Methods for reducing surface defects

• US 10,351,472 B2
• Filed: 08/09/2017
• Issued: 07/16/2019
• Est. Priority Date: 08/10/2016
• Status: Active Grant

• Current Assignee: Corning Incorporated
• Original Assignee: Corning Incorporated
• Inventors: Amin, Jaymin, Jin, Yuhui, Smith, Kristy Lynn
• Primary Examiner(s): Herring, Lisa L
• Application Number:
  US15/672,567
• Publication Number:
  US 20180044231A1
• Time in Patent Office: 706 Days
• Field of Search: None
• CPC Class Codes: C03C 21/002 to perform ion-exchange between alkali ions C03C21/005 takes precedence
• CPC Class Codes: C03C 21/005 to introduce in the glass such metals or metallic ions as Ag, Cu
• CPC Class Codes: C03C 2204/00 Glasses, glazes or enamels with special properties
• CPC Class Codes: C03C 3/093 containing zinc or zirconium
• CPC Class Codes: C03C 3/097 containing phosphorus, niobium or tantalum
• CPC Class Codes: C03C 4/18 for ion-sensitive glass

Abstract

Methods for reducing a defective area in a strengthened substrate to produce a non-defective substrate are provided. The methods include contacting a strengthened defective substrate with a heated salt bath containing at least one monovalent salt, and removing the strengthened substrate from the bath. The strengthened substrate, before being contacted with the salt bath, is a defective substrate having at least one defective area and one or more non-defective area. Upon removal from the salt bath, at least one defective area has been reduced or substantially removed to produce a non-defective substrate.

Claims

1. A method for removing a defective area in a strengthened substrate comprising:

heating a salt bath comprising at least one monovalent salt to a temperature of from greater than or equal to 95°

C.;

contacting at least a portion of a strengthened substrate with the salt bath, wherein, before the strengthened substrate is contacted with the salt bath, the strengthened substrate has one or more non-defective areas having an average concentration of total metal monovalent cations, and at least one defective area having an average concentration of total metal monovalent cations that deviates from the average concentration of the one or more non-defective areas by greater than or equal to 10 mol %; and

removing the at least a portion of the strengthened substrate from the salt bath, wherein, after removal, the at least one defective area has an average concentration of total metal monovalent cations that deviates from the average concentration of total metal monovalent cations of the one or more non-defective areas by less than 10 mol %, and wherein the strengthened substrate has an Arithmetic Average Roughness (Ra) of greater than or equal to 0.002 μ

m before contact with the salt bath and an Ra of less than 0.002 μ

m after removal from the salt bath, as measured over an area having dimensions of 0.18 mm by 0.13 mm.

2. The method of claim 1, wherein the average concentration of the at least one defective area comprises greater than or equal to 60 mol % of a first metal monovalent cation before the strengthened substrate is contacted with the salt bath and after removing the at least a portion of the strengthened substrate from the salt bath, the average concentration of the at least one defective area comprises less than 60 mol % of the first metal monovalent cation.

3. The method of claim 2, wherein the first metal monovalent cation comprises an alkali metal.

4. The method of claim 1, wherein, before the strengthened substrate is contacted with the salt bath, the at least one defective area has a first metal monovalent cation concentration that deviates from the average metal monovalent cation concentration of the one or more non-defective areas by greater than or equal to 20 mol %.

5. The method of claim 1, wherein, upon removing the at least a portion of the strengthened substrate from the salt bath the at least one defective area has a second metal monovalent cation concentration that deviates from the average metal monovalent cation concentration of total metal monovalent cations of the one or more non-defective areas by less than 5 mol %.

6. A method for producing a non-defective ion-exchanged substrate comprising:

heating a salt bath comprising at least one monovalent salt to a temperature of from greater than or equal to 95°

C. and less than or equal to 430°

C.;

contacting at least a portion of a defective ion-exchanged substrate with the salt bath, wherein, the defective ion-exchanged substrate has an Arithmetic Average Roughness (Ra) of greater than or equal to about 0.002 μ

m, as measured over an area having dimensions of 0.18 mm by 0.13 mm; and

removing the at least a portion of the defective ion-exchanged substrate from the salt bath to produce a non-defective ion-exchanged substrate having an Ra of less than 0.002 μ

m.

