315A), and the materials have the advantages of corrosion resistance, easiness in operation, strong designability and the like, but the defects are very obvious, namely the mechanical property is poor, so that the prepared artificial tooth is easy to crack in the using process and causes bad influence on a user. Zirconia is of wide interest because of its good mechanical, biological and aesthetic properties. CN109199872a discloses an artificial tooth material containing zirconia and yttria, but straw powder is used as a main component, and the use environment in the oral cavity is not considered, so that various problems are caused in the sintering process of the material.
Disclosure of Invention
In order to solve the problems of the existing artificial tooth material, the invention provides the artificial tooth material and the preparation method thereof, the sol-gel method is combined with the cold isostatic pressing and vacuum sintering process, the zirconium, the yttrium, the aluminum and the silver are mixed in the atomic scale, and the prepared material has high purity, less defects, good uniformity, stable property, good biocompatibility, excellent mechanical property and antibacterial sterilization, and completely meets the oral use environment and the daily occlusion of users.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a method for preparing a material for artificial teeth, comprising the steps of:
(1) Mixing and stirring a zirconium source, acid and water, and heating for reaction to obtain sol A;
(2) Mixing and stirring yttrium source, acid and water, and heating for reaction to obtain sol B;
(3) Mixing and stirring an aluminum source, acid and water, and heating for reaction to obtain sol C;
(4) Mixing the sol A, B with the sol C, adding a silver source, uniformly stirring to obtain a mixture D, concentrating and drying the mixture D to obtain a mixture E, and heating the mixture E to 700-900 ℃ to remove impurities to obtain a mixture F;
(5) Mixing the mixture F and paraffin, ball-milling, drying and sieving to obtain powder G;
(6) And (3) carrying out cold isostatic pressing on the powder G, and then carrying out vacuum sintering to obtain the material for the artificial teeth.
Further, in the step (1), the zirconium source is selected from at least one of zirconium acetate, zirconium oxychloride and zirconium nitrate, the acid is selected from at least one of formic acid, acetic acid, nitric acid and hydrochloric acid, and the mass ratio of the zirconium source to the acid to the water is 1:0.1 to 0.6:30 to 50 ℃ and the temperature of the heating reaction is 60 to 90 ℃.
Further, in the step (2), yttrium source is yttrium acetate, acid is at least one selected from formic acid, acetic acid, nitric acid and hydrochloric acid, and the mass ratio of yttrium source, acid and water is 1:0.1 to 0.8: 30-40 ℃, and the heating reaction temperature is 60-120 ℃.
Further, in the step (3), the aluminum source is at least one selected from elemental aluminum, aluminum nitrate and basic aluminum acetate, the acid is at least one selected from formic acid, acetic acid, propionic acid, nitric acid and hydrochloric acid, and the mass ratio of the aluminum source to the acid to the water is 1:0.2 to 1.2:20 to 40 percent, and the temperature of the heating reaction is 60 to 90 ℃.
Further, in the step (4), zrO is added 2 ：Y 2 O 3 ：Al 2 O 3 In terms of mass ratio of sol A, B to C is 1:0.1 to 0.3:0.3 to 0.6; the silver source is at least one of silver nitrate, silver chlorate and silver perchlorate, and the addition amount of the silver source is 0.01 to 5wt percent of the sum of A, B and C, preferably 0.5 to 2wt percent.
Further, in the step (4), the mixture E is heated to 300-500 ℃ at a heating rate of 5-10 ℃/min, and is kept warm for 0.5-3 h, and then is heated to 700-900 ℃ at a heating rate of 10-20 ℃/min, and is kept warm for 1-3 h, and then the mixture F is obtained after impurity removal.
Further, in the step (5), the addition amount of the paraffin is 1 to 5wt% of the mixture F, preferably 1.5 to 3%; the ball milling time is 9 to 20 hours, preferably 9 to 12 hours; the number of the sieving meshes is 100 to 400 meshes, preferably 100 to 200 meshes.
Further, in the step (6), the temperature of vacuum sintering is 1400-1800 ℃, preferably 1600-1800 ℃; the time is 2 to 15 hours, preferably 5 to 10 hours.
The invention also provides the artificial tooth material prepared by the preparation method.
According to the invention, a precursor is prepared by adopting a sol-gel method, all raw materials are added and mixed on the surface of a sol layer, the preparation process is simple and controllable, the purity of each component can be effectively improved, the influence of impurities is reduced, the biocompatibility of the material is improved, the zirconium, yttrium, aluminum and silver can be mixed at an atomic scale, the mixing uniformity of each component is improved, and the generation of material defects is reduced; the density and strength of the artificial teeth are improved by further combining the cold isostatic pressing forming and vacuum sintering processes, and the defect of insufficient mechanical strength of the traditional material is effectively overcome; moreover, the addition of silver in the invention not only plays a role of a sintering aid in sintering to improve the strength of the material, but also has the functions of bacteriostasis and sterilization, thus obtaining the artificial tooth material which completely meets the use environment of the oral cavity and the daily occlusion of a user.
