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    • 专利摘要:
    abstract patent of invention: "dental restoration, method for its production and ingot". the present invention relates to a method for producing a dental restoration comprising lithium silicate glass or glass ceramics, as well as a dental restoration itself. the invention also relates to an ingot with the same composition that has a defined resistance.
    公开号:BR112013032786B1
    申请号:R112013032786
    申请日:2012-06-21
    公开日:2018-05-08
    发明作者:Durschang Bernhard；Probst Jörn；Vollmann Markus；Gödiker Michael；Hackner Michael；Thiel Norbert；Schusser Udo
    申请人:Degudent Gmbh；Vita Zahnfabrik H Rauter Gmbh & Co Kg；
    IPC主号:
    专利说明:

    (54) Title: DENTAL RESTORATION, AND METHOD FOR ITS PRODUCTION (51) Int.CI .: A61K 6/027; C03B 32/02; C03C 10/00 (30) Unionist Priority: 06/22/2011 US 61 / 499,843, 06/22/2011 EP 11005104.2 (73) Holder (s): VITA ZAHNFABRIK H. RAUTER GMBH & CO. KG. DEGUDENT GMBH (72) Inventor (s): BERNHARD DURSCHANG; JÕRN PROBST; NORBERT THIEL; MICHAEL GÓDIKER; MARKUS VOLLMANN; UDO SCHUSSER; MICHAEL HACKNER
    1/23
    Descriptive Report of the Invention Patent for DENTAL RESTORATION, AND METHOD FOR ITS PRODUCTION.
    [001] The present invention relates to a method for the production of a dental restoration comprising a lithium silicate glass or glass ceramic, as well as a dental restoration itself. The invention also relates to an ingot with the same composition that has a defined resistance.
    [002] In the lithium oxide and silicon dioxide system, lithium disilicate glass ceramics (Li 2 O '2 SiO 2 (Li 2 Si 2 O 5 )) are well known in the literature and several patents use this glass ceramic system as a base. In EP 0 536 479 B1, self-glazing lithium disilicate glass ceramic objects are thus described for the production of tableware and, in EP 0 536 572 B1, lithium disilicate glass ceramics that can be used by dispersing a colored glass of fine particles on the surface of them as coating elements for construction purposes.
    [003] The main focus of publications on lithium disilicate glass ceramics lies in dental applications. The lithium disilicate system is very suitable here for the production of processable CAD / CAM glass ceramics since crystallization is done here through the lithium metasilicate phase (see SD Stookey: Chemical Machining of Photosensitive Glass, Ind. Eng. Chem., 45, 115 to 118 (1993) and SD Stookey: Photosensitively Opacifiable Glass US-A-2 684 911 (1954)).
    [004] These lithium metasilicate glass ceramics have such low resistance at this intermediate stage that they can be easily processed using CAD / CAM (M.-P. Borom, AM Turkalo, RH Doremus: 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.
    Petition 870180011081, of 02/09/2018, p. 10/40
    2/23 [005] This principle is exploited in order to produce, first, a glass ceramic, in a two-phase crystallization process, whose glass ceramic can be readily processed mechanically, for example, by means of CAD / CAM processes and, in order to process this later, in a second crystallization step, form the dental glass ceramic. This method is suitable in order to be able to use dental restorations according to the so-called side chair method. In this method, an individually adapted crown / implant / obturation is ground from a glass ceramic block, after the first crystallization phase by means of CAD / CAM, in dental practice, they are sub-injected for the second phase of crystallization. crystallization in a special muffle, and used directly on the first and only visit to the dentist by the patient (DE 10 2005 028 637).
    [006] In a first stage, a glass ceramic is produced, which is machined with CAM. After the ceramic glass is machined, it is finally crystallized, resulting in a highly resistant material. Pre-crystallization to a glass ceramic that is machined by CAM is necessary, for three reasons.
    [007] In the first, the starting glasses are not directly machined by CAM since in the homogeneous amorphous system, flaking and ruptures can occur due to the widening of the fracture. Second, the final crystallization needs to be carried out in a very short period, which can only be guaranteed by pre-crystallization. Third, by using the glasses, the necessary precision during the final crystallization cannot be achieved.
    [008] Thereafter, it was the aim of the present invention to provide glass ceramics that have improved strength values and also improved translucency and chemical resistance.
    [009] This objective is achieved through the method for production 870180011081, of 02/09/2018, p. 11/40
    A dental restoration having the characteristics of claim 1, the ingot which has the characteristics of claim 12 and the dental restoration according to claim 14. The other dependent claims reveal the advantageous embodiments.
