• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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    • 专利摘要:
    invention patent: "lithium disiloicate glass ceramic, method for its manufacture and use". the invention relates to glass ceramics based on the lithium disilicate system which can be easily processed in an intermediate crystallization stage and which after complete crystallization represent a chemically stable, highly resistant, highly translucent glass ceramic. the invention also relates to a method for making said glass ceramics. the glass ceramics according to the invention are used as dental material.
    公开号:BR112012015576B1
    申请号:R112012015576
    申请日:2010-12-23
    公开日:2020-04-22
    发明作者:Durschang Bernhard；Bibus Joachim；Probst Jorn；Vollmann Markus；Thiel Norbert；Schusser Udo
    申请人:Degudent Gmbh；Fraunhofer Ges Forschung；Vita Zahnfabrik H Rauter Gmbh & Co Kg；
    IPC主号:
    专利说明:

    (54) Title: LITHIUM DISSILICATE GLASS CERAMICS, ITS USE AND ITS MANUFACTURING METHOD, AND MOLDED DENTAL PRODUCT (51) Int.CI .: C03C 10/00; A61C 13/00; C03B 32/02; C04B 41/00.
    (30) Unionist Priority: 12/23/2009 DE 10 2009 060 274.7.
    (73) Holder (s): FRAUNHOFER-GESELLSCHAFT ZUR FOERDERUNG DER ANGEWANDTEN FORSCHUNG E.V .; VITA ZAHNFABRIK H. RAUTER GMBH & CO. KG; DEGUDENT GMBH.
    (72) Inventor (s): BERNHARD DURSCHANG; JORN PROBST; NORBERT THIEL; JOACHIM BIBUS; MARKUS VOLLMANN; UDO SCHUSSER.
    (86) PCT Application: PCT EP2010007918 of 12/23/2010 (87) PCT Publication: WO 2011/076422 of 06/30/2011 (85) Date of the Beginning of the National Phase: 06/25/2012 (57) Summary: Invention Patent: LITHIUM DISILOICATE GLASS CERAMICS, METHOD FOR ITS MANUFACTURE AND USE. The invention relates to glass ceramics based on the 1'thio disilicate system which can be easily processed in an intermediate crystallization stage and which after complete crystallization represent a chemically stable, highly resistant, highly translucent glass ceramic. The invention also relates to a method for making said glass ceramics. The glass ceramics according to the invention are used as dental material.
    1/7
    Descriptive Report of the Invention Patent for LITHIUM DISSILICATE GLASS CERAMICS, ITS USE AND ITS MANUFACTURING METHOD, AND MOLDED DENTAL PRODUCT.
    [001] The invention relates to glass ceramics based on the lithium disilicate system that are easily mechanically processable in an intermediate stage of crystallization and after complete crystallization represent a chemically stable, highly rigid and translucent glass ceramic. The invention also relates to a method of making these glass ceramics.
    [002] Glass ceramics can be used as dental material.
    [003] Lithium disilicate glass ceramics are well known in the specialized literature and several patents are based on this glass ceramic system. Thus, for example, EP-B-536 479 describes self-glazed lithium disilicate glass ceramic objects for the manufacture of tableware, in EP-B-536 572 lithium disilicate glass ceramics that can be used by dispersing a fine-particle pigmented glass over its surface as a coating element for civil construction purposes.
    [004] A key point of the patented lithium disilicate glass ceramics lies in dental applications. This is because the crystallization of lithium disilicate crystals is done through a minimum stability phase (lithium metasilicate) and the material system is accessible, among others, through the Chairside method (see SD Stookey: Chemical achining of Photosensitive Glass, Ind Eng. Chem., 45, S. 115-118 (1993) and SD Stookey: Photosensitively Opacifiable Glass US-A-2,684,911 (1954)). Borom's research, z.B. M.P. Borom, A.M. Turkalo, R.H. Doremus: Strength and Microstructure in Lithium Disilicate Glass-Ceramics, J. Am. Ceream. Soc, 58, Nr. 910, S. 385-391 (1975) and M.-P. Borom, A.M. Turkalo, R.H.Doremus:
    Petition 870190095511, of 24/09/2019, p. 4/19
    2/7
    Verfahren zum Herstellen von Glaskeramiken DE-A-24 51 121 (1974) show that glass ceramics, which contains lithium metasilicate as the main phase, have a reduced stability compared to glass ceramics, which contains lithium disilicate as the only crystalline phase.
