CN113816610A - Lithium silicate glass ceramic restoration and preparation method thereof - Google Patents
Lithium silicate glass ceramic restoration and preparation method thereof Download PDFInfo
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- CN113816610A CN113816610A CN202111183678.4A CN202111183678A CN113816610A CN 113816610 A CN113816610 A CN 113816610A CN 202111183678 A CN202111183678 A CN 202111183678A CN 113816610 A CN113816610 A CN 113816610A
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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 42
- 229910052912 lithium silicate Inorganic materials 0.000 title claims abstract description 42
- 239000006017 silicate glass-ceramic Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000003086 colorant Substances 0.000 claims abstract description 31
- 239000011858 nanopowder Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000011521 glass Substances 0.000 claims abstract description 13
- 239000006121 base glass Substances 0.000 claims abstract description 12
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 11
- 238000005245 sintering Methods 0.000 claims description 40
- 239000000919 ceramic Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 25
- 239000003103 lithium disilicate glass Substances 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005266 casting Methods 0.000 claims description 7
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 7
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 6
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims description 6
- 238000003825 pressing Methods 0.000 claims description 6
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 6
- 150000002910 rare earth metals Chemical class 0.000 claims description 6
- 239000011029 spinel Substances 0.000 claims description 6
- 229910052596 spinel Inorganic materials 0.000 claims description 6
- 229910052726 zirconium Inorganic materials 0.000 claims description 6
- 238000000462 isostatic pressing Methods 0.000 claims description 5
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims description 5
- KOPBYBDAPCDYFK-UHFFFAOYSA-N Cs2O Inorganic materials [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000604 Ferrochrome Inorganic materials 0.000 claims description 4
- AKUNKIJLSDQFLS-UHFFFAOYSA-M dicesium;hydroxide Chemical compound [OH-].[Cs+].[Cs+] AKUNKIJLSDQFLS-UHFFFAOYSA-M 0.000 claims description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-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
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 238000010791 quenching Methods 0.000 claims description 4
- 230000000171 quenching effect Effects 0.000 claims description 4
- 229910001953 rubidium(I) oxide Inorganic materials 0.000 claims description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 3
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims description 3
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims description 3
- 238000007731 hot pressing Methods 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 229910052573 porcelain Inorganic materials 0.000 claims description 3
- 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 3
- 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 3
- 230000007704 transition Effects 0.000 claims description 3
- 229910000314 transition metal oxide Inorganic materials 0.000 claims description 3
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 239000001054 red pigment Substances 0.000 claims description 2
- 150000003754 zirconium Chemical class 0.000 claims description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 abstract description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052593 corundum Inorganic materials 0.000 abstract description 2
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 abstract description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000009472 formulation Methods 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- WVMPCBWWBLZKPD-UHFFFAOYSA-N dilithium oxido-[oxido(oxo)silyl]oxy-oxosilane Chemical compound [Li+].[Li+].[O-][Si](=O)O[Si]([O-])=O WVMPCBWWBLZKPD-UHFFFAOYSA-N 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000004512 die casting Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011960 computer-aided design Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000011351 dental ceramic Substances 0.000 description 1
- 239000005548 dental material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007850 fluorescent dye Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 229910002077 partially stabilized zirconia Inorganic materials 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000001062 red colorant Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/70—Preparations for dentistry comprising inorganic additives
- A61K6/78—Pigments
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
- A61K6/833—Glass-ceramic composites
-
- 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
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Glass Compositions (AREA)
Abstract
The invention provides a lithium silicate glass ceramic restoration and a preparation method thereof, wherein the lithium silicate glass ceramic restoration comprises the following basic glass components in percentage by mass: SiO 22：50‑80wt％、Li2O：5‑25wt％、K2O：0.4‑10.5wt％、Al2O3：0.4‑6wt％、P2O5: 0.5 to 6 wt%, ZnO: 0.4-6 wt%, other components: 0 to 11 wt%; the glass ceramic prosthesis further comprises Y2O3ZrO of2The nano powder, the coloring agent and/or the fluorescent agent; based on the total mass of the base glass, contains Y2O3ZrO of2Nano powder: 0.5-8%, colorant and fluorescent agent: 0 to 9 percent. The lithium silicate glass ceramic restoration provided by the invention has high fracture toughness.
