Lithium disilicate glass ceramic restoration and preparation method thereof

Abstract

The invention provides a lithium disilicate glass ceramic restoration and a preparation method thereof. The lithium disilicate glass ceramic restoration is prepared from the following raw material components in percentage by mass: 50 to 74 weight percent of SiO2, 9 to 20 weight percent of Li2O, 0.1 to 10 weight percent of ZrO2, 2 to 15 weight percent of Al2O3, 0 to 8.5 weight percent of ZnO, 0.5 to 10 weight percent of MgO, 0.1 to 10 weight percent of P2O5, 0.1 to 10 weight percent of fluxing agent, 0 to 5 weight percent of coloring agent, 0.5 to 4.9 weight percent of fluorescent agent and 0 to 10 weight percent of other additives. According to the lithium disilicate glass ceramic restoration provided by the invention, precipitation of sub-crystalline phases is controlled by regulating and controlling the content of Al2O3, Li2O, MgO and other components, so that the sub-crystalline phases SiO2, Li2SiO3, Li3PO4 and AlPO4 are converted to the crystalline phases of aluminosilicate and aluminate such as LiAlSi3O8, Li0. 6Al0. 6Si2. 4O6, LiXAlXSi3-XO6, MgAl2Si3O10 and the like, the composition of the sub-crystalline phases is improved, the influence of miscellaneous sub-crystalline phases on the mechanical properties of the material is reduced, and the performance of the lithium disilicate glass ceramic restoration is improved. Further, the mechanical property of the lithium disilicate glass ceramic restoration is improved.

Description

Technical Field

[0001] The present application relates to the technical field of dental materials, and in particular to a lithium disilicate glass ceramic restoration and a preparation method thereof. Background Art

[0002] Lithium disilicate glass ceramics are a polycrystalline composite material composed of a crystal phase and a glass matrix. 2 Si 2 O 5 As the main crystal phase, lithium disilicate glass ceramics are widely used in the field of denture restoration because of its semi-transparent characteristics and excellent mechanical properties, as well as outstanding aesthetic properties and excellent biocompatibility.

[0003] At present, the secondary crystalline phase precipitated in the preparation process of lithium disilicate glass ceramics cannot be completely eliminated, and the secondary crystalline phase is mostly lithium metaphosphate (LiPO 3 ), some products also have more lithium orthophosphate (Li 3 PO 4 ) and other residual crystal phases, and the content of these residual crystal phases often affects the mechanical properties of the material. When the content of lithium orthophosphate and lithium metaphosphate is high, compared with the fully transformed lithium disilicate glass ceramics, the strength and hardness of the lithium disilicate glass ceramics containing the secondary crystalline phases are reduced, the fracture toughness is reduced, and the mechanical properties are significantly reduced. The strength of the dental restoration using this material needs to be improved. Summary of the invention

[0004] The purpose of this application is to provide a lithium disilicate glass ceramic restoration and a preparation method thereof, so as to improve the mechanical properties of the lithium disilicate glass ceramic restoration. The specific technical solution is as follows:

[0005] The first aspect of the present application provides a lithium disilicate glass ceramic restoration, which comprises the following raw material components in percentage by mass:

[0006] SiO 2 50-74wt%

[0007] Li 2 O 9-20wt%

[0008] ZrO 2 0.1-10wt%

[0009] Al 2 O 3 2-15wt%

[0010] ZnO 0-8.5wt%

[0011] MgO 0.5-10wt%

[0012] P 2 O 5 0.1-10wt%

[0013] Flux 0.1-10wt%

[0014] Colorant 0-5wt%

[0015] Fluorescent agent 0.5-4.9wt%

[0016] Other additives 0-10wt%

[0017] in,

[0018] The flux is selected from Rb 2 O、Cs 2 O.K 2 O and Na 2 At least one of O;

[0019] The other additives are selected from B 2 O 3 、CaO、BaO、SrO、Y 2 O 3 ,La 2 O 3 At least one of .

[0020] In some embodiments of the first aspect of the present application, the lithium disilicate glass ceramic restoration comprises the following raw material components in percentage by weight:

[0021] SiO 2 55-72wt%

[0022] Li 2 O 9-17wt%

[0023] ZrO 2 0.3-6.5wt%

[0024] Al 2 O 3 2.5-10wt%

[0025] ZnO 0-6wt%

[0026] MgO 0.5-8wt%

[0027] P 2 O 5 1-7wt%

[0028] Flux 2-8wt%

[0029] Colorant 0.3-4.2wt%

[0030] Fluorescent agent 0.6-4.9wt%

[0031] Other additives 0-10wt%.

[0032] In some embodiments of the first aspect of the present application, the colorant is selected from V 2 O 5 , Er 2 O 3 、CeO 2 Cr 2 O 3 、MnO 2 , NiO; the fluorescent agent is selected from Tb 4 O 7 、Nd 2 O 3 , Pr 6 O 11 、Sm 2 O 3 、Dy 2 O 3 、Tm 2 O 3 、Eu 2 O 3 At least one of .

[0033] The second aspect of the present application provides a method for preparing the lithium disilicate glass ceramic restoration provided in the first aspect of the present application, which comprises the following steps:

[0034] 1) The raw material components are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a frit;

[0035] 2) heating the frit at 1350-1650° C. for 50-120 min to melt into molten glass;

[0036] 3) pouring the glass liquid into a mold for casting to obtain a glass block;

[0037] 4) subjecting the glass block to a first crystallization heat treatment, and obtaining a restoration blank through molding, and then subjecting the restoration blank to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

[0038] In some embodiments of the second aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 500-900°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C.

[0039] In some embodiments of the second aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 600-850°C, and the heat treatment temperature of the second crystallization heat treatment is 800-950°C.

[0040] In some embodiments of the second aspect of the present application, the molding process is computer-aided design (CAD) or computer-aided manufacturing (CAM) molding process.

[0041] The third aspect of the present application provides another method for preparing the lithium disilicate glass ceramic restoration provided in the first aspect of the present application, which comprises the following steps:

[0042] 1) mixing the raw material components uniformly, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain a glass powder with an average particle size of 1-30 μm;

[0043] Alternatively, the raw material components except the colorant are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a glass frit, which is ground to obtain a powder with an average particle size of 1-30 μm, and the colorant is mixed with the powder to obtain a glass powder;

[0044] 2) placing the glass powder into a mold, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body;

[0045] 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain a lithium disilicate glass ceramic restoration.

