Method and apparatus for low-temperature annealing of metallization microstructures in the production of a microelectronic device

• US 7,001,471 B2
• Filed: 08/31/1999
• Issued: 02/21/2006
• Est. Priority Date: 02/04/1998
• Status: Expired due to Fees

• Current Assignee: Applied Materials Incorporated
• Original Assignee: Semitool Incorporated (Applied Materials Incorporated)
• Inventors: Ritzdorf, Thomas L., Dundas, Curt, Stevens, E. Henry, Graham, Lyndon W., Chen, LinLin
• Primary Examiner(s): WYSZOMIERSKI, GEORGE P
• Application Number:
  US09/386,734
• Publication Number:
  US 20020000271A1
• Time in Patent Office: 2,366 Days
• Field of Search: 148/518, 148/536, 148/679, 205/157, 205/224, 205/227
• US Class Current: 148/518
• CPC Class Codes: C25D 17/001 Apparatus specially adapted for electrolytic coating of wafers, e.g. semiconductors or solar cells
• CPC Class Codes: C25D 5/022 using masking means
• CPC Class Codes: C25D 5/50 by heat-treatment
• CPC Class Codes: C25D 7/123 Semiconductors first coated with a seed layer or a conductive layer
• CPC Class Codes: H01L 21/2885 using an external electrical current, i.e. electro-deposition
• CPC Class Codes: H01L 21/67173 in-line arrangement
• CPC Class Codes: H01L 21/6723 comprising at least one plating chamber electroless plating apparatuses C23C, electroplating apparatuses C25D
• CPC Class Codes: H01L 21/76838 characterised by the formation and the after-treatment of the conductors etching for patterning the conductors H01L21/3213
• CPC Class Codes: H01L 21/76877 Filling of holes, grooves or trenches, e.g. vias, with conductive material
• CPC Class Codes: H01L 21/76883 Post-treatment or after-treatment of the conductive material

Abstract

A method for filling recessed microstructures at a surface of a microelectronic workpiece, such as a semiconductor wafer, with metallization is set forth. In accordance with the method, a metal layer is deposited into the microstructures with a process, such as an electroplating process, that generates metal grains that are sufficiently small so as to substantially fill the recessed microstructures. The deposited metal is subsequently subjected to an annealing process at a temperature below about 100 degrees Celsius, and may even take place at ambient room temperature to allow grain growth which provides optimal electrical properties. Various novel apparatus for executing unique annealing processes are also set forth.

Claims

1. A method for reducing voids in a metal material that has been electrolytically deposited into recessed microstructures defined in a surface of a microelectronic workpiece comprising:

electrolytically depositing a metal to substantially fill recessed sub-micron structures in the surface of the workpiece; and

then

subjecting the workpiece to an annealing process at a temperature that is at or below about 250 degrees Celsius, the workpiece being subjected to a controlled temperature gradient in which the temperature decreases along a cross-section of the workpiece in a direction that is opposite to the direction of formation of the metal material during its deposition.

2. A method as set forth in claim 1 wherein the metal material comprises copper.

3. The method of claim 1, further comprising depositing a barrier layer on the surface of the workpiece in which the recessed microstructures are formed prior to depositing metal to substantially fill the recessed microstructures.

4. The method of claim 1, further comprising depositing a seed layer, substantially comprised of the same metal to be deposited to substantially fill the recessed microstructures, onto the surface of the workpiece prior to depositing the metal to substantially fill the recessed microstructures.

5. A method for reducing voids in a metal material that has been electrolytically deposited into recessed microstructures defined on a surface of a microelectronic workpiece comprising:

electrolytically depositing a metal to substantially fill recessed sub-micron structures on the surface of the workpiece; and

then

subjecting the workpiece to an annealing process to generate a controlled temperature gradient in which the temperature decreases along a cross-section of the workpiece in a direction that is toward the surface in which the recessed sub-micron structures are formed.

6. The method of claim 5, further comprising depositing a seed layer, substantially comprised of the same metal to be deposited to substantially fill the recessed microstructures, onto the surface of the workpiece prior to depositing the metal to substantially fill the recessed microstructures.

7. A method of processing a microelectronic workpiece having a surface including a sub-micron recessed microstructure, comprising:

electroplating copper at an electroplating station to substantially fill the recessed microstructure and to deposit excess copper above the recessed microstructure;

thereafter, robotically transferring the workpiece from the electroplating station for at least one further process that includes thermal processing at a thermal processing station, the thermal processing comprising thermally treating the electroplated copper by establishing a temperature gradient through the electroplated copper having a maximum gradient temperature of about 60 degrees Celsius to about 100 degrees Celsius for no longer than 15 minutes, thereby reducing resistivity of the copper and reducing voids which may be present in the copper.

