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EP4298071A1 - Vitrocéramique comprenant une phase cristalline mixte de quartz - Google Patents

Vitrocéramique comprenant une phase cristalline mixte de quartz

Info

Publication number
EP4298071A1
EP4298071A1 EP22706599.2A EP22706599A EP4298071A1 EP 4298071 A1 EP4298071 A1 EP 4298071A1 EP 22706599 A EP22706599 A EP 22706599A EP 4298071 A1 EP4298071 A1 EP 4298071A1
Authority
EP
European Patent Office
Prior art keywords
glass
weight
glass ceramic
ceramic according
particularly preferably
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP22706599.2A
Other languages
German (de)
English (en)
Inventor
Markus Rampf
Marc Dittmer
Christian Ritzberger
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ivoclar Vivadent AG
Original Assignee
Ivoclar Vivadent AG
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ivoclar Vivadent AG filed Critical Ivoclar Vivadent AG
Publication of EP4298071A1 publication Critical patent/EP4298071A1/fr
Pending legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0018—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents
    • C03C10/0027—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing SiO2, Al2O3 and monovalent metal oxide as main constituents containing SiO2, Al2O3, Li2O as main constituents
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • C03C10/0009—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing silica as main constituent
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/0003—Making bridge-work, inlays, implants or the like
    • A61C13/0004—Computer-assisted sizing or machining of dental prostheses
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/0003—Making bridge-work, inlays, implants or the like
    • A61C13/0006—Production methods
    • A61C13/0021—Production methods using stamping techniques
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C5/00—Filling or capping teeth
    • A61C5/70—Tooth crowns; Making thereof
    • A61C5/77—Methods or devices for making crowns
    • 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
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/005—Hot-pressing vitrified, non-porous, shaped glass products
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
    • C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
    • 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
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • 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
    • 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
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
    • 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
    • C03C2204/00—Glasses, glazes or enamels with special properties
    • C03C2204/04—Opaque glass, glaze or enamel

Definitions

  • Glass ceramic with a quartz mixed crystal phase The invention relates to glass ceramic with a quartz mixed crystal phase, which is particularly suitable for use in dentistry and preferably for the production of dental restorations, and preliminary stages for the production of this glass ceramic.
  • Glass ceramics with a quartz mixed crystal phase are known in principle from the prior art.
  • DE 2507 131 A1 describes special magnesium aluminosilicate glass ceramics which contain 20 to 35% by weight Al 2 O 3 and 9 to 15% by weight MgO.
  • Bodies made from the glass ceramics have a heterogeneous structure in that the crystal structure of the surface layer differs from that of the interior of the body. The surface compressive stress generated in this way has a significant influence on the mechanical properties, so that machining the surface layer has an adverse effect. the mechanical properties would result.
  • JP 2000/063144 A discloses magnesium aluminosilicate glasses for the production of substrates for storage media, which have 30 to 60 mol % SiO 2 and large amounts of B 2 O 3 .
  • GB 2172282 A describes magnesium aluminosilicate glass ceramics which contain 10 to 40% by weight Al 2 O 3 .
  • the glass ceramics are intended for microelectronic applications and in particular as a coating for substrates such as aluminum and, in addition to high strength, they have a suitable dielectric constant in the range from 7 to 10 and high electrical resistance.
  • WO 2012/143137 A1 describes glass-ceramic bodies which contain at least 10.1% by weight Al 2 O 3 and have different crystal phases in different areas.
  • the article by M. Dittmer and C. Rüssel in J. Biomed. mater Res. Part B:100B:463-470 (2012) describes glass-ceramics with a high-quartz or low-quartz mixed-crystal phase as the main crystal phase, which contain at least 25.9% by weight Al 2 O 3 .
  • the strengths achieved with these known glass ceramics and also their optical properties are not entirely satisfactory for use as dental material.
  • the invention is therefore based on the object of providing a glass ceramic which has a combination of high strength and good translucency.
  • the glass ceramic should also have a thermal expansion coefficient that can be adjusted over a wide range.
  • the glass ceramic should also be easy to process into dental restorations and should therefore be excellently suited as a restorative dental material.
  • This object is achieved by the glass ceramic with a quartz mixed crystal phase according to claims 1 to 16 and 19.
