Method for preparing a coating for protecting a part against oxidation

Patent metadata

Field	Value
Publication number	US-9493873-B2
Application number	US-201214360407-A
Country	US
Kind code	B2
Filing date	Nov 23, 2012
Priority date	Nov 25, 2011
Publication date	Nov 15, 2016
Grant date	Nov 15, 2016

Abstract

A method is disclosed for coating, by means of a chemical vapor deposition (CVD) technique, a part with a coating (PAO) for protecting against oxidation. The method enables the preparation of a refractory coating for protecting against oxidation, having a three-dimensional microstructure, which ensures the protection against oxidation at a high temperature, generally at a temperature above 1200° C., for materials that are sensitive to oxidation, such as composite materials, and in particular carbon/carbon composite materials.

First claim

The invention claimed is:

1. Method for preparing a multilayer coating for protecting against oxidation on at least one surface of at least one part made of at least one material capable of being oxidized, wherein the following successive steps are carried out:
(a) on the surface is deposited a layer of a catalyst enabling the growth of short fibres made of a ceramic that resists oxidation;
(b) on the surface is grown, using a chemical vapour deposition CVD method or a chemical vapour infiltration CVI method, a first layer constituted of particles of a ceramic that resists oxidation, said particles comprising a majority of short fibres made of a ceramic that resists oxidation;
(c) the first layer is coated, using a chemical vapour deposition CVD method or a chemical vapour infiltration CVI method, in a totally homogeneous manner, fibre by fibre and without leaving any porosity, with a second layer made of a refractory ceramic;
(d) the second layer is coated, using a chemical vapour deposition CVD method or a chemical vapour infiltration CVI method, with a third layer made of a ceramic that resists oxidation;
(e) optionally, the third layer is coated, using a chemical vapour deposition CVD method or a chemical vapour infiltration CVI method, with a fourth layer made of a refractory ceramic;
(f) optionally the fourth layer is coated, using a chemical vapour deposition CVD method or a chemical vapour infiltration CVI method, with a fifth layer made of a ceramic that resists oxidation;
(g) optionally steps (e) and (f) are repeated 1 to 100 times;
(h) the part, coated on at least one of its surfaces with a refractory coating for protecting against oxidation, is recovered, said coating having a three-dimensional microstructure up to the third layer or up to the optional fifth layer; the ceramic that resists oxidation being different to the refractory ceramic.

2. Method according to claim 1 , wherein said particles of the first layer comprise 100% short fibres.

3. Method according to claim 1 , wherein the short fibres comprise a majority proportion of short fibres that are substantially perpendicular, or perpendicular, to the surface.

4. Method according to claim 1 , wherein the material capable of being oxidized is selected from materials based on carbon; ceramics, carbide ceramics with the exception of SiC, nitride ceramics; composite ceramics; ultrarefractory metals; and carbon/ceramic composites.

5. Method according to claim 1 , wherein the catalyst enabling the growth of short fibres is selected from particles of diamond; particles of at least one metal, and particles of mixtures and alloys thereof.

6. Method according to claim 1 , wherein the short fibres have a length of 1 nm to 200 μm and a diameter of 50 nm to 1 μm.

7. Method according to claim 1 , wherein the second layer has a thickness of 1 nm to 10 μm.

8. Method according to claim 1 , wherein the third layer has a thickness of 1 nm to 10 μm.

9. Method according to claim 1 , wherein the fourth layer has a thickness of 1 nm to 10 μm.

10. Method according to claim 1 , wherein the fifth layer has a thickness of 1 nm to 10 μm.

11. Method according to claim 1 , wherein all the layers from the second layer have the same thickness.

12. Method according to claim 1 , wherein the refractory ceramic is selected from oxide ceramics, nitride ceramics, boride ceramics, carbide ceramics; mixtures thereof; and composite ceramics thereof.

13. Method according to claim 12 , wherein the refractory ceramic is selected from metal carbides with the exception of SiC; mixtures of said metal carbides with each other, and mixtures of one or more of said metal carbides with SiC; composite ceramics of said metal carbides with each other, and composite ceramics of one or more of said metal carbides with SiC.

14. Method according to claim 1 , wherein the ceramic that resists oxidation is selected from carbide ceramics, nitride ceramics, boride ceramics, oxide ceramics; mixtures thereof; and composite ceramics thereof; the ceramic that resists oxidation being different to the refractory ceramic.

15. Method according to claim 14 , wherein the ceramic that resists oxidation is selected from SiC, TiN, ZrN, HfB 2 , ZrB 2 ; mixtures thereof; and composite ceramics thereof.

16. Method according to claim 1 , wherein the ceramic that resists oxidation is SiC and the refractory ceramic is HfC.

17. Method according to claim 1 , wherein the particles of the first layer, the third layer, the fifth layer and the optional layers made of a ceramic that resists oxidation prepared during step (g) are constituted of a same ceramic; and the second layer, the fourth layer and the optional layers made of a refractory ceramic prepared during step (g) are constituted of a same ceramic.

18. Method according to claim 1 , wherein the refractory coating for protecting against oxidation has a thickness of 4 nm to 1000 μm.

19. Method according to claim 1 , wherein steps (b) to (g) are all carried out continuously in a same chemical vapour deposition CVD or chemical vapour infiltration CVI reactor.

20. Method according to claim 19 , wherein steps (b) to (g), are all carried out at a same pressure of 0.5 to 50 kPa and at a same temperature of 700° C. to 1500° C.

21. Method according to claim 1 , wherein the at least one material capable of being oxidized comprises a carbon/carbon composite material.

22. Method according to claim 1 , wherein the part recovered in step (h) is protected against oxidation from 1200° C. to 2500° C. for up to 10 minutes.

Assignees

• Commissariat Energie Atomique
• Centre Nat Rech Scient

Inventors

• Allemand Alexandre
• Szwedek Olivier
• Epherre Jean-Francois
• Le Petitcorps Yann

Classifications

• C04B41/5057

  Carbides · CPC title

• C23C16/32

  Carbides · CPC title

• C04B41/89 Primary

  for obtaining at least two superposed coatings having different compositions · CPC title

• C04B41/009

  characterised by the material treated · CPC title

• C04B41/5002

  Diamond · CPC title