Optical quality diamond material

FIELD: technological process.

SUBSTANCE: invention pertains to the technology of obtaining monocrystalline diamond material and can be used in optics for making optical and laser windows, optical reflectors and refractors, diffraction grating and calibration devices. The diamond material is obtained using chemical vapour deposition method (CVDM) in the presence of a controlled nitrogen level, which allows for controlling development of crystal defects and therefore obtain diamond material with basic characteristics, necessary for use in optics.

EFFECT: material with basic characteristics, necessary for use in optics.

75 cl, 8 tbl, 15 ex, 9 dwg

 

The text descriptions are given in facsimile form.

1. Single crystal diamond material obtained by the method of chemical vapour deposition (CVD), which at room temperature is about 20°has at least one of the following characteristics:

I) high optical homogeneity, where the last wave front is different from the expected geometric wavefront passing through the diamond with a certain thickness of at least 0.5 mm, machined to the required flatness, when measured at a particular area, at least 1.3×1.3 mm, less than two bands, one band corresponds to the difference of optical path length equal to 1/2 the wavelength of 633 nm, which perform the measurement;

II) low optical birefringence, indicating a low deformation, so that in about what ASCE with a certain thickness, at least 0.5 mm, when measured by the method described in the present invention, in a particular area, at least 1.3×1.3 mm, the modulus of the sine of the phase shift |sin δ| for, at least 98% of the investigated area of the sample remains of the first order, i.e. δ does not exceed π/2 |sin δ| does not exceed 0,9;

III) low optical birefringence, indicating a low deformation, so that in the sample with a certain thickness of at least 0.5 mm, when measured by the method described in the present invention, in a particular area, at least 1.3×1.3 mm, for 100% of the investigated area of the sample birefringence remains of the first order, i.e. δ does not exceed π/2, and the maximum value of the average value of Δn[average]the difference of the refractive index for light polarized parallel to the slow and fast axes averaged over the entire sample thickness, not exceeding 1,5×10-4;

IV) effective refractive index, which in the sample with a certain thickness of at least 0.5 mm, when measured by the method described in the present invention in a particular area, which constitutes at least 1.3×1.3 mm, has a value 2,3964 when exactly ±0,002;

V) a combination of optical properties, such that the diamond plate is made of diamond material in the form of the coupon with a certain thickness, at least 0.5 mm, when measured by a laser beam with a wavelength near 1.55 mm and a nominal diameter of 1.2 mm in a particular area, at least 1.3×1.3 mm, has an area free of dispersion, which in different parts of the plate varies less than 5×10-3cm-1;

VI) a combination of optical properties, such that the diamond plate is made of diamond material in the form of a solid Etalon Fabry-Perot with a certain thickness of at least 0.5 mm, when measured by a laser beam with a wavelength near 1.55 mm and a nominal diameter of 1.2 mm in a particular area, at least 1.3×1.3 mm, not containing coatings on optical prepared surfaces, has a contrast ratio in different parts of the plate, exceeding 1,5;

VII) a combination of optical properties, such that the insertion loss of the diamond plate, made of diamond material in the form of a standard thickness of at least 0.5 mm, when measured by a laser beam with a wavelength near 1.55 mm and a nominal diameter of 1.2 mm in a particular area, at least 1.3×1.3 mm, not more than 3 dB;

VIII) a change in the refractive index in the analyzed volume containing layer with a certain thickness of at least 0.5 mm, when measured by the method described in this izopet the Institute in a particular area, at least 1.3×1.3 mm, is less than 0,002.

2. Single crystal diamond material according to claim 1, obtained by the CVD method, for which the last wave front is different from the expected geometric wavefront less than 0.5 bars.

3. Single crystal diamond material according to claim 2, obtained by the CVD method, in which the last wave front is different from the expected geometric wavefront less than 0.2 bars.

4. Single crystal diamond material according to claim 1, obtained by the CVD method, in which the module sine of the phase shift |sin δ| for at least 98% of the investigated area remains first order and does not exceed 0,4.

5. Single crystal diamond material according to claim 4 obtained by the method of the HOPF bifurcation, in which the module sine of the phase shift [sin δ| for 100% of the investigated area remains first order and Δn[average]does not exceed 5×10-5.

6. Single crystal diamond material according to claim 1, obtained by the method of the HOPF bifurcation, which is the magnitude of the effective refractive index equal to 2,3964 with accuracy of +/-0,001.