  • the invention also relates to the starting glass according to claims 17 to 19, the methods according to claims 20 and 23 and the use according to claims 21 and 22.
  • the glass ceramic according to the invention is characterized in that it contains the following components: component weight % SiO 2 54.1 to 67.0 Li 2 O 13.1 to 18.5 K 2 O 0.1 to 2.0 Al 2 O 3 1.6 to 4.0 P 2 O 5 4.1 to 6.5 ZrO 2 7.0 to 13.5 and contains at least one quartz mixed crystal phase.
  • This glass ceramic also referred to below as “glass ceramic with a quartz mixed crystal phase”, surprisingly shows an advantageous combination of mechanical and optical properties that are desirable for a restorative dental material.
  • the glass-ceramic has high strength and yet it can be easily shaped into a dental restoration by pressing or machining. Furthermore, it was not to be expected that very good optical properties could nevertheless be achieved by the provision of one or more quartz mixed crystal phases. This is because many secondary crystal phases have a negative effect on the optical properties of glass ceramics. For example, they can reduce the translucency and they can also impair the ability to color the glass ceramic, which can lead to considerable difficulties when imitating the color of the natural tooth material to be replaced.
  • quartz mixed crystal phase means a crystal phase of SiO 2 in which foreign atoms are built into the lattice of the SiO 2 either in interstitial sites or in lattice sites. These foreign atoms can in particular be Al, as well as Li, Mg and/or Zn.
  • Al can preferably be present in a molar concentration which corresponds to the sum of the molar concentration of Li, twice the molar concentration of Mg and twice the molar concentration of Zn.
  • the glass ceramic contains at least two different quartz mixed crystal phases.
  • the at least one quartz mixed crystal phase can be both a stoichiometric and a non-stoichiometric quartz mixed crystal phase.
  • Stoichiometric quartz mixed crystal phases are those crystal phases in which the number of silicon atoms and the number of one of the foreign atoms are in the ratio x:y, where x and y are integers in the range from 1 to 8 and in particular in the range from 1 to 5 are.
  • the glass ceramic contains at least one and preferably at least two non-stoichiometric quartz mixed crystal phases.
  • the at least one quartz mixed crystal phase can be a stoichiometric or non-stoichiometric aluminosilicate crystal phase.
  • contains the glass-ceramic has at least one and preferably at least two stoichiometric or non-stoichiometric aluminosilicate crystal phases.
  • the glass ceramic contains at least one and preferably at least two non-stoichiometric aluminosilicate crystal phases.
  • Stoichiometric aluminosilicate crystal phases are understood as meaning crystal phases in which the number of silicon atoms and the number of aluminum atoms are in the ratio x:y, where x and y are integers in the range from 1 to 8 and in particular in the range from 1 to 5 are.
  • Examples of stoichiometric aluminosilicate crystal phases are eucryptite (LiAlSiO 4 ), spodumene (LiAlSi 2 O 6 ), petalite (LiAlSi 4 O 10 ) and cordierite (Mg 2 Al 4 Si 5 O 18 ).
  • the quartz mixed crystal phases of the glass ceramic according to the invention can be detected in particular by X-ray powder diffraction using Cu K ⁇ radiation.
  • the quartz mixed crystal phases show characteristic peak patterns, which are derived from the peak pattern of deep quartz, but are shifted towards other 2 ⁇ values.
  • the glass ceramic according to the invention with a quartz mixed crystal phase contains in particular 57.0 to 66.5% by weight, preferably 59.0 to 66.0% by weight and particularly preferably 62.1 to 65.5% by weight SiO 2 . It is further preferred that the glass ceramic according to the invention contains 13.3 to 18.0% by weight, preferably 16.1 to 17.5% by weight and particularly preferably 16.5 to 17.0% by weight Li 2 O.
  • the glass ceramic contains 0.5 to 1.7% by weight, preferably 1.1 to 1.5% by weight and particularly preferably 1.2 to 1.4% by weight of K 2 O.
  • the glass ceramic according to the invention contains 2.0 to 3.8% by weight and preferably 1.6 to 3.6% by weight Al 2 O 3 .
  • the glass ceramic contains 4.3 to 6.0, preferably 4.5 to 5.9 and particularly preferably 5.1 to 5.8% by weight of P 2 O 5 . It is believed that the P 2 O 5 acts as a nucleating agent.