[0046] In some embodiments of the third aspect of the present application, the preparation method comprises:

[0047] 1) using at least two raw material components of different colors and / or transparencies, respectively mixing the different raw material components, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, then quenching with water to form glass frit, grinding to obtain at least two glass powders of different colors and / or transparencies with an average particle size of 1-30 μm;

[0048] Or, using at least two raw material components of different colors and / or transparencies, respectively, mixing the different raw material components except the colorant, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain different powders with an average particle size of 1-30 μm, and then respectively mixing the colorant with the powder to obtain at least two glass powders of different colors and / or transparencies;

[0049] 2) placing the at least two glass powders of different colors and / or transparencies into a mold layer by layer, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body;

[0050] 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

[0051] In some embodiments of the third aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 500-750°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C.

[0052] In some embodiments of the third aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 500-700°C, and the heat treatment temperature of the second crystallization heat treatment is 830-950°C.

[0053] In some embodiments of the third aspect of the present application, the molding process is CAD or CAM molding process.

[0054] The present application provides a lithium disilicate glass ceramic restoration and a preparation method thereof, without changing the precipitation state of the main crystalline phase lithium disilicate, by regulating the Al 2 O 3 , Li 2 The content of O and MgO and other components is used to control the precipitation of the secondary crystalline phase, so that the secondary crystalline phase Li 3 PO 4 、SiO 2 、AlPO 4 , Li 2 SiO 3 Towards LiAlSi 3 O 8 , Li 0.6 Al 0.6 Si 2.4 O 6 , Li X Al X Si 3-X O 6 (0.5≤x≤1) and MgAl 2 Si 3 O 10 The transformation of aluminosilicate and aluminate crystal phases improves the composition of the secondary crystal phase, thereby reducing the influence of the residual secondary crystal phase on the mechanical properties of the material, and further improving the mechanical properties of lithium disilicate glass-ceramic restorations.

[0055] Of course, implementing any product or method of the present application does not necessarily require achieving all of the advantages described above at the same time. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] In order to more clearly illustrate the technical solutions in the present application or the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application, and for ordinary technicians in this field, other embodiments can also be obtained based on these drawings.

[0057] Figure 1 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 1;

[0058] Figure 2 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 2;

[0059] Figure 3 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 3;

[0060] Figure 4 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 8;

[0061] Figure 5 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 9;

[0062] Figure 6 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 10;

[0063] Figure 7 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 17;

[0064] Figure 8 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 18;

[0065] Fig. 9 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 20;

[0066] Fig.10 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 24;

[0067] Fig.11 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Example 26;

[0068] Fig.12 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Comparative Example 1;

[0069] Fig.13 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Comparative Example 2;

[0070] Fig.14 This is the XRD pattern of the lithium disilicate glass ceramic restoration of Comparative Example 4;

[0071] Fig.15 This is the XRD diagram of the lithium disilicate glass ceramic restoration of comparative example 5. DETAILED DESCRIPTION

[0072] The following will be combined with the drawings in the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. All other embodiments obtained by ordinary technicians in this field based on the present application belong to the scope of protection of this application.

[0073] In a first aspect, the present application provides a lithium disilicate glass ceramic restoration, which comprises the following raw material components in percentage by mass:

[0074] SiO 2 50-74wt%

[0075] Li 2 O 9-20wt%

[0076] ZrO 2 0.1-10wt%

[0077] Al 2 O 3 2-15wt%

[0078] ZnO 0-8.5wt%

[0079] MgO 0.5-10wt%

[0080] P 2 O 5 0.1-10wt%

[0081] Flux 0.1-10wt%

[0082] Colorant 0-5wt%

[0083] Fluorescent agent 0.5-4.9wt%

[0084] Other additives 0-10wt%

[0085] in,

[0086] The flux is selected from Rb 2 O、Cs 2 O.K 2 O and Na 2 At least one of O;

[0087] Other additives selected from B 2 O 3 、CaO、BaO、SrO、Y 2 O 3 ,La 2 O 3 At least one of .

[0088] The present application provides a lithium disilicate glass ceramic restoration, which does not change the precipitation state of the main crystalline phase lithium disilicate by regulating the Al 2 O 3 , Li 2 The content of O and MgO and other components is used to control the precipitation of the secondary crystalline phase, so that the secondary crystalline phase Li 3 PO 4 、SiO 2 、AlPO 4 , Li 2 SiO 3 Towards LiAlSi 3 O 8 , Li 0.6 Al 0.6 Si 2.4 O 6 , Li X Al X Si 3-X O 6 (0.5≤x≤1) and MgAl 2 Si 3 O 10 Aluminosilicate and aluminate phase transformation. 2 Si 2 O 5 Incompletely converted Li is often present in glass-ceramics. 2 SiO 3 Secondary crystalline phase, this application adjusts Al 2 O 3 , Li 2 The contents of O and MgO are within the above ranges, so that Mg and Al are enriched at the grain boundaries or directly participate in the nucleation and crystallization of the secondary crystalline phase. 2 O 3 Easy to use with SiO 2 Formation of [AlSiO 4 ] - Network skeleton, which has a quartz-type topological structure and is easy to build a structural network with the glass phase; small-charge cation Li + Mg 2+It is easy to compensate into the framework, and at the same time has a structural tendency to occupy the gaps between the framework ligands, thereby forming relatively energy-stable aluminum silicate or aluminate fine crystals and accumulating at the grain boundaries of the main phase. These fine crystals are not only beneficial to improving the density of microcrystalline glass, but also play a role in dispersion strengthening, so that the dislocations generated by the microcrystalline glass under external force cause accumulation at the grain boundaries or the energy is lost when the dislocation slip process cuts through the second phase, so that the extension of cracks in the microcrystalline glass is stagnant or delayed, thereby achieving the improvement of the bending strength and other mechanical properties of lithium disilicate glass-ceramic restorations, improving the composition of the secondary crystal phase, reducing the influence of the residual secondary crystal phase on the mechanical properties of the material, and improving the mechanical properties of lithium disilicate glass-ceramic restorations.