8. The method of claim 7 further comprising removing the excess copper after the thermal processing.

9. The method of claim 8 wherein the excess copper is removed via chemical mechanical polishing.

10. The method of claim 7 wherein the workpiece is thermally treated with a plurality of other workpieces in batch processing fashion.

11. The method of claim 7 wherein the workpiece is thermally treated by flowing a temperature-controlled fluid over a surface of the workpiece.

12. The method of claim 11 wherein the temperature-controlled fluid comprises a gas.

13. The method of claim 11 wherein the temperature-controlled fluid comprises a cooling fluid.

14. The method of claim 7 wherein the workpiece is thermally treated by radiant heating.

15. The method of claim 7 wherein the workpiece is thermally treated by a hot plate.

16. The method of claim 7 further comprising sensing a control temperature and controlling heating of the workpiece in response to the sensed temperature.

17. The method of claim 16 wherein the control temperature is a temperature of a coolant fluid after the fluid is brought into thermal contact with the workpiece.

18. The method of claim 7 wherein the temperature in the temperature gradient decreases in a direction outwardly from the filled recessed microstructure toward the excess copper.

19. The method of claim 7 wherein the temperature gradient induces a stress gradient in the electroplated copper.

20. A method of treating a workpiece having a base having a surface, a dielectric layer carried on the surface of the base, and recessed sub-micron structures formed in the dielectric layer, comprising:

depositing a conductive seed layer exterior to the dielectric layer and in the recessed sub-micron structures;

contacting the seed layer with a copper-containing electroplating solution;

applying electroplating power to the seed layer to electrolytically deposit copper metal from the electroplating solution to substantially fill the recessed sub-micron structures and to deposit excess copper metal which extends beyond an exterior surface of the dielectric layer;

then

subjecting the electroplated workpiece to an elevated temperature annealing process comprising establishing a temperature gradient in which the temperature decreases in a direction moving outwardly from the base toward the dielectric layer, the annealing process having a maximum gradient temperature which is no greater than about 250 degrees Celsius.

21. The method of claim 20 wherein the maximum temperature of the annealing process is at or below about 100 degrees Celsius.

22. The method of claim 20 wherein the maximum temperature of the annealing process is between about 60 degrees Celsius and about 100 degrees Celsius.

23. The method of claim 20 wherein the workpiece is subjected to the annealing process for no longer than 15 minutes.

24. The method of claim 20 wherein the workpiece is subjected to the annealing process for less than one minute.

25. The method of claim 20 further comprising depositing a barrier layer on the dielectric layer and in the sub-micron structures prior to depositing the seed layer.

26. The method of claim 20 wherein the temperature gradient induces a stress gradient in the electroplated copper.

27. The method of claim 20 wherein the electroplating power is initially applied at a first current for a predetermined first period of time, then applied at a higher second current for a predetermined second period of time.

28. The method of claim 20 wherein the electroplating power is applied as a direct current.

29. The method of claim 20 wherein the electroplating power is applied as a pulsed waveform at a frequency of between 1 and 1000 Hz.

30. The method of claim 29 wherein the frequency of the pulsed waveform is between 5 and 20 Hz with a duty cycle of at least 50 percent.

31. The method of claim 20 wherein the workpiece is spun while electroplating power is applied.

32. The method of claim 20 further comprising removing the excess copper after the workpiece is subjected to the elevated temperature annealing process.

33. A method of treating a microelectronic workpiece having a base having a surface including a sub-micron recessed microstructure, comprising:

contacting the surface of the workpiece with a copper-containing electroplating solution;

applying electroplating power at a first power level for a first period of time, then applying electroplating power at a higher second power level for a time sufficient to substantially fill the recessed sub-micron structures with electroplated copper metal and to deposit excess copper metal above the sub-micron recessed microstructures;

then

subjecting the electroplated workpiece to an elevated temperature annealing process comprising establishing a temperature gradient through the electroplated copper metal in which the temperature decreases in a direction moving outwardly from the base toward the workpiece surface, the annealing process having a maximum gradient temperature which is no greater than about 250 degrees Celsius.

34. The method of claim 33 wherein the maximum temperature of the annealing process is at or below about 100 degrees Celsius.

35. The method of claim 33 wherein the maximum temperature of the annealing process is between about 60 degrees Celsius and about 100 degrees Celsius.

36. The method of claim 33 wherein the workpiece is subjected to the annealing process for no longer than 15 minutes.

37. The method of claim 33 wherein the workpiece is subjected to the annealing process for less than one minute.

38. The method of claim 33 further comprising depositing a barrier layer on the dielectric layer and in the sub-micron structures prior to depositing the seed layer.

39. The method of claim 33 wherein the temperature gradient induces a stress gradient in the electroplated copper.

40. The method of claim 33 wherein the seed layer is contacted with the electroplating solution for a predetermined dwell period before the electroplating power is applied.

