CN113087389A - Method for preparing lithium silicate glass or lithium silicate glass ceramic body with different light transmittances - Google Patents
Method for preparing lithium silicate glass or lithium silicate glass ceramic body with different light transmittances Download PDFInfo
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- CN113087389A CN113087389A CN202110348250.4A CN202110348250A CN113087389A CN 113087389 A CN113087389 A CN 113087389A CN 202110348250 A CN202110348250 A CN 202110348250A CN 113087389 A CN113087389 A CN 113087389A
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- lithium silicate
- glass
- silicate glass
- glass ceramic
- ceramic body
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- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910052912 lithium silicate Inorganic materials 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000005368 silicate glass Substances 0.000 title claims abstract description 31
- 239000006017 silicate glass-ceramic Substances 0.000 title claims abstract description 29
- 238000002834 transmittance Methods 0.000 title claims abstract description 22
- 239000011521 glass Substances 0.000 claims abstract description 166
- 238000005245 sintering Methods 0.000 claims abstract description 68
- 239000000843 powder Substances 0.000 claims abstract description 56
- 238000002156 mixing Methods 0.000 claims abstract description 54
- 238000002844 melting Methods 0.000 claims abstract description 41
- 230000008018 melting Effects 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 28
- 238000000227 grinding Methods 0.000 claims abstract description 27
- 238000003825 pressing Methods 0.000 claims abstract description 27
- 238000000462 isostatic pressing Methods 0.000 claims abstract description 19
- 239000003086 colorant Substances 0.000 claims abstract description 15
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 238000010791 quenching Methods 0.000 claims abstract description 5
- 230000000171 quenching effect Effects 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 238000000465 moulding Methods 0.000 claims description 50
- 239000000049 pigment Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 26
- 229910044991 metal oxide Inorganic materials 0.000 claims description 20
- 150000004706 metal oxides Chemical class 0.000 claims description 20
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000006121 base glass Substances 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 4
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 4
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 4
- 239000011029 spinel Substances 0.000 claims description 4
- 229910052596 spinel Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- GXTNDOSGOPRCEO-UHFFFAOYSA-N [Cr].[Fe].[Zn] Chemical compound [Cr].[Fe].[Zn] GXTNDOSGOPRCEO-UHFFFAOYSA-N 0.000 claims description 2
- NDUKHFILUDZSHZ-UHFFFAOYSA-N [Fe].[Zr] Chemical compound [Fe].[Zr] NDUKHFILUDZSHZ-UHFFFAOYSA-N 0.000 claims description 2
- USEGQPUGEPSVQL-UHFFFAOYSA-N [Pr].[Zr] Chemical compound [Pr].[Zr] USEGQPUGEPSVQL-UHFFFAOYSA-N 0.000 claims description 2
- 239000001058 brown pigment Substances 0.000 claims description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 2
- 239000005548 dental material Substances 0.000 claims description 2
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 2
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims description 2
- 239000001054 red pigment Substances 0.000 claims description 2
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims description 2
- ZIKATJAYWZUJPY-UHFFFAOYSA-N thulium (III) oxide Inorganic materials [O-2].[O-2].[O-2].[Tm+3].[Tm+3] ZIKATJAYWZUJPY-UHFFFAOYSA-N 0.000 claims description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910000604 Ferrochrome Inorganic materials 0.000 claims 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 38
- 239000003103 lithium disilicate glass Substances 0.000 abstract description 38
- 230000008569 process Effects 0.000 abstract description 7
- 230000008859 change Effects 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 100
- 229910052697 platinum Inorganic materials 0.000 description 50
- 239000002994 raw material Substances 0.000 description 50
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 24
- 238000001035 drying Methods 0.000 description 24
- 125000002467 phosphate group Chemical class [H]OP(=O)(O[H])O[*] 0.000 description 24
- 238000004321 preservation Methods 0.000 description 17
- 238000012545 processing Methods 0.000 description 16
- 238000002425 crystallisation Methods 0.000 description 10
- 230000008025 crystallization Effects 0.000 description 10
- 238000005266 casting Methods 0.000 description 8
- 238000011960 computer-aided design Methods 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010309 melting process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000013022 formulation composition Substances 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/02—Compositions for glass with special properties for coloured glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Ceramic Engineering (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a preparation method of lithium silicate glass or lithium silicate glass ceramic body with different light transmittances, belonging to the technical field of lithium silicate glass. The method comprises the following steps: weighing the basic glass components according to the formula, uniformly mixing, and melting at high temperature; water quenching the fully melted glass liquid into glass frit, and grinding the glass frit into glass powder with required granularity; uniformly mixing the obtained glass powder with a coloring agent and/or a fluorescent agent, and carrying out dry pressing or isostatic pressing; sintering the formed blank in a vacuum atmosphere, and obtaining lithium silicate glass or lithium silicate glass ceramic blanks with different light transmittances by adjusting the vacuum degree in the vacuum atmosphere. The method provided by the invention can realize the adjustment of the light transmittance of the lithium disilicate glass ceramic under the same formula by controlling the vacuum degree in the vacuum sintering process, and compared with the method for realizing the change of the light transmittance by adjusting the formula in the prior art, the method is simpler and has stronger operability.
