Process for manufacturing glazing comprising a porous layer

Patent metadata

Field	Value
Publication number	US-9394602-B2
Application number	US-201214126767-A
Country	US
Kind code	B2
Filing date	Jun 15, 2012
Priority date	Jun 17, 2011
Publication date	Jul 19, 2016
Grant date	Jul 19, 2016

Abstract

A process for manufacturing glazing including a substrate provided with a coating including a layer consisting of a porous material, includes depositing on the substrate, via a physical vapor deposition (PVD) process in a vacuum chamber, a coating including a layer of a material including an element selected from Si, Ti, Sn, Al, Zr, In or a mixture of at least two of these elements, oxygen and carbon, the layer in addition optionally including hydrogen, heat treatment of the layer thus deposited, under conditions that enable at least one portion of the carbon to be removed and the layer of porous material to be obtained, wherein the deposition is carried out, on the substrate passing through the chamber, by the sputtering of a carbon target, under a reactive plasma atmosphere including a precursor of the element or elements.

First claim

The invention claimed is:

1. A process for manufacturing glazing comprising a substrate provided with a coating comprising at least one layer consisting of a porous material, for which the refractive index is thus reduced thereby, comprising:
depositing on the substrate, via a physical vapor deposition (PVD) process in a vacuum chamber, a coating comprising a layer of a material comprising at least one element selected from Si, Ti, Sn, Al, Zr, In or a mixture of at least two of said elements, oxygen and carbon, said layer in addition optionally comprising hydrogen,
heat treatment of the layer thus deposited, under conditions that enable at least one portion of the carbon to be removed and said layer of porous material to be obtained,
wherein said deposition is carried out, on the substrate passing through said chamber, by the sputtering of a carbon target, under a reactive, plasma atmosphere comprising at least one precursor of the element or elements.

2. The process as claimed in claim 1 , wherein the power applied to the cathode is between 0.5 and 20 kW/m.

3. The process as claimed in claim 1 , wherein the total pressure of the gases in the vacuum chamber is between 0.1 and 2 Pa.

4. The process as claimed in claim 1 , wherein the partial pressure of the precursor or precursors in the chamber is between 0.05 and 1.5 Pa.

5. The process as claimed in claim 1 , wherein the reactive plasma atmosphere essentially consists of a neutral gas such as argon and at least one of the precursors comprises oxygen.

6. The process as claimed in claim 1 , wherein the atmosphere of the reactive plasma comprises the mixture of a neutral gas such as argon and an oxidizing gas such as oxygen.

7. The process as claimed in claim 1 , wherein the atmosphere of the reactive plasma essentially consists of precursors, at least one of which contains oxygen.

8. The process as claimed in claim 1 , wherein the heat treatment is carried out under conditions that enable at least one portion of the carbon to be removed, until a porous layer is obtained wherein the carbon content is less than 15 at %.

9. The process as claimed in claim 1 , wherein the heat treatment of the layer is carried out by heating between 300° C. and 800° C., for a period of less than 1 hour.

10. The process as claimed in claim 1 , wherein use is made, as the element, of silicon or of a mixture of elements predominantly including silicon.

11. The process as claimed in claim 10 , wherein the heat treatment is carried out under conditions that enable at least one portion of the carbon and of the hydrogen to be removed, until a porous layer having a refractive index of less than 1.42 is obtained.

12. The process as claimed in claim 10 , wherein the precursor or precursors are chosen from organometallic compounds of silicon, alkylsilanes, silicon alcoholates, or silicon hydrides, or silicon chlorides.

13. The process as claimed in claim 10 , wherein the thickness of the porous layer, after heat treatment, is between 30 and 150 nm.

14. The process as claimed in claim 1 , wherein use is made, as the element, of titanium or of a mixture of elements predominantly including titanium.

15. The process as claimed in claim 14 , wherein the heat treatment is carried out under conditions that enable at least one portion of the carbon and of the hydrogen to be removed, until a porous layer having a refractive index of less than 2.30 is obtained.

16. The process as claimed in claim 14 , wherein the precursor or precursors of titanium are chosen from organometallic compounds of titanium or titanium alkyl compounds and/or titanium alcoholates.

17. The process as claimed in claim 14 , wherein the porous layer has a photocatalytic activity of antisoiling type.

18. The process as claimed in claim 1 , wherein the substrate is a glass substrate.

19. The process as claimed in claim 1 , wherein the plasma atmosphere is oxidizing.

20. The process as claimed in claim 12 , wherein the organometallic compounds of silicon include siloxanes selected from the group consisting of hexamethyldisiloxane (HMDSO), and TDMSO (tetramethyldisiloxane), wherein the alkylsilanes are selected from the group consisting of diethoxymethylsilane (DEMS), (Si(CH 3 ) 3 ) 2 (HMDS), Si(CH 3 ) 4 (TMS), (SiO(CH 3 ) 2 ) 4 , and (SiH(CH 3 ) 2 ) 2 , wherein the silicon alcoholates are selected from the group consisting of Si(OC 2 H 5 ) 4 (TEOS), and Si(OCH 3 ) 4 (TMOS), wherein the silicon hydrides are selected from the group consisting of SiH 4 and Si 2 H 6 , and wherein the silicon chlorides are selected from the group consisting of SiCl 4 , CH 3 SiCl 3 , (CH 3 ) 2 SiCl 2 .

21. The process as claimed in claim 16 , wherein the precursor or precursors of titanium are selected from the group consisting of Ti tetraisopropylate, diisopropoxytitanium bis(acetylacetonate) and titanium tetraoctylene glycolate, titanium acetylacetonate, titanium methylacetoacetate and titanium ethylacetoacetate.

22. The process as claimed in claim 8 , wherein the heat treatment is carried out under conditions that enable at least one portion of the carbon to be removed, until a porous layer is obtained wherein the carbon content in the porous layer is less than 10 at %.

23. The process as claimed in claim 22 , wherein the heat treatment is carried out under conditions that enable at least one portion of the carbon to be removed, until a porous layer is obtained wherein the carbon content in the porous layer is less than 5 at %.

24. The process as claimed in claim 1 , wherein said deposition is carried out, on the substrate passing through said chamber, by the sputtering of a carbon target, under a reactive, plasma atmosphere comprising at least one precursor of Si, argon, and oxygen.

Assignees

• Kharchenko Andriy
• Rousseau Jean-Paul
• Jung Antje
• Petersen Christian Bernhard
• Saint Gobain

Inventors

• Kharchenko Andriy
• Rousseau Jean-Paul
• Jung Antje
• Petersen Christian Bernhard

Classifications

• C03C2217/425

  consisting of a porous layer · CPC title

• Y10T428/249969

  Of silicon-containing material [e.g., glass, etc.] · CPC title

• C03C17/006

  with materials of composite character · CPC title

• C23C14/0605

  Carbon · CPC title

• C23C14/06

  characterised by the coating material ({C23C14/0021} , C23C14/04 take precedence) · CPC title