    [005] This principle was explored in order to manufacture, in a biphasic crystallization process, first a glass ceramic that could be easily processed mechanically, for example by means of the CAD / CAM method, and then to process it in a second stage of crystallization to form dental glass ceramic. This method is suitable to be able to employ dental restorations according to the chair-side method mentioned above. In the case of this method, in the private dental practice, a ceramic glass block is milled after the first crystallization stage by means of CAD / CAM, an individually adapted crown / Onlay / Inlay is submitted to a special oven of the second crystallization stage. and inserted into the patient directly at the first and only visit to the dentist (DE 10 2005 028 637).
    [006] In addition, WO-A-95/32678 and US-A-5, 507, 981 describe lithium disilicate glass ceramics, which can be processed by applying a special crucible pressable by hot pressing forming molded dental products. In addition, DE-C-14 21 886 glass ceramics based on SiO2 and Li2O are known, which contain large amounts of very critical physiologically arsenic oxide. Also in US-A-4, 515, 634 and FR-A-2 655 264 are disclosed for the manufacture of appropriate dental crowns and ceramic lithium disilicate glass dental bridges.
    [007] All known lithium disilicate glass ceramics exhibit deficiencies in their processing in relation to molded products and / or mechanical or optical properties and / or stability
    Petition 870190095511, of 24/09/2019, p. 5/19
    3/7 mechanics. Especially when used in the dental field, equally high requirements must be met for all these properties.
    [008] Based on this, it is the task of the present invention to prepare a glass ceramic, which has improved mechanical and optical properties as well as an improved chemical stability in relation to the (glass) ceramics known in the prior art.
    [009] This task is solved through the lithium disilicate glass ceramic with the characteristics of claim 1, as well as through the method for manufacturing that glass ceramic with the characteristics of claim 9. In claim 12, applications are indicated according to with the invention. A molded dental product with the characteristics of claim 13 is also prepared. The remaining dependent claims show advantageous improvements.
    [0010] Within the scope of the present invention glass compositions have been developed, which can be represented in a two-phase manufacturing process, after the first crystallization stage they can be easily processed by means of CAD / CAM and after a very short second crystallization stage they are both highly transparent and highly resistant and also have better chemical stability than the known lithium disilicate glass ceramics.
    [0011] Surprisingly, it has been found that the addition of ZrO2 to certain glass compositions produces glass ceramics that can be very easily processed in an intermediate stage of crystallization and have excellent strength values in the final state, extraordinary translucency and quite chemical stability elevated.
    [0012] It has been found that it is possible to incorporate up to 20% by weight of a stabilizer selected from the group consisting of ZrO2, HfO2 or
    Petition 870190095511, of 24/09/2019, p. 6/19
    4/7 mixtures of these in the glass without the structure being significantly influenced. Contrary to all expectations, the stabilizer in this case is not removed by crystallization as the crystal phase itself, but remains in the remaining glass phase. Through the high percentage in the amorphous phase, in this phase the mechanical and chemical stability improve a lot, which also produces improved properties in the final product.
    [0013] Especially, the chemical stability can be improved through the composition of the remaining glass phase, since the glass phase has a much higher solubility than that of lithium disilicate and, therefore, represents the weak point in relation to chemical attack. The extremely high solubility of the stabilizer (ZrO2) in the glass phase is especially noticeable, since for example zirconium oxide in the case of many silicate glass ceramics acts as a nucleating agent, that is, in the case of a heat treatment it is removed by crystallization as the first phase and in these ZrO2 crystals, the crystal phase properly loosens and separates into a fine crystal.
    [0014] Through the high percentages of the stabilizer, which basically remain in the amorphous phase, the crystalline percentage is correspondingly limited. In this way, and due to the small crystallite size of the lithium disilicate crystals, a good translucency of the materials is formed after the second crystallization. However, translucency is further improved by the fact that the refractive index of the gas phase in turn is increased by the stabilizer and thus adapts to the refractive index of lithium disilicate. In the case of glass ceramics, in which the refractive index of the amorphous matrix phase is consistent with the refractive index of the crystalline phase (s), there are very good translucency properties, relatively independent of the crystallite size. In glass ceramics according to the invention, all three points for the generation of
    Petition 870190095511, of 24/09/2019, p. 7/19
    5/7 a glass of maximum translucency glass:
    - limited percentage of crystalline phase,
    - small crystals (<500 nm),
    - adjusted refractive index of amorphous and crystalline phase.