7. The method of claim 6, wherein the defective ion-exchanged substrate comprises at least one defect having a height or depth of greater than or equal to at least 1.2 nm and a width or length of greater than or equal to 5 μ

m.

8. The method of claim 6, wherein the non-defective ion-exchanged substrate does not comprise a defect having a height or depth of greater than or equal to at least 8 nm and a width or length of greater than or equal to 0.01 mm.

9. The method of claim 6, wherein the salt bath does not comprise a saturated salt.

10. The method of claim 6, wherein the salt bath does not comprise phosphate or calcium.

11. The method of claim 6, wherein the at least a portion of the defective ion-exchanged substrate is contacted with the salt bath for 10 minutes to 40 hours.

12. The method of claim 6, wherein the salt bath is a molten salt bath and is heated at a temperature of from greater than or equal to 360°

C. and less than or equal to 430°

C.

13. The method of claim 6, wherein the salt bath is an aqueous salt bath and is heated to a temperature of from greater than or equal to 95°

C. and less than or equal to 350°

C.

14. The method of claim 6, wherein the salt bath comprises at least one of Li, Na, K, Rb, Cs, Fr, Ag(I), Au(I), Cu(I), and combinations thereof.

15. The method of claim 6, wherein the salt bath comprises at least one of KNO₃ and NaNO₃.

16. The method of claim 15, wherein the salt bath comprises from about 45 mol % to about 55 mol % NaNO₃ and from about 45 mol % to about 55 mol % KNO₃.

17. The method of claim 6, wherein the defective ion-exchanged substrate comprises glass, glass-ceramic, or combinations thereof.

18. The method of claim 6, wherein the defective ion-exchanged substrate comprises

greater than or equal to 50 mol % SiO₂ and less than or equal to 80 mol % SiO₂;

greater than or equal to 0 mol % B₂O₃ and less than or equal to 5 mol % B₂O₃;

greater than or equal to 5 mol % Al₂O₃ and less than or equal to 30 mol % Al₂O₃;

greater than or equal to 2 mol % Li₂O and less than or equal to 25 mol % Li₂O;

greater than or equal to 0 mol % Na₂O and less than or equal to 15 mol % Na₂O;

greater than or equal to 0 mol % MgO and less than or equal to 5 mol % MgO;

greater than or equal to 0 mol % ZnO and less than or equal to 5 mol % ZnO;

greater than or equal to 0 mol % SnO₂ and less than or equal to 5 mol % SnO₂; and

greater than or equal to 0 mol % P₂O₅ and less than or equal to 10 mol % P₂O₅.

19. A method for removing a defective area in a strengthened substrate comprising:

heating a salt bath comprising at least one monovalent salt to a temperature of from greater than or equal to 95°

C.;

contacting at least a portion of a strengthened substrate with the salt bath, wherein, before the strengthened substrate is contacted with the salt bath, the strengthened substrate has one or more non-defective areas having an average concentration of total metal monovalent cations, and at least one defective area having an average concentration of total metal monovalent cations that deviates from the average concentration of the one or more non-defective areas by greater than or equal to 10 mol %; and

removing the at least a portion of the strengthened substrate from the salt bath, wherein, after removal, the at least one defective area has an average concentration of total metal monovalent cations that deviates from the an average concentration of total metal monovalent cations of the one or more non-defective areas by less than 10 mol %,

wherein the average concentration of the at least one defective area comprises greater than or equal to 60 mol % of a first metal monovalent cation before the strengthened substrate is contacted with the salt bath and after removing the at least a portion of the strengthened substrate from the salt bath, the average concentration of the at least one defective area comprises less than 60 mol % of the first metal monovalent cation.

20. The method of claim 19, wherein the first metal monovalent cation comprises an alkali metal.