CN113248153B - Lithium disilicate glass ceramic and preparation method and application thereof - Google Patents

Lithium disilicate glass ceramic and preparation method and application thereof Download PDF

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CN113248153B
CN113248153B CN202110582059.6A CN202110582059A CN113248153B CN 113248153 B CN113248153 B CN 113248153B CN 202110582059 A CN202110582059 A CN 202110582059A CN 113248153 B CN113248153 B CN 113248153B
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lithium disilicate
disilicate glass
ceramic
sintering
glass ceramic
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CN113248153A (en
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刘鸿琳
李一洪
李兆梅
傅宇宏
林燕喃
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Fuzhou Rick Brown Pharmaceutical Technology Co ltd
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Fuzhou Rick Brown Pharmaceutical Technology Co ltd
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    • 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
    • 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
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • 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
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/818—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising zirconium oxide
    • 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
    • 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
    • A61K6/838—Phosphorus compounds, e.g. apatite
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57—Improving the yield, e-g- reduction of reject rates

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Abstract

The invention relates to lithium disilicate glass ceramic and a preparation method and application thereof. The preparation method of the lithium disilicate glass ceramic comprises the following steps: mixing the lithium disilicate glass matrix raw material and the opacifier, melting and annealing to prepare a lithium disilicate glass-ceramic blank; sintering the lithium disilicate glass-ceramic blank for the first time at the temperature of 520-580 ℃; preparing an intermediate; sintering the lithium disilicate glass-ceramic blank for the second time at the temperature of 800-860 ℃; preparing the lithium disilicate glass ceramic. The preparation method can lead the prepared lithium disilicate glass ceramic to be free from further sintering after cutting the manufactured restoration blank body by introducing the opacifier into the lithium disilicate glass matrix raw material and combining the two sintering processes in a specific temperature range, thereby avoiding the influence of the deformation generated during the sintering of the restoration blank body on the fitting degree of the restoration body and a patient and simultaneously improving the manufacturing efficiency of the restoration body.

Description

Lithium disilicate glass ceramic and preparation method and application thereof
Technical Field
The invention relates to a tooth restoration material, in particular to lithium disilicate glass ceramic and a preparation method and application thereof.
Background
The dental prosthesis is a material blank used for tooth restoration (such as whitening and defect repair), is more common as a veneer, also called as a tooth veneer, and is a restoration method which adopts a bonding technology to directly or indirectly bond and cover a dental prosthesis on the surface of a tooth under the condition of preserving living marrow, few molar teeth or no molar teeth aiming at tooth surface defects, stained teeth, discolored teeth, deformed teeth and the like so as to restore the normal shape of the tooth and improve the color and luster of the tooth. The veneering has excellent aesthetic effect on dental problems such as dental fluorosis, light and medium tetracycline pigmentation, slight tooth arrangement disorder and the like, and has small damage to the teeth of patients, so more and more people select a veneering form to repair the teeth.
Conventional veneers include resin veneers and ceramic veneers. The resin veneer is prepared by resin in the mouth of a patient, and has the advantages of convenience, rapidness and low cost, but cannot be used for a long time and only can be used as a transient prosthesis for improving the attractiveness in a short time. The ceramic veneer is a repairing method for fixing the thin-layer ceramic dental restoration on the lip surface of an affected tooth by using a bonding material to cover defects of defect discoloration and the like which affect the attractiveness, has the advantages of attractive color, small tooth preparation amount, liquid absorption resistance, good biocompatibility, abrasion resistance, periodontal health care, firm and reliable bonding and the like, and is the mainstream veneer at present. The ceramic veneers can be divided into three types according to different manufacturing methods and materials: traditional porcelain veneering, cast porcelain veneering and CAD/CAM machine processed porcelain veneering. Wherein, the CAD/CAM machine processing porcelain facing can better accord with the tooth form of the patient.