[0089] Preferably, the lithium disilicate glass ceramic restoration comprises the following raw material components in percentage by mass:

[0090] SiO 2 55-72wt%

[0091] Li 2 O 9-17wt%

[0092] ZrO 2 0.3-6.5wt%

[0093] Al 2 O 3 2.5-10wt%

[0094] ZnO 0-6wt%

[0095] MgO 0.5-8wt%

[0096] P 2 O 5 1-7wt%

[0097] Flux 2-8wt%

[0098] Colorant 0.3-4.2wt%

[0099] Fluorescent agent 0.6-4.9wt%

[0100] Other additives 0-10wt%.

[0101] The lithium disilicate glass ceramic restoration provided by the present application, when the mass percentage of the raw material components is within the above range, the type of the precipitated secondary crystalline phase is controlled without changing the precipitation state of the main crystalline phase lithium disilicate, for example, the secondary crystalline phase Li 3 PO 4 、SiO 2 、AlPO 4 , Li 2 SiO 3Towards LiAlSi 3 O 8 , Li 0.6 Al 0.6 Si 2.4 O 6 , Li X Al X Si 3-X O 6 MgAl 2 Si 3 O 10 The isomorphous phase transformation improves the composition of the secondary crystalline phase, thereby reducing the influence of the residual secondary crystalline phase on the mechanical properties of the material. The obtained lithium disilicate glass-ceramic restoration has better mechanical properties, while also having excellent aesthetic properties and good biocompatibility.

[0102] The present application has no particular restrictions on the types of colorants and fluorescent agents, as long as the purpose of the present application can be achieved. For example, the colorant may include but is not limited to V 2 O 5 , Er 2 O 3 、CeO 2 Cr 2 O 3 、MnO 2 , NiO; the fluorescent agent may include but is not limited to Tb 4 O 7 、Nd 2 O 3 , Pr 6 O 11 、Sm 2 O 3 、Dy 2 O 3 、Tm 2 O 3 、Eu 2 O 3 At least one of .

[0103] In the present application, the raw material components used may be oxides, carbonates, phosphates or nitrates of various components, etc. This is a conventional technology in the art and the present application has no particular limitation on this, as long as the purpose of the present application can be achieved.

[0104] The second aspect of the present application provides a method for preparing the lithium disilicate glass ceramic restoration provided in the first aspect of the present application, which comprises the following steps:

[0105] 1) The raw material components are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a frit;

[0106] 2) heating the frit at 1350-1650°C for 50-120 min to melt it into molten glass;

[0107] 3) pouring the glass liquid into a mold for casting to obtain a glass block;

[0108] 4) subjecting the glass block to a first crystallization heat treatment, and obtaining a restoration blank through molding, and then subjecting the restoration blank to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

[0109] The water quenching in the above step 1) refers to the process of pouring the molten glass into cold water, and the fluorescent agent is directly mixed with other raw material components. 2 During the melting and heat treatment of MgO or alkaline earth metal, the metal ions of the fluorescent agent are doped in the alkali metal Li 2 O or alkaline earth metal MgO orthophosphate secondary crystal phase, thereby improving the mechanical properties of lithium disilicate glass ceramic restorations, while having excellent aesthetic properties and meeting the requirements of excellent biocompatibility. In the above step 1), the raw material components are melted at the above temperature to form matrix glass, and then poured into water and quickly cooled to form a glass frit. In the above step 3), the present application has no special restrictions on the mold, as long as the purpose of the present application can be achieved, for example, the mold is a casting mold.

[0110] In some embodiments of the second aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 500-900°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C, and the obtained lithium disilicate glass-ceramics has good mechanical properties; preferably, the heat treatment temperature of the first crystallization heat treatment is 600-850°C, and the heat treatment temperature of the second crystallization heat treatment is 800-950°C.

[0111] In some embodiments of the second aspect of the present application, the molding process is CAD or CAM molding process.

[0112] The third aspect of the present application provides another method for preparing the lithium disilicate glass ceramic restoration provided in the first aspect of the present application, which comprises the following steps:

[0113] 1) mixing the raw material components uniformly, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain a glass powder with an average particle size of 1-30 μm;

[0114] Alternatively, the raw material components except the colorant are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a glass frit, which is ground to obtain a powder with an average particle size of 1-30 μm, and the colorant is mixed with the powder to obtain a glass powder;

[0115] 2) placing the glass powder into a mold, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body;

[0116] 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

[0117] In some embodiments of the third aspect of the present application, the preparation method comprises:

[0118] 1) using at least two raw material components of different colors and / or transparencies, respectively mixing the different raw material components, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, then quenching with water to form glass frit, grinding to obtain at least two glass powders of different colors and / or transparencies with an average particle size of 1-30 μm;

[0119] Or, using at least two raw material components of different colors and / or transparencies, respectively, mixing the different raw material components except the colorant, heating at 1350-1650°C for 30-120min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain different powders with an average particle size of 1-30μm, and then mixing the colorant with the powder respectively to obtain at least two glass powders of different colors and / or transparencies; the content of the colorant is such that the weight gain of the glass powder does not exceed 4wt%;

[0120] 2) placing the at least two glass powders of different colors and / or transparencies into a mold layer by layer, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body;

[0121] 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

[0122] Under this process, a fluorescent lithium disilicate glass-ceramic restoration with N layers of color and / or transparency can be prepared, N≥2, preferably, N≥3; in step 2), a mixed glass powder of one color and / or transparency is added to a dry pressing mold, and after being scraped flat, a mixed glass powder of another color and / or transparency is added, until all the mixed glass powders of N colors and / or transparencies are added to the mold, and dry pressing is performed at a pressure of 20-30Mpa, and then isostatic pressing is performed at 100-240MPa to obtain a preformed body with multiple layers of color and / or transparency. By regulating the glass powders of different colors and / or transparencies and loading them into the mold in sequence according to the gradual change of color and / or transparency, the lithium disilicate glass-ceramic restoration can achieve the effect of gradually lighter color and gradually higher transparency from the neck to the cutting end.

