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

• US 6,783,875 B2
• Filed: 04/16/2001
• Issued: 08/31/2004
• Est. Priority Date: 04/18/2000
• Status: Expired due to Term

• Current Assignee: NGK Insulators Limited
• Original Assignee: NGK Insulators Limited
• Inventors: Katsuda, Yuji, Iwasaki, Hiroyuki, Harada, Masashi, Yamada, Hirotake, Ito, Shigenori, Masuda, Masaaki, Ohashi, Tsuneaki
• Primary Examiner(s): STEIN, STEPHEN J
• Application Number:
  US09/835,857
• Publication Number:
  US 20020018921A1
• Time in Patent Office: 1,233 Days
• Field of Search: 428/689, 428/697, 428/699, 428/701, 428/702, 428/304.1, 428/332, 428/334, 427/421, 427/427, 427/376.1, 427/248.1
• 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 laminate comprising an alumina substrate and a yttrium compound film formed on said alumina substrate, wherein a reaction product between said alumina and said yttrium compound exists along an interface between said alumina substrate and said yttrium compound film.

3. The laminate set forth in claim 1, wherein said yttrium compound comprises yttria.

4. The laminate set forth in claim 1, wherein said yttrium compound comprises yttrium fluoride.

14. The laminate set forth in claim 1, wherein a surface of said yttrium compound film has a center-line average surface roughness in a range of 3 to 6 μ

m and a surface waveness in a range of 1 to 3 μ

m.

15. The laminate set forth in claim 1, 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.

16. A corrosion-resistant member comprising the laminate set forth in claim 1.

17. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising the laminate set forth in claim 1 as a substrate.

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

5. The laminate set forth in claim 2, wherein said reaction product comprises a crystalline phase composed of a composite oxide of yttria and alumina.

6. The laminate set forth in claim 5, wherein said reaction product comprises a crystalline phase composed of Y₃Al₅O₁₂.

7. The laminate set forth in claim 5, wherein said reaction product comprises a crystalline phase composed of Y₄Al₂O₉.

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

9. The laminate set forth in claim 8, wherein said yttrium compound comprises yttria.

10. The laminate set forth in claim 8, wherein said yttrium compound comprises yttrium fluoride.

11. The laminate set forth in claim 8, wherein said reaction product comprises a crystalline phase composed of Y₃Al₅O₁₂.

12. The laminate set forth in claim 8, wherein said reaction product comprises a crystalline phase composed of Y₄Al₂O₉.

13. The laminate set forth in claim 8, further comprising a microstructure along an interface between said intermediate layer and said substrate, said microstructure comprising fine particles made of a material identical to that of said intermediate layer and voids existing among said fine particles.

18. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising a main body and a corrosion-resistant oxide ceramic film formed at least on a surface of said main body, wherein a peeling resistance of said corrosion-resistant film to said main body is not less than 15 MPa, and wherein a center-line average surface roughness Ra of an underlying face of said corrosion-resistant film is not less than 1.2 mm.

21. The member set forth in claim 18, wherein a relative density of said corrosion-resistant film is not less than 90%.

23. The member set forth in claim 18, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not more than 1.5 mm.

26. The member set forth in claim 18, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not less than 1.2 mm.

29. The member set forth in claim 18, said corrosion-resistant film having a waveness of not less than 1.2 mm.

32. The member set forth in claim 18, wherein an underlying face of said corrosion-resistant film is porous.

35. The member set forth in claim 18, wherein said center-line average surface roughness Ra of said underlying face of the corrosion-resistant film is not more than 2 mm.

36. The member set forth in claim 18, wherein an open porosity of said corrosion-resistant film is not more than 1.5 vol %.

37. The member set forth in claim 18, wherein said corrosion-resistant film is free from cracks having lengths greater than or equal to 3 mm and/or widths greater than or equal to 0.1 mm.