The traditional restoration material for the CAD/CAM machined ceramic veneering is lithium disilicate glass ceramic, and the clinical procedures of the CAD/CAM machined ceramic veneering are as follows: the technical personnel scans the teeth or the model of the patient to be mounted with the veneers, manufactures a three-dimensional model, designs the veneers, cuts glass ceramics according to the designed veneers, prepares veneering blanks, then sinters and finally mounts the veneers on the teeth of the patient. The sintering process cannot be omitted because: the glass ceramic without sintering process has low strength, and the direct bonding is easy to crack the ceramic, thereby influencing the service life. However, the degree of fit between the sintered veneering blank and the patient's teeth decreases, and the sintering process reduces the efficiency of the veneering.
Disclosure of Invention
Based on the above, the invention provides a preparation method of lithium disilicate glass ceramic which can be directly installed after cutting and manufacturing the dental restoration without sintering, and meanwhile, the lithium disilicate glass ceramic has high strength, long service life and high manufacturing and installing efficiency of the dental restoration.
The specific technical scheme is as follows:
in one aspect of the invention, a method for preparing a lithium disilicate glass ceramic is provided, which comprises the following steps:
Mixing the lithium disilicate glass matrix raw material and the opacifier, melting and annealing to prepare a lithium disilicate glass-ceramic blank;
sintering the lithium disilicate glass-ceramic blank for the first time at the temperature of 520-580 ℃; preparing an intermediate;
sintering the lithium disilicate glass-ceramic blank for the second time at the temperature of more than or equal to 800 ℃; preparing the lithium disilicate glass ceramic.
In one embodiment, the opacifying agent is selected from CaF 2 、Na 3 AlF 6 、Na 2 SiF 6 、Ca 3 (PO 4 ) 2 And BaSO 4 At least one of (1).
In one embodiment, the opacifier is Na 2 SiF 6 And BaSO 4 Combinations of (a) and (b).
In one embodiment, the temperature of the first sintering is 520 ℃ to 570 ℃.
In one embodiment, the temperature of the second sintering is 800 ℃ to 860 ℃.
In one embodiment, the time for the first sintering is 10min to 45 mi; and/or
The time of the second sintering is 5 min-15 min.
In one embodiment, the lithium disilicate glass matrix raw material comprises 50 to 65% SiO by weight percentage in the lithium disilicate glass ceramic 2 20 to 30 percent of Li 2 CO 3 1% -6% of K 2 CO 3 0.5 to 2 percent of Al 2 O 3 2 to 8 percent of ZrO 2 2% -10% of P 2 O 5 And 0% -4% of B 2 O 3 And (3) mixing the materials, wherein the weight percentage of the opacifier is 0.5-5%.
In one embodiment, the lithium disilicate glass matrix feedstock further comprises 0.5% to 3% by weight of a colorant in the lithium disilicate glass ceramic.
In one embodiment, the colorant is selected from TiO 2 、CeO 2 、Er 2 O 3 、Tb 4 O 7 、V 2 O 5 、MnO 2 And NiO.
In one embodiment, the melting temperature is 1400-1600 ℃ and the time is 1-2 h.
In another aspect of the invention, the lithium disilicate glass ceramic prepared by the preparation method is provided.
In another aspect of the invention, the application of the lithium disilicate glass ceramic in preparing dental restorations is provided.
In still another aspect of the present invention, there is provided a dental restoration method comprising the steps of:
scanning the teeth or the model of the patient to be provided with the dental prosthesis to manufacture a three-dimensional model;
designing a dental prosthesis model according to the three-dimensional model;
cutting the lithium disilicate glass ceramic according to the dental prosthesis model to prepare a dental prosthesis;
mounting the dental restoration to a tooth of a patient.
In one embodiment, the dental restoration does not require a sintering process.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of lithium disilicate glass ceramics, which is characterized in that an opacifier is introduced into a lithium disilicate glass matrix raw material, and the two-time sintering process under a specific temperature range is combined, so that the prepared lithium disilicate glass ceramics has small and more crystals, and can give consideration to the characteristics of easy cutting and strength compared with the traditional lithium disilicate glass ceramics.