    [0010] Within the scope of the present invention, glass compositions were developed in the basic system of SiO 2 -Li 2 O-ZrO 2 , which have lithium metasilicate as the only or main crystalline phase (> 50%).
    [0011] It has been surprisingly revealed that the use of specific compositions of lithium metasilicate allows direct machining with common CAD / CAM systems without flaking and breakage. In addition, these glasses can be transformed within an extremely short period of time for glass ceramics with a very high resistance. An additional advantage is that the glass ceramics of the invention have very good contour accuracy.
    [0012] According to the invention, a complete step in the process that consumes time and cost can be ignored during the production of a dental restoration, without having any unwanted impact on the other properties of the materials.
    [0013] The method of the invention does not need a muffle, so the purchase and maintenance costs can be reduced. In addition, the process time can be reduced by up to 2 hours.
    [0014] An additional advantage of the present invention refers to the fact that dental restorations can not only be produced by CAM, but also by pressing or molding green bodies in molds. The inventive process allows to directly press the glass, without a previous heat treatment that is used in the prior art. In addition, it is not necessary to modify the composition to
    Petition 870180011081, of 02/09/2018, p. 12/40
    4/23 can be used for different methods to produce dental restorations.
    [0015] The high translucency is guaranteed by the small size of the crystallite in glass ceramics. In addition, good chemical stability is guaranteed by the high proportion of zirconium oxide in the glass phase.
    [0016] According to the present invention, a method for producing a dental restoration comprising a lithium silicate glass or glass ceramic is provided with the following steps:
    [0017] a) an amorphous glass with the composition [0018] 50 to 70% by weight of SiO 2 ;
    [0019] 10 to 25% by weight of Li 2 O;
    [0020] 8 to 20% by weight of a stabilizer selected from the group consisting of oxides of Zr, Hf, Ge, La, Y, Ce, Ti, Zn or mixtures thereof;
    [0021] 0 to 10% by weight of AI 2 O 3 ;
    [0022] 0 to 10% by weight of K 2 O and / or Na 2 O; and [0023] 0 to 20% by weight of additives;
    [0024] is provided as an ingot; and [0025] b) the ingot is transformed into a dental restoration by at least one transformation process, in which during at least one transformation process, at least partial crystallization occurs due to the increase in temperatures.
    [0026] The temperature increase is at least 50 ° C, preferably at least 300Ό above the glass transformation temperature, that is, in general, at least 800Ό.
    [0027] In a preferred embodiment, amorphous glass has the following composition:
    [0028] 50 to 70% by weight of SiO 2 ;
    Petition 870180011081, of 02/09/2018, p. 13/40
    5/23 [0029] 10 to 25% by weight of Li 2 O;
    [0030] 8 to 20% by weight of a stabilizer from a group selected from ZrO 2 , HfO 2 , or mixtures thereof;
    [0031] 0 to 10% by weight of AI 2 O 3 ;
    [0032] 0 to 10% by weight of K 2 O and / or Na 2 O; and [0033] 0 to 20% by weight of additives.
    [0034] In an additional preferred mode, amorphous glass has the following composition:
    [0035] 55 and 64% by weight of SiO 2 ;
    [0036] 15 to 22% by weight of Li 2 O;
    [0037] 8 to 20% by weight of a stabilizer from a group selected from ZrO 2 , HfO 2 , or mixtures thereof;
    [0038] 0.1 to 8% by weight of AI 2 O 3 ;
    [0039] 0 to 8% by weight of K 2 O and / or Na 2 O; and [0040] 0 to 10% by weight of additives.
    [0041] More preferably, amorphous glass has the following composition:
    [0042] 55 to 64% by weight of SiO 2 ;
    [0043] 17 to 20% by weight of Li 2 O;
    [0044] 8 to 20% by weight of a stabilizer from a group selected from ZrO 2 , HfO 2 , or mixtures thereof;
    [0045] 0.1 to 5% by weight of AI 2 O 3 ;
    [0046] 0.1 to 5% by weight of K 2 O and / or Na 2 O;
    [0047] 2 to 8% by weight of P 2 O 5 ; and [0048] 0 to 10% by weight of additives.
    [0049] Preferably, during the transformation process, thermal energy is transported to the ingot, preferably by heating the ingot at temperatures between 850 ° C and 1,100X3. This heat treatment is preferably carried out over a period of 10 to 120 minutes.
    Petition 870180011081, of 02/09/2018, p. 14/40
    6/23 [0050] Pse states that in an additional step c) subsequent to the transformation process, the dental restoration is subjected to a second heat treatment with temperatures from 850 ° C to 1100Ό. [0051] The stabilizer is preferably ZrO 2 and / or HfO 2 . Preferably, the stabilizer is essentially present in an amorphous state.