  • the glass ceramic contains 7.2 to 13.0% by weight and preferably 9.0 to 12.0% by weight ZrO 2 . It is also preferred that the glass ceramic contains 1.0 to 8.0, preferably 1.0 to 5.5 and particularly preferably 1.5 to 2.5% by weight of oxide of monovalent elements Me I 2 O selected from the group of Na 2 O, Rb 2 O, Cs 2 O and mixtures thereof.
  • the glass ceramic particularly preferably contains at least one and in particular all of the following oxides of monovalent elements MeI 2 O in the stated amounts: Component % by weight Na 2 O 0 to 2.0 Rb 2 O 0 to 8.0 Cs 2 O 0 bis 7.0.
  • the glass ceramic according to the invention preferably contains 0.05 to 5.0, in particular 0.07 to 1.5, preferably 0.08 to 1.0, particularly preferably 0.09 to 0.4 and very particularly preferably 0.1 to 0 2 wt . It is assumed that oxides of divalent elements Me II O and in particular MgO promote the formation of one or more quartz solid solutions and avoid the formation of undesired crystal phases such as in particular cristobalite, which can have an adverse influence on the thermal expansion coefficient and the optical properties. In a further preferred embodiment, the glass ceramic contains less than 2.0% by weight of BaO. In particular, the glass ceramic is essentially free of BaO.
  • the glass ceramic preferably contains at least one and in particular all of the following oxides of divalent elements Me II O in the stated amounts: Component % by weight CaO 0 to 3.0 MgO 0 to 5.0 SrO 0 to 5.0 ZnO 0 bis 3.0
  • a glass ceramic is also preferred which contains 0 to 5.0, preferably 1.0 to 4.0 and particularly preferably 2.0 to 3.0% by weight of oxide of trivalent elements Me III 2 O 3 from the group of B 2 O 3 , Y 2 O 3 , La 2 O 3 , Ga 2 O 3 , In 2 O 3 and mixtures thereof.
  • the glass ceramic particularly preferably contains at least one and in particular all of the following oxides of trivalent elements Me III 2 O 3 in the specified amounts: Component % by weight B 2 O 3 0 to 4.0 Y 2 O 3 0 to 5.0 La 2 O 3 0 to 5.0 Ga 2 O 3 0 to 3.0 In 2 O 3 0 to 5.0 Furthermore, preference is given to a glass ceramic which has 0 to 10.0 and particularly preferably 0 to 8.0 wt. % Oxide of tetravalent elements Me IV O 2 selected from the group consisting of TiO 2 , SnO 2 , CeO 2 , GeO 2 and mixtures thereof.
  • the glass ceramic particularly preferably contains at least one and in particular all of the following oxides of tetravalent elements Me IV O 2 in the stated amounts: Component % by weight TiO 2 0 to 4.0 SnO 2 0 to 3.0 GeO 2 0 to 9.0 , especially 0 to 8.0 CeO 2 0 to 4.0.
  • the glass ceramic contains 0 to 8.0, preferably 0 to 6.0% by weight oxide of pentavalent elements MeV 2 O 5 selected from the group of V 2 O 5 , Ta 2 O 5 , Nb 2 O 5 and mixtures thereof.
  • the glass ceramic particularly preferably contains at least one and in particular all of the following oxides of pentavalent elements Me V 2 O 5 in the specified amounts: Component % by weight V 2 O 5 0 to 2.0 Ta 2 O 5 0 to 5.0 Nb 2 O 5 0 to 5.0
  • the glass ceramic contains 0 to 5.0, preferably 0 to 4.0% by weight of oxide of the hexavalent element Me VI O 3 selected from the group consisting of WO 3 , MoO 3 and mixtures thereof .
  • the glass ceramic particularly preferably contains at least one and in particular all of the following oxides Me VI O 3 in the stated amounts: Component % by weight WO 3 0 to 3.0 MoO 3 0 to 3.0
  • the glass ceramic according to the invention contains 0 to 1.0% by weight and in particular 0 to 0.5% by weight of fluorine.