Drawings
FIG. 1 is a crystal morphology of a lithium disilicate glass ceramic prepared in example 1 of the present invention;
FIG. 2 is a crystal morphology of a lithium disilicate glass ceramic prepared in comparative example 1 of the present invention;
FIG. 3 is a fitting degree investigation of a veneered blank prepared from the lithium disilicate glass ceramic in example 1 of the present invention;
FIG. 4 is a fitting degree examination of a faced green body prepared from a lithium disilicate glass ceramic of comparative example 1 of the present invention.
Detailed Description
The lithium disilicate glass ceramics of the present invention, their preparation and use are described in further detail below with reference to specific examples. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The invention provides a preparation method of lithium disilicate glass ceramic, which comprises the following steps:
mixing the lithium disilicate glass matrix raw material and the opacifier, melting and annealing to prepare a lithium disilicate glass-ceramic blank;
sintering the lithium disilicate glass-ceramic blank for the first time at the temperature of 520-580 ℃; preparing an intermediate;
sintering the lithium disilicate glass-ceramic blank for the second time at the temperature of more than or equal to 800 ℃; preparing the lithium disilicate glass ceramic.
According to the veneering process, the cutting of the lithium disilicate glass ceramic is required to be carried out according to the tooth model of the patient so as to obtain the dental restoration fitting the tooth of the patient, therefore, in the conventional technical cognition in the field, although the conventional lithium disilicate glass ceramic is also sintered twice during the preparation, the lithium disilicate glass ceramic still keeps a low-strength lithium metasilicate state after being sintered for the convenience of cutting (if the lithium disilicate glass ceramic is directly converted into the lithium orthosilicate, the lithium metasilicate state has high strength and hardness and is not easy to cut), and after the cutting, the lithium disilicate glass ceramic is converted into the lithium orthosilicate with high strength by utilizing the sintering again, so that the service life of the glass ceramic is ensured. The problems of the degree of fit of the dental prosthesis and the low efficiency of manufacturing and installing the dental prosthesis caused thereby have not been solved.
The invention departs from the conventional technical cognition, seeks a material of the dental prosthesis which does not need sintering after cutting, and finds out through systematic research: the opacifier is introduced on the basis of a lithium disilicate glass matrix raw material, and two times of sintering at proper temperature are combined, wherein in the process of the first sintering (at the temperature of 520-580 ℃), suspended crystal grains formed by melting and annealing of the opacifier can promote nucleation and slight growth of lithium phosphate and lithium metasilicate, and in the process of the second sintering (at the temperature of more than or equal to 800 ℃), lithium phosphate and lithium metasilicate crystals are directly converted into lithium orthosilicate, and the crystal grains of the lithium orthosilicate are many and fine. Therefore, the lithium disilicate glass ceramic prepared by the invention can meet the cutting requirement, has better hardness, can be directly installed after cutting, does not need to carry out a sintering process again, avoids the influence of deformation generated during sintering of the dental prosthesis on the fitting degree of the prosthesis and a patient, simplifies the manufacturing and installing processes of the prosthesis, improves the efficiency, shortens the waiting time of the patient, and does not need to be provided with a sintering furnace.
Furthermore, by using a suitable opacifying agent, the glass ceramic can be melted in a lithium disilicate glass matrix during melting, and can be precipitated into innumerable extremely fine suspended crystal grains during cooling, so that the amount of fine crystals is increased, and the phase separation of the glass liquid is promoted, so that the crystal amount in the finally prepared glass ceramic is smaller and more.
In some specific examples thereof, the opacifying agent is selected from CaF 2 、Na 3 AlF 6 、Na 2 SiF 6 、Ca 3 (PO 4 ) 2 And BaSO 4 At least one of (1). Further, the opacifier is Na 2 SiF 6 And BaSO 4 Combinations of (a) and (b).
Further, Na 2 SiF 6 And BaSO 4 In combination of (A) and (B), Na 2 SiF 6 And BaSO 4 The mass ratio of (1) to (0.1-0.3).
In some specific examples, the temperature of the first sintering is 520 ℃ to 580 ℃. Further, the temperature of the first sintering is 520-570 ℃. Furthermore, the temperature of the first sintering is 520-530 ℃. Specifically, the temperature of the first sintering includes, but is not limited to: 520 ℃, 525 ℃, 530 ℃, 535 ℃, 540 ℃, 545 ℃, 550 ℃, 555 ℃, 560 ℃, 565 ℃, 567 ℃, 568 ℃, 569 ℃, 570 ℃, 571 ℃, 572 ℃, 573 ℃, 574 ℃, 575 ℃, 580 ℃.
