WO2002047616A2 - Fully ceramic tooth replacement with a frame made of cer-stabilised zircon oxide - Google Patents

Fully ceramic tooth replacement with a frame made of cer-stabilised zircon oxide Download PDF

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Publication number
WO2002047616A2
WO2002047616A2 PCT/EP2001/014502 EP0114502W WO0247616A2 WO 2002047616 A2 WO2002047616 A2 WO 2002047616A2 EP 0114502 W EP0114502 W EP 0114502W WO 0247616 A2 WO0247616 A2 WO 0247616A2
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Prior art keywords
framework
zro
weight
proportion
infiltration
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PCT/EP2001/014502
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German (de)
French (fr)
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WO2002047616A3 (en
Inventor
Helga Hornberger
Norbert Thiel
Markus Vollmann
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Vita Zahnfabrik H. Rauter Gmbh & Co. Kg
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Priority to AU2002219170A priority Critical patent/AU2002219170A1/en
Publication of WO2002047616A2 publication Critical patent/WO2002047616A2/en
Publication of WO2002047616A3 publication Critical patent/WO2002047616A3/en

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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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/0007—Compositions for glass with special properties for biologically-compatible glass
    • C03C4/0021—Compositions for glass with special properties for biologically-compatible glass for dental use
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/70—Preparations for dentistry comprising inorganic additives
    • A61K6/78—Pigments
    • 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
    • A61K6/804—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising manganese 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
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/816—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising titanium 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
    • A61K6/802—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
    • A61K6/802—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics
    • A61K6/822—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising rare earth metal oxides
    • 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
    • A61K6/824—Preparations for artificial teeth, for filling teeth or for capping teeth comprising ceramics comprising transition metal oxides
    • 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
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/062—Glass compositions containing silica with less than 40% silica by weight
    • C03C3/064—Glass compositions containing silica with less than 40% silica by weight containing boron
    • C03C3/068—Glass compositions containing silica with less than 40% silica by weight containing boron containing rare earths
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
    • C04B41/5022—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials with vitreous materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
    • C04B41/81—Coating or impregnation
    • C04B41/85—Coating or impregnation with inorganic materials
    • C04B41/86—Glazes; Cold glazes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
    • C04B2111/00836—Uses not provided for elsewhere in C04B2111/00 for medical or dental applications