Compared with the existing ceramic powder mixing technology, the invention has the advantages that:
(1) The invention adopts the sol-gel method to prepare the precursor, and the addition and mixing of all the raw materials are placed on the sol layer, so that the preparation process is simple and controllable, the purity of each component can be effectively improved, the influence of impurities is reduced, the biocompatibility of the material is improved, the zirconium, the yttrium, the aluminum and the silver can be mixed at the atomic scale, the mixing uniformity of each component is improved, and the generation of material defects is reduced.
(2) The invention adopts the processes of cold isostatic pressing and vacuum sintering, improves the density and the strength of the artificial teeth, effectively solves the defect of insufficient mechanical strength of the traditional material, and can completely meet the daily occlusion of a user.
(3) The material for artificial teeth has stable property and acid and alkali corrosion resistance after high-temperature treatment, can completely meet the use environment of oral cavity, and cannot be discolored or deteriorated due to long-term use.
(4) The addition of silver in the invention not only plays a role of a sintering aid in sintering to improve the strength of the material, but also has the functions of bacteriostasis and sterilization to protect the oral health.
Detailed Description
The present invention will be described in further detail with reference to embodiments, including but not limited to.
The experimental procedures described in the examples are conventional unless otherwise specified, and reagents and materials used therefor are commercially available without otherwise specified.
Example 1
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 10 parts by mass of zirconium acetate, 10 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Selecting 5 parts by mass of simple substance aluminum, 5 parts by mass of aluminum nitrate, 5 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, mixing and stirring, and reacting at 80 ℃ to obtain sol C;
(4) The sol A, B and C were mixed at a mass ratio of 1 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
Example 2
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 20 parts by mass of zirconium acetate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Mixing and stirring 20 parts by mass of simple substance aluminum, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 60 parts by mass of water, and reacting at 80 ℃ to obtain sol C;
(4) Sol A, B and C were mixed in a mass ratio of 1.3 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 7 hours to obtain the artificial tooth material.
Example 3
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 20 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Mixing and stirring 15 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, and reacting at 80 ℃ to obtain sol C;
(4) Mixing sol A, B with C according to a certain ratio of 1.3 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
Example 4
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 10 parts by mass of zirconium acetate, 10 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Selecting 5 parts by mass of simple substance aluminum, 5 parts by mass of aluminum nitrate, 5 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, mixing and stirring, and reacting at 80 ℃ to obtain sol C;
(4) The sol A, B and C were mixed at a mass ratio of 1 2 :Y 2 O 3 :Al 2 O 3 Metering), and uniformly stirring to obtain a mixture D;
(5) Concentrating and drying the mixture D to obtain a mixture E, heating to 400 ℃ at the heating rate of 5 ℃/min, preserving heat for 2h, heating to 900 ℃ at the heating rate of 10 ℃/min, preserving heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
Comparative example 1
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 10 parts by mass of zirconium acetate, 10 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Selecting 5 parts by mass of simple substance aluminum, 5 parts by mass of aluminum nitrate, 5 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, mixing and stirring, and reacting at 80 ℃ to obtain sol C;
(4) The sol A, B and C were mixed at a mass ratio of 1 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then placing the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
Comparative example 2
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 10 parts by mass of zirconium acetate, 10 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Selecting 5 parts by mass of simple substance aluminum, 5 parts by mass of aluminum nitrate, 5 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, mixing and stirring, and reacting at 80 ℃ to obtain sol C;
(4) The sol A, B and C were mixed at a mass ratio of 1 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2wt% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
Comparative example 3
A preparation method of a material for artificial teeth comprises the following process steps:
(1) Mixing and stirring 10 parts by mass of zirconium acetate, 10 parts by mass of zirconium nitrate, 10 parts by mass of formic acid, 10 parts by mass of nitric acid and 60 parts by mass of water, and reacting at 70 ℃ to obtain sol A;
(2) Mixing and stirring 20 parts by mass of yttrium acetate, 10 parts by mass of nitric acid and 80 parts by mass of water, and reacting at 60 ℃ to obtain sol B;
(3) Selecting 5 parts by mass of simple substance aluminum, 5 parts by mass of aluminum nitrate, 5 parts by mass of basic aluminum acetate, 10 parts by mass of formic acid, 10 parts by mass of acetic acid and 65 parts by mass of water, mixing and stirring, and reacting at 80 ℃ to obtain sol C;
(4) The sol A, B and C were mixed at a mass ratio of 1 2 :Y 2 O 3 :Al 2 O 3 Calculated), then silver nitrate and silver chlorate (the mass ratio is 1:1) accounting for 2wt% of the sum of the sol A, B and the sol C are added, and a mixture D is obtained after uniform stirring;
(5) Concentrating and drying the mixture D to obtain a mixture E, then increasing the temperature to 400 ℃ at the heating rate of 5 ℃/min, preserving the heat for 2h, increasing the temperature to 900 ℃ at the heating rate of 10 ℃/min, preserving the heat for 2h, and removing impurities to obtain a mixture F;
(6) Adding paraffin accounting for 2% of the mixture F into the mixture F for ball milling, drying the mixture after ball milling for 10 hours, and sieving the mixture through a 200-mesh sieve to obtain powder G;
(7) And (3) carrying out cold isostatic pressing on the powder G, and then putting the powder G into a 1700 ℃ vacuum sintering furnace for sintering for 10 hours to obtain the artificial tooth material.