Description
Technical Field
The invention relates to the technical field of dental materials, in particular to a lithium silicate glass ceramic restoration and a preparation method thereof.
Background
Lithium disilicate glass ceramics are polycrystalline materials with a homogeneous distribution of crystalline and glassy phases. Therefore, glass ceramics, which have both the light transmittance of glass and the strength of ceramics, are widely used in the field of dental restoration, for example, glass ceramics are the first choice material for aesthetic restoration of anterior teeth. However, the brittleness of lithium silicate glass ceramics limits their applications.
At present, the main method for improving the toughness of the lithium disilicate glass ceramic is to prepare the lithium disilicate glass ceramic by a melting method, before melting, ZrO is added2The crystal and other raw materials are melted, clarified and cast together to obtain ZrO2Uniformly distributed in the base glass, ZrO during subsequent nucleation and crystallization heat treatment2The phases precipitating from the base glass acting to increase the toughness, the ZrO added in this way2On one hand, the glass easily reacts with raw materials such as silicon oxide in the glass at high temperature to lose the function of improving toughness, on the other hand, a monoclinic phase is finally formed, the toughness cannot be improved by utilizing phase change, and the toughening effect is not obvious.
Disclosure of Invention
The invention aims to provide a lithium silicate glass ceramic restoration and a preparation method thereof, so as to improve the toughness of the lithium silicate glass ceramic restoration. The specific technical scheme is as follows:
the invention provides a lithium silicate glass ceramic restoration, which comprises the following basic components in percentage by mass:
wherein the other component comprises Rb2O、Cs2O、MgO、BaO、In2O3、La2O3、GeO2、Nb2O5、WO3、MoO3At least one of;
the glass ceramic restoration further comprises Y2O3ZrO of2Nano-powder, colorant and/or fluorescent agent; based on the total mass of the base glass, the content of Y2O3ZrO of2The addition amount of the nano powder is 0.5-8 wt%; the addition amount of the coloring agent and/or fluorescent agent is 0-9 wt%.
In some embodiments of the invention, the Y-containing moiety2O3ZrO of2Y in the nanopowder2O3The content is 2-6 mol%;
the colorant and/or fluorescent agent comprises transition metal oxide, rare earth colorant, zirconium series colorant and spinel colorant.
In some embodiments of the invention, the Y-containing component is based on the total mass of the base glass2O3ZrO of2The addition amount of the nano powder is 1-6 wt%; the addition amount of the coloring agent and/or fluorescent agent is 1-5 wt%.
In some embodiments of the invention, the transition metal oxide and rare earth colorant comprise Fe2O3、V2O5、NiO、MnO、Cr2O3、Co2O3、CeO2、Pr2O3、Nd2O5、Er2O3、Tb4O7、Tm2O3、Sm2O3、Dy2O3、Bi2O3、Yb2O3At least one of zirconium pigment including at least one of zirconium iron red, zirconium praseodymium yellow and zirconium ash,the spinel pigment comprises at least one of a ferrochrome red pigment and an iron-chromium-zinc brown pigment.
In some embodiments of the invention, the lithium silicate glass ceramic restoration has a fracture toughness of 2.1 to 2.6 MPa-m1/2。
The second aspect of the invention provides a preparation method of a lithium silicate ceramic restoration, which comprises the following steps:
1) uniformly mixing the basic glass components, heating at 1200-1700 ℃ for 18-125min, and performing water quenching to obtain a frit;
2) grinding the frit to obtain frit powder with particle size of 1-50 μm, and mixing with Y-containing powder with particle size less than 100nm2O3ZrO of2Mixing the nano powder, a coloring agent and/or a fluorescent agent to obtain mixed powder;
3) carrying out dry pressing molding or isostatic pressing molding on the mixed powder at 20-260MPa to obtain a blank;
4) sintering the green body to obtain lithium silicate glass ceramic;
5) and processing the sintered block into the lithium disilicate glass ceramic restoration.
