• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    patent summary: "dental restoration, method for its production and ceramic glass". The present invention relates to ceramic glasses which show high strength, high translucency, high chemical stability and are still mechanically processable. The invention further relates to a method for the production of dental restoration which comprises such glass or ceramic glass as the dental restoration itself.
    公开号:BR112013032434B1
    申请号:R112013032434-1
    申请日:2012-06-18
    公开日:2018-05-15
    发明作者:Durschang Bernhard；Probst Jörn；Thiel Norbert；Gödiker Michael；Vollmann Markus；Schusser Udo；Wiesner Carsten
    申请人:Vita Zahnfabrik H. Rauter Gmbh & Co. Kg；
    IPC主号:
    专利说明:

    Invention Patent Descriptive Report for "DENTAL RESTORATION, ITS PRODUCTION METHOD, AND CERAMIC DENTAL GLASS". The present invention relates to ceramic glasses that show high resistance, high translucency, high chemical stability and which are still mechanically processable. The invention also relates to a method for the production of a dental restoration comprising such glass or ceramic glass as well as the dental restoration itself.
    In the lithium oxide-silicon dioxide system, lithium disilicate (UO2. 2S1O2 (LÍ2SÍ2O5)) - ceramic glasses are well known in the literature and several patents are based on this ceramic glass system. In EP 0 536 479 B1, self-glazing ceramic lithium disilicate glass objects are then described for the production of crockery and, in EP 0 536 572 B1, ceramic lithium disilicate glass that can be used for the dispersion of fine glass particles colored on its surface as cladding elements for construction purposes. The main focus of publications on ceramic lithium disilicate glasses lies in dental applications. The lithium disilicate system is very suitable here for the production of processable CAD / CAM ceramic glasses, since crystallisation is carried out here through the lithium metasilicate phase (see SD Stookey: "Chemical Machining of Photosensiti-ve Glass ", Ind. Eng. Chem., 45, 115-118 (1993) and SD Stookey:" Photo-sensitively Opacifiable Glass "US-A-2 684 911 (1954)).
    These ceramic lithium metasilicate glasses have resistances so low in their intermediate stage that they are readily processed using CAD / CAM (M.-P. Borom, AM Turkalo, RH Do-remus: "Strength and Microstructure in Lithium Disilicate Glass Ceramics ", J. Am. Ceram. Soc., 58, No. 9-10, 385 - 391 (1975) and DE 24 51 121 A1.
    Only by the subsequent conversion to lithium disilicate or by the growth of lithium metasilicate crystals in a second heat treatment, high-strength dental materials are obtained. The heat treatment that is carried out in a dental laboratory or in dental practice is a burden for the technician as well as for the patient in terms of time and costs. In particular, during the method at the clinic, inconvenient waiting times can occur.
    In this method, an individually adapted crown / onlay / inlay is milled from a ceramic glass block after the first crystallization stage by means of CAD / CAM, in dental practice this is subjected to a second crystallization stage in a special oven and used directly on the first and only visit to the patient's dentist (DE 10 2005 028 637).
    Such heat treatment requires an oven and the corresponding acquisition and maintenance costs. In addition, such heat treatment can be a source of defects in the final product. Another disadvantage is the time required for such treatment, which is between 30 and 60 minutes. For common CAD / CAM systems, a maximum strength of 170 MPa is the limit. Therefore, machinable materials cannot be used directly for high quality applications. Machinability is not only dependent on the strength of the material, but it is also dependent on additional properties, such as hardness, modulus of elasticity, resistance to fracture as well as the structure and microstructure of ceramic glass. It has to be differentiated between forms of intercrystalline and transcrystalline fraction.
    Based on that, it was an objective of the present invention to provide ceramic glasses that have improved resistance values and also improved translucency and chemical resistance.
    This objective is achieved by the method for producing a dental restoration that has the characteristics of claim 1, colored and translucent dental ceramic glass having the characteristics of claim 11 and the dental restoration of claim 14. The subsequent dependent claims reveal advantageous developments.