In some specific examples, the temperature of the second sintering is 800 ℃ to 860 ℃. Further, the temperature of the second sintering is 840-860 ℃. Furthermore, the temperature of the second sintering is 850-560 ℃. Specifically, the temperature of the second sintering includes, but is not limited to: 800 deg.C, 805 deg.C, 810 deg.C, 815 deg.C, 820 deg.C, 825 deg.C, 830 deg.C, 835 deg.C, 836 deg.C, 837 deg.C, 838 deg.C, 839 deg.C, 840 deg.C, 841 deg.C, 842 deg.C, 843 deg.C, 844 deg.C, 845 deg.C, 850 deg.C, 855 deg.C, 860 deg.C.
In some specific examples, the time for the first sintering is 25min to 35 min. Specifically, the time for the first sintering includes, but is not limited to: 25min, 26min, 27min, 28min, 29min, 30min, 31min, 32min, 33min, 34min, 35 min.
In some specific examples, the time for the second sintering is 5min to 15 min. Specifically, the time for the first sintering includes, but is not limited to: 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15 min.
In some specific examples, the time for the first sintering is 25min to 35min, and the time for the second sintering is 5min to 15 min.
In some specific examples, the lithium disilicate glass matrix material comprises 50% to 65% SiO by weight in the lithium disilicate glass ceramic 2 20 to 30 percent of Li 2 CO 3 1% -6% of K 2 CO 3 0.5 to 2 percent of Al 2 O 3 2 to 8 percent of ZrO 2 2% -10% of P 2 O 5 And 0% -4% of B 2 O 3 The materials are mixed, and the weight percentage of the opacifier is 0.5 to 5 percent.
In some specific examples, the opacifying agent is present in an amount of 0.5 to 5 weight percent, based on the weight percent in the lithium disilicate glass ceramic. Further, the weight percentage of the opacifier is 1 to 1.5 percent. Specifically, the weight percentages of opacifying agents include, but are not limited to: 0.5%, 0.8%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 2%, 3%, 4%, 5%.
In some specific examples, the opacifier includes 0.7% to 1.4% Na by weight in the lithium disilicate glass ceramic 2 SiF 6 And 0.1 to 0.3 percent of BaSO 4 。
In some specific examples, B is present as a weight percentage in the lithium disilicate glass ceramic 2 O 3 The weight percentage of the component (A) is 0.05-4%.
In some specific examples, the lithium disilicate glass matrix material comprises 57% to 60% SiO by weight in the lithium disilicate glass ceramic 2 25 to 28% of Li 2 CO 3 3% -4% of K 2 CO 3 0.5 to 1 percent of Al 2 O 3 2.5 to 4 percent of ZrO 2 4 to 5 percent of P 2 O 5 And 0.5 to 1 percent of B 2 O 3 And (5) burdening. Further, the lithium disilicate glass matrix raw material contains 59-60% of SiO in percentage by weight in the lithium disilicate glass ceramic 2 25 to 26% of Li 2 CO 3 3.5% -4% of K 2 CO 3 0.5 to 0.7 percent of Al 2 O 3 2.5% -3% of ZrO 2 4.5 to 5 percent of P 2 O 5 And 0.5 to 0.7 percent of B 2 O 3 And (5) burdening.
In some specific examples, the lithium disilicate glass matrix feedstock further comprises 0.5% to 3% by weight of a colorant in the lithium disilicate glass ceramic. Specifically, the weight percentages of the colorant include, but are not limited to: 0.5%, 0.6%, 0.7%, 0.8%, 0.9%, 1%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 2%, 2.5%, 3%.
In some specific examples thereof, the colorant is selected from TiO 2 、CeO 2 、Er 2 O 3 、Tb 4 O 7 、V 2 O 5 、MnO 2 And NiO. Further, the colorant is CeO 2 、Er 2 O 3 And V 2 O 5 Combinations of (a) and (b).
