MAYFIELD ROBERT L (US)
TOWSE ROSS W (US)
MAYFIELD ROBERT L (US)
| US6527938B2 | 2003-03-04 | |||
| US3468774A | 1969-09-23 |
WHAT IS CLAIMED IS:
1. A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone comprising the act of exposing the Ti 6/4 alloy in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and create the desired surface topography.
2. The method of claim 1 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
3. The method of claim 1 wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid. 4. The method of claim 3 wherein the aqueous solution comprises from about
16.0 to about 17.3 wt.% citric acid.
5. The method of claim 1 wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid.
6. The method of claim 5 wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid.
7. The method of claim 1 wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid and from about 0.16 to about 0.20 wt.% hydrofluoric acid.
8. The method of claim 1 wherein all of the native oxide is removed from the Ti 6/4 alloy.
9. The method of claim 1 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy.
10. A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone comprising the act of exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
11. The method of claim 10 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. 12. The method of claim 10 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. 13. The method of claim 11 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns.
14. The method of claim 10 wherein the irregularities are cone-shapes.
15. The method of claim 10 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
16. The method of claim 10 wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid.
17. The method of claim 16 wherein the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid. o 18. The method of claim 10 wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid.
19. The method of claim 18 wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid.
20. The method of claim 10 wherein the aqueous solution comprises from s about 16 to about 17.3 wt.% citric acid and from about 0.16 to about 0.20 wt.% hydrofluoric acid.
21. The method of claim 10 wherein all of the native oxide is removed from the Ti 6/4 alloy.
22. The method of claim 10 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. o 23. A method of preparing a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the act of: exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period, 5 wherein the aqueous solution of citric acid and hydrofluoric acid removes substantially all of the native oxide from the Ti 6/4 alloy and forms a modified surface with substantially uniform array of irregularities having peak-to-valley heights less than about 10 microns.
24. The method of claim 23 wherein the implant is a dental implant. 0 25. The method of claim 24 wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components.
26. The method of claim 24 wherein the exposing of the Ti 6/4 alloy is conducted only on a region of the dental implant located outside the gingival end. 27. The method of claim 24 wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
28. The method of claim 23 wherein the exposing of the Ti 6/4 alloy is conducted only on the bone-contacting surface. o 29. The method of claim 23 wherein the irregularities include cone-shaped elements.
30. The method of claim 23 wherein the substantially uniform array of irregularities has peak-to-peak distances of from about 1 to about 3 microns.
31. The method of claim 23 wherein the substantially uniform array of s irregularities has peak-to-valley heights of less than about 5 microns.
32. The method of claim 31 wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 3 microns.
33. The method of claim 23 further including rinsing the desired surface topography so as to remove the residual aqueous solution. o 34. The method of claim 23 wherein the aqueous solution comprises from aboiit 16.0 to about 17.3 wt.% citric acid.
35. The method of claim 34 wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid.
36. The method of claim 23 wherein the aqueous solution comprises from 5 about 0.16 to about 0.20 wt.% hydrofluoric acid.
37. The method of claim 23 wherein all of the native oxide is removed from the Ti 6/4 alloy.
38. The method of claim 23 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy.
39. A method of producing a uniformly roughened surface on Ti 6/4 alloy for 0 contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography.
40. The method of claim 39 wherein performing the initial treatment includes etching the surface with hydrofluoric acid.
41. The method of claim 39 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide.
42. The method of claim 39 further including rinsing the desired surface topography so as to remove the residual aqueous solution. o 43. The method of claim 39 wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid.
44. The method of claim 39 wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid. s 45. The method of claim 39 wherein all of the native oxide is removed from the
Ti 6/4 alloy.
46. The method of claim 39 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy.
47. A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone, the method comprising the acts of: o performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 s microns.
48. The method of claim 47 wherein performing the initial treatment includes etching the surface with hydrofluoric acid.
49. The method of claim 47 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. 0 50. The method of claim 47 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. 51. The method of claim 47 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns.