  • a glass ceramic which contains at least one and preferably all of the following components in the stated amounts: component % by weight SiO 2 54.1 to 67.0 Li 2 O 13.1 to 18.5 K 2 O 0, 1 to 2.0 Al 2 O 3 1.6 to 4.0 P 2 O 5 4.1 to 6.5 ZrO 2 7.0 to 13.5 Me I 2 O 1.0 to 8.0 Me II O 0 to 5.0 Me III 2 O 3 1.0 to 8.0 Me IV O 2 0 to 10.0 Me V 2 O 5 0 to 8.0 Me VI O 3 0 to 5.0 fluorine 0 to 1, 0, where Me I 2 O, Me II O, Me III 2 O 3 , Me IV O 2 , MeV 2 O 5 and Me VI O 3 have the meaning given above.
  • the glass-ceramic contains at least one and preferably all of the following components in the specified amounts: Component % by weight SiO 2 54.1 to 67.0 Li 2 O 13.1 to 18.5 K 2 O 0 .1 to 2.0 Al 2 O 3 1.6 to 4.0 P 2 O 5 4.1 to 6.5 ZrO 2 7.0 to 13.5 Na 2 O 0 to 2.0 Rb 2 O 0 to 8.0 Cs 2 O 0 to 7.0 CaO 0 to 3.0 MgO 0 to 5.0 SrO 0 to 5, 0 ZnO 0 to 3.0 B 2 O 3 0 to 4.0 Y 2 O 3 0 to 5.0 La 2 O 3 0 to 5.0 Ga 2 O 3 0 to 3.0 In 2 O 3 0 to 5 .0 TiO 2 0 to 4.0 SnO 2 0 to 3.0 GeO 2 0 to 9.0, in particular 0 to 8.0 CeO 2 0 to 4.0 V 2 O 5 0 to 2.0 Ta 2 O 5 0 to 5.0 Nb
  • the glass-ceramic according to the invention can also contain other coloring agents and/or fluorescent agents. These can be made, for example, from Bi 2 O 3 or Bi 2 O 5 and in particular from other inorganic pigments and/or oxides of d and f elements, such as the oxides of Mn, Fe, Co, Pr, Nd, Tb, Er, Dy, Eu and Yb can be selected. With the help of these coloring agents and fluorescent agents, the glass ceramic can be easily colored in order to imitate the desired optical properties, in particular of natural tooth material. It is surprising that this is possible without any problems despite the presence of one or more quartz mixed crystal phases.
  • the molar ratio of SiO 2 to Li 2 O is in the range from 1.5 to 6.0, in particular 1.55 to 3.0, preferably 1.6 to 1.8 and particularly preferably 1.65 to 1.75. It is surprising that the production of the glass ceramic according to the invention with a quartz mixed crystal phase is successful within these broad ranges. It is further preferred that the glass ceramic according to the invention contains lithium disilicate or lithium metasilicate as further crystal phases and in particular as the main crystal phase. The glass ceramic according to the invention particularly preferably contains lithium disilicate as a further crystal phase and in particular as the main crystal phase.
  • the term "main crystal phase" refers to the crystal phase that has the highest proportion by weight of all the crystal phases present in the glass ceramic.
  • the determination of the amounts of the crystal phases is carried out in particular using the Rietveld method.
  • a suitable method for the quantitative analysis of the crystal phases using the Rietveld method is, for example, in the dissertation by M. Dittmer "Glasses and glass ceramics in the system MgO-Al 2 O 3 -SiO 2 with ZrO 2 as nucleating agent", University of Jena 2011, described. It is preferred that the glass ceramic according to the invention has at least 20% by weight, preferably 25 to 55% by weight and particularly preferably 30 to 55% by weight of lithium disilicate crystals. It is further preferred that the glass ceramic according to the invention has 0.2 to 28% by weight and preferably 0.2 to 25% by weight of quartz mixed crystals.
  • the glass ceramic according to the invention with a quartz mixed crystal phase is characterized by particularly good mechanical properties and optical properties and it can be formed by heat treating a corresponding starting glass or a corresponding starting glass with nuclei. These materials can therefore serve as precursors for the quartz solid solution glass-ceramic according to the invention.
  • the type and in particular the quantity of the crystal phases formed can be controlled by the composition of the starting glass and the heat treatment used to produce the glass-ceramic from the starting glass. The examples illustrate this by varying the composition of the starting glass and the heat treatment applied.
