Method of treating ceramic fibers by phosphating

Patent metadata

Field	Value
Publication number	US-9802870-B2
Application number	US-201214365255-A
Country	US
Kind code	B2
Filing date	Nov 27, 2012
Priority date	Dec 14, 2011
Publication date	Oct 31, 2017
Grant date	Oct 31, 2017

Abstract

A method of treating silicon carbide fibers comprises phosphating heat treatment in a reactive gas so as to form a coating around each fiber for protection against oxidation. The coating comprises a surface layer of silicon pyrophosphate crystals and at least one underlying bilayer system comprising a layer of a phosphosilicate glass and a layer of microporous carbon.

First claim

The invention claimed is:

1. A method of treating silicon carbide fibers, the method comprising phosphating heat treatment in a reactive gas so as to form a coating around each fiber for protection against oxidation, the coating comprising a surface layer of silicon pyrophosphate crystals and at least one underlying bilayer system comprising a layer of a phosphosilicate glass and a layer of microporous carbon.

2. A method according to claim 1 , wherein before the phosphating heat treatment in a reactive gas, a micro-mesoporous or microporous carbon layer is formed on the surface of each fiber, and after the phosphating heat treatment said micro-mesoporous or microporous carbon layer is interposed between the surface layer of silicon pyrophosphate crystals and said at least one bilayer system comprising a layer of a phosphosilicate glass and a layer of microporous carbon.

3. A method according to claim 2 , wherein the micro-mesoporous carbon layer is formed by etching the surface of each fiber with a phosphorus-containing agent in a gas followed by treatment to eliminate the phosphosilicate glass and the silicon pyrophosphate formed during the etching with the phosphorus-containing agent in a gas.

4. A method according to claim 3 , wherein the treatment for eliminating the phosphosilicate glass and the silicon pyrophosphate is performed by etching the surface of the fibers with a basic compound.

5. A method according to claim 2 , wherein the microporous carbon layer formed before phosphating heat treatment is formed by heat treatment in a reactive gas performed with at least one reactive gas comprising a halogen atom.

6. A method according to claim 5 , wherein the reactive gas comprising a halogen atom further comprises chlorine gas, fluorine gas, or hydrogen chloride.

7. A method according to claim 1 , wherein the protective coating against oxidation presents thickness lying in the range 50 nm to 1 μm.

8. A method according to claim 1 , wherein the phosphating heat treatment in a reactive gas is performed at temperatures lower than the thermal stability temperature of silicon carbide fibers.

9. A method of fabricating a fiber preform comprising forming a fiber structure at least from silicon carbide fibers, wherein the fibers are treated in accordance with the treatment method of claim 1 .

10. A method according to claim 9 , wherein the fibers are treated before forming the fiber structure.

11. A method according to claim 9 , wherein the fibers are treated after forming the fiber structure.

12. A method of fabricating a composite material part comprising making a fiber preform according to the method of claim 9 , and densifying said preform.

Assignees

• Herakles
• Centre Nat Rech Scient

Inventors

• Mazerat Stephane
• Pailler Rene
• Loison Sylvie
• Philippe Eric

Classifications

• B29B11/16

  comprising fillers or reinforcement {(non-woven fabrics per se D04H1/00, D04H3/00)} · CPC title

• B29B15/10

  Coating or impregnating {independently of the moulding or shaping step}(applying liquids in general B05) · CPC title

• C04B2235/5244

  Silicon carbide · CPC title

• C04B35/62873

  Carbon · CPC title

• D06M11/68

  with phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof (with phosphines or diphosphines D06M11/01; with selenium or tellurium compounds D06M11/52; with polyphosphazene or derivatives thereof D06M15/673) · CPC title