Definitions

  • the present invention relates to an all-ceramic dental prosthesis with a framework made of a cerium-stabilized zirconium oxide, a framework material which is composed of a cerium-stabilized zirconium oxide (Ce-Zr0 2 ), a method for producing a framework in the all-ceramic dental prosthesis according to the invention, and Use of cerium-stabilized ZrO 2 for the production of framework materials.
  • DE 44207180 AI also relates to glass ceramics with oxide ceramic components.
  • the oxide-ceramic zirconium-containing crystals are distributed as precipitates in a glass matrix.
  • the invention is based on the object To manufacture multi-unit posterior bridges with the highest possible reliability (ie high breaking strength Klc and high bending strength). With the previous all-ceramic processes, only a fracture toughness with K lc values of 3 - 6 is achieved. Due to the brittleness and the unfavorable fatigue behavior of ceramics, a material with the highest possible fracture toughness (Kic) and at the same time high bending strength is required for multi-unit posterior bridges.
  • Kic fracture toughness
  • an all-ceramic dental prosthesis with a framework which is based on a framework material made of a cerium-stabilized zirconium oxide (Ce-ZrO 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 O 3 ) is based on the proportion of ZrO 2 and an infiltration glass proportion in the framework of 0-40 vol% based on the volume of the framework as well as veneering ceramics matched to the framework material.
  • Scaffolding means that there is a continuous, porous oxide-ceramic network.
  • the all-ceramic dental prosthesis according to the invention preferably contains 5.5-16 mol% Ce0 2 in ZrO 2 .
  • the invention also relates to a framework material which is composed of a cerium-stabilized zirconium oxide (Ce-ZrO 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 O 3 ) based on the proportion of ZrO 2 .
  • the framework material according to the invention preferably contains 5.5-16 mol% CeO 2 in ZrO 2 .
  • the easy workability of the scaffold material before infiltration is advantageous.
  • the addition of Al 2 O 3 (aluminum oxide) ensures compatibility with existing veneering ceramics.
  • the method according to the invention for producing a framework in the all-ceramic dental prosthesis according to the invention assumes that the framework material according to the invention is shaped as a densely sintered material.
  • the framework material according to the invention is first sintered porously and then shaped.
  • porous all-ceramic frameworks produced via the intermediate stage by means of reaction bandages as opposed to a sintering process have the advantage of being easy to machine or manually modeling while maintaining the shape and a damage-free surface. These advantages lead to a high accuracy of fit and an improved flexural strength of the dentures produced from them.
  • the infiltration glass for infiltration of the porous framework according to the invention preferably contains 15 to 35% by weight of La 2 O 3 , 10 to 25% by weight of SiO 2 , 10 to 25% by weight of Al 2 O 3 , 5 to 20% by weight of B 2 O 3 , 5 - 20% by weight CaO, 0-10% by weight ZrO 2 , 0-10% by weight TiO 2 and 0-15% by weight CeO 2 .
  • the infiltration glass contains further metal oxides in an oxidation stage which can stabilize ZrO 2 .
  • metal oxides include in particular MgO and Y 2 O 3 .
  • the advantages of adding Mg, Ce, Y are the stabilization of the tetragonal phase at room temperature and thus a significant increase in the K lc value.
  • the absorption capacity of the glass of cerium oxide influences the tension between the glass and the matrix.
  • the infiltration glass can also contain pigments. By adding pigments you can go from the pure white color of the oxide in the direction of the natural tooth color.
  • the invention is based on the use of cerium-stabilized ZrO 2 for producing framework materials which can be used as restorations in the dental field.
  • SEM scanning electron microscopic
  • the images show the network of cerium-stabilized zirconium oxide (bright grains) that was infiltrated with a glass.
  • the links between the individual zirconium oxide grains are clearly visible, which together with the glass infiltration cause increased strength.
  • some bright crystallizations can be seen, which are rich in zirconium oxide and can lead to further solidification.
  • Ce-stab pure ZrO 2 (approx. 15.5% by weight CeO 2 ) was pressed and sintered at 1500 ° C.
  • the fracture toughness (K ⁇ c value) is> 11 MPam 1/2 .
  • the ZrO 2 used is cerium-stabilized with a proportion of 15.5% by weight CeO 2 .
  • the powder mixture is shaped and sintered at 1500 ° C.
  • the sample is infiltrated at 1140 ° C. with a lanthanum glass which has a CeO 2 content of less than 4% by weight and contains no further stabilizing oxides such as MgO, CaO, Y 2 O 3 etc.
  • the resulting bending tensile strength is 650 MPa.
  • the fracture toughness lies
  • a zirconia / alumina mixture with the composition 33% by weight of ZrO 2 and 67% by weight of Al 2 0 3 is produced.
  • This powder mixture is shaped and sintered at 1180 ° C.
  • the sample is infiltrated at 1140 ° C and lanthanum and has a bending strength of 580 MPa and a fracture toughness with a K ⁇ C value of 4.4 MPam 1/2.

Abstract

The invention relates to a fully ceramic tooth replacement with a frame made of a frame material which is constructed from cer-stabilised zircon oxide (Ce-ZrO2) with up to 25 wt. % aluminium oxide (Al2O3) in relation to the ZrO2 content and an infiltration glass content in the frame of 0-40 vol. % in relation to the volume of the frame, in addition to a facing ceramic which matches the frame material. The invention relates to the use of cer-stabilised ZrO2 for producing frame materials, which can be used in dental restoration.