    [0052] The components selected from the group consisting of nucleating agents, fluorescent agents, dyes, in particular oxides of glass dyes, colored pigments and mixtures thereof, may be contained as additives in glass or ceramic. of glass.
    [0053] The nucleating agents are preferably selected from the group consisting of phosphorus oxide, titanium oxide, tin oxide, mixtures thereof, and noble metals, preferably in an amount of 1 to 10% by weight, more preferably 2 to 8% by weight and more preferably, 4 to 8% by weight.
    [0054] Fluorescent agents are preferably selected from the group consisting of strontium oxides, bismuth, rare earth elements such as neodymium, praseodymium, samarium, erbium, europium and mixtures thereof, preferably in an amount of 0.1 to 5% by weight, more preferably 0.5 to 4% by weight and, more preferably, 1 to 3% by weight.
    [0055] Glass-colored oxides are preferably selected from the group of iron oxides, titanium, cerium, copper, chromium, cobalt, nickel, manganese, selenium, silver, indium, gold, vanadium. rare earths such as neodymium, praseodymium, samarium, europium, terbium, dysprosium, holmium, erbium, yttrium, and mixtures thereof, preferably in an amount of 0.1 to 6% by weight, more preferably 0.5 to 5% by weight and, more preferably, 1 to
    Petition 870180011081, of 02/09/2018, p. 15/40
    7/23
    4% by weight.
    [0056] The colored pigments can be doped spinel, which are preferably constituted in an amount of 0.1 to 6% by weight, more preferably, 0.5 to 5% by weight and, more preferably, 1 to 4% by weight.
    [0057] Other additives are preferably selected from the group consisting of boron oxide, phosphorus oxide, fluorine, sodium oxide, barium oxide, strontium, magnesium oxide, zinc oxide, calcium oxide, yttrium oxide, titanium oxide, niobium oxide, tantalum oxide, lanthanum oxide and mixtures thereof, which are preferably constituted in an amount of 0.1 to 5% by weight.
    [0058] The transformation process is preferably a lost wax process, for example, a molding, casting, pressing or combinations thereof.
    [0059] In another preferred modality, the dental restoration is submitted to a finishing process before the dental application. Such a finishing process can be a polishing, glazing, sealing, coating and capping with a ceramic cap or enamel.
    [0060] Dental restoration is preferably an internal inlay, an external inlay, a bridge, a pillar, a face, a varnish, a veneer, a crown, a partial crown, a frame or a copy.
    [0061] According to the present invention, also of an ingot, that is, a pressed pellet, with the following composition is provided: [0062] 55 to 70% by weight of SiO 2 ;
    [0063] 10 to 25% by weight of Li 2 O;
    [0064] 8 to 20% by weight of a stabilizer selected from the group consisting of oxides of Zr, Hf, Ge, La, Y, Ce, Ti, Zn or mixtures thereof;
    Petition 870180011081, of 02/09/2018, p. 16/40
    8/23 [0065] 0 to 10% by weight of AI 2 O 3 ;
    [0066] 0 to 10% by weight of K 2 O and / or Na 2 O; and [0067] 0 to 20% by weight of additives.
    [0068] Preferably, the ingot has the following composition:
    [0069] 50 to 70% by weight of SiO 2 ;
    [0070] 10 to 25% by weight of Li 2 O;
    [0071] 8 to 20% by weight of a stabilizer from a selected group of ZrO 2 , HfO 2 , or mixtures thereof;
    [0072] 0 to 10% by weight of AI 2 O 3 ;
    [0073] 0 to 10% by weight of K 2 O and / or Na 2 O; and [0074] 0 to 20% by weight of additives.
    [0075] More preferably, the ingot has the following composition:
    [0076] 55 to 64% by weight of SiO 2 ;
    [0077] 15 to 22% by weight of Li 2 O;
    [0078] 8 to 20% by weight of a stabilizer from a group selected from ZrO 2 , HfO 2 , or mixtures thereof;
    [0079] 0.1 to 8% by weight of AI 2 O 3 ;
    [0080] 0 to 8% by weight of K 2 O and / or Na 2 O and [0081] 0 to 10% by weight of additives.
    [0082] In an additional preferred mode, the ingot has the following composition:
    [0083] 55 to 64% by weight of SiO 2 ;
    [0084] 17 to 20% by weight of Li 2 O;
    [0085] 8 to 20% by weight of a stabilizer from a selected group of ZrO 2 , HfO 2 , or mixtures thereof;
    [0086] 0.1 to 5% by weight of AI 2 O 3 ;
    [0087] 0.1 to 5% by weight of K 2 O and / or Na 2 O;
    [0088] 2 to 8% by weight of P 2 O 5 ; and [0089] 0 to 10% by weight of additives.
