Lithium disilicate glass-ceramic compositions and methods thereof

Patent metadata

Field	Value
Publication number	US-2024026296-A1
Application number	US-202318376260-A
Country	US
Kind code	A1
Filing date	Oct 3, 2023
Priority date	May 27, 2016
Publication date	Jan 25, 2024
Grant date	—

Abstract

A glass-ceramic composition as defined herein. The glass-ceramic composition includes a first crystalline phase comprising lithium disilicate. The glass-ceramic composition can include up to 10 wt % CaO, up to 5 wt % Na2O, up to 10 wt % B2O3, and greater than 0.5 wt % ZrO2. The glass-ceramic composition can also include from 50 to 75 wt % SiO2, from 1 to 5 wt % Al2O3, from 1 to 8 wt % P2O5, and from 5 to 20 wt % Li2O. In aspects, the glass-ceramic composition can include a second crystalline phase including wollastonite, apatite, cristobalite, β-quartz, lithiophosphate, or a combination thereof. Also disclosed are methods of making and using the disclosed compositions.

First claim

What is claimed is:

1 . A glass-ceramic article, comprising:
a first crystalline phase comprising lithium disilicate; a second crystalline phase selected from a group consisting of: wollastonite, apatite, cristobalite, β-quartz, lithiophosphate, or a combination thereof; and a glass-ceramic composition comprising, based on a 100 wt % total of the glass-ceramic composition:
50 to 75 wt % SiO 2 ,
1 to 5 wt % Al 2 O 3 ,
1 to 8 wt % P 2 O 5 ,
up to 10 wt % CaO,
5 to 20 wt % Li 2 O,
up to 5 wt % Na 2 O,
greater than 0.5 wt % ZrO 2 , and
up to 10 wt % B 2 O 3 .

2 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition comprises, based on a 100 wt % total of the glass-ceramic composition:
50 to 60 wt % SiO 2 , 1 to 3 wt % Al 2 O 3 , 2 to 6 wt % P 2 O 3 , 4 to 8 wt % CaO, 7.5 to 12.5 wt % Li 2 O, 0.5 to 2 wt % Na 2 O, and 1 to 8 wt % ZrO 2 .

3 . The glass-ceramic article of claim 1 , further comprising a compressive stress layer on at least one surface of the glass-ceramic article.

4 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition comprises, based on a 100 wt % total of the glass-ceramic composition, further comprising at least one of:
2 to 10 wt % CaO; 0.5 to 5 wt % Na 2 O; 0.1 to 10 wt % B 2 O 3 ; or combinations thereof.

5 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition comprises, based on a 100 wt % total of the glass-ceramic composition, 2 to 10 wt % CaO.

6 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition comprises, based on a 100 wt % total of the glass-ceramic composition, 0.5 to 5 wt % Na 2 O.

7 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition comprises, 0.1 to 10 wt % B 2 O 3 based on a 100 wt % total of the glass-ceramic composition:

8 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition further comprises from 0.1 to 1.0 wt % F − , based on a 100 wt % total of the glass-ceramic composition.

9 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition has a fracture toughness greater than 1.5 MPa·m 1/2 .

10 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition has a fracture toughness of from 1.4 to 2.0 MPa·m 1/2 .

11 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition has a flexural strength greater than 300 MPa.

12 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition has a strength of from 200 MPa to 500 MPa.

13 . The glass-ceramic article of claim 1 , wherein the glass-ceramic composition further comprises a crystallinity of greater than 80% by volume.

14 . A method of making the glass-ceramic article of claim 1 , the method comprising:
ceramming a precursor glass mixture comprising, based on a 100 wt % total of the precursor glass mixture:
50 to 75 wt % SiO 2 ,
1 to 5 wt % Al 2 O 3 ,
1 to 8 wt % P 2 O 5 ,
up to 10 wt % CaO,
5 to 20 wt % Li 2 O,
up to 5 wt % Na 2 O,
greater than 0.5 wt % ZrO 2 , and
up to 10 wt % B 2 O 3 , by heating the precursor glass mixture at 650° C. to 750° C. for from 0.5 hours to 10 hours and then heating at 750° C. to 850° C. for 0.5 hours to 20 hours; and
ion exchanging the resulting glass-ceramic composition to create at least one compressive stress layer on at least one surface of the glass-ceramic composition to increase mechanical strength, wherein the glass-ceramic article further comprises a second crystalline phase selected from a group consisting of: wollastonite, apatite, cristobalite, β-quartz, lithiophosphate, or a combination thereof.

15 . The method of claim 14 , wherein the precursor glass mixture comprises, based on a 100 wt % total of the precursor glass mixture:
50 to 60 wt % SiO 2 , 1 to 3 wt % Al 2 O 3 , 2 to 6 wt % P 2 O 3 , 4 to 8 wt % CaO, 7.5 to 12.5 wt % Li 2 O, 0.5 to 2 wt % Na 2 O, 1 to 8 wt % ZrO 2 , and 0.1 to 10 wt % B 2 O 3 .

16 . The method of claim 14 , wherein the glass-ceramic composition further comprises a crystallinity of greater than 80% by volume.

17 . The method of claim 14 , wherein the glass-ceramic composition comprises, based on a 100 wt % total of the glass-ceramic composition, further comprising at least one of:
2 to 10 wt % CaO; 0.5 to 5 wt % Na 2 O; 0.1 to 10 wt % B 2 O 3 ; or combinations thereof.

18 . The method of claim 14 , wherein the precursor glass mixture comprises, based on a 100 wt % total of the precursor glass mixture, 2 to 10 wt % CaO.

19 . The method of claim 14 , wherein the precursor glass mixture comprises, based on a 100 wt % total of the precursor glass mixture, 0.5 to 5 wt % Na 2 O.

20 . The method of claim 14 , wherein the precursor glass mixture further comprises a source of 0.1 to 10 wt % B 2 O 3 , based on a 100 wt % total of the precursor glass mixture.

Assignees

• Corning Inc

Inventors

• Deng Huayun
• Fu Qiang
• Mauro John Christopher

Classifications

• C03B32/02

  Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles {(C03B27/012 takes precedence)} · CPC title

• C03C10/0009 Primary

  containing silica as main constituent · CPC title

• C12N5/0654 Primary

  Osteocytes, Osteoblasts, Odontocytes; Bones, Teeth · CPC title

• C03C3/097 Primary

  containing phosphorus, niobium or tantalum · CPC title

• C03C3/111

  containing nitrogen · CPC title