7. Single crystal diamond material according to claim 6, obtained by the method of the HOPF bifurcation, which is the magnitude of the effective refractive index equal to 2,39695 with accuracy of +/-0,0005.

8. Single crystal diamond material according to claim 1, obtained by the method of CVD, whichhas a region free of dispersion, which when measured at different parts of the material changes less than 2×10-3cm-1.

9. Single crystal diamond material of claim 8, obtained by the CVD method, in which the area is free of dispersion varies by less than 5×10-4cm-1.

10. Single crystal diamond material according to claim 1, obtained by the method of the HOPF bifurcation, which is the variation of refractive index within the volume, which is limited to a certain thickness and a certain area, when measured by the method described in the present invention, less than 0,001.

11. Single crystal diamond material of claim 10, obtained by the method of the HOPF bifurcation, which is the variation of refractive index less than 0,0005.

12. Single crystal diamond material according to claim 1, obtained by the method of the HOPF bifurcation, which, if it be made of diamond plate in the form of a solid Etalon Fabry-Perot, has a contrast ratio measured on different areas of the plate with a certain thickness and a certain area in excess of 1.7.

13. Single crystal diamond material according to item 12, obtained by the method of the HOPF bifurcation, which has a contrast ratio exceeding 1.8.

14. Single crystal diamond material according to claim 1, obtained by the method of the HOPF bifurcation, which, if it be made of diamond plate in the form of a solid Etalon f the Bry-Pen, has insertion loss, measured by a laser beam with a wavelength near 1.55 mm in different parts of the plate with a certain thickness and the surface does not exceed 1 dB.

15. Single crystal diamond material according to 14 obtained by the CVD method, in which the insertion loss less than 0.5 dB.

16. Single crystal diamond material obtained by the method of the HOPF bifurcation, which at room temperature is about 20°has at least one of the following characteristics:

I) low and uniform optical scattering, such that the direct scattering 1,064 μm for sample thickness of at least 0.4 mm, measured by the method described in the present invention, in a particular area, at least 1.3×1.3 mm, integrated within the spatial angle of 3.5 87.5° from the last beam, is less than 0.4%;

II) low and uniform optical absorption, such that the coefficient of optical absorption at the wavelength of 1.06 µm sample with a certain thickness of at least 0.5 mm, less than 0,09 cm-1;

III) low and uniform optical absorption, such that the coefficient of optical absorption at the wavelength of 10.6 µm sample with a certain thickness of at least 0.5 mm, less than 0,04 cm-1.

17. Single crystal diamond material according to item 16, obtained IU the Odom CVD, for which direct scattering 1,064 μm, measured for a sample with a certain thickness and area, and is integrated within the spatial angle of 3.5 87.5° from the last beam, less than 0.2%.

18. Single crystal diamond material according to 17 obtained by the method of the HOPF bifurcation, which has a direct scattering 1,064 μm is less than 0.1%.

19. Single crystal diamond material according to item 16, obtained by the CVD method, for which the absorption coefficient at the wavelength of 1.06 μm is less than 0.05 cm-1.

20. Single crystal diamond material according to claim 19, obtained by the CVD method, for which the absorption coefficient at the wavelength of 1.06 μm is less than 0.02 cm-1.

21. Single crystal diamond material according to item 16, obtained by the CVD method, for which the absorption coefficient at a wavelength of 10.6 μm is less than 0.03 cm-1.

22. Single crystal diamond material according to item 21, obtained by the CVD method, for which the absorption coefficient at a wavelength of 10.6 μm is less than or 0.027 cm-1.

23. Single crystal diamond material obtained by the method of the HOPF bifurcation, which at room temperature is about 20°has at least one of the following characteristics:

I) the ability to be treated, providing a high degree of polishing surface, characterized by the value of the arithmetic mean what about the absolute deviation from the mean line of the profile, R ameasured on a particular area, at least 1.3×1.3 mm, less than 2 nm;

II) ability to be processed, providing a high flatness, which when measured in a particular area, at least 1.3×1.3 mm, using a 633 nm radiation, better than 10 bands;

III) the ability to undergo processing, providing high parallelism, which when measured in a particular area, at least 1.3×1.3 mm, better than 1 angular minute.

24. Single crystal diamond material according to item 23, obtained by the method of the HOPF bifurcation, which can be processed up to the surface with Raless than 1 nm.