[0123] The water quenching in the above step 1) refers to the process of pouring the molten glass into cold water, and the fluorescent agent is directly mixed with other raw material components. 2 During the melting and heat treatment of MgO or alkaline earth metal, the metal ions of the fluorescent agent are doped in the alkali metal Li 2 O or alkaline earth metal MgO orthophosphate secondary crystal phase, thereby improving the mechanical properties of lithium disilicate glass ceramic restorations, while having excellent aesthetic properties and meeting the requirements of excellent biocompatibility. The present application has no particular limitation on the grinding method, as long as the purpose of the present application can be achieved, for example, the glass frit is first coarsely ground and then finely ground.

[0124] In some embodiments of the third aspect of the present application, the colorants and powders are mixed separately, which may be different colorants are mixed with different powders respectively, or different powders are mixed in required proportions to obtain different mixed powders. The present application has no particular limitation on mixing different colorants with different mixed powders respectively, as long as the purpose of the present application can be achieved.

[0125] In some embodiments of the third aspect of the present application, the heat treatment temperature of the first crystallization heat treatment is 500-750°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C, and the obtained lithium disilicate glass-ceramics has good mechanical properties; preferably, the heat treatment temperature of the first crystallization heat treatment is 500-700°C, and the heat treatment temperature of the second crystallization heat treatment is 830-950°C.

[0126] In some embodiments of the third aspect of the present application, the molding process is CAD or CAM molding process.

[0127] In the present application, the lithium disilicate glass ceramic restoration is subjected to secondary heat treatment to improve the crystallinity of the lithium disilicate glass ceramic restoration, and by regulating Al2 O 3 , Li 2 The content of O and MgO and other components is used to control the precipitation of the secondary crystalline phase, so that the secondary crystalline phase Li 3 PO 4 , Li 2 SiO 3 Towards LiAlSi 4 O 10 、LiAlSiO 4 、LiAlSi 2 O 6 , Li 2 Al 2 Si 3 O 10 、ZnAl 2 O 4 MgAl 2 Si 4 O 12 The isomorphous phase transformation improves the composition of the secondary crystalline phase and enhances the mechanical properties of lithium disilicate glass-ceramic restorations.

[0128] In the present application, the dry pressing molding refers to loading glass powder into a mold, applying pressure on a press, so that the glass powders are close to each other in the mold, and firmly combined with the help of internal friction to form a blank of a certain shape. In the present application, the isostatic pressing molding refers to placing the sample to be pressed in a high-pressure container, using a liquid medium to uniformly pressurize the sample from all directions to form a blank of a certain shape. This application has no special restrictions on presses and high-pressure containers, as long as the purpose of this application can be achieved, for example, they can be commercially available presses and high-pressure containers.

[0129] In some embodiments of the present application, the molding processing technology may be CAD or CAM molding processing technology.

[0130] In this application, CAD molding technology refers to the use of computers and their graphics equipment to help designers perform design work, for example, scanning a defective tooth and then using CAD technology to design the defective part after scanning. CAM molding technology is a process or system that applies computers to the manufacturing process. For example, lithium disilicate glass ceramics are carved into the desired lithium disilicate glass ceramic restoration according to the morphology designed by CAD technology.

[0131] Example

[0132] The following examples and comparative examples are given to more specifically describe the embodiments of the present application. Various tests and evaluations were performed according to the following methods. In addition, unless otherwise specified, "parts" and "%" are based on mass.

[0133] Test methods and equipment

[0134] Biaxial bending strength test:

[0135] According to the content of Chapter 7 of the national standard GB 30367-2013 / ISO 6872:2015 "Dental Ceramic Materials", the biaxial bending strength is determined by the biaxial bending ball-on-ring method. The formula is:

[0136]

[0137] Wherein, bending strength σ: maximum central tensile stress, in megapascals (MPa); P: total load at fracture, in Newtons (N); b: thickness of the specimen at fracture, in millimeters (mm); v: Poisson's ratio (if the Poisson's ratio of the ceramic is unknown, v = 0.25); r 1 : The radius of the support ring, in millimeters (mm); r 2 : The radius of the load zone (precision round pin), in millimeters (mm); r 3 :

[0138] The radius of the specimen, in millimeters (mm).

[0139] X-ray diffraction (XRD) test:

[0140] The D8 Advance X-ray diffractometer produced by Bruker, Germany, was used to analyze the crystal phase of lithium disilicate glass-ceramic restorations with a scanning speed of 2°·min -1 , the scanning range 2θ is 10-80° and the radiation source is CuKα (λ=0.15406nm).

[0141] Example 1

[0142] 1) According to the raw material composition in Table 1, the raw material components are mixed evenly and put into a platinum crucible, and the platinum crucible is placed in a heating furnace, and the heating temperature is controlled to be 1350° C. and the heating time is 60 min, so that the components are melted and homogenized into glass liquid (the heating temperature and time are referred to as the first heating temperature and the first heating time in Table 3), and then poured into cold water for quenching to form a molten block;

[0143] 2) After being dried in a drying oven, the frit is put into a heating furnace again, and the heating temperature is controlled to be 1350° C. and the heating time is 120 min to melt it into glass liquid (the heating temperature and time are referred to as the second heating temperature and the second heating time in Table 3);

[0144] 3) pouring the molten glass into a mold for casting to obtain a glass block;

[0145] 4) subjecting the glass block to a first crystallization heat treatment at 630° C. in a box furnace to obtain a ceramic block whose main crystal phase is lithium metasilicate; then, the ceramic block is designed using CAD technology, and then processed using a Sirona processing machine to obtain a restoration blank, and then the restoration blank is subjected to a second crystallization heat treatment at 820° C. to obtain a lithium disilicate glass-ceramic restoration.

[0146] Example 2-Example 15

[0147] Except for adjusting the raw material components according to Table 1 and adjusting the preparation process parameters according to Table 3, the rest is the same as Example 1.