In some embodiments of the present invention, the sintering is performed under vacuum condition, the vacuum degree is 45-6000Pa, the sintering temperature is 340-; and hot-pressing and casting the pressed block to obtain the lithium disilicate glass ceramic restoration at the casting temperature of 870-.
In some embodiments of the invention, the sintering is performed under the following conditions: the sintering temperature is 350-750 ℃, and the sintering time is 15-150 min;
then, carrying out CAD/CAM processing on the porcelain block;
and sintering the processed ceramic block for the second time to obtain the lithium disilicate glass ceramic restoration, wherein the sintering temperature is 780-930 ℃, and the sintering time is 5-60 min.
The invention has the beneficial effects that: the lithium silicate glass ceramic restoration and the preparation method thereof provided by the invention regulate and control the Y content by regulating and controlling the variety and the content of each component in the base glass2O3ZrO of2Y in the nanopowder2O3The content in the basic glass can improve the fracture toughness of the lithium silicate glass ceramic restoration, so that the lithium silicate glass ceramic restoration has better application prospect. Of course, not all of the advantages described above need to be achieved at the same time in the practice of any one product or method of the invention.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention are within the scope of the present invention.
The invention provides a lithium silicate glass ceramic restoration, wherein the basic glass comprises the following components in percentage by mass:
in the present invention, the other component includes Rb2O、Cs2O、MgO、BaO、In2O3、La2O3、GeO2、Nb2O5、WO3、MoO3At least one of;
the glass ceramic restoration further comprises Y2O3ZrO of2Nano-powder, colorant and/or fluorescent agent; based on the total mass of the base glass, the content of Y2O3ZrO of2The adding amount of the nano powder is 0.5-8 wt%, preferably 1-6 wt%; the colorants and/or fluorescent agents are added in an amount of 0 to 9 wt.%, preferably 1 to 5 wt.%.
The inventors have found that by adding Y-containing compounds to the base glass2O3ZrO of2Nano powder for regulating Y content2O3ZrO of2Y in the nanopowder2O3The content of the base glass is within the range of the invention, and the fracture toughness of the lithium silicate glass ceramic restoration can be improved. Without being limited to any theory, the reason is probably that Y-TZP (yttria stabilized tetragonal zirconia) or Y-PSZ (yttria partially stabilized zirconia) is formed in the lithium silicate glass ceramic after the blank body is sintered, the Y-TZP or Y-PSZ is uniformly distributed in the lithium silicate glass ceramic to play a role in toughening the particles in a dispersion way, meanwhile, the Y-TZP has a phase change toughening role, and the two mechanisms comprehensively play a role in improving the toughness of the lithium silicate glass ceramic restoration body.
In some embodiments of the invention, Y is2O3ZrO of2Y in the nanopowder2O3In an amount of 2 to 6 mol%, i.e., in the above-mentioned Y-containing2O3ZrO of2In the nano-powder, the Y is2O3The content of the silicon dioxide is 2-6 mol%, and the fracture toughness of the lithium silicate glass ceramic restoration is improved.
In some embodiments of the invention, the colorants and/or fluorescers include transition group metal oxides and rare earth colorants, zirconium based colorants, spinel colorants.
In some embodiments of the invention, the lithium silicate glass ceramic restoration has a fracture toughness of 2.1 to 2.6 MPa-m1/2。
In the present invention, the kind of the lithium silicate glass ceramic is not particularly limited as long as the object of the present invention can be achieved, and a lithium disilicate glass ceramic or a lithium metasilicate ceramic is preferable.
In one embodiment of the present invention, the transition group metal oxides and rare earth colorants can include, but are not limited to, Fe2O3、V2O5、NiO、MnO、Cr2O3、Co2O3、CeO2、Pr2O3、Nd2O5、Er2O3、Tb4O7、Tm2O3、Sm2O3、Dy2O3、Bi2O3、Yb2O3Etc., the zirconium-based colorant may include, but is not limited to, at least one of zircoferrite red, zircopr yellow, zirco grey, etc., and the spinel colorant may include, but is not limited to, at least one of ferrochrome red colorant, ferrochrome zinc brown colorant, etc.
