Lithium silicate glass ceramic material, process of production and use thereof

Patent metadata

Field	Value
Publication number	US-9351807-B2
Application number	US-201214356761-A
Country	US
Kind code	B2
Filing date	Dec 6, 2012
Priority date	Dec 8, 2011
Publication date	May 31, 2016
Grant date	May 31, 2016

Abstract

The invention relates to a lithium silicate glass ceramic comprising CsO2 in an amount from about 6 to about 30 wt.-%. The invention also relates to a three-dimensional article comprising at least two layers (I) and (II), each layer (I) and (II) comprising a lithium silicate glass ceramic, the lithium silicate glass ceramics of layer (I) having a different translucency than the lithium silicate glass ceramic of layer (II).

First claim

The invention claimed is:

1. A lithium silicate glass ceramic comprising
Cs2O about 11 wt.-% and
SiO2 from about 55 to about 80 wt.-%,
Al2O3+B2O3 from about 1 to about 5 wt.-%,
Li2O from about 7 to about 16 wt.-%,
P2O5 from about 1 to about 5 wt.-%,
wt.-% with respect to the weight of the glass ceramic.

2. The lithium silicate glass ceramic according to claim 1 comprising a further metal oxide in a total amount from about 0.1 to about 10 wt.-%, the further metal oxide being selected from SrO, BaO, TiO2, ZrO2, HfO2, Fe2O3, VO2, Y2O3, CeO2, Sm2O3, Er2O3, Dy2O3, or mixtures thereof.

3. The lithium silicate glass ceramic according to claim 1 not comprising K2O, MgO, ZnO, La2O3 or a mixture of thereof in an amount above about 0.4 wt.-% with respect to the weight of the lithium silicate glass ceramic.

4. The lithium silicate glass ceramic according to claim 1 being characterized by at least one of the following parameters:
having a translucency from about 0.03 to about 0.60;
having a radiopacity of more than about 200%, determined according to ISO 6872;
having a coefficient of thermal expansion from about 8 to about 12×10 −6 /K, determined according to ISO 6872;
having a Vickers hardness of at least about 500 (0.2 kg load);
having a flexural strength of at least about 250 MPa, determined according to ISO 6872;
having a refractive index from about 1.545 to about 1.525.

5. The lithium silicate glass ceramic according to claim 1 not comprising either of the following crystal phases in an amount above about 50% apatite, tetragonal or cubic leucite.

6. A three-dimensional article comprising a lithium silicate glass ceramic as described in claim 1 , the three-dimensional article having the shape of a dental mill blank or ingot.

7. The three-dimensional article of claim 6 comprising at least two layers (I) and (II), each layer (I) and (II) comprising a lithium silicate glass ceramic, the lithium silicate glass ceramics of layer (I) having a different translucency than the lithium silicate glass ceramic of layer (II).

8. The three-dimensional article according to claim 6 comprising at least two layers (I) and (II), layer (I) comprising a lithium silicate glass ceramic (GC I) and layer (II) comprising a lithium silicate glass ceramic (GC II), the lithium silicate glass ceramics (GC I) and (GC II) having coefficients of thermal expansion (CTE I) and (CTE II) fulfilling the equation: (CTE I)−(CTE II)≦±1.2×10 −6 /K.

9. The three-dimensional article of claim 6 having the shape of a dental mill blank being fixed to or in a holder.

10. A method of producing a lithium silicate glass ceramic of claim 1 , the method of comprising the steps of:
a) melting a composition comprising SiO2, Li2O, Al2O3, P2O5, and Cs2O, wherein the Cs2O is present in an amount of about 11 wt.-%,
b) firing the composition at about 1500 to about 1600° C. for about 5 to 30 min,
c) optionally casting the composition into a mold,
d) annealing the composition at about 500 to about 600° C. for about 30 min to about 2 h,
e) heating the composition to about 600 to about 700° C. for about 1 to about 30 h,
f) heating the composition to about 750 to about 950° C. for about 5 min to about 2 h,
g) cooling the composition down to room temperature.

11. A kit of parts comprising a part A and a part B, part A comprising a lithium silicate glass ceramic as described in claim 1 or the three-dimensional article as described in claim 6 and part B comprising a zirconia based ceramic article.

12. A dental article formed from the lithium silicate glass ceramic as described in claim 1 or the three dimensional article as described in claim 6 .

13. The dental article according to claim 12 selected from crown(s), bridge(s), veneer(s), facing(s), implant(s), abutment(s), root-pin(s), orthodontic bracket(s), dental support structure(s), inlay(s), onlay(s), full arch prostheses and parts or combinations thereof.

14. A method of producing a multi-layered block, the method comprising the steps of
melting compositions A and B of claim 11 ,
casting composition A into a mold to obtain a layer I,
cooling the composition of layer I to about 700 to about 800° C.,
casting composition B on top of layer I to obtain a layer II,
cooling the composition of layer II to about 700 to about 800° C.

15. A dental restoration comprising at least two sections A and B, section A comprising a zirconia based ceramic and section B comprising a lithium silicate glass ceramic as described in claim 1 .

16. The lithium silicate glass ceramic according to claim 1 , the three-dimensional article having the shape of a dental mill blank or ingot and comprising at least two layers (I) and (II), each layer (I) and (II) comprising a lithium silicate glass ceramic, the lithium silicate glass ceramics of layer (I) having a different translucency than the lithium silicate glass ceramic of layer (II), wherein the lithium silicate glass ceramic does not comprise either of the following crystal phases in an amount above about 50% apatite, tetragonal or cubic leucite.

17. A method of producing a lithium silicate glass ceramic, the method comprising the steps of:
a) melting a composition of claim 1 ,
b) firing the composition at about 1500 to about 1600° C. for about 5 to 30 min,
c) optionally casting the composition into a mold,
d) annealing the composition at about 500 to about 600° C. for about 30 min to about 2 h,
e) heating the composition to about 600 to about 700° C. for about 1 to about 30 h,
f) heating the composition to about 750 to about 950° C. for about 5 min to about 2 h,
g) cooling the composition down to room temperature.

Assignees

• 3M Innovative Properties Co

Inventors

• Höscheler Stefan

Classifications

• A61K6/822

  comprising rare earth metal oxides · CPC title

• C03C4/0021 Primary

  for dental use · CPC title

• A61K6/824

  comprising transition metal oxides · CPC title

• A61K6/807

  comprising magnesium oxide · CPC title

• A61K6/818

  comprising zirconium oxide · CPC title