[0148] Example 16

[0149] 1) According to the raw material composition in Table 2, all raw material components except the colorant were mixed evenly and put into a platinum crucible, and the platinum crucible was placed in a heating furnace, and the heating temperature was controlled to be 1550° C. and the heating time was 50 min to melt all the components and homogenize them into glass liquid, and then poured into cold water for quenching to form a glass frit;

[0150] 2) drying the frit in a drying oven, and then coarsely grinding and finely grinding the frit to obtain a powder with an average particle size D50 of 5 μm;

[0151] 3) The colorant and the powder are fully mixed to obtain glass powder, which is then placed in a mold at room temperature, dry pressed at a pressure of 20 MPa, and then isostatically pressed at a pressure of 100 MPa to obtain a green body;

[0152] 4) The green body is subjected to the first crystallization heat treatment at 700°C in a box furnace, and then designed using CAD technology, and then processed using a Sirona processing machine to obtain a restoration body, and then the restoration body is subjected to the second crystallization heat treatment at 950°C in a vacuum atmosphere furnace with a vacuum degree of 3000Pa and heat treatment for 10 minutes to obtain a lithium disilicate glass-ceramic restoration.

[0153] Example 17-Example 27

[0154] Except for adjusting the raw material components according to Table 2 and adjusting the preparation process parameters according to Table 4, the rest is the same as Example 16.

[0155] Embodiment 28

[0156] 1) According to the raw material composition in Table 5, the raw material components of the base material a and the base material b except the colorant are mixed uniformly and put into a platinum crucible, and the platinum crucible is placed in a heating furnace, and the heating temperature is controlled to be 1550° C. and the heating time is 50 min, so that the components are melted and homogenized into glass liquid, and then poured into cold water for quenching to form a glass frit; the glass frit is dried in a drying oven and then coarsely ground and finely ground to obtain basic glass powders a and b with an average particle size D50 of 5 μm;

[0157] 2) According to the formula in Table 6, the basic glass powders a and b are mixed with the colorant to form 1#-5# glass powders, the color of 1#-5# glass powders gradually deepens and the transparency gradually decreases, the evenly mixed 1# glass powder is added to the dry pressing mold, and after being scraped flat, the evenly mixed 2# glass powder is added, and the operation is repeated until the evenly mixed 5# glass powder is all added to the mold, dry pressing is performed at a pressure of 20MPa, and then isostatic pressing is performed at a pressure of 100MPa to obtain a green body with 5 layers of color and transparency;

[0158] 3) The green body is subjected to the first crystallization heat treatment at 650°C in a box furnace, and then designed using CAD technology, and then processed using a Sirona processing machine to obtain a restoration body, and then the restoration body is subjected to the second crystallization heat treatment at 900°C in a vacuum atmosphere furnace with a vacuum degree of 3000Pa and a heat treatment time of 0.5h to obtain a lithium disilicate glass-ceramic restoration.

[0159] Example 29-Example 31

[0160] Except for adjusting the raw material components except the colorant according to Table 7 / Table 9 / Table 11, and adjusting the composition of the basic glass powder a, b and the colorant according to Table 8 / Table 10 / Table 12, the rest is the same as Example 28.

[0161] Embodiment 32

[0162] 1) According to the raw material composition in Table 13, the raw material components of base material a, base material b, and base material c were mixed evenly and put into a platinum crucible, and the platinum crucible was placed in a heating furnace, and the heating temperature was controlled to be 1550° C. and the heating time was 50 min to melt the components and homogenize them into glass liquid, and then poured into cold water for quenching to form a glass frit; the glass frit was dried in a drying oven and then coarsely ground and finely ground to obtain glass powders a, b, and c with an average particle size D50 of 5 μm;

[0163] 2) adding glass powder a into a dry pressing mold, adding glass powder b after flattening, repeating the operation until all glass powder c is added into the mold, performing dry pressing molding at a pressure of 20 MPa, and then performing isostatic pressing molding at a pressure of 100 MPa to obtain a green body;

[0164] 3) The green body is subjected to the first crystallization heat treatment at 650°C in a box furnace, and then designed using CAD technology, and then processed using a Sirona processing machine to obtain a restoration body, and then the restoration body is subjected to the second crystallization heat treatment at 900°C in a vacuum atmosphere furnace with a vacuum degree of 3000Pa and a heat treatment time of 0.5h to obtain a lithium disilicate glass-ceramic restoration.

[0165] Embodiment 33

[0166] Except for adjusting the raw material components according to Table 14, the rest is the same as Example 32.

[0167] Comparative Example 1-Comparative Example 3

[0168] Except for adjusting the raw material components according to Table 1 and adjusting the preparation process parameters according to Table 3, the rest is the same as Example 1.

[0169] Comparative Example 4-Comparative Example 5

[0170] Except for adjusting the raw material components according to Table 2 and adjusting the preparation process parameters according to Table 4, the rest is the same as Example 16.

[0171] Comparative Example 6

[0172] Except for adjusting the raw material components of base materials a and b according to Table 15, and adjusting the composition of base glass powders a, b and colorants according to Table 16, the rest is the same as Example 28.

[0173] Comparative Example 7

[0174] Except for adjusting the raw material components of base materials a, b, and c according to Table 15, the rest is the same as Example 32.

[0175]

[0176]

[0177] Table 5

[0178] Example 28 Components Base material a Basic material b <![CDATA[SiO 2 > 68 70 <![CDATA[Li 2 The]]> 9.5 14.9 <![CDATA[ZrO 2 ]]> 2.2 0.3 <![CDATA[Al 2 THE 3 ]]> 4.8 4.0 ZnO 0.9 0.8 MgO 4.5 2.0 <![CDATA[P 2 O 5 > 1.5 3.3 <![CDATA[Cs 2 The]]> 2.6 0.5 <![CDATA[K 2 O]]> 4.5 3.0 <![CDATA[Eu 2 THE 3 ]]> 0.7 0.6 <![CDATA[Tb 4 THE 7 ]]> 0.8 0.6

[0179] Table 6

[0180] Part Number Example 28 Ingredients 1# <![CDATA[(80% base glass powder a + 20% base glass powder b) + 0.08% Er 2 O 3 + 0.06% V 2 O 5 + 0.05% CeO 2 > 2# <![CDATA[(70% base glass powder a + 30% base glass powder b) + 0.05% Er 2 O 3 + 0.08% V 2 O 5 + 0.12% CeO 2 > 3# <![CDATA[(50% base glass powder a + 50% base glass powder b) + 0.12% Er 2 O 3 + 0.15% V 2 O 5 + 0.30% CeO 2 > 4# <![CDATA[(30% base glass powder a + 70% base glass powder b) + 0.3% Er 2 O 3 + 0.35% V 2 O 5 + 0.50% CeO 2 > 5# <![CDATA[(10% basic glass powder a + 90% basic glass powder b) + 0.4% Er 2 O 3 + 0.50% V 2 O 5 + 0.90% CeO 2 >

