Halogen gas plasma-resistive members and method for producing the same, laminates, and corrosion-resistant members

• US 20020018921A1
• Filed: 04/16/2001
• Published: 02/14/2002
• Est. Priority Date: 04/18/2000
• Status: Active Grant

• Current Assignee: NGK Insulators Limited
• Original Assignee: NGK Insulators Limited
• Inventors: Katsuda, Yuji, Masuda, Masaaki, Iwasaki, Hiroyuki, Ohashi, Tsuneaki, Harada, Masashi, Yamada, Hirotake, Ito, Shigenori
• Granted Patent: US 6,783,875 B2
• Time in Patent Office: Days
• US Class Current: 428/697
• CPC Class Codes: B32B 18/00 Layered products essentially comprising ceramics, e.g. refractory products
• CPC Class Codes: C04B 2111/00405 Materials with a gradually increasing or decreasing concentration of ingredients or property from one layer to another
• CPC Class Codes: C04B 2111/20 Resistance against chemical, physical or biological attack
• CPC Class Codes: C04B 2235/656 characterised by specific heating conditions during heat treatment
• CPC Class Codes: C04B 2235/6567 Treatment time
• CPC Class Codes: C04B 2237/34 Oxidic
• CPC Class Codes: C04B 2237/343 Alumina or aluminates
• CPC Class Codes: C04B 2237/348 Zirconia, hafnia, zirconates or hafnates
• CPC Class Codes: C04B 2237/52 Pre-treatment of the joining surfaces, e.g. cleaning, machining
• CPC Class Codes: C04B 2237/704 of one or more of the ceramic layers or articles
• CPC Class Codes: C04B 2237/708 of one or more of the interlayers
• CPC Class Codes: C04B 35/10 based on aluminium oxide
• CPC Class Codes: C04B 35/48 based on zirconium or hafnium oxides, zirconates, zircon or hafnates
• CPC Class Codes: C04B 35/63 using additives specially adapted for forming the products , e.g.. binder binders
• CPC Class Codes: C04B 35/63416 Polyvinylalcohols [PVA]; Polyvinylacetates
• CPC Class Codes: C04B 35/63424 Polyacrylates; Polymethacrylates
• CPC Class Codes: C04B 35/6365 Cellulose or derivatives thereof
• CPC Class Codes: C04B 37/005 consisting of glass or ceramic material
• CPC Class Codes: C04B 38/00 Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof treating slag with gases or gas generating material C04B5/06 ; expanded graphite C04B35/536
• CPC Class Codes: C04B 41/0072 Heat treatment
• CPC Class Codes: C04B 41/009 : characterised by the material treated
• CPC Class Codes: C04B 41/4527 : Plasma spraying deposition from the gas phase using plasma C04B41/4533
• CPC Class Codes: C04B 41/4556 : coating or impregnating with a product reacting with the substrate, e.g. generating a metal coating by surface reduction of a ceramic substrate
• CPC Class Codes: C04B 41/5011 : containing halogen in the anion
• CPC Class Codes: C04B 41/5031 : Alumina
• CPC Class Codes: C04B 41/5032 : Aluminates aluminate spinels C04B41/5046
• CPC Class Codes: C04B 41/5045 : Rare-earth oxides
• CPC Class Codes: C04B 41/52 : Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
• CPC Class Codes: C04B 41/522 : Multiple coatings, for one of the coatings of which at least one alternative is described
• CPC Class Codes: C04B 41/87 : Ceramics
• CPC Class Codes: C04B 41/89 : for obtaining at least two superposed coatings having different compositions
• CPC Class Codes: C23C 16/40 : Oxides
• CPC Class Codes: C23C 16/4404 : Coatings or surface treatment on the inside of the reaction chamber or on parts thereof
• CPC Class Codes: C23C 24/08 : by application of heat or pressure and heat C23C24/04 takes precedence
• CPC Class Codes: C23C 26/00 : Coating not provided for in groups C23C2/00 - C23C24/00
• CPC Class Codes: C23C 30/00 : Coating with metallic material characterised only by the composition of the metallic material, i.e. not characterised by the coating process C23C26/00, C23C28/00 take precedence
• CPC Class Codes: C23C 4/00 : Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge build-up welding B23K, e.g. B23K5/18, B23K9/04
• CPC Class Codes: C23C 4/18 : After-treatment
• CPC Class Codes: Y10T 428/249953 : Composite having voids in a component [e.g., porous, cellular, etc.]
• CPC Class Codes: Y10T 428/26 : Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
• CPC Class Codes: Y10T 428/263 : Coating layer not in excess of 5 mils thick or equivalent