    Within the scope of the present invention, glass compositions were developed in the basic Si02-Li20-Zr02 system, which has lithium meta-silicate as the only or the main crystalline phase (> 50%).
    Surprisingly, it was discovered that the use of specific compositions of lithium metasilicate together with specific heat treatments for its crystallization can result in finally crystallized ceramic glasses with high resistance, which can be machined with CAD / CAM techniques.
    In addition, it has been shown that up to 20% by weight of ZrÜ2 can be incorporated into the glass without the structure being significantly influenced. Contrary to all expectations, ZrC> 2 does not crystallize as a separate crystalline phase, but remains completely or considerably in the residual amorphous glass phase. Due to the high proportion of Zr02, the mechanical and chemical resistances are immensely improved in this amorphous phase, which also leads to improved properties of the complete dental ceramic glass (crystalline phase and residual glass phase), such as, for example, final resistance and acid solubility. The method is also suitable for a two-stage production process from the initial glass, a partial crystallization of lithium meta-silicate being carried out in the first stage of processing, which allows for good processing by CAD / CAM. In the second processing stage, an increase in the proportion of the crystalline phase (primary lithium metasilicate) is carried out, which leads to high resistance values. The most important cause for the surprisingly high resistance values in the lithium metasilicate system is attributed here to the high proportion of zirconia oxide (> 8 MA). High translucency is ensured by the small size of the crystallite in the ceramic glass. In addition, good chemical stability is ensured by the high proportion of zirconia oxide in the glass phase.
    In accordance with the present invention, a method for producing a dental restoration comprising a lithium silicate ceramic glass is provided, having the following steps: a) an amorphous glass is subjected to at least one heat treatment with temperatures between 450 to 1100 * 0, resulting in a colored and translucent dental ceramic glass with a resistance of at least 250 MPa (measured according to DIN ISO 6872) and with the color of the tooth, where during at least one heat treatment, at least a partial crystallization it occurs due to the increased temperatures, and b) the ceramic glass is formed for a dental restoration for immediate dental application and with resistance of at least 200 MPa (measured according to DIN ISO 6872) by using a material removal process.
    In the context of the present invention, a translucent ceramic glass is a ceramic that has a light transmission with a wavelength between 360 nm to 740 nm (measured according to DIN ISO 410 with a Minolta CM-3610d spectrometer). The tooth color is determined according to existing tooth color guides (for example, classic Vita color guide, Vita 3D master color guide). The stabilizer is preferably ZrC> 2 and / or Hf02. Preferably, the stabilizer is present essentially in the amorphous state.
    They can be contained as additives components selected from the group consisting of nucleating agents, fluorescent agents, dyes, in particular glass coloring oxides, colored pigments and their mixtures, in glass or ceramic glass.
    The nucleating agents are preferably selected from the group consisting of phosphorus oxide, titanium oxide, tin oxide, their mixtures and noble metals, preferably in an amount of 1 to 10% by weight, more preferably 2 to 8% by weight and most preferably 4 to 8% by weight.
    The fluorescent agents are preferably selected from the group consisting of bismuth oxides, rare earth elements such as neodymium, praseodymium, samarium, erbium and europium and mixtures thereof, preferably in an amount of 0.1 to 5% by weight, more preferably 0 , 5 to 4% by weight and most preferably 1 to 3% by weight.
    Glass dye oxides are preferably selected from the group of iron oxides, titanium, cerium, copper, chromium, cobalt, nickel, manganese, selenium, silver, indium, gold, vanadium, rare earth elements such as neodymium, praseodymium, samarium, erbium, europium, terbium, dysprosium, holmium, yttrium and mixtures thereof, preferably in an amount of 0.1 to 6% by weight, more preferably 0.5 to 5% by weight and most preferably 1 to 4% by weight Weight.
