IP Library › Granted Patent US 11,447,417
Granted Patent B2
US 11,447,417 · App. 16/585,190 · Granted Sep 20, 2022

Enhanced ion exchange methods

Inventors: Qiao Li (Horseheads, NY); Santona Pal (Corning, NY)
Assignee: CORNING INCORPORATED
C03C21/002C03C3/12C03C4/18C03C2201/50
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Quick Facts
Patent No.
US 11,447,417
App. No.
16/585,190
Granted
Sep 20, 2022
Kind
B2
Abstract

Methods of enhanced ion exchange (IOX) include exposing a substrate to a bath mixture that includes a second salt dissolved in a first salt, the second salt includes the same metal ion as the first salt with an anion different from the first salt. The first salts are conventional nitrate salts into which one or more second salts, for example, carbonate, sulfate, chloride, fluorine, borate, or phosphate salts are dissolved. The second salts remain at or below their solubility limits in the first salts. Any poisoning ions remain at or below their solubility limits in the bath mixture. Glass-based articles made therefrom and electronic devices incorporating the glass-based articles are also disclosed.

Claims (42)

1. A glass-based article, comprising:

opposing first and second surfaces defining a thickness (t);

a compressive stress region extending from the first surface of the glass-based article to a depth of compression (DOC);

a spike region extending from the first surface to a potassium depth of layer (DOL K ) of the spike region;

a sodium ion concentration profile, wherein the sodium ion concentration profile comprises a convex region in the spike region.

2. The glass-based article of claim 1 , wherein the convex region is located between the first surface and a depth of 5 μm.

3. The glass-based article of claim 1 , further comprising lithium.

4. The glass-based article of claim 1 , wherein the DOL K is greater than or equal to 5 micrometers.

5. The glass-based article of claim 1 , wherein the ratio of the DOC to the DOL K is greater than 1:1.

6. The glass-based article of claim 1 , wherein DOC is greater than or equal to 30 micrometers.

7. The glass-based article of claim 1 , comprising a compressive stress of greater than or equal to 350 MPa.

8. The glass-based article of claim 7 , wherein the compressive stress is greater than or equal to 500 MPa.

9. The glass-based article of claim 1 , wherein t is in the range of from 50 microns to 10 millimeters.

10. The glass-based article of claim 1 comprising potassium and sodium each at a non-zero concentration that varies from the first surface to at least a portion of the thickness (t).

11. The glass-based article of claim 1 comprising a maximum potassium ion concentration in the spike region.

12. The glass-based article of claim 11 , wherein the center of the glass-based article has a composition comprising:

from greater than or equal to 58 mol % to less than or equal to 65 mol % SiO 2 ;

from greater than or equal to 11 mol % to less than or equal to 19 mol % Al 2 O 3 ;

from greater than or equal to 5.5 mol % to less than or equal to 7 mol % Li 2 O;

from greater than or equal to 0.5 mol % to less than or equal to 3 mol % P 2 O 5 ;

from greater than or equal to 6 mol % to less than or equal to 18 mol % Na 2 O;

from greater than or equal to 0.01 mol % to less than or equal to 1 mol % SnO 2 ; and

from greater than or equal to 0.1 mol % to less than or equal to 2 mol % ZnO, and

the maximum potassium ion concentration of the glass-based article is 10% greater than a comparative glass-based article of the same composition at the center upon treatment in a comparative single molten salt bath comprising potassium nitrate (KNO 3 ) and sodium nitrate (NaNO 3 ) and no potassium carbonate (K 2 CO 3 ).

13. A consumer electronic product comprising:

a housing having a front surface, a back surface, and side surfaces;

electrical components provided at least partially within the housing, the electrical components including at least a controller, a memory, and a display, the display being provided at or adjacent the front surface of the housing; and

a cover disposed over the display;

wherein a portion of at least one of the housing and the cover comprises the glass-based article of claim 1 .

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

exposing a glass-based substrate to a molten salt bath to form the glass-based article, wherein the glass-based substrate contains an alkali metal oxide, the glass-based substrate has opposing first and second surfaces defining a substrate thickness (t), and the molten salt bath comprises:

a first salt including potassium and a first anion;

a second salt that is dissolved in the molten salt bath, and including potassium and a second anion, which is different from the first anion of the first salt; and

a third salt including sodium:

wherein after exposing the glass-based substrate to the molten salt bath, the glass-based article comprises a spike region extending from the first surface to a potassium depth of layer (DOL K ) of the spike region and a sodium ion concentration profile, wherein the sodium ion concentration profile comprises a convex region in the spike region.

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

exposing a glass-based substrate to a molten salt bath to form the glass-based article, wherein the glass-based substrate contains lithium, the glass-based substrate has opposing first and second surfaces defining a substrate thickness (t), and the molten salt bath comprises:

potassium nitrate (KNO 3 );

potassium carbonate (K 2 CO 3 ) that is dissolved in the molten salt bath; and

sodium nitrate (NaNO 3 );

wherein the concentration of the K 2 CO 3 remains at or below its solubility limit in the molten salt bath, and the concentration of lithium ions in the molten salt bath remains at or below their solubility limit in the molten salt bath; and

after exposing the glass-based substrate to the molten salt bath, the glass-based article comprises a spike region extending from the first surface to a potassium depth of layer (DOL K ) of the spike region and a sodium ion concentration profile, wherein the sodium ion concentration profile comprises a convex region in the spike region.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 18, 2021
From: LI, QIAO; PAL, SANTONA
To: CORNING INCORPORATED
Reel/Frame 056354/0561 →
Continuity (2)
Provisional Application 62738415 · Sep 28, 2018
Related Publication 20200102244A1 · Apr 2, 2020