41. The method of claim 33 wherein the electroplating power is applied as a direct current.

42. The method of claim 33 wherein the electroplating power is applied as a pulsed waveform at a frequency of between 1 and 1000 Hz.

43. The method of claim 42 wherein the frequency of the pulsed waveform is between 5 and 20 Hz with a duty cycle of at least 50 percent.

44. The method of claim 33 wherein the workpiece is spun while electroplating power is applied.

45. The method of claim 33 further comprising removing the excess copper after the workpiece is subjected to the elevated temperature annealing process.

46. A method of treating a microelectronic workpiece having a base having a surface including a sub-micron recessed microstructure, comprising:

contacting the surface of the workpiece with a copper-containing electroplating solution;

applying electroplating power to the workpiece in a pulsed waveform having a frequency of between about 1 and 1000 Hz to substantially fill the recessed sub-micron structures with electroplated copper metal and to deposit excess copper metal above the sub-micron recessed microstructures;

then

subjecting the electroplated workpiece to an elevated temperature annealing process comprising establishing a temperature gradient through the electroplated copper in which the temperature decreases in a direction moving outwardly from the base toward the surface of the workpiece, the temperature gradient having a maximum gradient temperature which is no greater than about 250 degrees Celsius.

47. The method of claim 46 wherein the frequency of the pulsed waveform is between 5 and 20 Hz with a duty cycle of at least 50 percent.

48. The method of claim 46 wherein the maximum temperature of the annealing process is at or below about 100 degrees Celsius.

49. The method of claim 48 wherein the maximum temperature of the annealing process is between about 60 degrees Celsius and about 100 degrees Celsius.

50. The method of claim 46 wherein the workpiece is subjected to the annealing process for no longer than 15 minutes.

51. The method of claim 46 wherein the workpiece is subjected to the annealing process for less than one minute.

52. The method of claim 46 wherein a dielectric is carried on a surface of the base, the sub-micron recessed microstructures being formed in the dielectric layer, the method further comprising depositing a conductive seed layer exterior to the dielectric layer and in the sub-micron recessed microstructues.

53. The method of claim 46 further comprising depositing a barrier layer on the dielectric layer and in the sub-micron structures prior to depositing the seed layer.

54. The method of claim 52 wherein the electroplating power is applied to the seed layer.

55. The method of claim 46 wherein the temperature gradient induces a stress gradient in the electroplated copper.

56. The method of claim 46 wherein the seed layer is contacted with the electroplating solution for a predetermined dwell period before the electroplating power is applied.

57. The method of claim 46 wherein the electroplating power is applied as a direct current.

58. The method of claim 46 wherein the electroplating power is initially applied at a first current for a predetermined first period of time, then applied at a higher second current for a predetermined second period of time.

59. The method of claim 46 wherein the workpiece is spun while electroplating power is applied.

60. The method of claim 46 further comprising removing the excess copper after the workpiece is subjected to the elevated temperature annealing process.

61. A method of processing a microelectronic workpiece having a surface including a sub-micron recessed microstructure and a conductive seed layer in the sub-micron recessed microstructure, comprising:

electroplating copper at an electroplating station to substantially fill the recessed microstructure and to deposit excess copper which extends above the sub-micron recessed microstructure;

robotically transferring the workpiece from the electroplating station for further processing;

removing the excess copper as one of the further processes; and

thereafter, robotically transferring the workpiece to a thermal processing station to thermally treat the electroplated copper by establishing a temperature gradient in the electroplated copper having a maximum temperature of about 60 degrees Celsius to about 100 degrees Celsius for no longer than 15 minutes, thereby reducing resistivity of the copper and reducing voids which may be present in the copper.

62. The method of claim 61 wherein the excess copper is removed via chemical mechanical polishing.

63. The method of claim 61 wherein the microelectronic workpiece is thermally treated with a plurality of other semiconductor workpieces in batch processing fashion.

64. The method of claim 61 wherein the microelectronic workpiece is thermally treated by flowing a temperature-controlled fluid over a surface of the workpiece.

65. The method of claim 64 wherein the temperature-controlled fluid comprises a gas.

66. The method of claim 64 wherein the temperature-controlled fluid comprises a cooling fluid.

67. The method of claim 61 wherein the semiconductor workpiece is thermally treated by radiant heating.

68. The method of claim 61 wherein the semiconductor workpiece is thermally treated by a hot plate.

69. The method of claim 61 further comprising sensing a control temperature and controlling heating of the workpiece in response to the sensed temperature.

70. The method of claim 69 wherein the control temperature is a temperature of a coolant fluid after the fluid is brought into thermal contact with the workpiece.

71. The method of claim 61 wherein the temperature in the temperature gradient decreases in a direction outwardly from the filled recessed microstructure toward the excess copper.