Description

Vollkeramischer Zahnersatz mit einem Gerüst aus einem cer- stabilisierten Zirkonoxid All-ceramic dentures with a framework made of a stabilized zirconium oxide
Die vorliegende Erfindung betrifft einen vollkeramischen Zahnersatz mit einem Gerüst aus einem cer-stabilisierten Zirkonoxid, einem Gerüstmaterial, das aus einem Cer-stabilisierten Zirkonoxid (Ce-Zr02) aufgebaut ist, einem Verfahren zur Herstellung eines Gerüstes in dem erfindungsgemäßen vollkeramischen Zahnersatz, sowie der Verwendung von cer-stabilisiertem ZrO2 zur Herstellung von Gerüstmaterialien.The present invention relates to an all-ceramic dental prosthesis with a framework made of a cerium-stabilized zirconium oxide, a framework material which is composed of a cerium-stabilized zirconium oxide (Ce-Zr0 2 ), a method for producing a framework in the all-ceramic dental prosthesis according to the invention, and Use of cerium-stabilized ZrO 2 for the production of framework materials.
Vollkeramische Massen sind heutzutage indiziert für Frontzähne, Inlays, Onlays und Veneers und max. 3-gliedrige Seitenzahnbrücken. Größere Arbeiten sind bisher nur mit dichtgesintertem Zirkonoxid möglich. Die Nachteile hier liegen in dem opaken Erscheinungsbild und der schweren Bearbeitbarkeit dϊchtgesin- terter (teilweise yttriumstabilisierter) Zirkonoxid,All-ceramic materials are nowadays indicated for anterior teeth, inlays, onlays and veneers and max. 3-unit posterior bridges. Larger jobs have so far only been possible with densely sintered zirconium oxide. The disadvantages here are the opaque appearance and the difficult workability of sintered (partially yttrium-stabilized) zirconium oxide,
Aus der DE4020893 AI sind Materialien bekannt, die Cer-stabilisiertes Zirkonium enthalten. Die Oxidkeramiken werden mit einer Glasphase zusammengeschmolzen. Dadurch entsteht ein Material aus einer amorphen Glasphase, in der die oxidkeramischen Partikel wie Inseln dispergiert sind.From DE4020893 AI materials are known which contain cerium-stabilized zirconium. The oxide ceramics are melted together with a glass phase. This creates a material from an amorphous glass phase in which the oxide-ceramic particles are dispersed like islands.
Die DE 44207180 AI betrifft ebenfalls Glaskeramiken mit oxidkeramischen Anteilen. Die oxidkeramischen zirkoniumhaltigen Kristalle sind als Ausfällungen in einer Glasmatrix verteilt.DE 44207180 AI also relates to glass ceramics with oxide ceramic components. The oxide-ceramic zirconium-containing crystals are distributed as precipitates in a glass matrix.
Ein Verfahren zur Herstellung von gesinterten porösen Gerüstmaterialien wird in EP 0 824879 A2 beschrieben.A method for producing sintered porous framework materials is described in EP 0 824879 A2.
Der Erfindung liegt die Aufgabe zugrunde, mehrgliedrige Seitenzahnbrücken mit möglichst hoher Zuverlässigkeit (d. h. hoher Bruchfestigkeit Klc und hohe Biegfestigkeiten) zahntechnisch herzustellen. Mit den bisherigen vollkeramischen Verfahren wird nur eine Bruchzä- higkeit mit Klc- Werten von 3 - 6 erreicht. Aufgrund der Sprödigkeit und dem ungünstigen Ermüdungsverhalten von Keramiken benötigt man für mehrgliedrige Seitenzahnbrücken ein Material mit möglichst hohen Bruchzähigkeiten (Kic) mit gleichzeitig hohen Biegefestigkeiten.The invention is based on the object To manufacture multi-unit posterior bridges with the highest possible reliability (ie high breaking strength Klc and high bending strength). With the previous all-ceramic processes, only a fracture toughness with K lc values of 3 - 6 is achieved. Due to the brittleness and the unfavorable fatigue behavior of ceramics, a material with the highest possible fracture toughness (Kic) and at the same time high bending strength is required for multi-unit posterior bridges.