The invention also provides a preparation method of the lithium silicate glass ceramic restoration in any scheme, which comprises the following steps:
1) uniformly mixing the basic glass components, heating at 1200-1700 ℃ for 18-125min, and performing water quenching to obtain a frit;
2) grinding the frit to obtain frit powder with particle size of 1-50 μm, and mixing with Y-containing powder with particle size less than 100nm2O3ZrO of2Mixing the nano powder, a coloring agent and/or a fluorescent agent to obtain mixed powder;
3) carrying out dry pressing molding or isostatic pressing molding on the mixed powder at 20-260MPa to obtain a blank;
4) sintering the green body to obtain lithium silicate glass ceramic;
5) and processing the sintered block into the lithium disilicate glass ceramic restoration.
In some embodiments of the present invention, the sintering is performed under vacuum condition, the vacuum degree is 45-6000Pa, the sintering temperature is 340-; and hot-pressing and casting the pressed block to obtain the lithium disilicate glass ceramic restoration at the casting temperature of 870-.
In some embodiments of the invention, the sintering is performed under the following conditions:
the sintering temperature is 350-750 ℃, and the sintering time is 15-150 min;
then, the porcelain block is processed by CAD/CAM (computer aided design/computer aided manufacturing);
and sintering the processed ceramic block for the second time to obtain the lithium disilicate glass ceramic restoration, wherein the sintering temperature is 780-930 ℃, and the sintering time is 5-60 min.
The water quenching in the above step 1) means a process of pouring the melted base glass component into cold water. In the step 2), the grinding method is not particularly limited, as long as the object of the present invention is achieved, and for example, the frit is subjected to coarse grinding and then fine grinding. When the lithium silicate glass ceramic restoration is prepared, the obtained lithium silicate glass ceramic restoration has higher fracture toughness by adopting the components and the content of the components provided by the invention.
In the present invention, dry press molding is a process in which frit powders are put into a mold, and the powders are pressed by a press machine so as to be close to each other in the mold and firmly bonded by an internal friction force, thereby forming a green body having a predetermined shape. In the invention, the isostatic pressing is to place a sample to be pressed in a high-pressure container, and uniformly pressurize the sample from all directions by using a liquid medium to form a blank body with a certain shape. The press and the high-pressure vessel of the present invention are not particularly limited, and may be those known in the art as long as the object of the present invention is achieved.
The die casting process may include, but is not limited to, the following steps: firstly, preparing a wax pattern of the restoration, then embedding the wax pattern of the restoration by using an embedding material, solidifying to obtain an embedding ring, heating the embedding ring to melt and volatilize the wax pattern, then putting the wax pattern into a die-casting furnace, and then putting lithium silicate glass ceramic into the embedding ring to die-cast the lithium silicate glass ceramic to obtain the lithium silicate glass ceramic restoration. Wherein the die casting temperature is 870-. The embedding material of the present invention is not particularly limited as long as the object of the present invention can be achieved, and for example, the embedding material is phosphate.
The CAD technology is a technology that helps a designer design a tooth by using a computer and a graphic device thereof, for example, scanning a defective tooth, and then designing the defective part by using the CAD technology. CAM technology is a process or system that applies computers to manufacturing processes. For example, the lithium silicate glass ceramic is carved into a lithium silicate glass ceramic restoration according to the designed morphology of the CAD technology.