In some specific examples, the colorant comprises 0.5% to 1.4% CeO by weight of the lithium disilicate glass ceramic 2 、0.01％～0.1％Er 2 O 3 And 0.5% -1.4% V 2 O 5 。
In some specific examples, the melting temperature is 1400 ℃ to 1600 ℃. Specifically, the temperature of melting includes, but is not limited to: 1400 deg.C, 1450 deg.C, 1480 deg.C, 1500 deg.C, 1520 deg.C, 1550 deg.C, 1600 deg.C.
In some specific examples, the melting time is 1h to 2 h. Specifically, the melting time includes, but is not limited to: 1h, 1.5h and 2 h.
In some specific examples, the melting temperature is 1400-1600 ℃ and the time is 1-2 h.
In some specific examples, the annealing temperature is 400 ℃ to 600 ℃. Specifically, the temperature of annealing includes, but is not limited to: 400 deg.C, 450 deg.C, 480 deg.C, 500 deg.C, 520 deg.C, 550 deg.C, 600 deg.C.
In some specific examples, the lithium disilicate glass matrix raw material and the opacifying agent are ball milled and then mixed.
The invention also provides the lithium disilicate glass ceramic prepared by the preparation method. The lithium disilicate glass ceramic does not need to be sintered, can be directly installed after being cut and manufactured into the dental restoration, and has high strength, long service life and high manufacturing and installing efficiency of the dental restoration.
The invention also provides the application of the lithium disilicate glass ceramic in preparing dental restorations. In particular, dental restorations include, but are not limited to, veneered embryos, inlays, onlays, crowns, and the like.
The invention also provides a manufacturing method of the dental prosthesis, which comprises the following steps:
scanning the teeth or the model of the patient to be provided with the dental prosthesis to manufacture a three-dimensional model;
designing a dental prosthesis model according to the three-dimensional model;
and cutting the lithium disilicate glass ceramic according to the dental restoration model to prepare the dental restoration.
The invention also provides a dental restoration method, which comprises the following steps:
scanning the teeth or the model of the patient to be provided with the dental prosthesis to manufacture a three-dimensional model;
designing a dental prosthesis model according to the three-dimensional model;
cutting the lithium disilicate glass ceramic according to the dental restoration model to prepare a dental restoration;
the dental restoration is mounted to a patient's tooth.
In some specific examples thereof, the dental restoration does not require a sintering process. Therefore, the manufacturing and mounting efficiency of the dental prosthesis is high, the waiting time of a patient is saved, and equipment such as a sintering furnace and the like does not need to be prepared.
Hereinafter, specific examples are described, and the raw materials used in the examples are all commercially available products unless otherwise specified.
Example 1
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 (opacifier), 0.2% BaSO 4 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic. The lithium disilicate glass ceramic is subjected to SEM detection, and the obtained morphology is shown in figure 1. As can be seen from FIG. 1, the crystals obtained in this example were fine and dense.
Example 2
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant), 0.1% of V 2 O 5 (coloring agent) 1.2% of Na 2 SiF 6 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 3
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 (opacifier) 0.2% Ca 3 (PO 4 ) 2 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 4
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 (opacifier), 0.2% BaSO 4 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation on the microcrystalline glass blank at 520 ℃ for 30min to realize nucleation, and finally carrying out heat preservation at 860 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 5
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 (opacifier), 0.2% BaSO 4 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 580 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 800 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 6
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) According to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant) 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 3 AlF 6 (opacifier), 0.2% CaF 2 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 7
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 55% SiO 2 30% of Li 2 CO 3 2% of K 2 CO 3 1.5% of Al 2 O 3 4.15% of ZrO 2 3% of P 2 O 5 2% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 (opacifier), 0.2% BaSO 4 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Example 8
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 60% SiO 2 25% of Li 2 CO 3 4% of K 2 CO 3 0.5% of Al 2 O 3 2.65% of ZrO 2 5% of P 2 O 5 0.5% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 2 SiF 6 Opacifier), 0.2% of BaSO 4 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min on the microcrystalline glass blank to realize nucleation, and finally carrying out heat preservation at 840 ℃ for 10min to obtain the lithium disilicate glass ceramic.