Das der Erfindung zugrunde liegende technische Problem wird gelöst durch einen vollkeramischen Zahnersatz mit einem Gerüst, das aus einem Gerüstmaterial aus einem Cer-stabilisierten Zirkonoxid (Ce-ZrO2) mit einem Anteil von bis zu 25 Gew% Aluminiumoxid (Al203) bezogen auf den Anteil an ZrO2 aufgebaut ist und einem Infiltrationsglasanteil im Gerüst von 0-40 Vol% bezo- gen auf das Volumen des Gerusts sowie einer auf das Gerüstmaterial abgestimmten Verblendkeramik. Gerüst bedeutet, dass ein durchgängiges, poröses oxidkeramisches Netzwerk vorliegt.The technical problem on which the invention is based is solved by an all-ceramic dental prosthesis with a framework, which is based on a framework material made of a cerium-stabilized zirconium oxide (Ce-ZrO 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 O 3 ) is based on the proportion of ZrO 2 and an infiltration glass proportion in the framework of 0-40 vol% based on the volume of the framework as well as veneering ceramics matched to the framework material. Scaffolding means that there is a continuous, porous oxide-ceramic network.
Überraschenderweise ergab sich bei Verwendung von Mischungen von Cer- dotiertem Zirkonoxid zu Aluminiumoxid (α-AI2O3) eine besondere Steigerung des Kιc-Wertes unter Verwendung passender Infiltrationsgläser.Surprisingly, when using mixtures of cerium-doped zirconium oxide to aluminum oxide (α-Al 2 O 3 ), there was a particular increase in the K 1 c value using suitable infiltration glasses.
Vorzugsweise enthält der erfindungsgemäße vollkeramische Zahnersatz 5,5 - 16 mol % Ce02 in ZrO2.The all-ceramic dental prosthesis according to the invention preferably contains 5.5-16 mol% Ce0 2 in ZrO 2 .
Die Vorteile liegen hier in der Reproduzierbarkeit der Metastabilität der tetra- gonalen Phase des cerstabilisierten Zirkonoxides (Ce-ZrO2).The advantages here lie in the reproducibility of the metastability of the tetrahedral phase of the cerstabilized zirconium oxide (Ce-ZrO 2 ).
Gegenstand der Erfindung ist auch ein Gerustmaterial, das aus einem Cer- stabilisierten Zirkonoxid (Ce-ZrO2) mit einem Anteil von bis zu 25 Gew% Aluminiumoxid (AI2O3) bezogen auf den Anteil an ZrO2 aufgebaut ist. Das erfindungsgemäße Gerüstmaterial enthält vorzugsweise 5,5 - 16 mol % CeO2 in ZrO2.The invention also relates to a framework material which is composed of a cerium-stabilized zirconium oxide (Ce-ZrO 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 O 3 ) based on the proportion of ZrO 2 . The framework material according to the invention preferably contains 5.5-16 mol% CeO 2 in ZrO 2 .
Vorteilhaft ist die leichte Bearbeitbarkeit des Gerüstmaterials vor dem Infilt- rieren. Die Zugabe von AI2O3 (Aluminiumoxid) gewährleistet die Kompatibilität zu bisher existierenden Verblendkeramiken.The easy workability of the scaffold material before infiltration is advantageous. The addition of Al 2 O 3 (aluminum oxide) ensures compatibility with existing veneering ceramics.
In einer Alternative geht das erfindungsgemäße Verfahren zur Herstellung eines Gerüstes in dem erfindungsgemäßen vollkeramischen Zahnersatz davon aus, dass das erfindungsgemäße Gerüstmaterial als dichtgesintertes Material formbearbeitet wird.In an alternative, the method according to the invention for producing a framework in the all-ceramic dental prosthesis according to the invention assumes that the framework material according to the invention is shaped as a densely sintered material.
Der Vorteil ist hier die formtreue Bearbeitung. Ein aus diesem Material hergestellter vollkeramischer Zahnersatz hätte eine deutlich höhere Bruchzähigkeit (Kic) als vergleichbare yttriumstabilisierte Zirkonoxide.The advantage here is the form-true processing. All-ceramic dentures made from this material would have a significantly higher fracture toughness (Ki c ) than comparable yttrium-stabilized zirconium oxides.
