Reducing the susceptibility of titanium nitride optical layers to crack

• US 6,707,610 B1
• Filed: 09/20/2002
• Issued: 03/16/2004
• Est. Priority Date: 09/20/2002
• Status: Active Grant

• Current Assignee: Solutia Singapore Pte. Ltd. (Eastman Chemical Company)
• Original Assignee: Hüper Optik International Pte Ltd. (Eastman Chemical Company), Southwall Technologies, Inc. (Eastman Chemical Company)
• Inventors: Dai, Yisheng, Woodard, Floyd E.
• Primary Examiner(s): Juba, Jr., John
• Application Number:
  US10/251,248
• Time in Patent Office: 543 Days
• Field of Search: 359/360, 359/582, 359/585, 359/900, 427/162
• US Class Current: 359/582
• CPC Class Codes: B32B 15/043 of metal B32B15/01 takes precedence
• CPC Class Codes: B32B 15/08 of synthetic resin
• CPC Class Codes: B32B 17/10018 comprising only one glass sheet
• CPC Class Codes: B32B 17/10174 Coatings of a metallic or dielectric material on a constituent layer of glass or polymer
• CPC Class Codes: B32B 2311/18 Titanium
• CPC Class Codes: B32B 2311/22 Nickel or cobalt
• CPC Class Codes: B32B 2367/00 Polyesters, e.g. PET, i.e. polyethylene terephthalate
• CPC Class Codes: B32B 27/36 comprising polyesters
• CPC Class Codes: C03C 17/42 at least one coating of an organic material and at least one non-metal coating
• CPC Class Codes: C23C 14/562 for coating elongated substrates
• CPC Class Codes: Y10S 359/90 Methods

Abstract

In a titanium nitride-based optical coating, the structural stability of the coating is enhanced by providing a damage-retardation base layer between the titanium nitride layer and a substrate. Where the optical coating is to provide solar control, the titanium nitride layer is selected primarily for achieving desired optical characteristics, while the thickness of the damage-retardation layer is selected primarily for achieving desired mechanical characteristics. The damage-retardation layer is formed of a grey metal, with nickel chromium being the preferred metal. The grey metal layer reduces the likelihood that the titanium nitride layer will crack. The tendency of such a layer to crack and form worm tracks is further reduced by exposing the substrate to a plasma preglow and/or by using a slip agent on the side of the substrate on which the layers are to be formed.

Claims

1. A method of providing solar control comprising:

providing a flexible substrate having a first surface; and

providing a damage-retardation layer at said first surface to protect a subsequently formed optical coating, said damage-retardation layer being a grey metal;

providing said optical coating as a titanium nitride-based structure having a titanium nitride layer on a side of said damage-retardation layer opposite to said flexible substrate, thereby forming a coated flexible substrate; and

attaching said coated flexible substrate to a rigid substrate through which solar control is sought;

wherein a thickness of said titanium nitride layer is selected primarily for achieving desired optical characteristics and a thickness of said grey metal is selected primarily for achieving desired mechanical characteristics in retarding damage to said titanium nitride layer, and wherein providing said damage-retardation layer includes selecting a material to achieve desired characteristics with regard to low reflectivity and physical bonding to said titanium nitride layer.

2. The method of claim 1 wherein providing said optical coating consists of depositing said titanium nitride layer as a single-layer solar control coating, said single-layer solar control coating and said damage-retardation layer combining to provide a visible light transmissivity in the range of ten percent to sixty percent.

3. The method of claim 1 wherein providing said grey metal layer is a step of depositing a nickel chromium layer.

4. The method of claim 3 wherein depositing said nickel chromium layer is to a thickness in the range of 1.04 nm to 3.12 nm and wherein providing said titanium nitride layer defines a thickness in the range of 10 nm to 50 nm.

5. The method of claim 3 wherein said nickel chromium and titanium nitride layers are sputter deposited and wherein providing said flexible substrate is a step of providing a generally transparent polymeric substrate having a slip agent on which said titanium nitride is sputter deposited.

6. The method of claim 1 wherein providing said damage-retardation layer includes selecting at least one material from the group Ni, Cr, Ti, W, Zr, Hf, Ta, Nb, Fe, V and Mo in order to achieve said desired characteristics with regard to physical bonding and low reflectivity, wherein a ratio of said thickness of said grey metal to said thickness of said titanium nitride is in the range of 1:

3 to 1;

20.

7. The method of claim 6 further comprising exposing said flexible substrate to a plasma preglow prior to forming said damage-retardation layer on said first surface, thereby reducing susceptibility of said titanium nitride layer to stress cracking after said optical coating is provided.

8. The method of claim 7 further comprising providing a slip agent at said first surface of said flexible substrate such that said susceptibility is further reduced.

9. An optical member comprising:

a flexible polymeric substrate;

a grey metal layer on said polymeric substrate, said grey metal layer having a thickness in the range of 1 nm to 20 nm;

a single-layer optical coating of titanium nitride, said optical coating having a thickness in the range of 10 nm to 50 nm and having a visible light transmissivity in the range of ten percent to sixty percent, said single-layer optical coating being on a side of said grey metal layer opposite to said flexible polymeric substrate; and

a slip agent on a surface of said flexible polymeric substrate upon which said grey metal layer is formed.

10. The optical member of claim 9 wherein said grey metal layer is formed of at least one material selected from the group consisting of Ni, Cr, Ti, W, Zr, Hf, Ta, Nb, Fe, V and Mo.

11. The optical member of claim 9 wherein said grey metal layer is a nickel chromium layer.

12. The optical member of claim 9 wherein said flexible polymeric substrate is a transparent web of PET.

13. A method of forming an optical member comprising:

providing a generally transparent substrate;

forming a layer of NiCr on a first surface of said substrate; and

forming a single-layer solar control coating in contact with said layer of NiCr, said solar control coating being a TiN layer;

wherein forming said layer of NiCr includes selecting a layer thickness at least partially based upon inhibiting cracking of said TiN layers, and wherein forming said single-layer solar control coating includes selecting a layer thickness primarily based on achieving a target level of transmissivity of visible light, said layer thickness of said NiCr thereby functioning to provide structural stability of said TiN layer which is dimensioned to determine optical characteristics.

14. The method of claim 13 wherein:

forming said layer of NiCr includes sputtering NiCr to said layer thickness in the range of 1 nm to 20 nm; and

forming said TiN layer includes sputtering TiN to a thickness in the range of 10 nm to 50 nm, said TiN layer and said layer of NiCr combining to provide a visible light transmissivity in the range of ten percent to sixty percent.

15. The method of claim 13 further comprising exposing said transparent substrate to a plasma preglow prior to forming said layer of NiCr.

16. The method of claim 15 wherein said step of exposing includes using at least one of oxygen, nitrogen and argon in providing said plasma preglow.

17. The method of claim 15 wherein providing said generally transparent substrate includes using a polymeric substrate having a slip agent on a side upon which said layer of NiCr is formed.