48. A method for producing the halogen gas plasma-resistant member set forth in claim 18, comprising the steps of preparing said main body of said member, and forming said corrosion-resistant film on at least a surface of said main body by melting a material of said corrosion-resistant film and spraying said melted material of said corrosion-resistant film onto said surface of said main body to form a spray film on said surface of said main body.

49. The method set forth in claim 48, wherein said material of said corrosion-resistant film is sprayed in a low-pressure state.

50. The method set forth in claim 48, wherein said spray film is thermally treated.

51. The method set forth in claim 48, wherein said material of said corrosion-resistant film comprises a yttrium compound.

52. The method set forth in claim 50, wherein said thermal treatment is effected at a temperature of 1400 to 1600°

C.

53. The method set forth in claim 48, wherein pores located at a surface portion of said sprayed film are reduced by depositing said material of said corrosion-resistant film on said spray film according to a chemical gas phase growth method or an electrochemical gas phase growth method.

54. A method for producing the halogen gas plasma-resistant member set forth in claim 18, comprising the steps of preparing said main body of said member, and forming said corrosion-resistant film on at least a surface of said main body according to a chemical gas phase growth method or an electrochemical gas phase growth method.

19. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising a main body and a corrosion-resistant oxide ceramic film formed at least on a surface of said main body, said member further comprising an intermediate layer between said main body and said corrosion-resistant film, said intermediate layer having a coefficient of thermal expansion between that of said member main body and said corrosion-resistant film, wherein a peeling resistance of said corrosion-resistant film to said main body is not less than 15 MPa.

22. The member set forth in claim 19, wherein a relative density of said corrosion-resistant film is not less than 90%.

24. The member set forth in claim 19, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not more than 1.5 mm.

27. The member set forth in claim 19, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not less than 1.2 mm.

30. The member set forth in claim 19, said corrosion-resistant film having a waveness of not less than 1.2 mm.

33. The member set forth in claim 19, wherein an underlying face of said corrosion-resistant film is porous.

38. The member set forth in claim 19, wherein said corrosion-resistant film is free from cracks having lengths greater than or equal to 3 mm and/or widths greater than or equal to 0.1 mm.

40. The member set forth in claim 19, wherein a thickness of said intermediate layer is not more than 20 mm.

42. The member set forth in claim 19, wherein said material of said corrosion-resistant film comprises a yttrium compound.

44. The member set forth in claim 19, wherein a concentration of iron atoms contained in said corrosion-resistant film is not more than 30 ppm.

46. The member set forth in claim 19, wherein said material of said main body is alumina.

20. A halogen gas plasma-resistant member to be exposed to a halogen gas plasma, comprising a main body and a corrosion-resistant oxide ceramic film formed at least on a surface of said main body, said member further comprising an intermediate layer between said main body and said corrosion-resistant film, said intermediate layer comprising a mixture, a solid solution or a reaction product of a material of said corrosion-resistant film and a material of said main body, wherein a peeling resistance of said corrosion-resistant film to said main body is not less than 15 MPa.

25. The member set forth in claim 20, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not more than 1.5 mm.

28. The member set forth in claim 20, wherein a center-line average surface roughness Ra of said corrosion-resistant film is not less than 1.2 mm.

31. The member set forth in claim 20, said corrosion-resistant film having a waveness of not less than 1.2 mm.

34. The member set forth in claim 20, wherein an underlying face of said corrosion-resistant film is porous.

39. The member set forth in claim 20, wherein said corrosion-resistant film is free from cracks having lengths greater than or equal to 3 mm and/or widths greater than or equal to 0.1 mm.

41. The member set forth in claim 20, wherein a concentration ratio of said material of said corrosion-resistant film to said material of said main body in said intermediate layer increases in a direction from a side of said main body to that of said corrosion-resistant film.

43. The member set forth in claim 20, wherein said material of said corrosion-resistant film comprises a yttrium compound.

45. The member set forth in claim 20, wherein a concentration of iron atoms contained in said corrosion-resistant film is not more than 30 ppm.

47. The member set forth in claim 20, wherein said material of said main body is alumina.