In einer anderen AUsführungsform des erfindungsgemäßen Verfahrens zur Herstellung eines Gerüstes in dem erfindungsgemäßen vollkeramischen Zahnersatz wird das erfindungsgemäße Gerüstmaterial zunächst porös gesintert und danach formbearbeitet.In another embodiment of the method according to the invention for producing a framework in the all-ceramic dental prosthesis according to the invention, the framework material according to the invention is first sintered porously and then shaped.
Die über die Zwischenstufe durch Reaktionsbinden in Abgrenzung zu einem Sinterprozess hergestellte poröse vollkeramische Gerüste haben den Vorteil der einfachen Maschinenbearbeitbarkeit oder des einfachen manuellen Model- lierens unter Beibehaltung der Form und einer beschädigungsfreien Oberfläche. Diese Vorteile führen zu einer hohen Passgenauigkeit und einer verbesserten Biegefestigkeit des daraus hergestellten Zahnersatzes.The porous all-ceramic frameworks produced via the intermediate stage by means of reaction bandages as opposed to a sintering process have the advantage of being easy to machine or manually modeling while maintaining the shape and a damage-free surface. These advantages lead to a high accuracy of fit and an improved flexural strength of the dentures produced from them.
Hieran schließt sich dann eine Verfestigung durch Dichtsinterung oder Infiltra- tion mit einem Infiltrationsglas an. Durch Infiltration ergibt sich die formtreue Wiedergabe ohne Schädigung der Oberfläche.This is then followed by solidification by dense sintering or infiltration with an infiltration glass. Infiltration results in true-to-shape reproduction without damaging the surface.
Das Infiltrationsglas zur Infiltration des erfindungsgemäßen porösen Gerüstes enthält vorzugsweise 15 bis 35 Gew% La2O3, 10 - 25 Gew% SiO2, 10 - 25 Gew% AI2O3, 5 - 20 Gew% B2O3, 5 - 20 Gew% CaO, 0 - 10 Gew% ZrO2, 0 - 10 Gew% TiO2 und 0 - 15 Gew% CeO2. In einer besonderen Ausführungsform enthält das Infiltrationsglas weitere Metalloxide in einer Oxidationsstufe, die ZrO2 stabilisieren kann. Dazu gehören als Metalloxide insbesondere MgO und Y2O3. Vorzugsweise sind bis zu 10 Gew% MgO und bis zu 10 Gew% Y2O3 in dem Infiltrationsglas vorhanden.The infiltration glass for infiltration of the porous framework according to the invention preferably contains 15 to 35% by weight of La 2 O 3 , 10 to 25% by weight of SiO 2 , 10 to 25% by weight of Al 2 O 3 , 5 to 20% by weight of B 2 O 3 , 5 - 20% by weight CaO, 0-10% by weight ZrO 2 , 0-10% by weight TiO 2 and 0-15% by weight CeO 2 . In a special embodiment, the infiltration glass contains further metal oxides in an oxidation stage which can stabilize ZrO 2 . As metal oxides, these include in particular MgO and Y 2 O 3 . Preferably up to 10 wt% MgO and up to 10 wt% Y 2 O 3 are present in the infiltration glass.
Die Vorteile der Zugabe von Mg, Ce, Y ist die Stabilisierung der tetragonalen Phase bei Raumtemperatur und somit zu einer deutlichen Erhöhung des Klc- Wertes. Das Aufnahmevermögen des Glases von Ceroxid beeinflusst die Verspannung zwischen Glas und Matrix.The advantages of adding Mg, Ce, Y are the stabilization of the tetragonal phase at room temperature and thus a significant increase in the K lc value. The absorption capacity of the glass of cerium oxide influences the tension between the glass and the matrix.
Das Infiltrationsglas kann auch Pigmente enthalten. Durch Zugabe von Pigmenten kann man von der rein weißen Farbe des Oxides in Richtung der na- türlichen Zahnfarbe gehen.The infiltration glass can also contain pigments. By adding pigments you can go from the pure white color of the oxide in the direction of the natural tooth color.
Der Erfindung liegt als allgemeiner Gedanke die Verwendung von Cer- stabilisiertem ZrO2 zur Herstellung von Gerüstmaterialien, die als Restauration im Dentalbereich einsetzbar sind, zugrunde.As a general idea, the invention is based on the use of cerium-stabilized ZrO 2 for producing framework materials which can be used as restorations in the dental field.
