IP Library › Granted Patent US 9,561,982
Granted Patent B2
US 9,561,982 · App. 14/244,570 · Granted Feb 7, 2017

Method of cleaning glass substrates

Inventors: Darwin Gene Enicks (Corning, NY); Yoshihiro Nakamura (Shizuoka, JP); Siva Venkatachalam (Painted Post, NY); Wanda Janina Walczak (Big Flats, NY); Liming Wang (Painted Post, NY)
Assignee: CORNING INCORPORATED
C03C23/0075B08B3/08B08B3/12B08B11/04H01L21/02041
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Quick Facts
Patent No.
US 9,561,982
App. No.
14/244,570
Granted
Feb 7, 2017
Kind
B2
Abstract

A method of cleaning thin glass substrates comprises applying a sequence of chemical washing steps as the thin glass substrate is being conveyed in a conveyance direction. In addition, surfaces of the glass substrate may be treated to enhance electrostatic discharge properties of the glass substrates.

Claims (33)

1. An in-line method of removing contaminants from a surface of a glass substrate comprising the steps of:

conveying the glass substrate with a conveying device along a conveyance direction, wherein during the conveying at least one surface of the glass substrate is subjected to a surface treatment comprising, sequentially:

a) exposing the at least one surface of the glass substrate to a liquid discharge comprising ozonated water;

b) exposing the at least one surface of the glass substrate to a liquid discharge of a first base solution, wherein ultrasonic energy is applied to the first base solution at a frequency in a range from about 20 kHz to about 200 kHz;

c) exposing the at least one surface of the glass substrate to a liquid discharge of a second base solution;

d) exposing the at least one surface of the glass substrate to a liquid discharge of a first acid solution to remove metallic ions from the at least one surface of the glass substrate, wherein the first acid solution comprises HCl; and

e) drying the at least one surface of the glass substrate.

2. The method according to claim 1 , further comprising increasing an average surface roughness of the glass substrate by exposing the glass substrate to a liquid discharge of a second acid solution after step d).

3. The method according to claim 2 , wherein the second acid solution comprises HF.

4. The method according to claim 2 , wherein the second acid solution comprises an ammonium bifluoride solution having a molar concentration in a range from about 0.2 M to about 2 M.

5. The method according to claim 2 , wherein the average surface roughness Ra of the glass substrate after increasing the average surface roughness of the glass substrate is in a range from equal to or greater than about 0.2 nm to about 0.8 nm.

6. The method according to claim 1 , wherein the first base solution comprises NH 4 OH:H 2 O 2 :H 2 O having a mixture ratio in a range from about 1:1:5 to about 1:2:80 by volume.

7. The method according to claim 1 , wherein the first base solution is at a temperature in a range from about 40° C. to about 80° C. and the glass substrate is exposed to the first base solution for a time in a range from about 1 minute to about 30 minutes.

8. The method according to claim 1 , wherein a pH of the first base solution is greater than about 10.

9. The method according to claim 1 , further comprising applying megasonic energy to the second base solution at a frequency in a range from about 850 kHz to about 1.2 MHz.

10. The method according to claim 1 , wherein the glass substrate comprises less than 1.6×10 12 atoms/cm 2 of Na, K, Fe, Cu and Zn within 5 nm of the at least one surface after step e).

11. The method according to claim 1 , wherein the at least one surface of the glass substrate comprises less than 0.02 particles/cm 2 having an effective diameter greater than 0.3 microns after step e).

12. An in-line method of removing contaminants from a surface of a glass substrate comprising the steps of:

conveying the glass substrate with a conveying device along a conveyance direction, wherein during the conveying at least one surface of the glass substrate is subjected to a surface treatment comprising, sequentially:

a) exposing the at least one surface of the glass substrate to a liquid discharge comprising ozonated water;

b) exposing the at least one surface of the glass substrate to a liquid discharge of a first base solution;

c) exposing the at least one surface of the glass substrate to a liquid discharge of a second base solution;

d) exposing the at least one surface of the glass substrate to a liquid discharge of a first acid solution to remove metallic ions from the at least one surface of the glass substrate, wherein the first acid solution comprises HCl;

e) drying the at least one surface of the glass substrate; and

wherein an average surface roughness of the glass substrate is increased by exposing the glass substrate to a liquid discharge of a second acid solution.

13. The method according to claim 12 , wherein exposing the glass substrate to a liquid discharge of a second acid solution is performed after step c).

14. The method according to claim 12 , wherein exposing the glass substrate to a liquid discharge of a second acid solution is performed before step c).

15. The method according to claim 12 , wherein the second acid solution comprises HF.

16. The method according to claim 12 , wherein the second acid solution comprises an ammonium bifluoride solution having a molar concentration in a range from about 0.2 M to about 2 M.

17. The method according to claim 12 , wherein the glass substrate comprises less than 1.6×10 12 atoms/cm 2 of Na, K, Fe, Cu and Zn within 10 nm of the at least one surface after step e).

18. The method according to claim 12 , wherein the at least one surface of the glass substrate comprises less than 0.02 particles/cm 2 having an effective diameter greater than 0.3 microns after step e).

19. The method according to claim 12 , further comprising applying ultrasonic energy to the first base solution at a frequency in a range from about 20 kHz to about 200 kHz.

20. The method according to claim 12 , further comprising applying megasonic energy to the second base solution at a frequency in a range from about 850 kHz to about 1.2 MHz.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 7, 2014
From: ENICKS, DARWIN GENE; NAKAMURA, YOSHIHIRO; VENKATACHALAM, SIVA; WALCZAK, WANDA JANINA; WANG, LIMING
To: CORNING INCORPORATED
Reel/Frame 032617/0294 →
Continuity (2)
Provisional Application 61817532 · Apr 30, 2013
Related Publication 20140318578A1 · Oct 30, 2014