Example 1
According to the formula 1 in the table 1, the components are fully and uniformly mixed and then put into a platinum crucible, the platinum crucible is put into a heating furnace, the heating temperature is controlled to be 1200 ℃, and the heating time is 1And (5) pouring the melted glass liquid into cold water for 25min to obtain the frit. The frit was dried and ground to an average particle size of 1.5 μm to obtain frit powder. And fully and uniformly mixing the frit powder with the components in the formula a in the table 2, performing dry pressing molding under 20MPa, performing isostatic pressing molding under 260MPa to obtain a blank, and performing vacuum sintering on the blank at the vacuum degree of 45MPa, the sintering temperature of 955 ℃ and the sintering time of 2min to obtain the glass ceramic containing the lithium disilicate crystal nucleus. Then the lithium disilicate glass ceramic is made into the lithium disilicate glass ceramic restoration by a hot-press casting process. Wherein, Y-ZrO2Middle Y2O3The content was 2 mol%.
Example 2
Except for Y-ZrO2Middle Y2O3The procedure of example 1 was repeated except that the content was 3 mol%.
Example 3
Except for Y-ZrO2Middle Y2O3The procedure of example 1 was repeated except that the content was 4 mol%.
Example 4
Except for Y-ZrO2Middle Y2O3The procedure of example 1 was repeated except that the content was 5 mol%.
Example 5
Except for Y-ZrO2Middle Y2O3The procedure of example 1 was repeated except that the content was 6 mol%.
Example 6
According to the formula 2 in the table 1, the components are fully and uniformly mixed and then placed into a platinum crucible, the platinum crucible is placed into a heating furnace, the heating temperature is controlled to be 1700 ℃, the heating time is 18min, and the melted glass liquid is poured into cold water to obtain the frit. The frit was dried and ground to an average particle size of 22 μm to obtain frit powder. Mixing the frit powder with the components in the formula b shown in the table 2, performing dry pressing under 260MPa to obtain a blank, sintering the blank at 350 ℃ for 15min to obtain glass ceramic containing lithium disilicate crystal nuclei, and performing secondary sintering on the ceramic block obtained by CAD/CAM processing to obtain the lithium disilicate glassThe sintering temperature of the glass ceramic restoration is 780 ℃ and the sintering time is 5 min. Wherein, Y-ZrO2Middle Y2O3The content was 2 mol%.
Example 7
Except for Y-ZrO2Middle Y2O3The procedure of example 6 was repeated except that the content was 3 mol%.
Example 8
Except for Y-ZrO2Middle Y2O3The procedure of example 6 was repeated except that the content was 4 mol%.
Example 9
Except for Y-ZrO2Middle Y2O3The procedure of example 6 was repeated except that the content was 5 mol%.
Example 10
Except for Y-ZrO2Middle Y2O3The procedure of example 6 was repeated except that the content was 6 mol%.
Example 11
According to the formula 3 in the table 1, the components are fully and uniformly mixed and then placed into a platinum crucible, the platinum crucible is placed into a heating furnace, the heating temperature is controlled at 1550 ℃, the heating time is 70min, and the melted glass liquid is poured into cold water to obtain the frit. The frit was dried and ground to an average particle size of 12 μm to obtain frit powder. And fully and uniformly mixing the frit powder with the components in the formula c in the table 2, carrying out dry pressing molding under 140MPa to obtain a blank, sintering the blank at the sintering temperature of 550 ℃ for 80min to obtain the glass ceramic containing lithium disilicate crystal nuclei, and carrying out secondary sintering on the ceramic block prepared by CAD/CAM processing to obtain the lithium disilicate glass ceramic restoration, wherein the sintering temperature is 850 ℃ and the sintering time is 30 min. Wherein, Y-ZrO2Middle Y2O3The content was 2 mol%.
Example 12
Except for Y-ZrO2Middle Y2O3The procedure of example 11 was repeated except that the content was 3 mol%.
Example 13
Except for Y-ZrO2Middle Y2O3The procedure of example 11 was repeated except that the content was 4 mol%.
Example 14
Except for Y-ZrO2Middle Y2O3The procedure of example 11 was repeated except that the content was 5 mol%.
Example 15
Except for Y-ZrO2Middle Y2O3The procedure of example 11 was repeated except that the content was 6 mol%.
Comparative example 1
Except for Y-ZrO2Does not contain Y2O3I.e. Y2O3The procedure of example 1 was repeated except that the content was 0 mol%.