[0181] Table 7

[0182] Example 29 Components Base material a Basic material b <![CDATA[SiO 2 ]]> 61.5 65 <![CDATA[Li 2 The]]> 10 15 <![CDATA[ZrO 2 ]]> 3.5 0.6 <![CDATA[Al 2 THE 3 ]]> 4.5 3.5 ZnO 4.6 1.3 MgO 2.4 2 <![CDATA[P 2 THE 5 ]]> 4.2 5.8 <![CDATA[Cs 2 The]]> 2.6 1.1 <![CDATA[K 2 The]]> 5.3 4.3 <![CDATA[Eu 2 THE 3 ]]> 0.4 0.6 <![CDATA[Tb 4 THE 7 ]]> 1 0.8

[0183] Table 8

[0184] Part Number Example 29 Ingredients 1# <![CDATA[(80% base glass powder a + 20% base glass powder b) + 0.03% Er 2 O 3 + 0.05% V 2 O 5 + 0.06% CeO 2 > 2# <![CDATA[(70% base glass powder a + 30% base glass powder b) + 0.06% Er 2 O 3 + 0.08% V 2 O 5 + 0.15% CeO 2 > 3# <![CDATA[(50% base glass powder a + 50% base glass powder b) + 0.10% Er 2 O 3 + 0.15% V 2 O 5 + 0.30% CeO 2 > 4# <![CDATA[(30% base glass powder a + 70% base glass powder b) + 0.25% Er 2 O 3 + 0.25% V 2 O 5 + 0.60% CeO 2 > 5# <![CDATA[(10% base glass powder a + 90% base glass powder b) + 0.5% Er 2 O 3 + 0.6% V 2 O 5 + 1.0% CeO 2 >

[0185] Table 9

[0186] Example 30 Components Base material a Basic material b <![CDATA[SiO 2 ]]> 71 60 <![CDATA[Li 2 The]]> 12 11 <![CDATA[ZrO 2 ]]> 1.1 1 <![CDATA[Al 2 THE 3 ]]> 9.4 10 ZnO 0.5 5 MgO 0.5 3.5 <![CDATA[P 2 THE 5 ]]> 0.5 3.2 <![CDATA[Cs 2 The]]> 1.2 2.1 <![CDATA[K 2 The]]> 2.5 3 <![CDATA[Eu 2 THE 3 ]]> 0.4 0.5 <![CDATA[Tb 4 THE 7 ]]> 0.9 0.7

[0187] Table 10

[0188] Part Number Example 30 Ingredients 1# <![CDATA[(80% base glass powder a + 20% base glass powder b) + 0.3% Er 2 O 3 + 0.2% V 2 O 5 > 2# <![CDATA[(70% base glass powder a + 30% base glass powder b) + 0.6% Er 2 O 3 + 0.4% V 2 O 5 > 3# <![CDATA[(60% base glass powder a + 40% base glass powder b) + 0.9% Er 2 O 3 + 0.8% V 2 O 5 > 4# <![CDATA[(30% base glass powder a + 70% base glass powder b) + 1.0% Er 2 O 3 + 1.1% V 2 O 5 + 0.8% CeO 2 > 5# <![CDATA[(15% base glass powder a + 85% base glass powder b) + 1.2% Er 2 O 3 + 1.0% V 2 O 5 + 1.0% CeO 2 >

[0189] Table 11

[0190] Example 31 Components Base material a Basic material b <![CDATA[SiO 2 > 55 65 <![CDATA[Li 2 The]]> 10 14 <![CDATA[ZrO 2 ]]> 6.5 2 <![CDATA[Al 2 THE 3 ]]> 8.9 7.5 ZnO 6 1.5 MgO 1 2.5 <![CDATA[P 2 THE 5 ]]> 1 1.8 <![CDATA[Cs 2 The]]> 3 2.4 <![CDATA[K 2 The]]> 2.5 1 <![CDATA[Eu 2 THE 3 ]]> 1 0.8 <![CDATA[Tb 4 THE 7 ]]> 1.6 1.5 <![CDATA[B 2 THE 3 ]]> 3.5 -

[0191] Table 12

[0192] Part Number Example 31 Ingredients 1# <![CDATA[(75% base glass powder a + 25% base glass powder b) + 0.1% Er 2 O 3 + 0.1% V 2 O 5 > 2# <![CDATA[(65% base glass powder a + 35% base glass powder b) + 0.3% Er 2 O 3 + 0.2% V 2 O 5 > 3# <![CDATA[(50% base glass powder a + 50% base glass powder b) + 0.5% Er 2 O 3 + 0.7% V 2 O 5 + 0.2% CeO 2 > 4# <![CDATA[(30% base glass powder a + 70% base glass powder b) + 0.8% Er 2 O 3 + 1.1% V 2 O 5 + 0.8% CeO 2 <!-- 13 -->]]> 5# <![CDATA[(15% base glass powder a + 85% base glass powder b) + 1.2% Er 2 O 3 + 1.0% V 2 O 5 + 1.0% CeO 2 >

[0193] Table 13

[0194] Example 32 Components Base material a Basic material b Base material c <![CDATA[SiO 2 ]]> 68.5 66 60 <![CDATA[Li 2 The]]> 12.5 15 14.5 <![CDATA[ZrO 2 ]]> 1.5 2.5 0.5 <![CDATA[Al 2 THE 3 ]]> 5.8 5.5 4.6 ZnO 1.1 1.6 1.8 MgO 1.1 1.2 2.6 <![CDATA[P 2 THE 5 ]]> 2 1.5 3.1 <![CDATA[Cs 2 The]]> 0.5 0.5 1.4 <![CDATA[K 2 The]]> 3.4 0.5 5.3 <![CDATA[V 2 THE 5 ]]> - 0.5 0.7 <![CDATA[Er 2 THE 3 ]]> - 0.5 0.5 <![CDATA[CeO 2 ]]> - 1.5 1.9 <![CDATA[Tm 2 THE 3 ]]> - 0.5 0.5 <![CDATA[Eu 2 THE 3 ]]> 0.5 - 0.5 <![CDATA[Tb 4 THE 7 ]]> 0.9 0.8 0.8 <![CDATA[B 2 THE 3 ]]> 1.4 1.4 0.8 CaO 0.8 0.5 0.5