  • the glass ceramic has a high biaxial breaking strength of preferably at least 200 MPa and particularly preferably 250 to 460 MPa. The biaxial fracture strength was determined according to ISO 6872 (2008) (piston on three balls test).
  • the glass ceramic according to the invention has in particular a thermal expansion coefficient CTE (measured in the range from 100 to 500° C.) of 3.0 to 14.0 ⁇ 10 -6 K -1 , preferably 5.0 to 14.0 ⁇ 10 -6 K -1 and more preferably 7.0 to 14.0 x 10 -6 K -1 .
  • the CTE is determined according to ISO 6872 (2008).
  • the thermal expansion coefficient is adjusted to a desired value in particular by the type and quantity of the crystal phases present in the glass ceramic and the chemical composition of the glass ceramic.
  • the translucency of the glass ceramic was determined in the form of the contrast value (CR value) according to British Standard BS 5612, and this contrast value was preferably 40 to 92.
  • the present glass ceramic according to the invention special combination of properties allows it even as a dental material and to be used in particular as a material for the production of dental restorations.
  • the invention also relates to precursors with a corresponding composition, from which the glass-ceramic according to the invention with a quartz mixed crystal phase can be produced by heat treatment. These precursors are a correspondingly composed starting glass and a correspondingly composed starting glass with nuclei.
  • corresponding composition means that these precursors contain the same components in the same amounts as the glass ceramic, with the components being calculated as oxides as is usual with glasses and glass ceramics, with the exception of fluorine.
  • the invention therefore also relates to a starting glass which contains the components of the glass-ceramic according to the invention with a quartz mixed crystal phase.
  • the starting glass according to the invention therefore contains, in particular, suitable amounts of SiO 2 , Li 2 O, K 2 O, Al 2 O 3 , P 2 O 5 and ZrO 2 which are required to form the glass ceramic according to the invention with a quartz mixed crystal phase.
  • the starting glass can also contain other components, as specified above for the glass-ceramic with quartz mixed crystal phase according to the invention. All such embodiments for the components of the starting glass are preferred which are also indicated as preferred for the components of the glass ceramic according to the invention with a quartz mixed crystal phase.
  • the starting glass is particularly preferably in the form of a powder, a granulate or a powder compact pressed from a powder or granulate.
  • the starting glass in the molds mentioned has a large inner surface on which the later crystallization of one and preferably several quartz mixed crystal phases can take place. This can have the advantage that compared to crystallization of glass monoliths, fewer heat treatment steps are required to form one or more quartz solid solutions.
  • the invention also relates to such a starting glass containing nuclei for the crystallization of quartz mixed crystal phase.
  • the starting glass preferably also contains nuclei for the crystallization of lithium disilicate or lithium metasilicate.
  • the starting glass is produced in particular by melting a mixture of suitable starting materials, such as carbonates and oxides, at temperatures of, in particular, around 1500 to 1700° C.
  • the glass melt obtained can be poured into water to form a glass frit, and the resulting frit is then melted again.
  • the melt can then be poured into molds, eg steel or graphite molds, in order to produce blanks of the starting glass, so-called bulk glass blanks or monolithic blanks.
  • These monolithic blanks are usually first stress-relieved, for example by being held at 800 to 1200° C. for 5 to 60 minutes, and then slowly cooled to room temperature.
  • the melt is poured into water to make a frit. This glass frit can be processed into a powder or granules by grinding.
  • the powder or granulate obtained in this way can preferably be pressed to give a blank, a so-called powder compact, optionally after the addition of further components such as colorants and fluorescent agents.
  • multicolored blanks can be obtained in a simple manner, which have several areas with different color properties.
  • the invention enables the production of highly aesthetic multicolored dental restorations, which can imitate the optical properties of natural tooth material particularly well.
  • the further preliminary stage, starting glass with nuclei can first be produced by heat treatment of the starting glass.
  • the glass ceramic according to the invention with a quartz mixed crystal phase can then be produced by heat treatment of this further preliminary stage.
  • the quartz solid solution glass-ceramic of the present invention can be formed by heat treating the starting glass.