Comparative example 1
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 58.2% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3.65% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation at 570 ℃ for 30min to realize nucleation on the microcrystalline glass blank, and carrying out crystallization at 630 ℃ for 30 min.
Comparative example 2
The preparation method of the lithium disilicate glass ceramic comprises the following steps:
(1) according to 57% SiO 2 28% of Li 2 CO 3 3% of K 2 CO 3 1% of Al 2 O 3 3% of ZrO 2 4% of P 2 O 5 1% of B 2 O 3 1% of CeO 2 (colorant), 0.05% Er 2 O 3 (colorant) 0.1% of V 2 O 5 (colorant) 1% Na 3 AlF 6 (opacifier), 0.2% CaF 2 (opacifier) burdening, ball-milling and mixing, putting into a high-temperature furnace at 1500 ℃ for melting for 2h, and then annealing at 500 ℃ to obtain a microcrystalline glass blank;
(2) and (3) carrying out heat preservation on the microcrystalline glass blank at 600 ℃ for 30min to realize nucleation, and finally carrying out heat preservation at 880 ℃ for 10min to obtain the lithium disilicate glass ceramic.
And (4) performance testing:
(1) and (3) testing the strength: the lithium disilicate glass ceramics prepared in examples 1 to 8 and comparative examples 1 to 2 were subjected to a strength test.
The test method comprises the following steps: test samples were prepared and tested according to the three-point bending test method in GB 30367-2013.
The test results are shown in table 1 below:
TABLE 1
Three point bending strength (MPa)
Example 1 318±26
Example 2 280±28
Example 3 300±19
Example 4 333±22
Example 5 280±21
Example 6 305±18
Example 7 275±29
Example 8 328±23
Comparative example 1 312±31
Comparative example 2 257±27
(2) And (3) testing the fitting degree: the lithium disilicate glass ceramics prepared in example 1 and comparative example 1 were subjected to a conformity test.
The test method comprises the following steps: selecting the same set of prosthesis data, respectively adopting the lithium disilicate glass ceramics prepared in the embodiment 1 and the comparative example 1 to carry out cutting preparation on the prosthesis, wherein the prosthesis cut in the embodiment 1 is not further sintered, the prosthesis cut in the comparative example 1 is further subjected to heat preservation at 840 ℃ for 10min, the three-point bending strength (MPa) tested at the moment is 312 +/-31, and SEM detection is carried out on the lithium disilicate glass ceramics at the moment, and the obtained morphology graph is shown in figure 2, so that the crystal grains are thicker and the crystal distribution is looser. And (4) photographing and comparing the fitting degree of the prepared veneering blank and the dental cast.
The fitting degree between the dental cast and the veneer blank prepared from the lithium disilicate glass ceramic of example 1 is shown in fig. 3, and it can be seen from fig. 3 that the veneer blank which is not required to be sintered after cutting completely retains the shape at the time of design and is completely fitted with the dental cast.
The fitting degree between the veneering blank prepared from the lithium disilicate glass ceramic of the comparative example 1 and the dental cast is shown in fig. 4, and as can be seen from fig. 4, the veneering sintered after cutting generates obvious gaps with the dental cast due to sintering shrinkage and deformation, and the prepared veneering can not be fitted with the teeth of a patient.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.

Claims (14)

1. A preparation method of lithium disilicate glass ceramics is characterized by comprising the following steps:
mixing the lithium disilicate glass matrix raw material and the opacifier, melting and annealing to prepare a lithium disilicate glass-ceramic blank;
sintering the lithium disilicate glass-ceramic blank for the first time at the temperature of 520-580 ℃; preparing an intermediate;
sintering the lithium disilicate glass-ceramic blank for the second time at the temperature of more than or equal to 800 ℃; preparing the lithium disilicate glass ceramic.
2. The method of claim 1, wherein the opacifying agent is selected from CaF 2 、Na 3 AlF 6 、Na 2 SiF 6 、Ca 3 (PO 4 ) 2 And BaSO 4 At least one of (1).