[0195] Table 14

[0196] Example 33 Components Base material a Basic material b Base material c <![CDATA[SiO 2 ]]> 72 65 58 <![CDATA[Li 2 The]]> 9.1 11.5 13 <![CDATA[ZrO 2 ]]> 1.5 1.9 0.8 <![CDATA[Al 2 THE 3 ]]> 5 6 8.5 ZnO 1.5 2.5 1.6 MgO 3.1 1.6 2.5 <![CDATA[P 2 THE 5 ]]> 1.1 1.9 4.5 <![CDATA[Cs 2 The]]> 2.8 2.1 1.3 <![CDATA[K 2 The]]> 2.2 2.6 2.1 <![CDATA[V 2 THE 5 ]]> - 0.6 0.7 <![CDATA[Er 2 THE 3 ]]> - 0.5 0.5 <![CDATA[CeO 2 ]]> 0.2 0.8 1.9 <![CDATA[Tm 2 THE 3 ]]> - 0.9 0.6 <![CDATA[Eu 2 THE 3 ]]> 0.6 0.6 0.5 <![CDATA[Tb 4 THE 7 ]]> 0.9 1.5 1.8 <![CDATA[B 2 THE 3 ]]> - - 1.2 CaO - - 0.5

[0197] Table 15

[0198]

[0199]

[0200] Table 16

[0201] Part Number Comparative Example 6 Ingredients 1# <![CDATA[(75% base glass powder a + 25% base glass powder b) + 0.1% Er 2 O 3 + 0.1% V 2 O 5 > 2# <![CDATA[(65% base glass powder a + 35% base glass powder b) + 0.3% Er 2 O 3 + 0.2% V 2 O 5 > 3# <![CDATA[(50% base glass powder a + 50% base glass powder b) + 0.5% Er 2 O 3 + 0.7% V 2 O 5 + 0.2% CeO 2 > 4# <![CDATA[(30% base glass powder a + 70% base glass powder b) + 0.8% Er 2 O 3 + 1.1% V 2 O 5 + 0.8% CeO 2 > 5# <![CDATA[(15% base glass powder a + 85% base glass powder b) + 1.2% Er 2 O 3 + 1.0% V 2 O 5 + 1.0% CeO 2 >

[0202] Note: The content of each substance in Table 5-Table 16 is the mass percentage, and “-” means that the corresponding substance does not exist in the raw materials.

[0203] The biaxial bending strength results of the lithium disilicate glass ceramic restorations in Examples 1-15 and Comparative Examples 1-3 are shown in Table 17.

[0204] Table 17

[0205] Example Biaxial bending strength (MPa) Example 1 425 Example 2 438 Example 3 448 Example 4 456 Example 5 417 Example 6 457 Example 7 429 Example 8 426 Example 9 397 Example 10 418 Embodiment 11 426 Example 12 434 Example 13 407 Embodiment 14 403 Embodiment 15 420 Comparative Example 1 287 Comparative Example 2 300 Comparative Example 3 293

[0206] The biaxial bending strength results of the lithium disilicate glass ceramic restorations in Examples 16-27 and Comparative Examples 4-5 are shown in Table 18.

[0207] Table 18

[0208] Example Biaxial bending strength (MPa) Example 16 326 Embodiment 17 322 Embodiment 18 319 Embodiment 19 341 Embodiment 20 322 Embodiment 21 357 Embodiment 22 324 Embodiment 23 327 Embodiment 24 320 Embodiment 25 338 Embodiment 26 312 Embodiment 27 315 Comparative Example 4 280 Comparative Example 5 274

[0209] The biaxial bending strength results of the lithium disilicate glass-ceramic restorations in Examples 28-33 and Comparative Examples 6-7 are shown in Table 19.

[0210] Table 19

[0211] Example Biaxial bending strength (MPa) Embodiment 28 323 Embodiment 29 315 Embodiment 30 307 Embodiment 31 319 Embodiment 32 310 Embodiment 33 326 Comparative Example 6 240 Comparative Example 7 276

[0212] Referring to Table 17, it can be seen from Examples 1 to 15 and Comparative Examples 1 to 3 that when the lithium disilicate glass-ceramic restoration is prepared by the melting method, the biaxial bending strength of the lithium disilicate glass-ceramic restoration using the composition and content of the present application is significantly higher, indicating that the lithium disilicate glass-ceramic restoration of the present application has more excellent mechanical properties.

[0213] Referring to Table 18, it can be seen from Examples 16 to 27 and Comparative Examples 4 to 5 that when the lithium disilicate glass-ceramic restoration is prepared by the sintering method, the biaxial bending strength of the lithium disilicate glass-ceramic restoration using the composition and content of the present application is significantly higher, indicating that the lithium disilicate glass-ceramic restoration of the present application has more excellent mechanical properties.

[0214] Referring to Table 19, it can be seen from Examples 28 to 33 and Comparative Examples 6 to 7 that when the lithium disilicate glass-ceramic restoration is prepared by the sintering method, the biaxial bending strength of the lithium disilicate glass-ceramic restoration using the composition and content of the present application is significantly higher, indicating that the lithium disilicate glass-ceramic restoration of the present application has more excellent mechanical properties; among them, the lithium disilicate glass-ceramic restorations obtained in Examples 28 to 33 all have a fluorescent effect and have excellent aesthetic properties.