  • the starting glass prefferably to subject the starting glass to a heat treatment at a temperature of 400 to 600° C., in particular 450 to 550° C., for a period of in particular 5 to 120 min, preferably 10 to 60 min, in order to nucleate the starting glass with nuclei for to produce the crystallization of quartz solid solution phase. It is further preferred that the starting glass or the starting glass with nuclei undergoes at least one heat treatment at a temperature of 600 to 1000° C., preferably 650 to 900° C. and particularly preferably 750 to 900° C., for a period of in particular 1 to 240 min, preferably 5 to 120 min, and more preferably 10 to 60 min to produce the quartz solid solution glass-ceramic.
  • the starting glass or the starting glass with nuclei undergoes a first heat treatment at a temperature of 600 to 800° C., preferably 650 to 750° C. and particularly preferably 650 to 700° C., for a period of in particular 1 to 120 min, preferably 5 to 120 min and more preferably 10 to 60 min, and then a second heat treatment at a temperature of 750 to 950°C, preferably 800 to 900°C and more preferably 800 to 850°C for Duration of in particular 1 to 120 min, preferably 5 to 120 min and more preferably 10 to 60 min subjected.
  • the invention therefore also relates to a method for producing the glass ceramic according to the invention with quartz mixed crystal phase in which the starting glass or the starting glass with nuclei, in particular in particulate form, preferably in the form of a powder and particularly preferably in the form of a powder compact, is subjected to at least one heat treatment in the range from 600 to 1000° C., preferably 650 to 900° C., for a duration of in particular 1 to 240 min, preferably 5 to 120 min and particularly preferably 10 to 60 min, and in particular sintered.
  • the at least one heat treatment carried out in the method according to the invention can also be carried out as part of a hot pressing or sintering of the starting glass according to the invention or the starting glass according to the invention with nuclei.
  • the glass ceramics according to the invention and the glasses according to the invention are present in particular as powders, granules or blanks in any shape and size, for example monolithic blanks such as platelets, cuboids or cylinders, or powder compacts. In these forms they can easily be further processed, eg to form dental restorations. However, they can also be present in the form of dental restorations, such as inlays, onlays, crowns, veneers, shells or abutments.
  • the glass ceramics according to the invention are particularly preferably in the form of multicolored blanks, in particular multicolored presintered or sintered powder compacts.
  • Dental restorations such as bridges, inlays, onlays, crowns, veneers, shells or abutments can be produced from the glass ceramics according to the invention and the glasses according to the invention.
  • the invention therefore also relates to their use for producing dental restorations, in particular multicolored dental restorations.
  • the glass ceramic or the glass is given the shape of the desired dental restoration by pressing or machining.
  • the pressing usually takes place under increased pressure and increased temperature. It is preferable that the pressing is carried out at a temperature of 700 to 1200°C. It is also preferred to carry out the pressing at a pressure of 2 to 10 bar.
  • the desired shape change is achieved through the viscous flow of the material used.
  • the starting glass according to the invention, the starting glass with nuclei according to the invention and the glass-ceramic with quartz mixed crystal phase according to the invention can be used for the pressing.
  • the glasses and glass ceramics according to the invention can be used in particular in the form of blanks of any shape and size, eg powder compacts, eg in unsintered, partially sintered or densely sintered form.
  • the machining usually takes place by means of material-removing processes and in particular by milling and/or grinding. It is particularly preferred that the machining is carried out as part of a CAD/CAM process.
  • the starting glass according to the invention, the starting glass with nuclei according to the invention and the glass-ceramic with quartz mixed crystal phase according to the invention can be used.
  • the glasses and glass ceramics according to the invention can be used in particular in the form of blanks, eg powder compacts, eg in unsintered, partially sintered or densely sintered form. After the desired shaped dental restoration has been produced, eg by pressing or machining, it can still be heat treated in order to reduce the porosity, eg of an inserted porous powder compact.
  • the glass ceramics according to the invention and the glasses according to the invention are also suitable as a coating material for ceramics and glass ceramics, for example.
  • the invention is therefore also based on the use of the glasses according to the invention or the invention directed according glass ceramics for coating ceramics and glass ceramics in particular.
  • the invention also relates to a method for coating ceramics, metals, metal alloys and glass ceramics, in which glass ceramic according to the invention or glass according to the invention is applied to the corresponding substrate and exposed to elevated temperature.