    The colored pigments can be doped spinels, which are comprised, preferably in an amount of 0.1 to 6% by weight, more preferably 0.5 to 5% by weight and most preferably 1 to 4% by weight.
    Additional additives are preferably selected from the group consisting of boron oxide, phosphorus oxide, fluorine, barium oxide, strontium oxide, magnesium oxide, zinc oxide, calcium oxide, yttrium oxide, titanium oxide, oxide of niobium, tantalum oxide, lanthanum oxide and mixtures thereof, which are preferably comprised in an amount of 0.1 to 5% by weight.
    In a preferred embodiment, amorphous glass has the following composition: 55 to 70% by weight of S1O2, 10 to 25% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group consisting of Zr oxides, Hf, Ge, La, Y, Ce, Ti or Zn or their mixtures, 0 to 10% by weight of Al2O3, 0 to 10% by weight of K2O and / or Na20 and 0 to 20% by weight of additives.
    In a further preferred embodiment, the amorphous glass has the following composition: 55 to 70% by weight of S1O2, 10 to 25% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of ZrC> 2, HfC > 2 or mixtures thereof, 0 to 10% by weight of AI2O3, 0 to 10% by weight of K2O and / or Na2Ü and 0 to 20% by weight of additives.
    In a further preferred embodiment, amorphous glass has the following composition: 55 to 64% by weight of S1O2, 15 to 22% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of ZrC> 2, ΗΙΌ2 or mixtures thereof, 0.1 to 8% by weight of Al2O3, 0 to 8% by weight of K20 and / or Na20 and 0 to 15% by weight of additives.
    In a further preferred embodiment, the amorphous glass has the following composition: 55 to 64% by weight of S1O2, 17 to 20% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of ZrC> 2, Hf02 or mixtures thereof, 0.1 to 5% by weight of AI2O3, 0.1 to 5% by weight of K2O and / or Na2Ü, 2 to 8% by weight of P2O5 and 0 to 10% by weight of additives.
    In a preferred embodiment, the heat treatment is a single stage treatment with a temperature between 600 * C to 950 * 0, preferably 780 to 900 * 0. It is another preferred embodiment that the heat treatment is a two-stage treatment with a first temperature between 600 to 800 * 0 and a second temperature between 780 to 900 * 0.
    Lithium silicate glasses or ceramic glasses according to the invention are used as dental material or as components of a dental material. The material removal process is a subtractive process, preferably selected from the group consisting of milling, grinding and laser ablation, preferably as a CAM process.
    In an additional preferred embodiment, the dental restoration is subjected to a finishing process before dental application. Such a finishing process can be polishing, glazing, waterproofing, coating and covering with a ceramic or covering enamel. The dental restoration is preferably an inlay, an onlay, a bridge, a side support, jacket, cover, a crown, a partial crown, a structure or "coping".
    According to the present invention, a colored and translucent dental ceramic glass with a resistance of at least 250 MPa (measured according to DIN ISO 6872) which has the following composition is also provided: 55 to 70% by weight of S1O2, 10 to 25% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of Zr, Hf, Ge, La, Y, Ce, Ti, Zn or their mixtures, 0 to 10% by weight of AI2O3, 0 to 10% by weight of K20 and / or Na20 and 0 to 20% by weight of additives.
    In a preferred embodiment, the ceramic glass has the following composition: 55 to 70% by weight of S1O2, 10 to 25% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of Zr02, Hf02 or mixtures thereof , 0.1 to 10% by weight of Al2O3, 0 to 10% by weight of K2O and / or Na20 and 0 to 20% by weight of additives.
    Preferably, the ceramic glass has the following composition: 55 to 64% by weight of S1O2, 15 to 22% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of ZrC> 2, HfC> 2 or its mixtures, 0.1 to 8% by weight of Al203, 0 to 8% by weight of K2O and / or Na20 and 0 to 15% by weight of additives.
