Process for treatment of thin films based upon metallic oxide or nitride

• US 5,569,362 A
• Filed: 12/13/1993
• Issued: 10/29/1996
• Est. Priority Date: 12/11/1992
• Status: Expired due to Term

• Current Assignee: Saint-Gobain Vitrage International
• Original Assignee: Saint-Gobain Vitrage International
• Inventors: Lerbet, Francois, Pillias, Daniele
• Primary Examiner(s): Kunemund, Robert
• Assistant Examiner(s): MCDONALD, RODNEY GLENN
• Application Number:
  US08/165,493
• Time in Patent Office: 1,051 Days
• Field of Search: 204/192.1, 204/192.11, 204/192.12, 204/192.15, 204/192.23, 204/192.26, 204/192.27, 204/192.28, 204/192.34, 204/298.02, 204/298.04 , 204/298.23, 204/298.25, 204/298.26, 204/192.16, 204/192.3
• US Class Current: 204/192.16
• CPC Class Codes: C03C 17/22 with other inorganic material C03C17/34, C03C17/44 take precedence
• CPC Class Codes: C03C 17/225 Nitrides
• CPC Class Codes: C03C 17/245 by deposition from the vapour phase
• CPC Class Codes: C03C 2217/21 Oxides
• CPC Class Codes: C03C 2217/281 Nitrides
• CPC Class Codes: C03C 2217/282 Carbides, silicides
• CPC Class Codes: C03C 2218/154 by sputtering
• CPC Class Codes: C03C 2218/32 After-treatment

Abstract

A treatment process for the purpose of improving the chemical and/or physical durability of film containing one or more metallic oxides, nitrides, oxynitrides or oxycarbides deposited on a transparent substrate by a cathodic sputtering technique, notably assisted by a magnetic field and preferably reactive in the presence of oxygen. Said process consists of subjecting the film to a low energy ion beam.

Claims

1. A process for increasing the chemical or physical durability of a film deposited on a transparent substrate by a reactive cathodic sputtering technique comprising:

subjecting the film after the deposition to an ion beam wherein the energy of the ions at impact on the film is 200 eV or less, and obtaining a film having a root mean square rugosity of 1.4 nm or less,

wherein the deposition of the film is carried out in sequential steps and at least one of the sequential deposition steps is followed by at least one step of treatment with said ion beam, and

wherein said film comprises a member selected from the group consisting of titanium oxide, titanium nitride, tantalum oxide, tin oxide, zinc oxide, silicon oxide and silicon nitride.

2. The process according to claim 1, wherein the deposition of the film is preceded by a step of pretreating the substrate with an ion beam.

3. The process according to claim 1, wherein at least a portion of said ion beam is selected from the group consisting of ionized oxygen, argon, ionized argon and ionized nitrogen.

4. The process of claim 1 wherein said energy is between 200 and 50 electron-volt.

5. The process of claim 1 wherein said energy is between 80 and 100 electron-volt.

6. The process according to claim 1, wherein the ion beam current density is from 1 to 2.2 mA/cm².

7. The process according to claim 1 wherein, said film has a final thickness of at least 30 nm and each step of sequential deposition is 15 to 25 nanometers;

and each deposition step is followed by said ion beam treatment step.

8. The process according to claim 1 wherein each sequential deposition step has a duration of at most 30 minutes.

9. The process of claim 7 wherein each deposition step has a duration between 1 and 10 minutes.

11. The process of claim 1, wherein the film has a final thickness of less than 30 nm and each step of sequential deposition is approximately 5 nm;

and each deposition step is followed by said ion beam treatment step.

10. A process for the production of panes containing at least one treated film comprising:

forming a film comprising a member selected from the group consisting of titanium oxide, titanium nitride, tantalum oxide, tin oxide, zinc oxide, silicon oxide and silicon nitride on a pane, followed by;

subjecting the film to an ion beam, wherein the energy of the ion beam at impact on the film is 200 eV or less and obtaining panes having a root mean square rugosity of 1.4 nm or less;

wherein the deposition of the film is carried out in sequential steps and at least one of the sequential deposition steps is followed by at least one step of treatment with said ion beam.

12. A process comprising:

forming a film on a transparent substrate by reactive cathodic sputtering, followed by

subjecting the film to an ion beam, thereby forming a film with a root mean square rugosity of 1.4 nm or less,

wherein the energy of the ions at impact on the film is 200 eV or less, and the film comprises a material selected from the group consisting of titanium oxide, titanium nitride, tantalum oxide, tin oxide, zinc oxide, silicon oxide and silicon nitride, and

the deposition of the film is carried out in sequential steps and at least one of the sequential deposition steps is followed by at least one step of treatment with said ion beam.