    Petition 870180011081, of 02/09/2018, p. 17/40
    9/23 [0090] According to the present invention, in addition, a dental restoration is provided, which can be produced by the method described above.
    [0091] It is preferable that the dental restoration has a degree of crystallization of at least 5%, preferably at least 50%. [0092] It is also preferred that the dental restoration has a strength of at least 200 MPa, preferably 250 MPa (measured according to DIN ISO 6872).
    [0093] Dental restoration can have a finish. Such a finish is preferably a polish, a glass, a seal, a coating and a cap with a ceramic cap or enamel. This finished dental restoration preferably has a strength of at least 250 MPa, preferably 300 MPa (measured according to DIN ISO 6872).
    [0094] Dental restorations, with the following compositions, are the additional aspects of the present invention:
    Composition 1
    SÍO 2 50 to 75% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight AI 2 O 3 0 to 8% by weight K 2 O 0 to 8% by weight additions 0 to 15% by weight
    Composition 2
    SiO 2 50 to 64% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight AI 2 O 3 0 to 8% by weight K 2 O 0 to 8% by weight additions 0 to 15% by weight
    Petition 870180011081, of 02/09/2018, p. 18/40
    10/23
    Composition 3
    SiO2 55 to 60% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight AI2O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Composition 4
    SiO2 50 to 75% by weight Li2O 15 to 22% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Composition 5
    SiO2 50 to 75% by weight Li2O 17 to 20% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Composition 6
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Petition 870180011081, of 02/09/2018, p. 19/40
    11/23
    Composition 7
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 10 to 15% by weight AI2O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Composition 8
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0.1 to 5% by weight K2O 0 to 8% by weight Additions 0 to 15% by weight
    Composition 9
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 1 to 3% by weight K2O 0 to 8% by weight additions 0 to 15% by weight
    Composition 10
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0.1 to 5% by weight Additions 0 to 15% by weight
    Petition 870180011081, of 02/09/2018, p. 20/40
    12/23
    Composition 11
    SI2 50 to 75% by weight LI2 10 to 25% by weight ZrO2 8 to 20% by weight AI2O3 0 to 8% by weight K2O 1 to 3% by weight Additions 0 to 15% by weight
    Composition 12
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 1 to 10% by weight
    Composition 13
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight additions 2 to 8% by weight
    Composition 14
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 4 to 6% by weight
    Petition 870180011081, of 02/09/2018, p. 21/40
    13/23
    Composition 15
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight P2O5 1 to 10% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 16
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight P2O5 2 to 8% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 7% by weight
    Composition 17
    SiO2 50 to 75% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight P2O5 4 to 6% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight additions 0 to 9% by weight
    Composition 18
    SiO2 55 to 64% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight P2O5 1 to 10% by weight Al2O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Petition 870180011081, of 02/09/2018, p. 22/40
    14/23
    Composition 19
    SI2 55 to 64% by weight LI2 15 to 22% by weight ZrO2 8 to 20% by weight P2O5 1 to 10% by weight AI2O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 20
    SiO2 55 to 64% by weight Li2O 17 to 20% by weight ZrO2 8 to 20% by weight P2O5 1 to 10% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 21
    SiO2 55 to 64% by weight Li2O 10 to 25% by weight ZrO2 8 to 20% by weight P2O5 1 to 10% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 22
    SiO2 55 to 64% by weight Li2O 10 to 25% by weight ZrO2 8 to 15% by weight P2O5 1 to 10% by weight A ^ O3 0 to 8% by weight K2O 0 to 8% by weight Additions 0 to 5% by weight
    Petition 870180011081, of 02/09/2018, p. 23/40
    15/23
    Composition 23
    SÍO 2 55 to 64% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight P2O5 1 to 10% by weight AI 2 O3 0.1 to 5% by weight K 2 O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 24
    SiO 2 55 to 64% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight P2O5 1 to 10% by weight AI 2 O3 1 to 3% by weight K 2 O 0 to 8% by weight Additions 0 to 5% by weight
    Composition 25
    SiO 2 55 to 64% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight P2O5 1 to 10% by weight AI 2 O3 0 to 8% by weight K 2 O 0.1 to 5% by weight Additions 0 to 5% by weight
    Composition 26
    SiO 2 55 to 64% by weight li 2 O 10 to 25% by weight ZrO 2 8 to 20% by weight P2O5 1 to 10% by weight AI 2 O3 0 to 8% by weight K 2 O 1 to 3% by weight Additions 0 to 5% by weight
    [0095] The objective according to the application is intended to be displayed 870180011081, of 02/09/2018, p. 24/40
    16/23 in more detail with reference to the figures and the following examples, without limiting the said subject to these variations.