52. The method of claim 51 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. 53. The method of claim 47 wherein the irregularities are cone-shapes.
54. The method of claim 47 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
55. The method of claim 47 wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid. o 56. The method of claim 47 wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid.
57. The method of claim 47 wherein all of the native oxide is removed from the • Ti 6/4 alloy. s 58. The method of claim 47 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy.
59. A method of preparing a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide o from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. 5 60. The method of claim 59 wherein the implant is a dental implant.
61. The method of claim 60 wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components. 0 62. The method of claim 61 wherein the exposing of the Ti 6/4 alloy is conducted only on a region of the dental implant located outside the gingival end. 82
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63. The method of claim 61 wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
64. The method of claim 59 wherein the exposing of the Ti 6/4 alloy is conducted only on the bone-contacting surface.
65. The method of claim 59 wherein performing the initial treatment includes etching the surface with hydrofluoric acid.
66. The method of claim 59 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. Q 67. The method of claim 59 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns.
68. The method of claim 59 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns.
69. The method of claim 68 wherein the roughened surface has irregularities s with peak-to-valley heights of less than about 3 microns.
70. The method of claim 59 wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid.
71. The method of claim 59 wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. o 72. A method of producing a generally uniformly roughened surface on titanium for contact with living bone comprising the act of exposing the titanium in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium metal surface and create the desired surface topography. 5 73. The method of claim 72 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
74. The method of claim 72 wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid.
75. The method of claim 74 wherein the aqueous solution comprises from Q about 22 to about 23 wt.% citric acid.
76. The method of claim 72 wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid. 77. The method of claim 76 wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid.
78. The method of claim 72 wherein the aqueous solution further includes sulfuric acid. 79. The method of claim 72 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt.% sulfuric acid.
80. The method of claim 72 wherein all of the native oxide is removed from the titanium. o 81. A method of producing a generally uniformly roughened surface on titanium for contact with living bone comprising the act of exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley s heights of less than about 10 microns.
82. The method of claim 81 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns.
83. The method of claim 81 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. o 84. The method of claim 83 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns.
85. The method of claim 81 wherein the irregularities are cone-shapes.
86. The method of claim 81 further including rinsing the desired surface topography so as to remove the residual aqueous solution. 5 87. The method of claim 81 wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid.
88. The method of claim 81 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid.
89. The method of claim 81 wherein the aqueous solution comprises from o about 0.01 to about 1.0 wt.% hydrofluoric acid.
90. The method of claim 89 wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid. 82
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91. The method of claim 81 wherein the aqueous solution further includes sulfuric acid.
92. The method of claim 81 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20% sulfuric acid.
93. The method of claim 81 wherein all of the native oxide is removed from the titanium.
94. A method of preparing a surface of a titanium implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the act of: exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period, wherein the aqueous solution of citric acid and hydrofluoric acid removes substantially all of the native oxide from the titanium and forms a modified surface with substantially uniform array of irregularities having peak-to-valley heights less than about 10 microns.
95. The method of claim 94 wherein the implant is a dental implant.
96. The method of claim 95 wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components.
97. The method of claim 96 wherein the exposing of the titanium is conducted only on a region of the dental implant located outside the gingival end.
98. The method of claim 96 wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
99. The method of claim 94 wherein the exposing of the titanium is conducted only on the bone-contacting surface.
100. The method of claim 94 wherein the irregularities include cone-shaped elements.
101. The method of claim 94 wherein the substantially uniform array of irregularities has peak-to-peak distances of from about 1 to about 3 microns. 102. The method of claim 94 wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 5 microns.
103. The method of claim 102 wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 3 microns. 104. The method of claim 94 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
105. The method of claim 94 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid.
106. The method of claim 105 wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid.
107. The method of claim 94 wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid.
108. The method of claim 94 wherein all of the native oxide is removed from the titanium. 109. A method of producing a generally uniformly roughened surface on titanium for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and after performing the initial treatment, exposing the titanium in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography.