    [0015] The high percentage of the stabilizer acts on the glass ceramic also in
    - improved chemical stability,
    - higher resistance values and
    - with an improved translucency forming corresponding glass ceramic materials without or with a minimum percentage of ZrO2- or HfO2.
    [0016] The glass ceramics according to the invention can preferably be manufactured using a method in which [0017] a starting glass is made, which contains components of the glass ceramic, [0018] the starting glass is subjected to a first heat treatment at a first temperature, to manufacture a glass ceramic, which presents lithium metasilicate as a single or main crystal phase and [0019] this glass ceramic is subjected to a second heat treatment, in which the metasilicate of lithium with SiO2 from the glass phase is converted into lithium disilicate and then lithium dislicate is present as the single or main crystal phase.
    [0020] Crystallization from lithium metasilicate is preferably carried out at temperatures between 620 ° C and 800 ° C, with times between 1 and 200 minutes, preferably between 650 ° C and 750 ° C for 10 to 60 minutes.
    [0021] Crystallization from lithium disilicate is preferably carried out at temperatures between 800 ° C and 1040 ° C, with times of 5 to 200 minutes, preferably between 800 ° C and 870 ° C for 5 to 30
    Petition 870190095511, of 24/09/2019, p. 8/19
    6/7 minutes.
    [0022] Based on the following examples, the object according to the invention will be clarified in more detail without it being intended to be restricted to the special embodiments shown here. Examples 1 to 6 [0023] In examples 1 to 6, glass compositions containing superior zirconium oxide are presented, which are converted through a biphasic heat treatment into first easily mechanically processable lithium metasilicate glass ceramics and then into ceramics of highly translucent, highly resistant and chemically stable lithium disilicate glass.
    [0024] The compositions with their components are shown in table 1.
    Table 1
    Bl B2 B3 B4 B5 B6 SiO2 66, 9 65, 8 65, 5 63.7 63.5 63.5 Li2O 13, 9 13, 7 13, 6 13.2 14.4 12, 9 ZrO2 10.0 10.0 12, 0 11.7 12, 7 13, 5 Al2O3 3.2 3.1 3.1 3.0 3.3 3, 5 P2O5 3.0 3.0 3.0 2.9 3.1 3.4 K2O 2.9 2.9 2.9 2.8 3.0 3.2 CeO2 - 1.0 - 2.0 - - Er2O3 - 0.2 - 0.3 - - Tb2O3 - 0.3 - 0.3 - -
    [0025] The glasses were melted at 1500 ° C and in metallic forms forming blocks. The blocks were relaxed at 560 ° C in the oven and slowly cooled. For the different characterization methods, the glass blocks were fractionated and submitted to a first crystallization treatment. In this case, the glasses were stored for 10 to 120 minutes under 600 ° C to 750 ° C. In this way, the ceramics of
    Petition 870190095511, of 24/09/2019, p. 9/19
    7/7 glass were manufactured with strength values from 150 MPa to 220 MPa. As a crystal phase, only lithium metasilicate was found. In this state, processing using CAD / CAM methods is perfectly possible.
    [0026] With a second short crystallization at 800 ° C to 950 ° C for 3 to 15 minutes, recrystallization of the lithium metasilicate with SiO2 from the glass phase forming lithium disilicate and an increase in strength of 300 MPa at 450 MPa. In addition to the lithium disilicate phase, there may also be a secondary crystal phase containing zirconium oxide. In addition, minimal residues of lithium metasilicate may also be present. The main unambiguous crystal phase is lithium disilicate.
    [0027] Table 2 shows the crystallization conditions of individual glasses as well as the crystal phases that are formed and resistance values.
    Table 2
    Glass B1 B2 B3 B4 B5 B6 1. Crystallization 650 ° C 700 ° C 650 ° C 700 ° C 700 ° C 700 ° C 20 min 40 min 30 min 20 min 40 min 40 min 2. Crystallization 850 ° C 830 ° C 870 ° C 850 ° C 820 ° C 830 ° C 10 min 10 min 20 min 8 min 10 min 10 min Crystal phases- Main Stage(> 80%) Disilicate Disilicate Disilicate Disilicate Disilicate Disilicate - Secondary Phase - - - - Metasilicate Metasilicate (<20%) Translucency great very good Great very good Great Great 3. Resistance to flexion refraction at 3 points 375 MPa 413 MPa 380 MPa 418 MPa 356 MPa 385 MPa
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    权利要求:
    Claims (10)
    [1]
    1. Lithium disilicate glass ceramics, characterized by the fact that it has the following composition:
    55 to 70% by weight of SiO2,
    10 to 15% by weight of LiO2,
    10 to 20% by weight of the stabilizer selected from the group consisting of ZrO2, HfO2, or mixtures thereof,
    0.1 to 5% by weight of K2O,
    0.1 to 5% by weight of ALO3,
    0 to 10% by weight of additives selected from the group consisting of boron oxide, phosphorus oxide, fluorine, sodium oxide, barium oxide, strontium oxide, magnesium oxide, zinc oxide, calcium oxide, yttrium oxide , titanium oxide, niobium oxide, tantalum oxide, marsh oxide and mixtures thereof, and
    0 to 10% by weight of dyes.