Comparative example 2
Except for Y-ZrO2Does not contain Y2O3I.e. Y2O3The procedure of example 6 was repeated except that the content was 0 mol%.
Comparative example 3
Except for Y-ZrO2Does not contain Y2O3I.e. Y2O3The procedure of example 11 was repeated except that the content was 0 mol%.
TABLE 1
| Composition (I) | Formulation 1 | Formulation 2 | Formulation 3 |
| SiO2 | 80 | 50 | 60 |
| Li2O | 5 | 25 | 10 |
| K2O | 10.5 | 0.5 | 5 |
| Al2O3 | 0.5 | 5 | 3 |
| P2O5 | 1 | 5 | 10 |
| ZnO | 3 | 3.5 | 6 |
| Rb2O | - | - | 1.5 |
| Cs2O | - | 1.5 | - |
| MgO | - | 2 | - |
| BaO | - | - | 1 |
| In2O3 | - | 1 | 0.5 |
| La2O3 | - | 2 | - |
| GeO2 | - | 1.5 | 1.5 |
| Nb2O5 | - | 1.5 | 1 |
| MoO3 | - | - | 0.5 |
| WO3 | - | 1.5 | - |
Note: the contents of the respective substances in table 1 are mass percentages, "-" indicates that no corresponding substance is present in the formulation.
TABLE 2
Note: Y-ZrO in Table 22Is represented by containing Y2O3ZrO of2The content of each substance of the nano powder is mass percent, and the < - > indicates that no corresponding substance exists in the formula.
The test method and the test equipment are as follows:
and (3) testing fracture toughness:
according to the national standard GB30367-2013 unilateral V-groove beam method (SEVNB) of the dental ceramic material, a universal material testing machine (TH-8201S) is adopted to measure the fracture toughness of the glass ceramic restoration with the unit of MPa.m1/2。
The relevant parameter and property pairs for the lithium disilicate glass ceramic restorations in the examples and comparative examples are shown in table 3:
TABLE 3
As can be seen from the data in table 3, the fracture toughness of examples 1 to 5 is higher than that of comparative example 1, the fracture toughness of examples 6 to 10 is higher than that of comparative example 2, and the fracture toughness of examples 11 to 15 is higher than that of comparative example 3. It can be seen that the fracture toughness of the lithium disilicate glass ceramic restoration follows Y-ZrO2Y in the nanopowder2O3Change of the contentAlternatively, when the same formulation is used to prepare the lithium disilicate glass ceramic, Y is added2O3And the content of the lithium disilicate glass ceramic restoration is controlled, so that the fracture toughness of the lithium disilicate glass ceramic restoration can be improved.
As can be seen from examples 1 to 15 and comparative examples 1 to 3, Y-ZrO in the formulation for preparing a lithium disilicate glass ceramic restoration2Y in the nanopowder2O3The content of (A) is within the range of the invention, and the lithium disilicate glass ceramic restoration with high fracture toughness can be obtained.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (8)
1. A lithium silicate glass ceramic restoration comprises the following components in percentage by mass in basic glass:
wherein the other component comprises Rb2O、Cs2O、MgO、BaO、In2O3、La2O3、GeO2、Nb2O5、WO3、MoO3At least one of;
the glass ceramic restoration further comprises Y2O3ZrO of2Nano-powder, colorant and/or fluorescent agent; based on the total mass of the base glass, the content of Y2O3ZrO of2The adding amount of the nano powder is 0.5-8 wt%; the addition amount of the coloring agent and/or fluorescent agent is 0-9 wt%.
2. The lithium silicate glass ceramic restoration of claim 1, wherein the Y-containing is2O3ZrO of2Y in the nanopowder2O3The content is 2-6mol％；
The colorant and/or fluorescent agent comprises transition metal oxide, rare earth colorant, zirconium series colorant and spinel colorant.