Die Struktur eines erfindungsgemässen Gerusts aus Cer-stabilisiertem Zirkoniumoxid wird durch Figur 1 und 2 verdeutlicht. Es handelt sich dabei um raster- elektronenmikroskopische (REM) Aufnahmen (Rückstreuelektronen, Detector = QBSD) mit unterschiedlicher Auflösung. Die Aufnahmen zeigen das Netzwerk aus Cer-stabilisiertem Zirkoniumoxid (helle Körner), das mit einem Glas infiltriert wurde. Deutlich sichtbar sind die Verknüpfungen der einzelnen Zirkoniumoxidkörner untereinander, die zusammen mit der Glasinfiltration eine er- höhte Festigkeit bewirken. Außerdem sind im Glas (grauer Anteil) teilweise helle Auskristallisierungen zu sehen, die reich an Zirkoniumoxid sind und zu einer weiteren Verfestigung führen können.The structure of a framework made of cerium-stabilized zirconium oxide according to the invention is illustrated by FIGS. 1 and 2. These are scanning electron microscopic (SEM) recordings (backscattered electrons, detector = QBSD) with different resolutions. The images show the network of cerium-stabilized zirconium oxide (bright grains) that was infiltrated with a glass. The links between the individual zirconium oxide grains are clearly visible, which together with the glass infiltration cause increased strength. In addition, in the glass (gray part) some bright crystallizations can be seen, which are rich in zirconium oxide and can lead to further solidification.
Die Erfindung wird anhand der folgenden Beispiele näher erläutert:The invention is illustrated by the following examples:
Beispiel 1 :Example 1 :
Ce-stab. pures ZrO2 (ca. 15.5 Gew% CeO2) wurde gepresst und gesintert bei 1500 °C.Ce-stab. pure ZrO 2 (approx. 15.5% by weight CeO 2 ) was pressed and sintered at 1500 ° C.
Die Bruchzähigkeit (Kιc-Wert) liegt bei >11 MPam1/2.The fracture toughness (Kι c value) is> 11 MPam 1/2 .
Beispiel 2:Example 2:
Ein Zirconia/Aluminium Gemisch mit der Zusammensetzung 20 Gew.% AI2O3, 80 Gew.% ZrO2 mit einer Korngröße von d = 3,0 μm der Mischung wird hergestellt. Das verwendete ZrO2 ist Cer-stabilisiert mit einem Anteil von 15,5 Gew.% CeO2. Die Pulvermischung wird geformt und bei 1500 °C gesintert. Die Probe wird bei 1140 °C mit einem Lanthanglas infiltriert, das einen CeO2-Anteil unter 4 Gew.% hat und keine weiteren stabilisierenden Oxide wie MgO, CaO, Y2O3 etc. enthält.A zirconia / aluminum mixture with the composition 20% by weight Al 2 O 3 , 80% by weight ZrO 2 with a grain size of d = 3.0 μm of the mixture is produced. The ZrO 2 used is cerium-stabilized with a proportion of 15.5% by weight CeO 2 . The powder mixture is shaped and sintered at 1500 ° C. The sample is infiltrated at 1140 ° C. with a lanthanum glass which has a CeO 2 content of less than 4% by weight and contains no further stabilizing oxides such as MgO, CaO, Y 2 O 3 etc.
Die resultierende Biegezugfestigkeit liegt bei 650 MPa. Die Bruchzähigkeit liegt
Figure imgf000007_0001
The resulting bending tensile strength is 650 MPa. The fracture toughness lies
Figure imgf000007_0001
Vergleichsbeispiel:Comparative Example:
Ein Zirconia/Alumina Gemisch mit der Zusammensetzung 33 Gew. % ZrO2 und 67 Gew. % Al203 wird hergestellt. Das Gemisch hat eine mittlere Korngröße d50 = 2,3 μm. Diese Pulvermischung wird geformt und bei 1180 °C gesintert. Die Probe wird bei 1140 °C mit Lanthanglas infiltriert und hat eine Biegefestigkeit von 580 MPa und eine Bruchzähigkeit mit einem KιC-Wert von 4,4 MPam1/2. A zirconia / alumina mixture with the composition 33% by weight of ZrO 2 and 67% by weight of Al 2 0 3 is produced. The mixture has an average grain size d 50 = 2.3 μm. This powder mixture is shaped and sintered at 1180 ° C. The sample is infiltrated at 1140 ° C and lanthanum and has a bending strength of 580 MPa and a fracture toughness with a Kι C value of 4.4 MPam 1/2.