    [0096] Figure 1 shows a scanning electron microscope (SEM) micrograph of a glass according to the present invention, after pre-crystallization;
    [0097] Figure 2 shows a scanning electron microscope (SEM) micrograph of a glass according to the present invention, after pressing at a temperature of 950Ό; and [0098] figure 3 shows a scanning electron microscope (SEM) micrograph of a glass according to the present invention, after pressing at a temperature of 970Ό.
    Example 1 [0099] In Table 1, the fixed compositions given by way of example for a different stabilizer are mentioned, from which the metasilicate glass ceramics containing the high stabilizers can be produced for the dental field.
    Table 1
    % by weight Sio 2 60.0 li 2 O 19.0 P2O5 6.0 AI2O3 2.0 K 2 O 2.0 CeO 2 1.0 SX Stabilizer * 10.0
    * SX represents the stabilizer compositions S1 to S5 (see table 2) [00100] Table 2 shows the stabilizers used by way of example for dental applications, with the composition of Table 1.
    Petition 870180011081, of 02/09/2018, p. 25/40
    17/23
    Table 2
    SX Stabilizers S1 Zirconium oxide: 10% S2 Germanium oxide: 10% S3 Lanthanum oxide: 10% S4 Yttrium oxide: 10% S5 Zirconium oxide: 6%Titanium oxide: 4%
    [00101] The glasses were melted at 1500Ό and poured into metal molds to form blocks. The blocks were relieved from the muffle strain at 560Ό and cooled slowly. For the various characterization processes, the glass blocks are divided and subjected to a first crystallization treatment. For this purpose, the cups were stored for 10 to 120 minutes at 600Ό to 750Ό. As a result, glass ceramics with strength values of 150 MPa and 220 MPa were produced. Exclusively lithium metasilicate was instituted as a crystalline phase. In this state, processing using CAD / CAM methods is very easy.
    [00102] In Table 3, the compositions that are given by way of example are mentioned, from which metasilicate glass ceramics containing zirconium oxide can be produced for the dental field.
    Table 3
    G1 ‘ G2 * G3 * G4 ‘ G5 ‘ G6 * SiO 2 63.5 63.5 59.0 59.0 63.5 63.5 li 2 O 12.9 13.9 18.0 19.0 12.9 12.9 ZrO 2 10.0 9.0 12.0 12.0 12.3 11.0 AI 2 O 3 4.7 5.1 4.5 4.5 3.9 4.4 P 2 O 5 4.5 4.5 3.5 3.5 3.7 4.2 K 2 O 4.4 4.0 3.0 2.0 3.6 4.0
    * (Data in% by weight)
    Petition 870180011081, of 02/09/2018, p. 26/40
    18/23 [00103] The glasses were melted at 1500Ό and poured into metal molds to form blocks. The blocks were relieved from the muffle strain at 560Ό and cooled slowly. For the various characterization processes, the glass blocks are divided and subjected to a first crystallization treatment. For this purpose, the cups were stored for 10 to 120 minutes at 600Ό to 750Ό. As a result, glass ceramics with strength values of 150 MPa and 220 MPa were produced. Exclusively lithium metasilicate was instituted as a crystalline phase. In this state, processing using CAD / CAM methods is very easy.
    Example 2 [00104] A dental restoration of the invention was produced according to the following process steps:
    [00105] 1. Fusion of components for homogeneous liquid glass [00106] 2. Molding of glass blocks [00107] 3. Strain relief within glass block [00108] 4. Optional: pre-crystallization of the glass block (process is not necessary for the result of high strength press) [00109] The glass blocks are placed in firing trays, for example, made from glass fibers. A heat treatment of 550 to 700Ό, the residence time from 0 to 60 min, the heating rate from 10 to 100 ° / min and the final temperature from 800 to 850Ό, the residence time from 8 to 30 min in an atmosphere .
    [00110] The microstructure shows a polycrystalline state with crystals <5 pm (see figure 1).
    [00111] The XRD analysis shows the phases of lithium silicate (Li 2 SiO 3 ) and lithium phosphate (Li 3 PO 4 ).
    [00112] 5. Modeling of the desired prosthesis in wax [00113] The modeling in complete anatomical wax of the prosthesis will be
    Petition 870180011081, of 02/09/2018, p. 27/40
    19/23 made of wax free burning residue. The minimum thickness of the wax modeling should not be less than 0.4 mm and should not exceed 2.0 mm on the occlusal side. The wax pieces will be added to the modeling with a length of 5 to 6 mm and a thickness of 3 to 4 mm. [00114] 6. Investment of wax modeling [00115] The investment mass will be agitated and poured free of bubbles in the muffle under the vibration where the wax modeling is fixed until the wax modeling is completely covered by the investment mass. After that, the muffle will be filled completely without the application of vibration. The muffle with the liquid investment mass will be stored to define the hardening process.