    In a further preferred embodiment, the ceramic glass has the following composition: 55 to 64% by weight of S1O2, 17 to 20% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group of ZrC> 2, HfC > 2 or mixtures thereof, 0.1 to 5% by weight of AI2O3, 0.1 to 5% by weight of K2O and / or Na20, 2 to 8% by weight of P2O5, and 0 to 10% by weight of additives . The ceramic glass preferably has a dimensional stability that allows the processing of the ceramic glass with a process of removing the material.
    In accordance with the present invention, in addition, a dental restoration is provided which is producible by the method described above. It is preferred that the dental restoration has a degree of crystallization of at least 5%, preferably at least 50%. It is preferred that the dental restoration has a strength of at least 200 MPa, preferably at least 300 MPa. Dental restoration can have a finish. Such a finish is preferably a polishing, glazing, waterproofing, cladding and coating with a ceramic or enamel coating. Such finished dental restoration preferably has a strength of at least 250 MPa, preferably of at least 300 MPa.
    Dental restorations with the following compositions are additional aspects of the present invention: Composition 1 The purpose according to the application is intended to be explained in more detail with reference to the subsequent examples without restricting said purpose to those variants.
    Example 1 In Table 1, a fixed composition given by way of example for different stabilizers is mentioned, from which ceramic metasilicate glasses containing a large amount of stabilizer can be produced in the dental area.
    Table 1 * SX represents stabilizer compositions S1 to S5 (see Table 2) Table 2 shows stabilizers used as an example for dental applications with the composition of Table 1.
    The glasses were melted at 1500Ό and poured into metal molds to form blocks. The blocks were allowed to rest in the oven at 560Ό and cooled slowly. For the various characterization processes, the glass blocks were divided and subjected to a first crystallization treatment. For this purpose, the glasses were stored for 10 to 120 minutes from 600Ό to 7500. As a result, ceramic glasses with resistance values from 150 MPa to 220 MPa were produced. Here, lithium metasilicate was instituted exclusively as the crystalline phase. In this state, processing using CAD / CAM methods is possible very quickly.
    In Table 3, the compositions that are given are mentioned as an example, from which ceramic glasses containing a large amount of zirconium oxide can be produced for use in the dental field.
    Table 3 * (Data are in% by weight) The glasses were melted at 15000 and poured into metal molds to form blocks. The blocks were allowed to rest in the oven at 560 * C and cooled slowly. For the various characterization processes, the glass blocks were divided and subjected to a first crystallization treatment. For this purpose, the glasses were stored for 10 to 120 minutes from 600 * 0 to 7500. As a result, ceramic glasses with resistance values from 150 MPa to 220 MPa were produced. Here, lithium metasilicate was instituted exclusively as the crystalline phase. In this state, processing using CAD / CAM methods is possible very quickly.
    Example 2 A molten glass with a composition of 60% by weight of Si-O2, 19% by weight of UO2, 10% by weight of ZrÜ2, 6% by weight of P2O5, 2% by weight of AI2O3, 2% by weight of K2O and 2% by weight of Ce02 is molded into a block shape. This block is completely crystallized by a two-stage firing process. The heat treatment is carried out at 620 * 0 and 8500. After this procedure, a block support (for example, a metal accessory) is glued to the block to fix it on a CAM machine.
    For this application, a dental grinding machine (Sirona inLab MCXL) is used. For a first test, the pre-installed parameters for pre-sintered IPS e.max CAD (program version 3.85) were chosen. A previously designed crown was ground using typical diamond tools. The expected grinding time was 17 minutes; The actual grinding time was 28 min. The chosen drills and the resulting crown showed no problems.
    In a second test, an identical crown was ground on the same machine by selecting pre-installed parameters for VITA In-Ceram Spinell. The grinding process also took approximately 10 minutes longer than the calculated time. The crown and emeralds showed no defects.