Claims

Patentansprüche claims
1. Vollkeramischer Zahnersatz mit einem Gerüst, das aus einem Gerüstmaterial aus einem Cer-stabilisierten Zirkonoxid (Ce-Zr02) mit einem Anteil von bis zu 25 Gew% Aluminiumoxid (Al203) bezogen auf den Anteil an ZrO2 aufgebaut ist und einem Infiltrationsglasanteil im Gerüst von 0-40 Vol% bezogen auf das Volumen des Gerusts sowie einer auf das Gerustmaterial abgestimmten Verblendkeramik.1. All-ceramic dentures with a framework that is made up of a framework material made of a cerium-stabilized zirconium oxide (Ce-Zr0 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 0 3 ) based on the proportion of ZrO 2 and an infiltration glass content in the framework of 0-40 vol% based on the volume of the framework as well as veneering ceramics matched to the framework material.
2. Vollkeramischer Zahnersatz nach Anspruch 1, mit einem Anteil von 5,5 - 16 mol % CeO2 in ZrO2.2. All-ceramic dental prosthesis according to claim 1, with a proportion of 5.5-16 mol% CeO 2 in ZrO 2 .
3. Gerüstmaterial, das aus einem Cer-stabilisierten Zirkonoxid (Ce-Zr02) mit einem Anteil von bis zu 25 Gew% Aluminiumoxid (AI2O3) bezogen auf den Anteil an Zr02 aufgebaut ist.3. Framework material which is composed of a cerium-stabilized zirconium oxide (Ce-Zr0 2 ) with a proportion of up to 25% by weight aluminum oxide (Al 2 O 3 ) based on the proportion of Zr0 2 .
4. Gerüstmaterial nach Anspruch 3, mit einem Anteil von 5,5 - 16 mol % Ce02 in ZrO2.4. Framework material according to claim 3, with a proportion of 5.5-16 mol% Ce0 2 in ZrO 2 .
5. Verfahren zur Herstellung eines Gerüstes in einem vollkeramischen Zahnersatz nach Anspruch 1 oder 2, wobei das Gerüstmaterial nach einem der Ansprüche 3 oder 4 als dichtgesintertes Material form bearbeitet wird.5. A method for producing a framework in an all-ceramic dental prosthesis according to claim 1 or 2, wherein the framework material according to one of claims 3 or 4 is machined as a densely sintered material.
6. Verfahren zur Herstellung eines Gerüstes in einem vollkeramischen Zahnersatz nach Anspruch 1 oder 2, wobei das Gerüstmaterial nach einem der Ansprüche 3 oder 4 porös gesintert wird, danach formbearbeitet wird, gefolgt von einer Verfestigung durch Dichtsinterung oder Infiltration mit einem Infiltrationsglas.6. A process for producing a framework in an all-ceramic dental prosthesis according to claim 1 or 2, wherein the framework material according to one of claims 3 or 4 is sintered porously, is then shaped, followed by solidification by sealing sintering or infiltration with an infiltration glass.
Verfahren nach Anspruch 6, wobei das Infiltrationsglas 15 bis 35 Gew% La2O3, 10 - 25 Gew% SiO2, 10 - 25 Gew% AI2O3, 5 - 20 Gew% B2O3, 5 - 20 Gew% CaO, 0 - 10 Gew% ZrO2, 0 - 10 Gew% TiO2 und 0 - 15 Gew% CeO2 enthält.The method of claim 6, wherein the infiltration glass 15 to 35 wt% La 2 O 3 , 10 to 25 wt% SiO 2 , 10 to 25 wt% Al 2 O 3 , 5 to 20 wt% B 2 O 3 , 5 - 20% by weight of CaO, 0 - 10% by weight of ZrO 2 , 0 - 10% by weight of TiO 2 and 0 - 15% by weight of CeO 2 .
8. Verfahren nach Anspruch 6 oder 7, wobei das Infiltrationsglas weitere Metalloxide in einer Oxidationsstufe zur Stabilisierung des ZrO2. enthält.8. The method according to claim 6 or 7, wherein the infiltration glass further metal oxides in an oxidation stage to stabilize the ZrO 2nd contains.
9. Verfahren nach einem der Ansprüche 6 bis 8, wobei das Infiltrationsglas 0 - 10 Gew% MgO und/oder 0 - 10 Gew% Y2O3 enthält.9. The method according to any one of claims 6 to 8, wherein the infiltration glass contains 0-10 wt% MgO and / or 0-10 wt% Y 2 O 3 .
10. Verfahren nach einem der Ansprüche 6 bis 9, wobei das Infiltrationsglas Pigmente enthält.10. The method according to any one of claims 6 to 9, wherein the infiltration glass contains pigments.
11. Verwendung von cer-stabilisiertem ZrO2 zur Herstellung von Gerüstmaterialien, die als Restauration im Dentalbereich einsetzbar sind. 11. Use of cerium-stabilized ZrO 2 for the production of framework materials that can be used as a restoration in the dental field.
PCT/EP2001/014502 2000-12-11 2001-12-11 Fully ceramic tooth replacement with a frame made of cer-stabilised zircon oxide WO2002047616A2 (en)

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US10214443B2 (en) 2005-02-08 2019-02-26 Ivoclar Vivadent Ag Lithium silicate materials
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CN108395246A (en) * 2018-05-15 2018-08-14 钱兴 A kind of preparation method of high tenacity oral cavity Nano ceramic powder material

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