3. The lithium silicate glass ceramic restoration of claim 1, wherein the Y content is based on the total mass of the base glass2O3ZrO of2The addition amount of the nano powder is 1-6 wt%; the addition amount of the coloring agent and/or fluorescent agent is 1-5 wt%.
4. The lithium silicate glass ceramic restoration of claim 2, wherein the transition group metal oxide and rare earth colorant comprise Fe2O3、V2O5、NiO、MnO、Cr2O3、Co2O3、CeO2、Pr2O3、Nd2O5、Er2O3、Tb4O7、Tm2O3、Sm2O3、Dy2O3、Bi2O3、Yb2O3The zirconium system pigment comprises at least one of zirconium iron red, zirconium praseodymium yellow and zirconium ash, and the spinel pigment comprises at least one of ferrochrome red pigment and iron chromium zinc brown pigment.
5. The lithium silicate glass ceramic restoration of any one of claims 1-4, wherein the lithium silicate glass ceramic restoration has a fracture toughness of 2.1-2.6 MPa-m1/2。
6. A method of producing a lithium silicate glass ceramic restoration according to any one of claims 1 to 5, comprising the steps of:
1) uniformly mixing the basic glass components, heating at 1200-1700 ℃ for 18-125min, and performing water quenching to obtain a frit;
2) grinding the frit to obtain frit powder with particle size of 1-50 μm, and mixing with the powder with particle size of less than 100nmY2O3ZrO of2Mixing the nano powder, a coloring agent and/or a fluorescent agent to obtain mixed powder;
3) carrying out dry pressing molding or isostatic pressing molding on the mixed powder at 20-260MPa to obtain a blank;
4) sintering the green body to obtain lithium silicate glass ceramic;
5) and processing the sintered block into the lithium disilicate glass ceramic restoration.
7. The preparation method according to claim 6, wherein the sintering is performed under vacuum condition, the vacuum degree is 45-6000Pa, the sintering temperature is 340-955 ℃, and the sintering time is 20-125min, so as to obtain the pressed block; and hot-pressing and casting the pressed block to obtain the lithium disilicate glass ceramic restoration at the casting temperature of 870-.
8. The production method according to claim 6, wherein the sintering is performed under the following conditions: the sintering temperature is 350-750 ℃, and the sintering time is 15-150 min;
then, carrying out CAD/CAM processing on the porcelain block;
and sintering the processed ceramic block for the second time to obtain the lithium disilicate glass ceramic restoration, wherein the sintering temperature is 780-930 ℃, and the sintering time is 5-60 min.
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| CN114477774A (en) * | 2022-03-01 | 2022-05-13 | 山东国瓷功能材料股份有限公司 | Lithium disilicate glass ceramic with color gradient effect and preparation method thereof |
| WO2023061045A1 (en) * | 2021-10-11 | 2023-04-20 | 深圳爱尔创口腔技术有限公司 | Lithium silicate glass-ceramic prosthesis and preparation method therefor |
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| CN110981204B (en) * | 2019-12-27 | 2022-09-02 | 深圳爱尔创口腔技术有限公司 | Fluorescent lithium silicate glass material and preparation method and application thereof |
| CN113816610A (en) * | 2021-10-11 | 2021-12-21 | 深圳爱尔创口腔技术有限公司 | Lithium silicate glass ceramic restoration and preparation method thereof |
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| WO2023061045A1 (en) * | 2021-10-11 | 2023-04-20 | 深圳爱尔创口腔技术有限公司 | Lithium silicate glass-ceramic prosthesis and preparation method therefor |
| CN114028240A (en) * | 2021-12-24 | 2022-02-11 | 深圳爱尔创口腔技术有限公司 | Lithium disilicate glass ceramic restoration and preparation method thereof |
| CN114477774A (en) * | 2022-03-01 | 2022-05-13 | 山东国瓷功能材料股份有限公司 | Lithium disilicate glass ceramic with color gradient effect and preparation method thereof |
| CN114477774B (en) * | 2022-03-01 | 2023-10-31 | 山东国瓷功能材料股份有限公司 | Lithium disilicate glass ceramic with color gradient effect and preparation method thereof |
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