Organic substrate having optical layers deposited by magnetron sputtering and method for preparing it

• US 6,596,368 B1
• Filed: 01/30/2001
• Issued: 07/22/2003
• Est. Priority Date: 03/26/1998
• Status: Expired due to Term

• Current Assignee: Essilor International SA
• Original Assignee: Essilor International SA
• Inventors: Keller, Gerhard, Comble, Pascal, Liebig, Jöm-Steffen, Kirchhoff, Volker, Bosmans, Richard, Goedicke, Klaus
• Primary Examiner(s): KILIMAN, LESZEK B
• Application Number:
  US09/647,053
• Time in Patent Office: 903 Days
• Field of Search: 428/412, 428/694.XS, 428/64.4, 428/64.7, 428/300, 427/128-130, 359/580, 359/582, 359/586, 359/588, 204/192.15, 204/192.26
• US Class Current: 428/64.4
• CPC Class Codes: C23C 14/0036 Reactive sputtering
• CPC Class Codes: G02B 1/115 Multilayers
• CPC Class Codes: Y10S 428/90 Magnetic feature
• CPC Class Codes: Y10T 428/31507 Of polycarbonate

Abstract

An organic substrate having optically-active layers deposited by magnetron sputtering and a preparation process for it are provided. Gas pressure used for carrying out better adhesion by sputtering is high, comprised between 0.8 and 5.0 Pa. Sputtering is particularly suitable for targets of Si, Ti, Zr and organic substrates with or without anti-abrasive coating. Improved adhesion of thin films is obtained.

Claims

1. An organic substrate having an optically-active stack on at least one side thereof wherein said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, said at least one high refractive index layer being deposited by magnetron sputtering at a pressure of from 1.5 Pa to 5.0 Pa.

2. An organic substrate according to claim 1, wherein said at least one low refractive index layer is deposited by magnetron sputtering at a pressure of from 1.5 Pa to 5.0 Pa.

3. An organic substrate according to claim 1 wherein said magnetron sputtering is carried out at a pressure ranging from 1.5 to 3.5 Pa.

4. An organic substrate according to claim 1 wherein said sputtering is carried out with the substrate being located at least at 90 mm from the magnetron.

6. An organic substrate according to claim 1 wherein said substrate is provided with a scratch resistant hard coating prior to deposition of said optical layers.

7. An organic substrate according to claim 6 wherein said scratch resistant hard coating comprises a polysiloxane matrix including inorganic particles.

8. An organic substrate according to claim 6 wherein said scratch resistant hard coating is obtained by one selected from the group consisting of UV, thermal and electrom beam polymerization.

9. An organic substrate according to claim 1 wherein said substrate is firstly exposed to a low pressure plasma of one selected from the group consisting of argon, oxygen, nitrogen and mixtures thereof, before depositing said optical layers.

10. An organic substrate according to claim 1 wherein said optical layers comprise SiO₂ and TiO₂.

11. An organic substrate according to claim 1 wherein said optical layers comprise SiO₂ and ZrO₂.

12. An organic substrate according to claim 1 wherein said optical layers comprise SiO₂ and Nb₂O₅.

13. An organic substrate according to claim 1 comprising between 2 and 15 optical layers.

14. An organic substrate according to claim 1 wherein said substrate includes an antireflective optically-active stack.

15. An organic substrate according to claim 1 wherein said substrate includes a mirror-like optically-active stack.

16. An organic substrate according to claim 1 wherein said substrate is an ophthalmic lens.

17. An organic substrate according to claim 16 wherein the substrate comprises a polymer obtained by polymerization of one selected from to group consisting of acrylic, allylic, methacrylic and vinylic monomers.

18. An organic substrate according to claim 16 wherein the substrate comprises polycarbonate.

35. An organic substrate according to claim 4 wherein sputtering is carried out with the substrate being located between 90 mm and 200 mm from the magnetron.

42. An organic substrate according to claim 13 wherein all the optical layers are obtained by magnetrons sputtering.

5. An organic substrate having an optically-active stack on at least one side thereof wherein said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index, at least one of said layers being deposited by magnetron sputtering at high pressure from 1.5 to 5.0 Pa, said sputtering being carried out with the substrate being located at least at 90 mm from the magnetron.

36. An organic substrate according to claim 5 wherein at least one of said layers is deposited by magnetron sputtering at high pressure between 1.5 to 3.5 Pa.

37. An organic substrate according to claim 5 wherein sputtering is carried out with the substrate being located between 90 mm and 200 mm from the magnetron.

38. An organic substrate according to claim 36 wherein sputtering is carried out with the substrate being located between 90 mm and 200 mm from the magnetron.

39. An organic substrate according to claim 5 wherein said optical layer comprise SiO₂ and TiO₂.

40. An organic substrate according to claim 5 wherein said optical layer comprise SiO₂ and ZrO₂.

41. An organic substrate according to claim 5 wherein said optical layers comprise SiO₂ and Nb₂O₅.

43. An organic substrate according to claim 5 wherein said substrate is an ophthalmic lens.

44. An organic substrate according to claim 43 wherein the substrate comprises a polymer obtained by polymerization of one selected from the group consisting of acrylic, allylic, methacrylic and vinylic monomers.