  • glass ceramic according to the invention or glass according to the invention is applied to the corresponding substrate and exposed to elevated temperature.
  • This can be done in particular by sintering or by joining an overlay produced using CAD-CAM with a suitable glass solder or adhesive and preferably by pressing on.
  • the glass ceramic or the glass is applied to the material to be coated, such as ceramic or glass ceramic, in the usual way, for example as a powder, and then sintered at an elevated temperature.
  • glass ceramic according to the invention or glass according to the invention for example in the form of powder compacts, is pressed on at an elevated temperature, for example from 700 to 1200° C., and with the application of pressure, for example from 2 to 10 bar.
  • an elevated temperature for example from 700 to 1200° C.
  • pressure for example from 2 to 10 bar.
  • a suitable oven is, for example, the Programat EP 5000 from Ivoclar Vivadent AG, Liechtenstein. Due to the above-described properties of the glass ceramics according to the invention and the glasses according to the invention, these are particularly suitable for use in dentistry.
  • the invention therefore also relates to the use of the glass ceramics according to the invention or the glasses according to the invention as dental material, preferably for coating dental restorations and particularly preferably for producing dental restorations such as bridges, inlays, onlays, veneers, abutments, partial crowns, crowns or shells.
  • the invention therefore also relates to a method for producing a dental restoration, in particular a bridge, inlay, onlay, Veneer, abutment, partial crown, crown or shell, in which the glass ceramic according to the invention or the glass according to the invention is given the shape of the desired dental restoration by pressing or by machining, in particular as part of a CAD/CAM process. It is preferably a multicolored dental restoration.
  • Example 1 to 3 the melts of the starting glasses were poured into graphite or steel molds to produce glass monoliths. These glass monoliths were stress relieved and slowly cooled to room temperature. They were then subjected to a first heat treatment at temperature T Kb for a duration t Kb for nucleation and then to a further heat treatment at temperature T C for a duration t C for crystallization.
  • glass frits ie glass granules, were produced by pouring the molten starting glasses into water. The glass frits were ground to a particle size of ⁇ 45 ⁇ m using ball or mortar mills and pressed into powder compacts using powder presses.
  • the powder compacts were optionally subjected to a heat treatment at temperature T Kb for a duration t Kb , a first heat treatment at temperature T C1 for a duration t C1 and a second heat treatment at temperature T C2 for a duration for nucleation and crystallization t subject to C2 .
  • Table I QMK: quartz mixed crystal phase SP: spodumene (LiAlSi 2 O 6 )

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Abstract

L'invention concerne des vitrocéramiques à cristal mixte de quartz et leurs précurseurs, qui sont caractérisées par d'excellentes propriétés mécaniques et optiques et qui peuvent être utilisées, en particulier, comme matériau de restauration dentaire.
EP22706599.2A 2021-02-24 2022-02-17 Vitrocéramique comprenant une phase cristalline mixte de quartz Pending EP4298071A1 (fr)

Applications Claiming Priority (2)

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EP21159118.5A EP4049982A1 (fr) 2021-02-24 2021-02-24 Vitrocéramique comprenant une phase cristalline mixte de quartz
PCT/EP2022/054010 WO2022179936A1 (fr) 2021-02-24 2022-02-17 Vitrocéramique comprenant une phase cristalline mixte de quartz

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EP4368587A1 (fr) * 2022-11-08 2024-05-15 Ivoclar Vivadent AG Procédé de fabrication d'une ébauche multicolore en vitrocéramique pour usage dentaire, ébauche multicolore en vitrocéramique et son utilisation
EP4368586A1 (fr) * 2022-11-08 2024-05-15 Ivoclar Vivadent AG Moule multiple pour la fabrication d'au moins deux préformes en vitrocéramique à usage dentaire, utilisation d'un moule multiple, dispositif de pressage et installation de défilement
WO2025051863A1 (fr) 2023-09-05 2025-03-13 Vita Zahnfabrik H. Rauter Gmbh & Co. Kg Corps moulé en vitrocéramique à usage dentaire

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WO2022179936A1 (fr) 2022-09-01
EP4049982A1 (fr) 2022-08-31
JP2024508246A (ja) 2024-02-26
KR20230148339A (ko) 2023-10-24
CN116917245A (zh) 2023-10-20

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