110. The method of claim 109 wherein performing the initial treatment includes etching the surface with hydrofluoric acid.
111. The method of claim 109 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide.
112. The method of claim 109 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
113. The method of claim 109 wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid. 114. The method of claim 109 wherein the aqueous solution further includes sulfuric acid. 82
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115. The method of claim 109 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt. % sulfuric acid.
116. The method of claim 109 wherein all of the native oxide is removed from the titanium.
117. A method of producing a generally uniformly roughened surface on titanium for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and after performing the initial treatment, exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
118. The method of claim 117 wherein performing the initial treatment includes etching the surface with hydrofluoric acid. 119. The method of claim 117 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide.
120. The method of claim 117 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns.
121. The method of claim 117 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns.
122. The method of claim 121 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns.
123. The method of claim 117 wherein the irregularities are cone-shapes.
124. The method of claim 117 further including rinsing the desired surface topography so as to remove the residual aqueous solution.
125. The method of claim 117 wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid.
126. The method of claim 117 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt. % sulfuric acid.
127. The method of claim 117 wherein all of the native oxide is removed from the titanium. 128. A method of preparing a surface of a titanium implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide s from the surface of the titanium; and after performing the initial treatment, exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
129. The method of claim 128 wherein the implant is a dental implant. o 130. The method of claim 129 wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components.
131. The method of claim 130 wherein the exposing of the titanium is conducted s only on a region of the dental implant located outside the gingival end.
132. The method of claim 130 wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
133. The method of claim 130 wherein the exposing of the titanium is conducted 0 only on the bone-contacting surface.
134. The method of claim 130 wherein performing the initial treatment includes etching the surface with hydrofluoric acid.
135. The method of claim 130 wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. 5 136. The method of claim 130 wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns.
137. The method of claim 130 wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns.
138. The method of claim 137 wherein the roughened surface has irregularities 0 with peak-to-valley heights of less than about 3 microns. 82
45 139. The method of claim 128 wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt.% sulfuric acid. |
SURFACE TREATMENT METHODS FOR IMPLANTS MADE OF TITANIUM OR TITANIUM ALLOY
FIELD OF INVENTION
[0001] This present invention relates to methods of producing a surface using titanium 6/4 alloy or titanium and, more specifically, to methods of producing a surface of an implant such as a dental implant using titanium 6/4 alloy or titanium that improves the osseointegration of the implant surface with the bone.
BACKGROUND OF THE INVENTION
[0002] It is known to roughen the surface of implants. Various approaches have been suggested, each producing a unique surface. One approach has been to apply materials to the surface of the implant such as, for example hydroxyapitite, a material that is considered also to improve the bonding of the implant to bone because the hydroxyapitite is chemically related to bone. In a related approach, titanium particles have been sprayed onto a titanium implant to roughen the surface. Roughening can also be done by removing some of the surface. Grit blasting with fine particles has been proposed to create dents and to abrade away some of the surface.
[0003] Another method is the use of acid etching to create a roughened surface. At least one supplier of dental implants has proposed grit blasting to create a coarse roughened surface, followed by acid etching to form a superimposed fine roughening. In a series of U.S. patents, including U.S. Patent Nos. 5,603,338, 5,876,453, 5,863,201, assigned to Implant Innovations Inc., a unique two-step acid treatment was disclosed and is used on dental implants having an Osseotite® surface. The first acid treatment used aqueous hydrofluoric acid to remove the "native oxide", which is the titanium oxide found on titanium metal surfaces. Removing the native oxide is important since it makes the metal surface more easily accessible to etching by other acids that are otherwise unable to uniformly etch the surface of titanium containing native oxide. The second acid treatment desirably used a mixture of hydrochloric and sulfuric acids to etch the exposed titanium surface. A relatively fine etching was achieved, having peak-to-valley heights of 10 microns or less. The peak-to- peak distance typically is about from about 1 to about 3 microns. This Osseotite® surface has
achieved commercial success, having reduced the time required for osseointegration of the titanium implant with bone.