Description
Technical Field
The invention belongs to the technical field of lithium silicate glass, and particularly relates to a preparation method of lithium silicate glass or lithium silicate glass ceramic body with different light transmittances.
Background
The lithium disilicate glass ceramic has good mechanical property and optical property, has the texture similar to that of natural teeth and better aesthetic effect compared with zirconia materials, and is widely applied to the field of dental restoration.
At present, lithium disilicate glass ceramics are mostly prepared by a melting method, all raw materials are put in a platinum crucible, melted at high temperature to form glass liquid, then poured into a mould for forming, and then crystallized to obtain a final CAD/CAM porcelain block or a hot-pressed cast porcelain block. However, in this way, the raw materials are easy to volatilize or have poor price variation control during the high-temperature melting process, which can cause the phenomena of poor color stability, non-uniform crystallization and the like.
Based on the method, the lithium disilicate glass ceramic can be prepared by adopting a sintering method, the glass frits obtained by melting, water quenching and water quenching of basic glass powder are ground to a certain granularity, the ground glass frits are uniformly mixed with a colorant and then are pressed into a required geometric shape in a mould, and the final lithium disilicate glass ceramic is obtained by vacuum sintering. By the method, volatilization of the additive in the high-temperature melting process can be effectively avoided, the color stability is good, and crystal precipitation is more uniform. However, in all of the above methods, the transparency is adjusted by controlling the crystallization process by the formulation composition, and the search process is complicated, and further improvement of the transparency cannot be achieved.
Disclosure of Invention
The invention provides a preparation method of lithium silicate glass or lithium silicate glass ceramic blank with different light transmittances, the method can adjust the light transmittance of lithium disilicate glass ceramic under the same formula by adjusting the vacuum degree in the vacuum sintering process, and compared with the prior art that the light transmittance is changed by adjusting the formula, the method is simpler and has stronger operability.
In order to achieve the purpose, the invention provides a preparation method of lithium silicate glass or lithium silicate glass ceramic body with different light transmittances, which realizes the adjustment of the transmittancy of the lithium silicate glass or lithium silicate glass ceramic body by adjusting the vacuum degree of the body during sintering in vacuum atmosphere.
Preferably, the smaller the degree of vacuum adjusted, the higher the light transmission of the resulting lithium silicate glass or lithium silicate glass ceramic body under the same lithium silicate glass or lithium silicate glass ceramic body formulation conditions.
Preferably, the smaller the adjusted degree of vacuum, the higher the light transmission of the obtained lithium silicate glass or lithium silicate glass ceramic body, specifically:
the vacuum degree is more than or equal to 50Pa and less than or equal to 850Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic blank is 53.1-60.3 percent;
the vacuum degree is more than 850Pa and less than or equal to 2500Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic blank is 41.4-47.7 percent;
the vacuum degree is more than 2500Pa and less than or equal to 3500Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic body is 31.9-40.6 percent.