    [2]
    2. Lithium disilicate glass ceramics, according to claim 1, characterized by the fact that the dyes are oxide dyes for glass and / or pigments.
    [3]
    3. Lithium disilicate glass ceramics according to claim 1 or 2, characterized by the fact that the glass coloring oxides are selected from the group of iron, titanium, cerium, copper, chromium, cobalt, nickel oxides, manganese, selenium, silver, indium, rare gold earth metals, especially neodymium, praseodymium, samarium and europium.
    [4]
    4. Lithium disilicate glass ceramics according to any one of claims 1 to 3, characterized in that the pigments are doped spinel.
    [5]
    5. Lithium disilicate glass ceramic, according to any one of claims 1 to 4, characterized by the fact that it has the following composition:
    Petition 870190095511, of 24/09/2019, p. 11/19
    2/3
    58 to 64% by weight of SiO2,
    11 to 13% by weight of LIO2,
    10 to 15% by weight of the stabilizer selected from the group consisting of ZrO2, HfO2, or mixtures thereof,
    2 to 5% by weight of K2O,
    2 to 5% by weight of ALO3,
    2 to 5% by weight of P2O5,
    0 to 5% by weight of additives selected from the group consisting of boron oxide, phosphorus oxide, fluorine, sodium oxide, barium oxide, strontium oxide, magnesium oxide, zinc oxide, calcium oxide, yttrium oxide titanium oxide, niobium oxide, tantalum oxide, marsh oxide and mixtures thereof, and
    0 to 10% by weight of dyes.
    [6]
    6. Method for the manufacture of a lithium disilicate glass ceramic, as defined in any one of claims 1 to 5, characterized by the fact that:
    (a) a starting glass is made, which comprises the components of the glass ceramic, (b) the starting glass is subjected to a first heat treatment to manufacture a glass ceramic that has lithium metasilicate as the main crystalline phase, and (c) the glass ceramic of (b) is subjected to a second heat treatment, in which the lithium metasilicate is converted into lithium disilicate with SiO2 from the glass phase, and the lithium disilicate is then present as main crystalline phase.
    [7]
    7. Method according to claim 6, characterized by the fact that the first heat treatment is carried out at a temperature of 620 ° C to 800 ° C for a period of 1 to 200 minutes, especially from 650 ° C to 750 ° C, for a period of 10 to 60 minutes.
    [8]
    8. Method according to claim 6 or 7, characterized
    Petition 870190095511, of 24/09/2019, p. 12/19
    3/3 due to the fact that the second heat treatment is carried out at a temperature of 800 ° C to 1040 ° C for a period of 5 to 200 min, especially from 650 ° C to 750 ° C, for a period of 5 30 minutes.
    [9]
    9. Use of lithium disilicate glass ceramics, as defined in any one of claims 1 to 5, characterized by the fact that it is as a dental material or as a component of a dental material.
    [10]
    10. Molded dental product, characterized by the fact that it comprises a lithium disilicate glass ceramic, as defined in any one of claims 1 to 5, especially in the form of an Inlay, an Onlay, a bridge, a structure pin, varnish and crown lining (partial).
    Petition 870190095511, of 24/09/2019, p. 13/19
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    法律状态:
    2018-06-12| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2018-12-11| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|
    2019-08-27| B06A| Notification to applicant to reply to the report for non-patentability or inadequacy of the application [chapter 6.1 patent gazette]|
    2020-02-27| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-04-22| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 23/12/2010, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
    申请号 | 申请日 | 专利标题
    DE102009060274A|DE102009060274A1|2009-12-23|2009-12-23|Lithium disilicate glass-ceramic, process for their preparation and their use|
    DE102009060274.7|2009-12-23|
    PCT/EP2010/007918|WO2011076422A1|2009-12-23|2010-12-23|Lithium disilicate glass ceramics, method for the production thereof and use thereof|
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