[0004] Previous U.S. patents have shown the titanium surface obtained by scanning electron microscopy (SEM). Another method of describing the surface is surface mapping microscopy (SMM), which produces a computer-generated three-dimensional picture of the region being examined, and several calculated measures of the roughness of the surface. It will be understood by those skilled in the art that acid treatment produces a surface that appears very uniform to the naked eye, but contains variations that become evident only when greatly magnified, as in the photomicrographs. Each region will not be precisely the same as the others, but nevertheless, the variations are small and fall within the general limits discussed above. By carefully controlling the treatment process, each implant has substantially the same surface.
[0005] It would be desirable to improve and simplify existing processes, while still producing a desirable uniform surface.
SUMMARY OF INVENTION
[0006] According to one method, a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone is produced. The Ti 6/4 alloy is exposed in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and create the desired surface topography.
[0007] According to another method, a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone is produced. The Ti 6/4 alloy is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
[0008] According to a further method, a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone is prepared. The surface has a native oxide layer thereon. The Ti 6/4 alloy is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period. The aqueous solution of citric acid and hydrofluoric acid removes substantially
all of the native oxide from the Ti 6/4 alloy and forms a modified surface with substantially uniform array of irregularities having peak-to-valley heights less than about 10 microns. [0009] According to yet another method, a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone is produced. An initial treatment is performed that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy. After performing the initial treatment, the Ti 6/4 alloy is exposed in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography, [0010] According to yet a further method, a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone is produced. An initial treatment is performed that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy. After performing the initial treatment, the Ti 6/4 alloy is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0011] According to another method, a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone is prepared. The surface has a native oxide layer thereon. An initial treatment is performed that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy. After performing the initial treatment, the Ti 6/4 alloy is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
[0012] According to one method, a generally uniformly roughened surface on titanium for contact with living bone is produced. The titanium is exposed in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium surface and create the desired surface topography. [0013] According to another method, a generally uniformly roughened surface on titanium for contact with living bone is produced. The titanium is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
[0014] According to a further method, a surface of a titanium implant that is surgically implantable in living bone is prepared. The titanium is exposed to an aqueous solution of
citric acid and hydrofluoric acid for a suitable time period. The aqueous solution of citric acid and hydrofluoric acid removes substantially all of the native oxide from the titanium and forms a modified surface with substantially uniform array of irregularities having peak-to- valley heights less than about 10 microns.
[0015] According to yet another method, a generally uniformly roughened surface on titanium for contact with living bone is produced. An initial treatment is performed that removes substantially all of the native oxide from the surface of the titanium. After performing the initial treatment, the titanium is exposed in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography. [0016] According to yet a further method, a generally uniformly roughened surface on titanium for contact with living bone is produced. An initial treatment is performed that removes substantially all of the native oxide from the surface of the titanium. After performing the initial treatment, the titanium is exposed to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0017] According to another method, a surface of a titanium implant that is surgically implantable in living bone is prepared. The surface has a native oxide layer thereon. An initial treatment is performed that removes substantially all of the native oxide from the surface of the titanium. After performing the initial treatment, exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
BRIEF DESCRIPTION OF THE DRAWINGS
[0018] FIG. 1 is a front plan view of a dental implant according to one embodiment.
[0019] FIGs. 2a-d are surfaces of a Ti 6/4 alloy dental implant after being exposed by a one step process using citric acid.
[0020] FIGs. 3a-d are surfaces of a Ti 6/4 alloy dental implant after being exposed by a two step process using citric acid.
[0021] FIGs. 4a-d are surfaces of a grade 3 titanium dental implant after being exposed by a one step process using citric acid.