Preferably, the blank is prepared by the following method:
weighing the basic glass components according to the formula, uniformly mixing, and melting at high temperature;
water quenching the fully melted glass liquid into glass frit, and grinding the glass frit into glass powder with required granularity;
and uniformly mixing the obtained glass powder with a coloring agent and/or a fluorescent agent, and carrying out dry pressing or isostatic pressing to obtain a molded blank.
Preferably, the melting temperature of the base glass is 1350-.
Preferably, the obtained glass powder has a particle size range D501-50 μm, preferably D502-20 μm. Preferably, the molding pressure is 10 to 300 MPa.
Preferably, the sintering temperature of the vacuum atmosphere sintering is 350-950 ℃, and the heat preservation time is 20-240 min.
Preferably, the base glass consists essentially of, in weight percent:
wherein the other component is selected from monovalent metal oxide Na2O, divalent metal oxides SrO, MgO, CaO, trivalent metal oxides B2O3、La2O3Tetravalent metal oxide TiO2Nb, an oxide of an invaluable metal2O5And hexavalent metal oxide WO3、MoO3At least one of (1).
Preferably, the base glass consists essentially of, in weight percent:
wherein the other component is selected from monovalent metal oxide Na2O, divalent metal oxides SrO, MgO, CaO, trivalent metal oxides B2O3、La2O3Tetravalent metal oxide TiO2Nb, an oxide of an invaluable metal2O5And hexavalent metal oxide WO3、MoO3At least one of (1).
Preferably, the dye also comprises 0 to 8.5 percent of colorant and/or fluorescent agent, preferably 1.5 to 4.5 percent by weight.
Preferably, the colorants and/or phosphors include transition metal oxides and rare earth colorants selected from the group consisting of Fe, zirconium-based colorants and spinel colorants2O3、V2O5、NiO、MnO、Cr2O3、Co2O3、CeO2、Pr2O3、Nd2O5、Er2O3、Tb4O7、Tm2O3、Sm2O3、Dy2O3、Bi2O3、Yb2O3At least one of zirconium pigment selected from at least one of zirconium iron red, zirconium praseodymium yellow and zirconium ash, and the spinel pigment selected from chromiumAt least one of iron red pigment and iron chromium zinc brown pigment.
The invention provides a lithium silicate glass or lithium silicate glass ceramic body prepared by the preparation method according to any one of the technical schemes.
The invention provides the use of the lithium silicate glass or lithium silicate glass ceramic body according to the above technical scheme as a dental material, preferably for the preparation of a dental restoration.
The invention provides a dental prosthesis which is prepared by adopting the lithium silicate glass or lithium silicate glass ceramic body in the technical scheme.
Preferably, the dental restoration is selected from the group of: crowns, abutments, inlays, onlays, veneers, facets, bridges and braces.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention provides a preparation method of lithium silicate glass or a lithium silicate glass ceramic body, which can adjust the light transmission of lithium disilicate glass ceramic under the same formula by controlling the vacuum degree in the vacuum sintering process, and has simpler method and stronger operability compared with the prior art that the light transmission needs to be changed by adjusting the formula. In addition, the mode can save the production and batching process, avoid cross contamination in the batching process, reduce the consumption of the platinum crucible and the maintenance cost, simultaneously avoid the volatilization of the pigment in the melting process and improve the color stability; further, the colorant and/or fluorescent component is added after the base glass frit is prepared, so that volatilization and price change during high-temperature melting can be avoided.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding under the molding pressure of 10MPa, then carrying out isostatic pressing molding under the pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 50Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 2
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding under the molding pressure of 10MPa, then carrying out isostatic pressing molding under the pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 800Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 3
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding under the molding pressure of 10MPa, then carrying out isostatic pressing molding under the pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 1200Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 4
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding under the molding pressure of 10MPa, then carrying out isostatic pressing molding under the pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 2000Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 5
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding at the molding pressure of 10MPa, performing isostatic pressing molding at the pressure of 300MPa, performing vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 2500Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 6
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding under the molding pressure of 15MPa, then carrying out isostatic pressing molding under the pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, the vacuum degree of 3000Pa and the heat preservation time of 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 7
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, and then carrying out dry pressing molding at the molding pressure of 300MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 950 ℃, keeping the vacuum degree of 3500Pa and keeping the temperature for 30min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Example 8
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. Drying the obtained glass frit, grinding into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder with a pigment, then carrying out dry pressing molding with the pressure of 200MPa, carrying out vacuum sintering on the molded blank at the sintering temperature of 850 ℃ and the vacuum degree of 50Pa for 120min to obtain the final lithium disilicate glass ceramic, processing by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment
Example 9
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 200MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃ and the vacuum degree of 850Pa for 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 10
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding under the pressure of 20MPa, performing isostatic pressing molding under the pressure of 200MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃, the vacuum degree of 1200Pa and the heat preservation time of 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 11
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding under the pressure of 20MPa, performing isostatic pressing molding under the pressure of 200MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃, the vacuum degree of 1600Pa, and the heat preservation time of 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 12
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding under the pressure of 20MPa, performing isostatic pressing molding under the pressure of 200MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃, the vacuum degree of 2000Pa and the heat preservation time of 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 13
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 200MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃ under the vacuum degree of 3000Pa for 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 14
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 250MPa, performing vacuum sintering on the molded blank at the sintering temperature of 850 ℃ under the vacuum degree of 3500Pa, and keeping the temperature for 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic by adopting a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization treatment.