Abstract

A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, includes a main body of said member, and a corrosion-resistant film formed at least a surface of said main body, wherein a peeling resistance of the corrosive film to said main body is not less than 15 MPa.

Claims

1. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising a main body of said member, and a corrosion-resistant film formed at least a surface of said main body wherein a peeling resistance of the corrosive film to said main body is not less than 15 MPa.

2. The member set forth in claim 1, wherein a relative density of the corrosion-resistive film is not less than 90%.

3. The member set forth in claim 1, wherein a center-line average surface roughness Ra of the corrosion-resistant film is not more than 1.5 μ

m.

4. The member set forth in claim 1, wherein a center-line average surface roughness Ra of the corrosion-resistant film is not less than 1.2 μ

m

7. The member set forth in any one of claims 1 to 6, wherein a waveness Wa of said corrosion-resistant film is not less than 1.2 μ

m.

8. The member set forth in any one of claims 1 to 6, wherein an underlying face of corrosion-resistant film is porous.

9. The member set forth in any one of claims 1 to 6, wherein a center-line average surface roughness Ra of the underlying face of the corrosion-resistant film is not less than 1.2 μ

m.

10. The member set forth in claim 9, wherein the center-line average surface roughness Ra of the underlying face of the corrosion-resistant film is not more than 2 μ

m

11. The member set forth in any one of claims 1 to 6, wherein an open porosity of said corrosion-resistant film is not more than 1.5 vol %.

12. The member set forth in any one of claims 1 to 6, wherein the corrosion-resistive film is free from cracks having lengths of not less than 3 μ

m and/or widths of not less than 0.1 μ

m.

13. The member set forth in any one of claims 1 to 6, which further comprises an intermediate layer between said main body of the member and said corrosion-resistive film, said intermediate layer having a coefficient of thermal expansion between those of said member main body and said corrosion-resistive film, respectively.

14. The member set forth in any one of claims 1 to 6, which further comprises an intermediate layer between said member main body and said corrosion-resistive film, said intermediate layer comprising a mixture, a solid solution or a reaction product of material of the corrosion-resistive film and a constituting material of the main body.

15. The member set forth in claim 13, wherein the thickness of said intermediate layer is not more than 20 μ

m.

16. The member set forth in claim 14, wherein a concentration ratio of the material of said corrosion-resistive film to the constituting material of the main body in the intermediate layer increases in a direction from a side of the main body to that of the corrosion-resistant film.

17. The member set forth in any one of claims 1 to 6, wherein the material of the corrosion-resistant film comprises a yttrium compound.

18. The member set forth in claim 17, wherein a concentration of iron atoms contained in the corrosion-resistive film is not more than 30 ppm.

19. The member set forth in claim 17, wherein the constituting material of the main body is alumina.

20. The member set forth in any one of claims 1 to 6, wherein the material of the corrosion-resistant film comprises a compound of a rare earth element.

21. The member set forth in any one of claims 1 to 6, wherein the material of the corrosion-resistant film comprises a zirconium compound.

22. A method for producing the halogen gas plasma-resistant member set forth in any one of claims 1 to 21, which comprises the steps of preparing the main body of the member, and forming the corrosion-resistant film on at least the surface of the main body by forming a spray film through melting and spraying the material of the corrosion-resistant film.