[0215] The XRD patterns of the lithium disilicate glass ceramic restorations of Examples 1, 2, 3, 8, 9, 10, 17, 18, 20, 24, and 26 are shown in Figures 1 and 2. Figure 1-Figure 11 As shown, the XRD patterns of the lithium disilicate glass ceramic restorations of Comparative Examples 1, 2, 4, and 5 are shown as follows: Figure 12-Figure 15 As shown in the figure, the horizontal axis is the diffraction angle 2θ (°), and the vertical axis is the intensity (Intensity (au)). Figure 1 and Fig.12 It can be seen that the main crystal phase of the lithium disilicate glass ceramic restoration of Example 1 of the present application is Li 2 Si 2 O 5 , the secondary crystalline phase is Li X Al X Si 3-X O 6 The main crystalline phase of the lithium disilicate glass ceramic restoration of Comparative Example 1 is Li 2 Si 2 O 5 , while the secondary crystalline phase is Li 3 PO 4 、SiO 2 、AlPO 4 .from Figure 2 and Fig.14 It can be seen that the main crystal phase of the lithium disilicate glass ceramic restoration of Example 2 of the present application is Li 2 Si 2 O 5 , the secondary phase is MgAl 2 Si 3 O 10 The main crystalline phase of the lithium disilicate glass ceramic restoration of Comparative Example 4 is Li 2 Si 2 O 5 , the secondary crystalline phase is Li 3 PO 4 , Li 2 SiO 3 .according to Figure 1-Figure 15 It can be seen that the lithium disilicate glass ceramic restoration of the present application does not change the main crystal phase of lithium disilicate Li 2 Si 2 O 5 Based on the precipitation state, by regulating the Al 2 O 3 , Li 2 The content of O and MgO and other components is used to control the precipitation of the secondary crystalline phase, so that the secondary crystalline phase Li 3 PO 4 、SiO 2 、AlPO 4 , Li 2 SiO 3 Towards LiAlSi 3 O 8 , Li 0.6 Al 0.6 Si 2.4 O 6 , Li X Al X Si 3-X O 6 MgAl 2 Si 3 O 10 The invention can control the precipitation of the secondary crystalline phase, thereby improving the composition of the secondary crystalline phase and reducing the influence of the secondary crystalline phase.

[0216] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a method or article including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such a method or article.

[0217] Each embodiment in this specification is described in a related manner, and the same or similar parts between the embodiments can be referenced to each other, and each embodiment focuses on the differences from other embodiments.

[0218] The above description is only a preferred embodiment of the present application and is not intended to limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application are included in the protection scope of the present application.

Claims

1. A lithium disilicate glass ceramic restoration comprising the following raw material components in percentage by mass: SiO2 50-74wt% Li2O 9-20wt% ZrO2 0.1-10wt% Al2O3 2-15wt% ZnO 0-8.5wt% MgO 0.5-10wt% P2O5 0.1-10wt% Flux 0.1-10wt% Colorant 0-5wt% Fluorescent agent 0.5-4.9wt% Other additives 0-10wt% in, The flux is selected from at least one of Rb2O, Cs2O, K2O and Na2O; The other additives are selected from at least one of B2O3, CaO, BaO, SrO, Y2O3, and La2O3.

2. The lithium disilicate glass-ceramic restoration according to claim 1, wherein: The lithium disilicate glass ceramic restoration comprises the following raw material components in percentage by mass: SiO2 55-72wt% Li2O 9-17wt% ZrO2 0.3-6.5wt% Al2O3 2.5-10wt% ZnO 0-6wt% MgO 0.5-8wt% P2O5 1-7wt% Flux 2-8wt% Colorant 0.3-4.2wt% Fluorescent agent 0.6-4.9wt% Other additives 0-10wt%.

3. The lithium disilicate glass-ceramic restoration according to claim 1 or 2, wherein: The colorant is selected from at least one of V2O5, Er2O3, CeO2, Cr2O3, MnO2, and NiO; The fluorescent agent is selected from Tb4O7, Nd2O3, Pr6O 11 , Sm2O3, Dy2O3, Tm2O3, Eu2O3.

4. A method for preparing a lithium disilicate glass ceramic restoration according to any one of claims 1 to 3, comprising the following steps: 1) The raw material components are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a frit; 2) heating the frit at 1350-1650° C. for 50-120 min to melt into molten glass; 3) pouring the glass liquid into a mold for casting to obtain a glass block; 4) subjecting the glass block to a first crystallization heat treatment, and obtaining a restoration blank through molding, and then subjecting the restoration blank to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

5. The preparation method according to claim 4, wherein: The heat treatment temperature of the first crystallization heat treatment is 500-900°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C; preferably, the heat treatment temperature of the first crystallization heat treatment is 600-850°C, and the heat treatment temperature of the second crystallization heat treatment is 800-950°C.

6. The preparation method according to claim 4 or 5, wherein: The molding process is CAD or CAM molding process.

7. A method for preparing a lithium disilicate glass ceramic restoration according to any one of claims 1 to 3, comprising the following steps: 1) mixing the raw material components uniformly, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain a glass powder with an average particle size of 1-30 μm; Alternatively, the raw material components except the colorant are mixed uniformly, heated at 1350-1650° C. for 30-120 min to melt into glass liquid, and then water quenched to form a glass frit, which is ground to obtain a powder with an average particle size of 1-30 μm, and the colorant is mixed with the powder to obtain a glass powder; 2) placing the glass powder into a mold, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body; 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

8. The preparation method according to claim 7, wherein: The preparation method comprises: 1) using at least two raw material components of different colors and / or transparencies, respectively mixing the different raw material components, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, then quenching with water to form glass frit, grinding to obtain at least two glass powders of different colors and / or transparencies with an average particle size of 1-30 μm; Or, using at least two raw material components of different colors and / or transparencies, respectively, mixing the different raw material components except the colorant, heating at 1350-1650° C. for 30-120 min to melt into glass liquid, and then quenching with water to form a glass frit, grinding to obtain different powders with an average particle size of 1-30 μm, and then respectively mixing the colorant with the powder to obtain at least two glass powders of different colors and / or transparencies; 2) placing the at least two glass powders of different colors and / or transparencies into a mold layer by layer, performing dry pressing at 20-30 MPa, and then performing isostatic pressing at 100-240 MPa to obtain a green body; 3) subjecting the green body to a first crystallization heat treatment, and obtaining a restoration body through molding, and then subjecting the restoration body to a second crystallization heat treatment to obtain the lithium disilicate glass ceramic restoration.

9. The preparation method according to claim 7 or 8, wherein: The heat treatment temperature of the first crystallization heat treatment is 500-750°C, and the heat treatment temperature of the second crystallization heat treatment is 800-1000°C; preferably, the heat treatment temperature of the first crystallization heat treatment is 500-700°C, and the heat treatment temperature of the second crystallization heat treatment is 830-950°C.

10. The preparation method according to any one of claims 7 to 9, wherein The molding process is CAD or CAM molding process.

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