3. The method of claim 2, wherein the opacifier is Na 2 SiF 6 And BaSO 4 Combinations of (a) and (b).
4. The method of claim 1, wherein the first sintering temperature is 520 ℃ to 570 ℃.
5. The method of claim 1, wherein the second sintering temperature is 800 ℃ to 860 ℃.
6. The method for preparing lithium disilicate glass-ceramics according to claim 1, wherein the time for the first sintering is 10min to 45 mi; and/or
The time of the second sintering is 5 min-15 min.
7. The method for preparing a lithium disilicate glass ceramic according to any one of claims 1 to 6, wherein the lithium disilicate glass matrix raw material contains 50 to 65% of SiO in terms of weight percentage in the lithium disilicate glass ceramic 2 20 to 30 percent of Li 2 CO 3 1% -6% of K 2 CO 3 0.5 to 2 percent of Al 2 O 3 2 to 8 percent of ZrO 2 2% -10% of P 2 O 5 And 0% -4% of B 2 O 3 And (3) mixing the materials, wherein the weight percentage of the opacifier is 0.5-5%.
8. The method of preparing a lithium disilicate glass-ceramic according to claim 7, wherein the lithium disilicate glass matrix raw material further comprises 0.5 to 3% of a colorant by weight percentage in the lithium disilicate glass-ceramic.
9. The method of claim 8, wherein the colorant is selected from the group consisting of TiO 2 、CeO 2 、Er 2 O 3 、Tb 4 O 7 、V 2 O 5 、MnO 2 And NiO.
10. The method of any of claims 1 to 6, wherein the melting temperature is 1400 ℃ to 1600 ℃ for 1h to 2 h.
11. A lithium disilicate glass-ceramic produced by the production method according to any one of claims 1 to 10.
12. Use of a lithium disilicate glass ceramic according to claim 11 for the preparation of a dental restoration.
13. A dental restoration method, comprising the steps of:
scanning the teeth or the model of the patient to be provided with the dental prosthesis to manufacture a three-dimensional model;
designing a dental prosthesis model according to the three-dimensional model;
cutting the lithium disilicate glass-ceramic of claim 11 according to the dental restoration model to produce a dental restoration;
mounting the dental restoration to a tooth of a patient.
14. The dental restoration method according to claim 13, wherein the dental restoration does not require a sintering process.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009156493A1 (en) * 2008-06-25 2009-12-30 University Of Sheffield Dental constructs and methods for their preparation
WO2016026580A1 (en) * 2014-08-22 2016-02-25 Pritidenta Gmbh Cubic stabilized zirconia compositions produced by a melting process for use in dental applications and dental articles comprising the same cubic stabilized zirconia compositions
CN108751721A (en) * 2018-06-15 2018-11-06 中国人民解放军第四军医大学 A kind of lithium bisilicate glass ceramics and its preparation method and application for dental zirconium oxide surface decorations porcelain
CN111904638A (en) * 2020-06-15 2020-11-10 福州瑞克布朗医药科技有限公司 Glass ceramic veneer and processing method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009156493A1 (en) * 2008-06-25 2009-12-30 University Of Sheffield Dental constructs and methods for their preparation
WO2016026580A1 (en) * 2014-08-22 2016-02-25 Pritidenta Gmbh Cubic stabilized zirconia compositions produced by a melting process for use in dental applications and dental articles comprising the same cubic stabilized zirconia compositions
CN108751721A (en) * 2018-06-15 2018-11-06 中国人民解放军第四军医大学 A kind of lithium bisilicate glass ceramics and its preparation method and application for dental zirconium oxide surface decorations porcelain
CN111904638A (en) * 2020-06-15 2020-11-10 福州瑞克布朗医药科技有限公司 Glass ceramic veneer and processing method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
CEREC椅旁CAD/CAM嵌体/高嵌体修复的短期临床观察;李晶等;《现代口腔医学杂志》;20170919(第05期);全文 *
锂云母型微晶玻璃可切削机理的探讨;黄文旵等;《功能材料》;19831231(第06期);全文 *

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