IP Library › Granted Patent US 11,884,581
Granted Patent B2
US 11,884,581 · App. 17/894,693 · Granted Jan 30, 2024

Scratch resistant glass and method of making

Inventors: Jaymin Amin (Corning, NY); Xiaoju Guo (Pittsford, NY); Pascale Oram (Hammondsport, NY); Rostislav Vatchev Roussev (Painted Post, NY); Ljerka Ukrainczyk (Ithaca, NY); Taylor Marie Wilkinson (Painted Post, NY)
Assignee: CORNING INCORPORATED
C03C21/002C03C3/093C03C3/125C03C4/18H05K5/0017H05K5/03C03C2204/00
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Quick Facts
Patent No.
US 11,884,581
App. No.
17/894,693
Granted
Jan 30, 2024
Kind
B2
Abstract

Methods of manufacturing a glass-based article includes exposing a glass-based substrate having a lithium aluminosilicate composition to an ion exchange treatment to form the glass-based article. The ion exchange treatment including a molten salt bath having a concentration of a sodium salt in a range from 8 mol % to 100 mol %. The glass-based article includes sodium having a non-zero varying concentration extending from a surface of the glass-based article to a depth of the glass-based article The glass-based article has compressive stress layer extending from the surface to a spike depth of layer from 4 micrometers to 8 micrometers. The glass-based article includes a molar ratio of potassium oxide (K 2 O) to sodium oxide (Na 2 O) averaged over a distance from the surface to a depth of 0.4 micrometers that is greater than or equal to 0 and less than or equal to 1.8.

Claims (60)

1. A method of manufacturing a glass-based article, comprising:

exposing a glass-based substrate having opposing first and second surfaces defining a substrate thickness (t) and having a lithium aluminosilicate composition to an ion exchange treatment comprising a first molten salt bath having a concentration of a sodium salt in a range from 8 mol % to 100 mol % to form the glass-based article,

wherein the glass-based article comprises:

sodium having a non-zero varying concentration extending from a surface of the glass-based article to a depth of the glass-based article;

a compressive layer extending from the surface to a spike depth of layer (DOL spike ) from 4 micrometers to 8 micrometers; and

a molar ratio of potassium oxide (K 2 O) to sodium oxide (Na 2 O) averaged over a distance from the surface to a depth of the glass-based article of 0.4 micrometers that is from 0 to 1.8; and

wherein at least one of the following is satisfied:

a base composition of the glass-based substrate comprises a molar ratio of sodium oxide (Na 2 O) to lithium oxide (Li 2 O) of less than or equal to 0.63; and

at a center of the glass-based article, a molar ratio of sodium oxide (Na 2 O) to lithium oxide (Li 2 O) is less than or equal to 0.63.

2. The method of claim 1 , wherein the glass-based article comprises an average compressive stress (CS avg ) of greater than or equal to 115 MPa over a depth from 15 micrometers to 40 micrometers.

3. The method of claim 1 , wherein the glass-based article comprises a depth of compression (DOC) that is greater than or equal to 0.19t and/or greater than or equal to 150 micrometers.

4. The method of claim 1 , wherein the molar ratio of potassium oxide (K 2 O) to sodium oxide (Na 2 O) is about 0.4 to 1.8.

5. The method of claim 1 , conducted using a single ion exchange treatment, wherein the first molten salt bath comprises:

from 8 mol % to 100 mol % of the sodium salt;

from 0 mol % to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt.

6. The method of claim 5 , wherein the first molten salt bath comprises from about 70 mol % to about 89 mol % of the potassium salt.

7. The method of claim 1 , wherein the exposing further comprises second molten salt bath that follows the first molten salt bath, wherein:

the first molten salt bath comprises:

from 8 mol % to 100 mol % of the sodium salt;

from 0 mol % to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt; and

the second molten salt bath comprises:

from 8 mol % to 100 mol % of a sodium salt;

from 0 mol % to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt.

8. The method of claim 7 , wherein the first molten salt bath comprises from 8 mol % to about 15 mol % of the sodium salt.