72. The method of claim 61 wherein the temperature gradient induces a stress gradient in the electroplated copper.

73. A method of treating a microelectronic workpiece having a base having a surface including a sub-micron recessed microstructure, comprising:

contacting the surface of the workpiece with a copper-containing electroplating solution;

applying electroplating power at a first power level for a first period of time, then applying electroplating power at a higher second power level for a time sufficient to substantially fill the recessed sub-micron structures with electroplated copper metal and to deposit excess copper metal above the sub-micron recessed microstructures;

then

subjecting the electroplated workpiece to an elevated temperature annealing process for a time sufficient to reduce resistivity of the electroplated copper metal.

74. The method of claim 73 wherein a maximum temperature of the annealing process is at or below about 250 degrees Celsius.

75. The method of claim 73 wherein a maximum temperature of the annealing process is at or below about 100 degrees Celsius.

76. The method of claim 73 wherein a maximum temperature of the annealing process is between about 60 degrees Celsius and about 100 degrees Celsius.

77. The method of claim 73 wherein the workpiece is subjected to the annealing process for no longer than 15 minutes.

78. The method of claim 73 wherein the workpiece is subjected to the annealing process for less than one minute.

79. The method of claim 73 further comprising depositing a barrier layer on the dielectric layer and in the sub-micron structures prior to depositing the seed layer.

80. The method of claim 73 wherein the annealing process comprises establishing a temperature gradient through the electroplated copper metal in which the temperature decreases in a direction moving outwardly from the base toward the workpiece surface, the temperature gradient inducing a stress gradient in the electroplated copper.

81. The method of claim 73 wherein the seed layer is contacted with the electroplating solution for a predetermined dwell period before the electroplating power is applied.

82. The method of claim 73 wherein the electroplating power is applied as a direct current.

83. The method of claim 73 wherein the electroplating power is applied as a pulsed waveform at a frequency of between 1 and 1000 Hz.

84. The method of claim 73 wherein the frequency of the pulsed waveform is between 5 and 20 Hz with a duty cycle of at least 50 percent.

85. The method of claim 73 wherein the workpiece is spun while electroplating power is applied.

86. The method of claim 73 further comprising removing the excess copper after the workpiece is subjected to the elevated temperature annealing process.

87. A method of treating a microelectronic workpiece having a base having a surface including a sub-micron recessed microstructure, comprising:

contacting the surface of the workpiece with a copper-containing electroplating solution;

applying electroplating power to the workpiece in a pulsed waveform having a frequency of between about 1 and 1000 Hz to substantially fill the recessed sub-micron structures with electroplated copper metal and to deposit excess copper metal above the sub-micron recessed microstructures;

then

subjecting the electroplated workpiece to an elevated temperature annealing process for a time sufficient to reduce resistivity of the electroplated copper metal.

88. The method of claim 87 wherein the frequency of the pulsed waveform is between 5 and 20 Hz with a duty cycle of at least 50 percent.

89. The method of claim 87 wherein a maximum temperature of the annealing process is at or below about 250 degrees Celsius.

90. The method of claim 87 wherein a maximum temperature of the annealing process is at or below about 100 degrees Celsius.

91. The method of claim 87 wherein a maximum temperature of the annealing process is between about 60 degrees Celsius and about 100 degrees Celsius.

92. The method of claim 87 wherein the workpiece is subjected to the annealing process for no longer than 15 minutes.

93. The method of claim 87 wherein the workpiece is subjected to the annealing process for less than one minute.

94. The method of claim 87 wherein a dielectric is carried on a surface of the base, the sub-micron recessed microstructures being formed in the dielectric layer, the method further comprising depositing a conductive seed layer exterior to the dielectric layer and in the sub-micron recessed microstructures.

95. The method of claim 94 further comprising depositing a barrier layer on the dielectric layer and in the sub-micron structures prior to depositing the seed layer.

96. The method of claim 99 wherein the electroplating power is applied to the seed layer.

97. The method of claim 87 wherein the annealing process comprises establishing a temperature gradient through the electroplated copper metal in which the temperature decreases in a direction moving outwardly from the base toward the workpiece surface, the temperature gradient inducing a stress gradient in the electroplated copper.

98. The method of claim 87 wherein the seed layer is contacted with the electroplating solution for a predetermined dwell period before the electroplating power is applied.

99. The method of claim 87 wherein the electroplating power is applied as a direct current.

100. The method of claim 87 wherein the electroplating power is initially applied at a first current for a predetermined first period of time, then applied at a higher second current for a predetermined second period of time.

101. The method of claim 87 wherein the workpiece is spun while electroplating power is applied.

102. The method of claim 87 further comprising removing the excess topper after the workpiece is subjected to the elevated temperature annealing process.