Example 15
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 50Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 16
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 800Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 17
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 1200Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank, and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 18
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 2000Pa and the heat preservation time of 240min to obtain a blank, performing CAD/CAM processing on the blank, and sintering at the temperature of 910 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 19
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 2500Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank, and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 20
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 3000Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank, and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Example 21
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder and a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, performing vacuum sintering on the molded blank at the sintering temperature of 350 ℃, the vacuum degree of 3500Pa and the heat preservation time of 240min to obtain a blank, and performing CAD/CAM processing on the blank, and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Comparative example 1
The raw materials are weighed according to the formula 1, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1350 ℃ for 240min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 2 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding under the molding pressure of 25MPa, performing isostatic pressing molding under the pressure of 250MPa, sintering the molded blank in the air atmosphere at the sintering temperature of 950 ℃ for 20min to obtain the final lithium disilicate glass ceramic, and preparing the restoration by adopting a hot press casting process.
Comparative example 2
The raw materials are weighed according to formula 2, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1550 ℃, melting for 20min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 20 mu m, uniformly mixing the glass powder and a pigment, and then carrying out dry pressing molding under the pressure of 250MPa, sintering the molded blank in the air atmosphere at the sintering temperature of 850 ℃ for 120min to obtain the final lithium disilicate glass ceramic, and processing the final lithium disilicate glass ceramic in a CAD/CAM (computer aided design/computer aided manufacturing) mode without secondary crystallization.
Comparative example 3
The raw materials are weighed according to formula 3, and the raw materials can be selected from oxides, carbonate compounds, phosphate compounds and the like. And (3) fully and uniformly mixing, adding the mixture into a platinum crucible, putting the platinum crucible into a furnace for melting at 1450 ℃ for 120min, and pouring the melted glass liquid into cold water to obtain the glass frit. And drying the obtained glass frit, grinding the glass frit into glass powder with the granularity of 10 mu m, uniformly mixing the glass powder with a pigment, performing dry pressing molding under the pressure of 25MPa, performing isostatic pressing under the molding pressure of 180MPa, sintering the molded blank at the sintering temperature of 350 ℃ in the air atmosphere for 240min to obtain a blank, and performing CAD/CAM processing and sintering at the temperature of 900 ℃ for 5min to obtain the final lithium disilicate glass ceramic restoration.
Performance testing
The light transmission tests are carried out on the restorations obtained in the above examples 1-21, and the method specifically comprises the following steps: the light transmission of the material was measured using a spectrophotometer (Perkin Elmer Lambda 900) according to standard GBT2680-1994, and the results are shown in Table 1.
TABLE 1 results of light transmittance test of the restorations obtained in examples 1 to 21
Claims (16)
1. The preparation method of the lithium silicate glass or lithium silicate glass ceramic body with different light transmittances is characterized in that the light transmittance of the lithium silicate glass or lithium silicate glass ceramic body is adjusted by adjusting the vacuum degree of the body during sintering in a vacuum atmosphere.
