Method for the preparation of lithium silicate glasses and lithium silicate glass ceramics

Patent metadata

Field	Value
Publication number	US-10737972-B2
Application number	US-201816156203-A
Country	US
Kind code	B2
Filing date	Oct 10, 2018
Priority date	May 13, 2014
Publication date	Aug 11, 2020
Grant date	Aug 11, 2020

Abstract

The invention also relates to a lithium silicate glass and a lithium silicate glass ceramic which can be obtained using the method according to the invention, the use thereof as dental material and in particular for the preparation of dental restorations, as well as a glass-forming composition which is suitable for use in the method according to the invention.

First claim

The invention claimed is:

1. Method for the preparation of a lithium silicate glass, a lithium silicate glass with nuclei which are suitable for forming lithium metasilicate and/or lithium disilicate crystals, or a lithium silicate glass ceramic, which comprises a step in which a melt of a starting glass which comprises cerium ions is reacted with at least one reducing gas.

2. Method according to claim 1 , wherein the gas comprises hydrogen or comprises hydrogen and nitrogen.

3. Method according to claim 1 , in which the starting glass comprises up to 5.0 wt.-% alkaline earth metal oxide.

4. Method according to claim 1 , in which the starting glass comprises up to 5.0 wt.-% alkaline earth metal oxide selected from CaO, BaO, MaO, SrO and mixtures thereof.

5. Method according to claim 1 , in which the starting glass comprises at least one of the following components:

Component
wt.-%

SiO 2
55.0 to 75.0

Li 2 O
 9.0 to 21.0

M 2 O
 1.0 to 12.0

Al 2 O 3
0.5 to 5.0

P 2 O 5
  0.5 to 12.0,

wherein M 2 O is selected from the group consisting of Na 2 O, K 2 O, Rb 2 O and Cs 2 O.

6. Method according to claim 5 , in which the starting glass comprises at least one of the following components:

Component
wt.-%

SiO 2
59.0 to 73.0

Li 2 O
13.0 to 19.0

M 2 O
2.0 to 5.0

Al 2 O 3
2.5 to 3.5

P 2 O 5
 2.5 to 7.0.

7. Method according to claim 1 , in which the starting glass furthermore comprises terbium ions.

8. Method according to claim 1 for the preparation of a lithium silicate glass with nuclei which are suitable for forming lithium metasilicate and/or lithium disilicate crystals.

9. Method according to claim 1 for the preparation of a lithium silicate glass ceramic which comprises lithium metasilicate as main crystal phase and/or comprises more than 10 vol.-% lithium metasilicate crystals.

10. Method according to claim 9 , wherein the lithium metasilicate glass ceramic comprises more than 20 vol.-% lithium metasilicate crystals.

11. Method according to claim 1 for the preparation of a lithium silicate glass ceramic which comprises lithium disilicate as main crystal phase and/or comprises more than 10 vol.-% lithium disilicate crystals.

12. Method according to claim 11 , wherein the lithium silicate glass ceramic comprises more than 20 vol.-% lithium disilicate crystals.

13. Method according to claim 1 , in which the starting glass is subjected to at least one heat treatment in the range of from 450 to 950° C. in order to form a lithium silicate glass with nuclei which are suitable for forming lithium metasilicate and/or lithium disilicate crystals, or a lithium silicate glass ceramic.

14. Method according to claim 1 , in which the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals or the lithium silicate glass ceramic is present in the form of a powder, a blank or a dental restoration.

15. Method according to claim 1 , wherein the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals and the lithium silicate glass ceramic have a fluorescence intensity at 430 nm which is at least 1.5 times the corresponding fluorescence intensity of a reference sample,
wherein the reference sample is obtainable melting a starting glass with the composition: 71.3 wt.-% SiO 2 , 15.1 wt.-% Li 2 O, 3.2 wt.-% K 2 O, 3.5 wt.-% Al 2 O 3 , 3.3 wt.-% P 2 O 5 , 1.5 wt.-% CeO 2 and 0.7 wt.-% Tb 4 O 7 on a scale of 200 g from suitable raw materials in a platinum-rhodium crucible at 1500° C. for 1 h, pouring 30 g of the glass melt into a pre-heated mould to produce a glass block, and converting the glass block into a glass ceramic by successive temperature treatments at 500° C. for 10 min, 700° C. for 20 min and 850° C. for 10 min, wherein the heating rates between the temperature treatments are 30 K/min in each case.

16. Method according to claim 1 , wherein the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals and the lithium silicate glass ceramic have a fluorescence intensity at 541 nm which is at least 1.5 times the corresponding fluorescence intensity of a reference sample,
wherein the reference sample is obtainable as defined in claim 15 .

17. Method according to claim 1 , which further comprises using the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals or the lithium silicate glass ceramic as dental material.

18. Method according to claim 1 , which further comprises using the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals or the lithium silicate glass ceramic for the preparation of dental restorations.

19. Method according to claim 18 , in which the lithium silicate glass, the lithium silicate glass with nuclei suitable for forming lithium metasilicate and/or lithium disilicate crystals or the lithium silicate glass ceramic is shaped by pressing or machining to form the desired dental restoration.

20. Method according to claim 19 , wherein the desired dental restoration is an inlay, onlay, veneer, partial crown, crown or facet.

Assignees

• Ivoclar Vivadent Ag

Inventors

• Krolikowski Sebastian
• Rampf Markus
• Ritzberger Christian
• Bürke Harald
• Holand Wolfram
• Schweiger Marcel

Classifications

• C09K11/77924

  Aluminosilicates · CPC title

• C09K11/7774

  Aluminates · CPC title

• C03C4/12 Primary

  for luminescent glass; for fluorescent glass · CPC title

• C03C4/0021

  for dental use · CPC title

• C03C3/112

  containing fluorine · CPC title