45. An organic substrate according to claim 43 wherein the substrate comprises polycarbonate.

19. An organic substrate having an optically-active stack on at least one side thereof wherein said optically-active stack comprises at least one optical layer having a high refractive index and at least one optical layer having a low refractive index comprising depositing at least one of said optical layers by magnetron sputtering at a pressure from 1.5 Pa to 5.0 Pa.

20. The method according to claim 19 wherein the substrate is located at least at 90 mm from the magnetron.

21. The method according to claim 19 wherein said magnetron sputtering is non-reactive magnetron sputtering in argon, followed by an oxidation step in a plasma containing oxygen, said sputtering and oxidation steps being optionally repeated.

22. The method according to claim 19 wherein said magnetron sputtering is partial reactive magnetron sputtering in argon-oxygen mixture, followed by an oxidation step in a plasma containing oxygen, said sputtering and oxidation steps being optionally repeated.

23. The method according to claim 19 wherein said magnetron sputtering is reactive sputtering in an argon-oxygen mixture at high pressure, using a voltage pulsed at a pulse rate of from 10 to 100 kHz.

24. The method according to claim 23 wherein said magnetron sputtering employs a pulsed voltage alternating between two neighboring magnetrons of the same type having the same target material, at a pulse rate of from 10 to 100 kHz.

25. The method according to claim 19 further comprising covering the substrate with a scratch resistant hard coating before depositing said optical layers.

26. The method according to claim 19 comprising exposing the substrate to a low pressure plasma of one selected from the group consisting of argon, oxygen, nitrogen and mixtures thereof, before deposition of said optical layers.

27. The method according to claim 19 comprising adjusting oxygen content of said optical layers by measuring the optical characteristics of the plasma emission, and controlling the oxygen supply as a function of a corresponding signal.

28. The method according to claim 19 comprising adjusting oxygen content of said optical layers by measuring the voltage of reactive magnetron discharge, and controlling the oxygen supply as a function of a corresponding signal.

29. The method according to claim 19 further comprising coating the substrate with an optically-inactive interface layer before deposition of said optical layer, said optically-inactive interface layer being deposited using sputtering technique in a non-reactive or partially reactive mode.

30. The method according to claim 29 wherein said interface layer is deposited by magnetron sputtering of silicon.

31. The method according to claim 29 wherein said interface layer is deposited by magnetron sputtering of titanium.

32. The method according to claim 29 wherein said interface layer is deposited by magnetron sputtering of zirconium.

33. The method according to claim 19 wherein said optically-active stack is simultaneously deposited on both sides of said substrate.

34. The method according to claim 19 wherein said optical layers include ZrO₂ and are deposited at a pressure of at least 1.5 Pa.

46. The method according to claim 19 comprising depositing at least one of said optical layers by magnetron sputtering at a pressure from 1.5 to 3.5 Pa.

47. The method according to claim 19 wherein the substrate is located between 90 mm and 200 mm from the magnetron.

48. The method according to claim 46 wherein the substrate is located between 90 mm and 200 mm from the magnetron.

49. The method according to claim 29 wherein the optically-inactive interface layer is 2 to 10 mm thick.

50. The method according to claim 19 wherein said optical layers comprise ZrO₂.

51. The method according to claim 20 wherein said magnetron sputtering is non-reactive sputtering in argon, followed by oxidation in a plasma containing oxygen, said sputtering and oxidation steps being optionally repeated.

52. The method according to claim 20 wherein said magnetron sputtering is partial reactive magnetron sputtering in argon-oxygen mixture, followed by an oxidation step in a plasma containing oxygen, said sputtering and oxidation steps being optionally repeated.

53. The method according to claim 20 wherein said magnetron sputtering is reactive sputtering in an argon-oxygen mixture at high pressure, using a voltage pulsed at a pulse rate of from 10 to 100 kHz.

54. The method according to claim 53 wherein said magnetron sputtering employs a pulsed voltage alternating between two neighboring magnetrons of the same type having the same target material, at a pulse rate of from 10 to 100 kHz.

55. The method according to claim 20 further comprising covering the substrate with a scratch resistant hard coating before depositing said optical layers.

56. The method according to claim 20 comprising exposing the substrate to a low pressure plasma of one selected from the group consisting of argon, oxygen, nitrogen and mixtures thereof, before deposition of said optical layers.

57. The method according to claim 20 comprising adjusting oxygen content of said optical layers by measuring the optical characteristics of the plasma emission, and controlling the oxygen supply as a function of a corresponding signal.

58. The method according to claim 20 comprising adjusting oxygen content of said optical layers by measuring the voltage of reactive magnetron discharge, and controlling the oxygen supply as a function of a corresponding signal.

59. The method according to claim 20 further comprising coating the substrate with an optically-inactive interface layer before deposition of said optical layer, said optically-inactive interface layer being deposited using sputtering technique in a non-reactive or partially reactive mode.

60. The method according to claim 53 wherein said interface layer is deposited by magnetron sputtering of silicon.

61. The method according to claim 53 wherein said interface layer is deposited by magnetron sputtering of titanium.

62. The method according to claim 53 wherein said interface layer is deposited by magnetron sputtering of zirconium.

63. The method according to claim 53 wherein said optically-active stack is simultaneously deposited on both sides of said substrate.

64. The method according to claim 53 wherein said optical layer comprise ZrO₂.