2. The method according to claim 1, wherein the smaller the degree of vacuum to be adjusted, the higher the light transmittance of the resulting lithium silicate glass or lithium silicate glass ceramic body under the same formulation conditions of the lithium silicate glass or lithium silicate glass ceramic body.
3. The method according to claim 2, wherein the smaller the degree of vacuum is adjusted, the higher the light transmittance of the resulting lithium silicate glass or lithium silicate glass ceramic body is, specifically:
the vacuum degree is more than or equal to 50Pa and less than or equal to 850Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic blank is 53.1-60.3 percent;
the vacuum degree is more than 850Pa and less than or equal to 2500Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic blank is 41.4-47.7 percent;
the vacuum degree is more than 2500Pa and less than or equal to 3500Pa, and the light transmittance of the obtained lithium silicate glass or lithium silicate glass ceramic body is 31.9-40.6 percent.
4. A production method according to any one of claims 1 to 3, wherein the green body is produced by:
weighing the basic glass components according to the formula, uniformly mixing, and melting at high temperature;
water quenching the fully melted glass liquid into glass frit, and grinding the glass frit into glass powder with required granularity;
and uniformly mixing the obtained glass powder with a coloring agent and/or a fluorescent agent, and carrying out dry pressing or isostatic pressing to obtain a molded blank.
5. The method according to claim 4, wherein the melting temperature of the base glass is 1350 ℃ and 1550 ℃ and the melting time is 20-240 min.
6. The method according to claim 4, wherein the obtained glass frit has a particle size in the range of D501-50 μm, preferably D50＝2-20μm。
7. The method according to claim 4, wherein the molding pressure is 10 to 300 MPa.
8. The method as claimed in claim 4, wherein the sintering temperature of the vacuum atmosphere sintering is 350-950 ℃, and the holding time is 20-240 min.
9. The method of claim 4, wherein the base glass consists essentially of, in weight percent:
wherein the other component is selected from monovalent metal oxide Na2O, divalent metal oxides SrO, MgO, CaO, trivalent metal oxides B2O3、La2O3Tetravalent metal oxide TiO2Nb, an oxide of an invaluable metal2O5And hexavalent metal oxide WO3、MoO3At least one of (1).
10. The method of claim 9, wherein the base glass consists essentially of, in weight percent:
wherein the other component is selected from monovalent metal oxide Na2O, divalent metal oxides SrO, MgO, CaO, trivalent metal oxides B2O3、La2O3Tetravalent metal oxide TiO2Nb, an oxide of an invaluable metal2O5And hexavalent metal oxide WO3、MoO3At least one of (1).
11. The method of claim 9 or 10, further comprising 0-8.5% by weight of a colorant and/or a fluorescent agent, preferably 1.5-4.5%.
12. The method of claim 11, wherein the colorant and/or phosphor comprises a transition metal oxide and rare earth colorant selected from the group consisting of Fe, a zirconium-based colorant, and a spinel colorant2O3、V2O5、NiO、MnO、Cr2O3、Co2O3、CeO2、Pr2O3、Nd2O5、Er2O3、Tb4O7、Tm2O3、Sm2O3、Dy2O3、Bi2O3、Yb2O3The zirconium pigment is selected from at least one of zirconium iron red, zirconium praseodymium yellow and zirconium ash, and the spinel pigment is selected from at least one of ferrochrome red pigment and iron chromium zinc brown pigment.
13. A lithium silicate glass or lithium silicate glass ceramic body prepared by the preparation method according to any one of claims 1 to 12.
14. Use of a lithium silicate glass or lithium silicate glass ceramic body according to claim 13 as dental material, preferably for the preparation of dental restorations.
15. Dental restoration, characterized in that it is produced using a lithium silicate glass or lithium silicate glass ceramic body according to claim 13.
16. Dental restoration according to claim 15, wherein the dental restoration is selected from the group of: crowns, abutments, inlays, onlays, veneers, facets, bridges and braces.
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| CN114940584A (en) * | 2022-05-05 | 2022-08-26 | 山东国瓷功能材料股份有限公司 | Dental glass ceramic and preparation method and application thereof |
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