25. Single crystal diamond material according to paragraph 24, obtained by the method of the HOPF bifurcation, which can be processed up to the surface with Raless than 0.6 nm.

26. Single crystal diamond material according to item 23, obtained by the method of the HOPF bifurcation, which can be processed up to a flatness of better than 1 page.

27. Single crystal diamond material according p obtained by means of CVD, which can be processed up to a flatness of better than 0.3 bars.

28. Single crystal diamond material according to item 23, obtained by the method of the HOPF bifurcation, which can be processed to parallelism better than +/-30 arcsec.

29. Single crystal diamond material according p obtained by the method of the HOPF bifurcation, which is can be processed to parallelism better than +/-15 arcsec.

30. Single crystal diamond material according to one of claims 1, 16 and 23 received by the CVD method, which has at least two of these characteristics.

31. Single crystal diamond material according to claim 1, obtained by the method of the HOPF bifurcation, which has at least three of these characteristics.

32. Single crystal diamond material according p obtained by means of CVD, which has at least four of these characteristics.

33. Single crystal diamond material according to item 16, obtained by the method of the HOPF bifurcation, which has all three of these characteristics.

34. Single crystal diamond material according to item 23, obtained by the method of the HOPF bifurcation, which has all three of these characteristics.

35. Single crystal diamond material according to one of claims 1, 16 and 23 received by the CVD method, for which a certain area of the sample for each of the respective characteristics, if given, is at least a 2.5×2.5 mm

36. Single crystal diamond material according p received by the CVD method, for which a certain area of the sample for each of the respective characteristics, if given, is at least 4×4 mm

37. Single crystal diamond material according to one of claims 1, 16 and 23 received by the CVD method, for which a certain thickness of the sample for each of the relevant the relevant characteristics, if given, is at least 0,8 mm

38. Single crystal diamond material according to clause 37, obtained by the CVD method, for which a certain thickness of the sample for each of the respective characteristics, if given, is at least 1,2 mm

39. Single crystal diamond material obtained by the method of the HOPF bifurcation, which has mechanical strength, as measured by the method described in the present invention, such that at least 70% of the tested samples from at least eight are destroyed when exposed to at least a 2.5 GPA.

40. Single crystal diamond material according to § 39, received by the CVD method, for which at least 70% of the tested samples from at least eight are destroyed when exposed to at least a 3.0 GPA.

41. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, in which the intensity of the luminescence lines 575 nm and 637 nm, normalized to the Raman line, less than 40.

42. Single crystal diamond material according to paragraph 41, received by the CVD method, in which the intensity of the luminescence lines 575 nm and 637 nm, normalized to the Raman line, less than 10.

43. Single crystal diamond material according to § 42, received by the CVD method, in which the intensity of the lines luminesce is of 575 nm and 637 nm, normalized to the Raman line, less than 3.

44. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, in which the conductivity measured at 20°With higher than 1800 WM-1To-1.

45. Single crystal diamond material according to item 44, obtained by the CVD method, in which the conductivity measured at 20°With higher than 2300 WM-1To-1.

46. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, in the form of a plate with opposite main faces, which is ready for use, with the average direction of the dislocations in the plate, constituting more than 30° and the normal to the major faces.

47. Single crystal diamond material according to one of claims 1, 16, 23 and 39, obtained by the method of the HOPF bifurcation, which was annealed, the annealing is part of the process of its receipt.

48. Single crystal diamond material according to one of claims 1, 16, 23 and 39, obtained by the method of the HOPF bifurcation, which was annealed after its receipt.

49. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, having the form of a mechanical layer or an optical layer, or faceted gemstone.

50. Single crystal diamond material according to § 49 received by the CVD method, having the form of a faceted precious stones is.

51. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, the size of which exceeds at least one of the following: (a) the transverse size of 1 mm; b) a second orthogonal transverse size of 1 mm; the thickness of 0.1 mm

52. Single crystal diamond material according to § 51 received by the CVD method, the transverse size of which exceeds 5 mm

53. Single crystal diamond material according to § 51 received by the CVD method, the thickness of which exceeds 0,8 mm

54. Single crystal diamond material according to § 51 received by the CVD method, the dimensions of which exceed at least two of these in a) - C).

55. Single crystal diamond material according to item 54, obtained by the CVD method, the dimensions of which exceed all three are listed in a) - C).

56. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, for use in an optical device or element or as an optical device or element.

57. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, in which according to electron paramagnetic resonance (EPR) of the single nitrogen atoms in the position of substitution of less than 5·1017atom/cm3.

58. Single crystal diamond material according to § 57, obtained by the CVD method, in which according to the EPR of the single atoms of azo is in the position of substitution of less than 2· 1017atom/cm3.

59. Single crystal diamond material according to one of claims 1, 16, 23 and 39 received by the CVD method, in which according to the EPR single nitrogen atoms in the position of substitution of more than 3·1015atom/cm3.

60. Single crystal diamond material according p received by the CVD method, in which according to the EPR single nitrogen atoms in the position of substitution is greater than 1·1016atom/cm3.

61. Single crystal diamond material according p received by the CVD method, in which according to the EPR single nitrogen atoms in the position of substitution is greater than 5·1016atom/cm3.

62. The method of obtaining single-crystal diamond material by the method of chemical vapour deposition (CVD), intended for use in optics, namely, that prepare a diamond substrate having a surface essentially free from crystalline defects, prepare the source gas by dissociation of the source gas to create an atmosphere for the synthesis of nitrogen, in terms of molecular nitrogen, 300 hours/bn up to 5 hours/million and spend homoepitaxially growth of diamond on the surface of the crystal, are essentially free from defect, where the defect density is such that the number of signs of etching the surface relating to defects less than 5·103/mm 2.

63. The method according to item 62, in which the content of nitrogen in the atmosphere, where the synthesis, in terms of molecular nitrogen greater than 500 ppm billion

64. The method according to p, in which the content of nitrogen in the atmosphere, where the synthesis, in terms of molecular nitrogen more than 800 hours/bln

65. The method according to one of PP-64, in which the content of nitrogen in the atmosphere, where the synthesis, in terms of molecular nitrogen is not more than 2 hours/million

66. The method according to p, in which the content of nitrogen in the atmosphere, where the synthesis, in terms of molecular nitrogen is not more than 1.5 hours/million

67. The method according to item 62, in which the nitrogen content is chosen sufficient to prevent or reduce the formation of defects, resulting in local deformation, and at the same time low enough to prevent or reduce unwanted absorption and deterioration in the quality of the crystal.

68. The method according to item 62, in which the defect density is such that the number of signs etching of the surface related to the etching, less than 102/mm2.

69. The method according to item 62, in which the growth of diamond by the method of the HOPF bifurcation occurs on the surface of the {100} diamond substrate.

70. The method according to item 62, in which the nitrogen content as a mole fraction in the total gas volume is determined with an error of less 300 hours/billion or 10% from the target value in the gas phase, while vibirayte value which is more.

71. The method according to item 70, in which the nitrogen content as a mole fraction in the total gas volume is determined with an error of less 100 hours/billion or 3% from the target value in the gas phase, thus choose a value that is greater.

72. The method according to p, in which the nitrogen content as a mole fraction in the total gas volume is determined with an error of less 50 PM/billion or 2% from the target value in the gas phase, thus choose a value that is greater.

73. The method according to item 62, in which the specified properties of the obtained single crystal diamond material is further improved its annealing.

74. Standard, made of single-crystal diamond material according to any one of claims 1 to 61, obtained by the CVD method.

75. Reference for p, which is a standard Fabry-Perot or a standard Fat-Tournoi.



 

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The invention relates to a technology of manufacturing products of high temperature dielectric, insulating materials and technologies of their production by chemical vapor deposition from the gas phase for the manufacture of various components for microwave applications and integrated circuits

FIELD: infra-red optics; production of zinc selenide specimens more than 20 mm in thickness used as passive optic elements of high-power CO2 lasers and other equipment working in infra-red range of long waves.

SUBSTANCE: proposed method includes delivery of hydrogen selenide and zinc vapor by argon flow to substrates heated to temperature of 650-750 C and sedimentation of zinc selenide on them at total pressure of 0.5-1.3 kPa, equimolar flow rates of zinc and hydrogen selenide is equal to 0.4-0.47 l/min and that of argon of 3-4 l/min; temperature of substrates is increased at rate of 0.1-0.15 deg./h throughout the entire period of selenide sedimentation. Zinc selenide obtained by this method has size of grains of 30-80 mcm and possesses the property of absorption at wave length of CO2 not above 5.10-4 cm-1.

EFFECT: enhanced efficiency.

2 cl, 1 ex

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