    After grinding, the surface of the crown can be improved manually. A typical procedure for a dental technician or dentist may be, for example, polishing, applying enamel, coloring and coating. Machine curved bars after the final crystallization and treated with an enamel showed fracture values of 370 MPa (flexural strength test in 3 points according to DIN EN ISO 6872).
    Comparative test The commercially available IPS e.max CAD product (Ivoclar-Vivadent, color LT A2) has been tested in a comparative manner. For this reason, the blocks were additionally heat treated at 850Ό. The support, which was removed before the final heat treatment, was re-coupled with glue.
    Then, the same crown model was loaded again and the parameters (usually only partially crystallized) for IPS e.max CAD were selected. The complete shredding process took approximately 90 minutes instead of the calculated 17 minutes. The process had to be restarted four times because the four diamond grinders broke during the process. This showed that it is not possible to process fully crystallized IPS e.max CAD crowns in a commercially successful manner.
    权利要求:
    Claims (16)
    [1]
    1. Method for producing a dental restoration, characterized by the fact that it comprises a ceramic glass of lithium silicate, being that: (a) an amorphous glass is subjected to at least one heat treatment with temperatures between 450 to HOOC, resulting in a colored and translucent ceramic glass tooth with a resistance of at least 250 MPa (measured according to DIN ISO 6872) and with the color of a tooth, during which the partial crystallization occurs due to high temperatures, and (b) ceramic glass is formed for dental restoration for immediate dental application and with a resistance of at least 200 MPa (measured according to DIN ISO 6872) by using a material removal process, with amorphous glass having the following composition : 55 to 70% by weight of SiC> 2, 15 to 22% by weight of U2O, 8 to 20% by weight of a stabilizer selected from the group consisting of ZrC> 2, Hf02 and their mixtures, 0 to 10% by weight weight of AI2O3, 0 to 10% in weight of K2O and / or Na20, 0 to 8% by weight of P2O5, and 0 to 20% by weight of additives.
    [2]
    2. Method according to claim 1, characterized in that the amorphous glass has the following composition: 55 to 64% by weight of S1O2, 17 to 20% by weight of U2O, 0.1 to 8% by weight , more preferably 0.5 to 5% by weight of Al2O3, 0.1 to 8% by weight, more preferably 0.5 to 5% by weight of K20 and / or Na20, 2 to 8% by weight of P2O5, and 0 to 10% by weight of additives.
    [3]
    3. Method according to claim 1 or 2, characterized by the fact that the heat treatment is a single stage treatment with a temperature between 600 ° C to 950 ° C, preferably 780 to 900 ° C or the treatment thermal is a two-stage treatment with a first temperature between 600 to 800 ° C and a second temperature between 780 to 900 ° C.
    [4]
    Method according to any one of claims 1 to 3, characterized in that the additives are selected from the group consisting of nucleating agents, fluorescent agents, dyes, preferably oxides for coloring glass and / or colored pigments and their mixtures.
    [5]
    5. Method according to claim 4, characterized by the fact that the nucleating agents are selected from the group consisting of phosphorus oxide, titanium oxide, tin oxide, their mixtures and noble metals, preferably in an amount of 1 to 10% by weight, more preferably 2 to 8% by weight and most preferably 4 to 8% by weight.
    [6]
    6. Method according to claim 4 or 5, characterized by the fact that the fluorescent agents are selected from the group consisting of bismuth oxides, rare earth elements such as neodymium, praseodymium, samarium, erbium and europium and their mixtures, preferably in an amount of 0.1 to 5% by weight, more preferably 0.5 to 4% by weight and most preferably 1 to 3% by weight.
    [7]
    Method according to any one of claims 4 to 6, characterized in that the oxides for staining glass are preferably selected from the group of oxides of iron, titanium, cerium, copper, chromium, cobalt, nickel, manganese, selenium, silver, indium, gold, vanadium, rare earth elements such as neodymium, praseodymium, samarium, erbium, europium, terbium, dysprosium, holmium, yttrium and mixtures thereof, preferably in an amount of 0.1 to 6% by weight, more preferably 0.5 to 5% by weight and most preferably 1 to 4% by weight.
