Process for making of glass articles with optical and easy-to-clean coatings

• US 9,957,609 B2
• Filed: 05/30/2013
• Issued: 05/01/2018
• Est. Priority Date: 11/30/2011
• Status: Active Grant

• Current Assignee: Corning Incorporated
• Original Assignee: Corning Incorporated
• Inventors: Lee, Christopher Morton, Lu, Xiao-feng, Ouyang, Xu, Zhang, Junhong
• Primary Examiner(s): Band, Michael A
• Application Number:
  US13/906,038
• Publication Number:
  US 20130334031A1
• Time in Patent Office: 1,797 Days
• CPC Class Codes: C03C 17/3482 comprising silicon, hydrogenated silicon or a silicide
• CPC Class Codes: C03C 17/42 at least one coating of an organic material and at least one non-metal coating
• CPC Class Codes: C03C 2217/76 Hydrophobic and oleophobic coatings
• CPC Class Codes: C03C 2218/154 by sputtering
• CPC Class Codes: C23C 14/0641 Nitrides C23C14/0617 takes precedence
• CPC Class Codes: C23C 14/0694 Halides
• CPC Class Codes: C23C 14/083 of refractory metals or yttrium
• CPC Class Codes: C23C 14/086 of zinc, germanium, cadmium, indium, tin, thallium or bismuth
• CPC Class Codes: C23C 14/18 on other inorganic substrates
• CPC Class Codes: C23C 14/56 Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
• CPC Class Codes: C23C 14/568 Transferring the substrates through a series of coating stations C23C14/562 takes precedence

Abstract

A process in which both an optical coating, for example, an AR coating, and an ETC coating are deposited on a glass substrate article, in sequential steps, with the optical coating being deposited first and the ETC coating being deposited second, using the same apparatus and without exposing the article to the atmosphere at any time during the application of the optical coating and ETC coating.

Claims

1. A process for vacuum depositing an optical coating and an easy-to-clean (ETC) coating onto a glass substrate, the process comprising:

providing a coating apparatus having an optical coating chamber for deposition of at least one optical coating and an ETC coating chamber for deposition of an ETC coating;

introducing a horizontally-oriented glass substrate to be coated into the optical coating chamber under a pressure of less than or equal to 10<sup>−

4</sup> Torr, the glass substrate having a first surface, a second surface opposite the first surface, and a thickness between the first surface and the second surface,

depositing at least one optical coating onto the glass substrate in the optical coating chamber;

transferring the glass substrate to the ETC coating chamber without breaking vacuum;

reorienting the glass substrate in the ETC coating chamber such that the glass substrate is vertically-oriented;

depositing an ETC coating on the at least one optical coating in the ETC coating chamber, the ETC coating selected from the group consisting of fluoroalkylsilanes, perfluoroalkylsilanes, perfluoroalkyl alkyl silanes, perfluoropolyethersilanes, perfluoropolyether alkoxy silanes, perfluoroalkyl alkoxy silanes, fluoroalkylsilane (non fluoroalkylsilane) copolymers, mixtures of fluoroalkylsilanes, and mixtures thereof; and

removing the glass substrate from the coating apparatus to provide a glass article having the optical coating formed thereon and the ETC coating formed on the optical coating.

2. The process of claim 1, wherein the glass article is post-treated at a temperature of from about 60°

C. to about 200°

C. for a period of time from about 5 minutes to about 60 minutes to facilitate cross-linking between ETC molecules.

3. The process of claim 1, wherein the at least one optical coating is deposited using inline sputtering.

4. The process of claim 3, wherein during inline sputtering, there is a distance between a sputtering source and the glass substrate, wherein the distance is from about 30 mm to about 100 mm.

5. The process of claim 1, wherein the ETC coating is deposited using chemical vapor deposition, physical vapor deposition, electron beam deposition or thermal evaporation source deposition.

6. The process of claim 1, wherein the optical coating is a multilayer coating comprising alternating layers of a high refractive index material H having a refractive index greater than 1.7 and less than or equal to 3.0, and one of (i) a low refractive index material L having a refractive index greater than or equal to 1.3 and less than or equal to 1.6 or (ii) a medium refractive index material M having a refractive index greater than 1.6 and less than or equal to 1.7, laid down in the order H(L or M) or (L or M)H, wherein each H(L or M) or (L or M)H pair of layers is a coating period;

and a thickness of an H layer and an (L or M) layer, independent of each other, in each coating period is from about 5 nm to about 200 nm.

7. The process of claim 6, wherein a number of coating periods in the multilayer coating is from 2 to 20, and the multilayer coating has a thickness from about 100 nm to about 2000 nm.

8. The process of claim 6, wherein if a last layer of a last coating period of the optical coating is a high refractive index layer, a capping layer of SiO₂ is applied over the high refractive index layer.

9. The process of claim 1, wherein the ETC coating source materials are selected from the group consisting of:

a perfluoroalkyl silane of formula (R_F)_ySiX_4-y, where R_F is a linear perfluoroalkyl having a carbon chain length of 6-130 carbon atoms from the silicon atom to an end of the carbon chain at its greatest length, X=Cl, acetoxy, —

OCH₃ or —

OCH₂H₃ and y=1 or 2; and

a perfluoropolyether silane.

10. The process of claim 1, wherein a thickness of the ETC coating is from about 1 nm to about 20 nm.

11. The process of claim 1, wherein the optical coating chamber is divided into an even number of sub-chambers of from 2 to 10, and a coating period of a multilayer optical coating is applied in an odd/even pair of sub-chambers;

wherein the odd numbered sub-chambers are used to deposit either a high refractive index material H or a low refractive index material L and the even numbered sub-chambers are used to deposit the other of the high refractive index material H or the low refractive index material L.

12. The process of claim 1, wherein the glass substrate is selected from the group consisting of borosilicate glass, aluminosilicate glass, soda-lime glass, chemically strengthened borosilicate glass, chemically strengthened aluminosilicate glass and chemically strengthened soda-lime glass, and wherein the glass substrate has a thickness of from about 0.2 mm to about 1.5 mm.

13. The process of claim 1, wherein the glass substrate is an aluminosilicate glass having a compressive stress of greater than 400 MPa and a depth of layer greater than 14 μ

m.