[0022] FIGs. 5a-d are surfaces of a grade 4 titanium dental implant after being exposed by a one step process using citric acid.
[0023] FIGs. 6a-d are surfaces of a grade 3 titanium dental implant after being exposed by a two step process using citric acid.
[0024] FIGs. 7a-d are surfaces of a grade 4 titanium dental implant after being exposed by a two step process using citric acid.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Titanium Alloys
[0025] Titanium alloys have been used in implants such as, for example, dental implants and are typically stronger than the commercially pure grades of titanium. One commonly used titanium alloy, Ti/6A1/4V, generally contains about 6 wt.% aluminum and about 4 wt.% vanadium, hereafter referred to herein as Ti 6/4. One example of a Ti 6/4 alloy that may be used is Ti 6/4 alloy E.L.I, (extra low interstitial). Ti 6/4 alloy E.L.I, is generally referred to as a controlled chemistry version of the standard 6-4 product with lower oxygen content. The aluminum and vanadium content of Ti 6/4 alloy may vary from exactly 6 wt.% aluminum and 4 wt.% vanadium. For example, the Ti 6/4 alloy may comprise from about 5.5 to about 6.5 wt.% aluminum and from about 3.5 to about 4.5 wt.% vanadium.
[0026] Ti 6/4 alloys may have other ingredients that are typically present in trace amounts including, but not limited to, nitrogen, carbon, hydrogen, iron and oxygen. Each of these trace amounts is generally less than 1 wt.% and, more specifically, less than 0.5 or 0.25 wt.%. For example, a Ti 6/4 E.L.I, alloy comprises less than 0.08 wt.% oxygen, less than 0.0125 wt.% hydrogen, less than 0.25 wt.% iron, and less than 0.13 wt.% oxygen. It is contemplated that other Ti 6/4 alloys may be used other than Ti 6/4 E.L.I, alloy.
[0027] One desirable characteristic of titanium alloys is the rapid formation of tenacious titanium oxide films on the surface, which contributes to titanium's resistance to corrosion. This oxide film is believed to be a combination of various oxides of titanium, including TiO, TiO 2 , Ti 2 O 3 , and Ti 3 O 4 . This oxide film is referred to as "native oxide" film. [0028] According to one method, a uniformly roughened surface may be obtained on a Ti 6/4 alloy, which is to contact living bone. One method for obtaining such a uniform roughened surface may be performed in a single step. This method involves exposing the Ti 6/4 alloy in an aqueous solution of citric acid and hydrofluoric (FfF) acid for a suitable time
period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and create the desired surface topography.
[0029] It is desirable to remove substantially all of the native oxide and even more desirable to remove all of the native oxide from the Ti 6/4 alloy during the exposure to the aqueous solution. It is understood by those of ordinary skill in the art, however, that some smaller bits of native oxide may still remain on the Ti 6/4 alloy after exposure to the citric acid and HF acid. The method typically also includes rinsing the desired surface topography so as to remove the residual aqueous solution.
[0030] The aqueous solution generally comprises from about 1 to about 50 wt.% citric acid. More specifically, the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid. Citric acid has a formula of C 6 H 8 O 7 -H 2 O and may be obtained commercially from a variety of sources. For example, citric acid may be obtained from chemical supply houses such as Cole-Parmer Instrument Company or Fisher Scientific, International. The use of citric acid is desirable because it is non-toxic. By using citric acid, it eliminates or reduces the use of more hazardous chemical in the aqueous solution.
[0031] The aqueous solution generally comprises from about 0.1 to about 1.0 wt.% HF acid. More specifically, the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid. Commercially available hydrofluoric acid may be used in the invention.
[0032] The aqueous solution may comprise from about 1 to about 50 wt.% citric acid and from about 0.1 to about 1.0 wt.% HF acid. More specifically, the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid and from about 0.16 to about 0.20 wt.% HF acid.