    [8]
    Method according to any one of claims 1 to 7, characterized in that the additives are preferably selected from the group consisting of boron oxide, phosphorus oxide, fluorine, barium oxide, strontium oxide, oxide of magnesium, zinc oxide, calcium oxide, yttrium oxide, titanium oxide, niobium oxide, tantalum oxide, lanthanum oxide and mixtures thereof, preferably in an amount of 0.1 to 5% by weight.
    [9]
    Method according to any one of claims 1 to 8, characterized in that the process of removing the material is a subtractive process, preferably selected from the group consisting of milling, grinding and laser ablation, preferably as a process CAM.
    [10]
    10. Method according to any one of claims 1 to 9, characterized by the fact that before dental application, the dental restoration is subjected to a finishing process, preferably a polishing, use of enamel, waterproofing, a coating and a re-coating such as ceramic or enamel coating.
    [11]
    11. Dental ceramic glass, characterized by the fact that it is colored and translucent with a resistance of at least 250 MPa (measured according to DIN ISO 6872) which has the following composition: 55 to 70% by weight of S1O2, 15 to 22% by weight of UO2, 8 to 20% by weight of a stabilizer selected from the group consisting of ZrÜ2, Hf02 and their mixtures, 0 to 10% by weight of AI2O3, 0 to 10% by weight of K2O and / or Na2Ü and 0 to 20% by weight of additives.
    [12]
    12. Ceramic glass according to claim 11, characterized by the fact that it has the following composition: 55 to 64% by weight of S1O2, 17 to 20% by weight of UO2, 10 to 15% by weight of a selected stabilizer of the group consisting of Ζ1Ό2, ΗΙΌ2 and mixtures thereof, 0.1 to 8% by weight and more preferably 1 to 5% by weight of AI2O3, 0.1 to 5% by weight of K20 and / or Na2Ü, 0 to 8 % by weight, preferably 2 to 8% by weight of P2O5, and 0 to 20% by weight, preferably 0.1 to 10% by weight of additives.
    [13]
    13. Ceramic glass, according to claim 11 or 12, characterized by the fact that it has a dimensional stability that allows the processing of ceramic glass with a material removal process.
    [14]
    14. Dental restoration, characterized by the fact that it is reproducible by the method, as defined in any of claims 1 to 10.
    [15]
    15. Dental restoration according to claim 14, characterized by the fact that it has a degree of crystallization of at least 5%, preferably 50% and / or dental restoration that has a strength of at least 200 MPa, preferably at least 300 MPa (measured according to DIN ISO 6872).
    [16]
    16. Dental restoration according to claim 14 or 15, characterized by the fact that it has a finish, preferably polishing, glazing, waterproofing, coating and covering with a ceramic or enamel coating and the completed dental restoration has a hair resistance minus 250 MPa, preferably 300 MPa (measured according to DIN ISO 6872).
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    法律状态:
    2017-11-07| B15K| Others concerning applications: alteration of classification|Free format text: AS CLASSIFICACOES ANTERIORES ERAM: A61K 6/027 , C03B 32/02 , C03C 10/00 Ipc: A61K 6/00 (1980.01), A61K 6/02 (1980.01), C03B 32/ Ipc: A61K 6/00 (1980.01), A61K 6/02 (1980.01), C03B 32/ |
    2017-11-07| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|
    2018-04-10| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2018-05-15| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|
    优先权:
    申请号 | 申请日 | 专利标题
    US201161499815P| true| 2011-06-22|2011-06-22|
    EP11005102|2011-06-22|
    US61/499,815|2011-06-22|
    EP11005102.6|2011-06-22|
    PCT/EP2012/061582|WO2012175450A1|2011-06-22|2012-06-18|Dental restoration, method for production thereof and glass ceramic|
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