9. The method of claim 7 , wherein the first molten salt bath comprises about 80 mol % to 90 mol % of the potassium salt.

10. The method of claim 7 , wherein the first molten salt bath comprises about 4 mol % or less of the lithium salt.

11. The method of claim 1 , wherein the glass-based article comprises a Knoop scratch initiation threshold of greater than or equal to 5 N.

12. The method of claim 1 , wherein the glass-based article comprises compressive stress at a knee (CS knee ) of greater than or equal to 115 MPa, and the DOL spike is greater than or equal to 4.4 micrometers and less than 8 micrometers.

13. The method of claim 1 , wherein the glass-based article has a maximum compressive stress (CS max ) of greater than or equal to 500 MPa.

14. A method of manufacturing a glass-based article, comprising:

exposing a glass-based substrate having opposing first and second surfaces defining a substrate thickness (t) and having a lithium aluminosilicate composition to an ion exchange treatment comprising a first molten salt bath having a concentration of a sodium salt in a range from 8 mol % to 100 mol % to form the glass-based article,

wherein the glass-based article comprises:

sodium having a non-zero varying concentration extending from a surface of the glass-based article to a depth of the glass-based article;

a compressive layer extending from the surface to a spike depth of layer (DOL spike ) from 4 micrometers to 8 micrometers; and

a molar ratio of potassium oxide (K 2 O) to sodium oxide (Na 2 O) averaged over a distance from the surface to a depth of the glass-based article of 0.4 micrometers that is from 0.4 to 1.8.

15. The method of claim 14 , wherein the glass-based article comprises an average compressive stress (CS avg ) of greater than or equal to 115 MPa over a depth from 15 micrometers to 40 micrometers.

16. The method of claim 14 , wherein the glass-based article comprises a depth of compression (DOC) that is greater than or equal to 0.19t and/or greater than or equal to 150 micrometers.

17. The method of claim 14 , conducted using a single ion exchange treatment, wherein the first molten salt bath comprises:

from 8 mol % to 100 mol % of the sodium salt;

from 0 mol % to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt.

18. The method of claim 17 , wherein the first molten salt bath comprises from about 70 mol % to about 89 mol % of the potassium salt.

19. The method of claim 14 , wherein the exposing further comprises a second molten salt bath that follows the first molten salt bath, wherein:

the first molten salt bath comprises:

from 8 mol % to 100 mol % of the sodium salt;

from 0 mol % to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt; and

the second molten salt bath comprises:

from 8 mol % to 100 mol % of a sodium salt;

from 0 mol% to 10 mol % of a lithium salt; and

from 0 mol % to 90 mol % of a potassium salt.

20. The method of claim 19 , wherein the first molten salt bath comprises from 8 mol % to about 15 mol % of the sodium salt.

21. The method of claim 19 , wherein the first molten salt bath comprises about 80 mol % to 90 mol % of the potassium salt.

22. The method of claim 19 , wherein the first molten salt bath comprises about 4 mol % or less of the lithium salt.

23. The method of claim 14 , wherein the glass-based article comprises a Knoop scratch initiation threshold of greater than or equal to 5 N.

24. The method of claim 14 , wherein the glass-based article comprises compressive stress at a knee (CS knee ) of greater than or equal to 115 MPa, and the DOL spike is greater than or equal to 4.4 micrometers and less than 8 micrometers.

25. The method of claim 14 , wherein the glass-based article has a maximum compressive stress (CS max ) of greater than or equal to 500 MPa.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 5, 2023
From: AMIN, JAYMIN; GUO, XIAOJU; ORAM, PASCALE; ROUSSEV, ROSTISLAV VATCHEV; UKRAINCZYK, LJERKA; WILKINSON, TAYLOR MARIE
To: CORNING INCORPORATED
Reel/Frame 065762/0397 →
Continuity (3)
Division 16826473 · Mar 23, 2020
Provisional Application 62826300 · Mar 29, 2019
Related Publication 20220411324A1 · Dec 29, 2022