    [00116] 7. Muffle heating and burning of the wax modeling.
    [00117] After defining the investment mass, any of the auxiliary plastic parts will be removed and the surfaces (upper / lower) will be cleaned to obtain a flat surface.
    [00118] The muffle will be positioned in the preheating oven. The base temperature depends on the type of investment stock used. Using the Dentsply investment mass, the muffle can be positioned immediately after setting 15 minutes in the oven preheated to 850Ό.
    [00119] 8. Pressing the restoration [00120] The muffle will then be cooled for 15 minutes at 700Ό. The starting temperature of the pressing process is 600Ό. Pressed TW4 pellets with a high resistance are positioned in the muffle. A heated press rod produced from alumina or investment mass is now defined on the pressed pellets. The muffle with the pellets and the pressure rod will now be positioned immediately in the oven and a pressing program with the following parameters will be started: The preheating temperature from 600 to 850Ό, heating rate from 30 to
    Petition 870180011081, of 02/09/2018, p. 28/40
    20/23 100o / min, pressing temperature from 890 to 995 Ό, dwell time from 10 to 35min, pressing time from 1 to 20min. After the pressing is finished, the muffle will be removed from the oven and cooled to room temperature.
    [00121] After pressing, the polycrystalline structure can be seen in figure 2.
    [00122] Due to a variation in the pressing temperature, the size of the crystal can be changed. Pressing temperatures from 950Ό to 970Ό result in crystal sizes from 1,500nm to 3,000nm (median) (see figure 3).
    [00123] The 3-point flexural test in accordance with DIN EN ISO 6872: 2008 shows a flexural strength of 370 MPa, and the thermal expansion coefficient of 25 to 400Ό is 10.6 to 10.9 pm / mK, for 25 500Ό, 11.0 to 11.3 pm / mK and for 25 to 600Ό, 11.4 to 11.8 pm / mK.
    [00124] XRD shows the phases of lithium silicate (Li 2 SiO 3 ) and lithium phosphate (Li 3 PO 4 ). Different pressing temperatures do not show significantly different crystalline phases.
    [00125] 9. Elimination of the pressed restoration [00126] The investment mass will be removed by removal with glass beads with a diameter of 50 mm with a pressure of 200 to 400 KPa (2 to 4 bar) or removal with alumina sand (110pm diameter, 50 to 200 KPa (0.5 to 2 bar)).
    [00127] 10. Removal of the reaction layer from the pressed restoration [00128] Residues from the reaction layer are removed in an ultrasonic bath with a hydrofluoric acid containing 0 solvent for 30 min at 30Ό.
    [00129] 11. Cutting the waste from the restoration [00130] The waste will be cut with a refrigre diamond sawPetition 870180011081, of 02/09/2018, pg. 29/40
    21/23 water and clean. The surface to be coated or glazed will be removed with alumina sand with an average diameter of 110pm and a pressure of 50 to 150 KPa (0.5 to 1.5 bar).
    [00131] 12. Protection with enamel / stains and capping technique, respectively [00132] The pressed restoration will be aesthetically individualized or with enamel / stains using 2 to 3 firing cycles or will be finished with ceramic capping, with the use cutting technique.
    Example 3 [00133] A dental restoration of the invention was produced according to the following process steps:
    [00134] 1. Fusion of components for homogeneous liquid glass [00135] 2. Molding of glass blocks [00136] 3. Strain relief within glass block [00137] 4. Optional: pre-crystallization of the glass block (process is not necessary for the result of high strength press) [00138] 5. Modeling of the desired prosthesis in wax.
    [00139] The complete modeling of the prosthetic anatomical wax will be made of residue-free burning wax. The minimum thickness of the wax modeling should not be less than 0.4 mm and should not exceed 2.0 mm on the occlusal side. The wax pieces will be added to the modeling with a length of 5 to 6 mm and a thickness of 3 to 4 mm.
    [00140] 6. Investment of wax modeling [00141] The investment mass (plaster or phosphate base) will be agitated and poured free of bubbles in the muffle under the vibration where the wax modeling is fixed until the wax modeling is fully covered by the investment mass. After that, the muffle will be completely filled without the application of vibrations. The muffle
    Petition 870180011081, of 02/09/2018, p. 30/40
    22/23 with the net investment mass will be stored to define the hardening process.
    [00142] 7. Muffle heating and burning of the wax modeling.