The artificial tooth materials obtained in examples 1 to 4 and comparative examples 1 to 3 were respectively subjected to tensile strength tests by the GBT 8489-2006 fine ceramic compressive strength test method, and the specific test results are shown in table 1:
TABLE 1 tensile Strength test results of the artificial tooth materials obtained in examples 1 to 4 and comparative examples 1 to 3
Claims (9)
1. A method for preparing a material for artificial teeth, comprising the steps of:
(1) Mixing and stirring a zirconium source, acid and water, and heating for reaction to obtain sol A;
(2) Mixing and stirring yttrium source, acid and water, and heating for reaction to obtain sol B;
(3) Mixing and stirring an aluminum source, acid and water, and heating for reaction to obtain sol C;
(4) Mixing the sol A, B with the sol C, adding a silver source, uniformly stirring to obtain a mixture D, concentrating and drying the mixture D to obtain a mixture E, and heating the mixture E to 700-900 ℃ to remove impurities to obtain a mixture F;
(5) Mixing the mixture F and paraffin wax, performing ball milling, drying and sieving to obtain powder G;
(6) And (3) carrying out cold isostatic pressing on the powder G, and then carrying out vacuum sintering to obtain the material for the artificial teeth.
2. The method according to claim 1, wherein in the step (1), the zirconium source is at least one selected from the group consisting of zirconium acetate, zirconium oxychloride and zirconium nitrate, the acid is at least one selected from the group consisting of formic acid, acetic acid, nitric acid and hydrochloric acid, and the mass ratio of the zirconium source to the acid to the water is 1:0.1 to 0.6: 30-50 ℃ and the heating reaction temperature is 60-90 ℃.
3. The method according to claim 1, wherein in the step (2), the yttrium source is yttrium acetate, the acid is at least one selected from formic acid, acetic acid, nitric acid and hydrochloric acid, and the mass ratio of the yttrium source, the acid and the water is 1:0.1 to 0.8:30 to 40 ℃, and the temperature of the heating reaction is 60 to 120 ℃.
4. The preparation method according to claim 1, wherein in the step (3), the aluminum source is at least one selected from elemental aluminum, aluminum nitrate and basic aluminum acetate, the acid is at least one selected from formic acid, acetic acid, propionic acid, nitric acid and hydrochloric acid, and the mass ratio of the aluminum source to the acid to the water is 1:0.2 to 1.2:20 to 40 percent, and the temperature of the heating reaction is 60 to 90 ℃.
5. The process according to claim 1, wherein in the step (4), zrO is used 2 ：Y 2 O 3 ：Al 2 O 3 In terms of mass ratio of sol A, B to C is 1:0.1 to 0.3:0.3 to 0.6; the silver source is at least one of silver nitrate, silver chlorate and silver perchlorate, and the adding amount of the silver source is 0.01 to 5 weight percent of the sum of the sol A, B and the C.
6. The preparation method according to claim 1, wherein in the step (4), the mixture E is heated to 300-500 ℃ at a heating rate of 5-10 ℃/min, and is kept at the temperature for 0.5-3 h, and then is heated to 700-900 ℃ at a heating rate of 10-20 ℃/min, and is kept at the temperature for 1-3 h, and then the mixture F is obtained after impurity removal.
7. The method according to claim 1, wherein in the step (5), the paraffin is added in an amount of 1 to 5wt% based on the mixture F; the ball milling time is 9-20 h; the number of the sieving meshes is 100-400 meshes.
8. The method according to claim 1, wherein in the step (6), the temperature of the vacuum sintering is 1400 to 1800 ℃; the time is 2 to 15 hours.
9. An artificial tooth material obtained by the production method according to any one of claims 1 to 8.
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