23. The method set forth in claim 22, wherein the material of the corrosion-resistant film is sprayed in a low-pressure state.

24. The method set forth in claim 22 or 23, wherein said spray film is thermally treated.

25. The method set forth in claim 22 or 23, wherein the material of the corrosion-resistant film comprises a yttrium compound.

26. The method set forth in claim 22 or 23, wherein the thermally treatment is effected at a temperature of 1400 to 1600°

C.

27. The method set forth in claim 22 or 23, wherein pores in a surface portion of the sprayed film are reduced by depositing the material of the corrosion-resistant film on the sprayed film according to a chemical gas phase growth or an electrochemical gas phase growth.

28. A method for producing the halogen gas plasma-resistant member set forth in any one of claims 1 to 6, which comprises the steps of preparing the main body of the member, and forming the corrosion-resistant film on at least the surface of the main body according to a chemical gas phase growth or an electrochemical gas phase growth.

31. The laminate set forth in claim 29 or 30, wherein said yttrium compound comprises yttria.

32. The laminate set forth in claim 29 or 30, wherein said yttrium compound comprises yttrium fluoride.

42. The laminate set forth in claim 29 or 30, wherein a center-line average surface roughness Ra and a waveness Wa of a surface of the yttrium compound film is 3 to 6 μ

m and 1 to 3 μ

m, respectively.

43. The laminate set forth in claim 29 or 30, wherein a peeling resistance of the yttrium compound film to the substrate is not less than 15 MPa when measured in a Sebastans test with a diameter of a bonded surface being 5.2 mm.

44. A corrosion-resistant member comprising the laminate set forth in claim 29 or 30.

45. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising the laminate set forth in claim 29 or 30 as a substrate.

5. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising a main body of the member, and a corrosion-resistant film formed at least a surface of said main body, wherein a center-line average surface roughness Ra of the corrosion-resistant film is not less than 1.2 μ

m.

6. The member set forth in claim 5, wherein a relative density of the corrosion-resistive film is not less than 90%.

29. A laminate comprising a substrate made of alumina, and a film of a yttrium compound formed on said substrate, wherein a reaction product between alumina and yttrium compound exists along an interface between the substrate and the yttrium compound film.

30. A laminate comprising a substrate made of alumina, a film of a yttrium compound formed on said substrate, and an intermediate layer along an interface between the substrate and the yttrium compound film, said intermediate layer being made of a reaction product between said alumina and said yttrium compound.

33. The laminate set forth in claim 30, wherein said reaction product comprises a crystalline phase composed of a composite oxide of yttria and alumina.

34. The laminate set forth in claim 33, wherein said reaction product comprises a crystalline phase composed of Y₃Al₅O₁₂.

35. The laminate set forth in claim 33, wherein said reaction product comprises a crystalline phase composed of Y₄Al₂O₉.

37. The laminate set forth in claim 36, wherein said yttrium compound comprises yttria.

38. The laminate set forth in claim 36 or 37, wherein said yttrium compound comprises yttrium fluoride.

39. The laminate set forth in claim 36 or 37, wherein said reaction product comprises a crystalline phase composed of Y₃Al₅O₁₂.

40. The laminate set forth in claim 36 or 37, wherein said reaction product comprises a crystalline phase composed of Y₄Al₂O₉.

41. The laminate set forth in claim 36 or 37, which further comprises a microstructure along an interface between the intermediate layer and the substrate, said microstructure comprising fine particles made of a material identical with that of the intermediate layer and voids existing among the fine particles.

36. A laminate comprising a substrate made of alumina, a film of a yttrium compound formed on said substrate, and an intermediate layer along an interface between the substrate and the yttrium compound film, said intermediate layer being made of a crystalline phase of a composite oxide between alumina and yttria.