    [00143] When using a plaster investment, the maximum temperature of around 700Ό needs to be considered.
    [00144] After setting the investment mass, any of the auxiliary plastic parts will be removed and the surfaces (upper / lower) will be cleaned to obtain a flat surface.
    [00145] The muffle will be positioned in the preheating oven. The base temperature depends on the type of investment stock used. Using the Dentsply investment mass, the muffle can be positioned immediately after setting 15 minutes in the oven preheated to 850Ό.
    [00146] 8. Casting the restoration [00147] The muffle will then be cooled for 15 minutes at 700Ό. For casting, a suitable casting machine will be used, for example, Prestomat from DeguDent. The TW4 blank or pellet produced as described above will be heated until reaching a temperature of 1150X3 and then it will be melted in the preheated muffle (700Ό). After the casting is completed, the muffle will be removed from the casting device and in a 660Ό preheat oven for 40 min for nucleation purposes. After that, either the muffle will be heated until it reaches the crystallization temperature (eg 850Ό, 5 min.), Or the muffle will be cooled to room temperature and the final crystallization takes place after being eliminated.
    [00148] Due to a variation of the nucleation and final crystallization temperature, the size of the crystal can be changed. Nucleation temperatures from 600Ό to 850Ό final crystallization from 750Ό to 850Ό resulting in crystal sizes from 1 OOnm to 3,000nm (median).
    Petition 870180011081, of 02/09/2018, p. 31/40
    23/23 [00149] The 3-point flexural test in accordance with DIN EN ISO 6872: 2008 shows a flexural strength of 370 MPa, and the thermal expansion coefficient of 25 to 400Ό is 10.6 to 10.9 pm / mK , for 25 500Ό, 11.0 to 11.3 pm / mK and for 25 to 600Ό, 11.4 to 11.8 pm / mK.
    [00150] XRD shows the phases of lithium silicate (Li 2 SiO 3 ) and lithium phosphate (Li 3 PO 4 ). Different pressing temperatures do not show significantly different crystalline phases.
    [00151] 9. Elimination of the molten restoration [00152] The investment mass will be removed by removing it with glass beads with a diameter of 50 mm with a pressure of 200 to 400 KPa (2 to 4 bar) or removing it with alumina sand (110pm diameter, 50 to 200 KPa (0.5 to 2 bar) or using 0 gypsum investment masses when dissolving in a water tank at room temperature.
    [00153] 10. Cutting the waste from the restoration [00154] The waste will be cut with a water-cooled and clean diamond saw. The surface to be coated or glazed will be removed with alumina sand with an average diameter of 110pm and a pressure of 50 to 150 KPa (0.5 to 1.5 bar). An advantage of casting is a significantly reduced reaction layer or no reaction layer at all. Therefore, the reproduction of precise surface details (for example, with thin margins) is superior, or especially if the plaster investment is used (easy to remove). [00155] 11. Protection with enamel / stains and capping technique, respectively [00156] The pressed restoration will be aesthetically individualized or with enamel / stains with the use of 2 to 3 firing cycles or will be finished with ceramic capping, with 0 use cutting technique.
    Petition 870180011081, of 02/09/2018, p. 32/40
    1/4
    权利要求:
    Claims (15)
    [1]
    1. Method for the production of a dental restoration, comprising a lithium silicate glass or glass ceramic, characterized by the fact that:
    (a) an amorphous glass with the composition
    50 to 70% by weight of SiO 2 ;
    17 to 25% by weight of Li 2 O;
    8 to 20% by weight of a stabilizer selected from the group consisting of ZrO 2 , HfO 2 , or mixtures thereof;
    0 to 10% by weight of AI 2 O 3 ;
    0 to 10% by weight of K 2 O and / or Na 2 O; and
    0 to 20% by weight of additives; it is supplied as an ingot; and (b) the ingot is transformed into a dental restoration by at least one transformation process, and during at least one transformation process, at least a partial crystallization occurs due to the increase in temperatures, and the said transformation process it is a lost wax process.
    [2]
    2. Method, according to claim 1, characterized by the fact that the amorphous glass has the following composition:
    55 to 64% by weight of SiO 2 ;
    17 to 22% by weight, preferably 17 to 20% by weight of
    Li 2 O;
    8 to 20% by weight, preferably 10 to 15% by weight of a stabilizer from a group selected from ZrO 2 , HfO 2 , or mixtures thereof;
    0 to 10% by weight, preferably 0.1 to 8% by weight and, more preferably, 1 to 5% by weight of AI 2 O 3 ;
    0 to 10% by weight, preferably 0.1 to 5% by weight of K 2 O and / or Na 2 O;
    Petition 870180011081, of 02/09/2018, p. 33/40
    2/4
    0 to 8% by weight of P 2 O 5 ; and
    0 to 20% by weight, preferably 0.1 to 10% by weight of additives.
    [3]
    3. Method according to claim 1 or 2, characterized by the fact that during the transformation process, thermal energy is transmitted to the ingot, preferably at temperatures of at least 800Ό, more preferably at temperatures of 850Ό to 1,100Ό, preferably, performed over a period of 10 to 120 min.
    [4]
    4. Method according to any one of claims 1 to 3, characterized by the fact that in an additional step (c), subsequent to the transformation process, the dental restoration is subjected to a thermal treatment with temperatures from 850Ό to 1100Ό .
    [5]
    Method according to any one of claims 1 to 4, characterized in that the additives are selected from the group consisting of nucleating agents, fluorescent agents, dyes, preferably glass-colored oxides and color pigments , and their mixtures.
    [6]
    6. Method according to claim 5, characterized by the fact that the nucleating agents are selected from the group consisting of phosphorus oxide, titanium oxide, tin oxide, and mixtures thereof, and metals noble, preferably in an amount of 1 to 10% by weight, more preferably 2 to 8% by weight and, more preferably, 4 to 8% by weight.
    [7]
    7. Method according to claim 5 or 6, characterized by the fact that fluorescent agents are selected from the group consisting of strontium oxides, bismuth, rare earth elements such as neodymium, praseodymium, samarium, europium, terbium, dysprosium, holmium, erbium, and their mixtures, prefectly 870180011081, of 02/09/2018, p. 34/40
    3/4 efficiency, in an amount of 0.1 to 5% by weight, more preferably 0.5 to 4% by weight and, more preferably, 1 to 3% by weight.
    [8]
    8. Method according to any one of claims 5 to 7, characterized in that the glass-colored oxides are selected from the group of oxides of iron, titanium, cerium, copper, chromium, cobalt, nickel, manganese, selenium , silver, indium, gold, vanadium, from rare earth elements such as neodymium, praseodymium, samarium, europium, terbium, dysprosium, holmium, erbium, yttrium, and mixtures thereof, preferably in an amount of 0.1 to 6% by weight, more preferably, 0.5 to 5% by weight and, more preferably, 1 to 4% by weight and / or the color pigments are doped spinels, which are constituted, preferably in an amount of 0 , 1 to 6% by weight, more preferably, 0.5 to 5% by weight and more preferably, 1 to 4% by weight.
    [9]
    Method according to any one of claims 1 to 8, characterized in that the additives are selected from the group consisting of boron oxide, fluorine, barium oxide, strontium oxide, magnesium oxide, 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.
    [10]
    Method according to any one of claims 1 to 9, characterized by the fact that the transformation process is a molding, casting, pressing or combinations thereof.
    [11]
    11. Method according to any one of claims 1 to 10, characterized by the fact that, prior to dental application, the dental restoration is subjected to a finishing process, preferably a polishing, a glazing, a sealing, a cladding and capping with a ceramic cap or a
    Petition 870180011081, of 02/09/2018, p. 35/40
    4/4 enamel.
    [12]
    12. Dental restoration, characterized by the fact that it is producible by the method, as defined in any of claims 1 to 11.
    [13]
    13. Dental restoration according to claim 12, characterized by the fact that it has a degree of crystallization of at least 5%, preferably 50% and / or the dental restoration has a strength of at least 200 MPa, preferably at least 250 MPa (measured according to DIN ISO 6872).
    [14]
    Dental restoration according to claim 12 or 13, characterized in that the dental restoration has a finish, preferably a polish, a glass, a seal, a coating, or a cap with a ceramic cap or enamel and the finished dental restoration has a resistance of at least 250 MPa, preferably 300 MPa (measured according to DIN ISO 6872).
    [15]
    15. Dental restoration according to any one of claims 12 to 14, characterized by the fact that it is an internal inlay, an external inlay, a bridge, a pillar, a face, a varnish, a veneer, a crown, a crown partial, frame or copy.
    Petition 870180011081, of 02/09/2018, p. 36/40
    1/3
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    法律状态:
    2017-11-21| B07A| Technical examination (opinion): publication of technical examination (opinion) [chapter 7.1 patent gazette]|
    2018-03-13| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2018-05-08| B16A| Patent or certificate of addition of invention granted|
    优先权:
    申请号 | 申请日 | 专利标题
    US201161499843P| true| 2011-06-22|2011-06-22|
    EP11005104|2011-06-22|
    PCT/EP2012/061971|WO2012175615A1|2011-06-22|2012-06-21|Dental restoration, method for its production and ingot|
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