[0033] The processing conditions for exposing the Ti 6/4 alloy in the aqueous solution of citric acid and HF acid may vary. One non-limiting example of processing conditions for exposing the Ti 6/4 alloy in the aqueous solution of citric acid and HF acid is at a temperature of from about 20 to about 35 0 C for a time period of from about 17 to about 20 minutes. One specific example is a temperature of about 30 0 C and a time period of from about 18 to about
19 minutes. It is contemplated that other temperatures and times may be used for exposing the aqueous solution of citric acid and HF acid to the Ti 6/4 alloy.
[0034] In one embodiment, the one step process of exposing the Ti 6/4 alloy in an aqueous solution of citric acid and HF acid for a suitable time period results in a generally uniform roughened surface having irregularities with peak-to-valley heights of less than about
10 microns. The peak-to-valley heights are measured from the top of the peak to the bottom of the valley. More specifically, the roughened surface has irregularities with peak-to-valley heights of less than about 5 or less than about 3 microns. In one embodiment, the roughened surface generally has irregularities with peak-to-peak distances of from about 1 to about 3 microns. The irregularities may be cone-shaped elements and it is contemplated that such irregularities may be of different shapes. It is contemplated that the irregularities may be in the form of a substantially uniform array.
[0035] As mentioned above, the method for preparing a uniformly roughened surface may be done on an implant (e.g., a dental implant), which is surgically implanted in living bone. One non-limiting example of a dental implant (a screw-type dental implant) is depicted in FIG. 1. A generally cylindrical implant 110 of FIG. 1 includes a bone-interfacing surface 112. The bone-interfacing surface 112 typically includes the entire implant surface beyond a narrow collar region 114 on a side wall of the implant 110 at a gingival end 116 thereof. This narrow collar region 114 desirably includes a first turn 118 of the threaded portion 120 of the implant 110. According to one method, the gingival end 116 and the narrow collar region 114 are not etched because these portions of the implant are normally fabricated with precise dimensions to match abutting components that are eventually attached to the gingival end 116 of the implant 110. Additionally, to minimize the risk of infection, it may be desirable to have a smooth surface on that portion of a dental implant that is not embedded in the bone. It is contemplated, however, that the gingival end and/or the narrow collar region may be etched.
[0036] It is important to remove substantially all the native oxide from the implant surface (e.g., a dental implant surface) that is intended to interface with the living bone so that a substantially uniform surface texture is formed that promotes uniform bonding to the living bone. Thus, the native oxide layer is desirably removed from substantially all of the entire bone-interfacing surface of the implant.
[0037] One method comprises exposing the bone-interfacing portion to an aqueous solution of citric acid and HF acid for a suitable time period. The aqueous solution of citric acid and HF acid removes substantially all of the native oxide from the Ti 6/4 alloy and forms a modified surface. The modified surface generally has irregularities with peak-to-valley heights of less than about 10 microns.
[0038] According to another method, the modified surface may be located only on a portion of the plurality of turns of the thread, hi another method, the modified surface may be located only below a first turn of the plurality of turns that is adjacent to the gingival end. hi yet another embodiment, the aqueous solution of citric acid and HF acid may be exposed to the gingival end.
[0039] Another method of preparing a dental implant involves using a blank of a Ti 6/4 alloy. The blank is machined to produce a desired structure of the dental implant. One example of a dental implant has been discussed and is shown in FIG. 1. It is contemplated that other dental implants may be used instead of dental implant 110 shown in FIG. 1. A surface of the desired structure is exposed to oxygen to naturally form a native oxide layer thereon. After machining, at least a portion of the surface is immersed in a single solution of citric acid and HF acid to remove the native oxide and to produce surface irregularities having a peak-to-valley height less than about 10 microns and, more typically, less than about 5 microns or less than about 3 microns.
[0040] According to another method, a uniformly roughened surface on Ti 6/4 alloy for contact with living bone comprises (a) performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and (b) after performing the initial treatment, exposing the Ti 6/4 alloy in an aqueous solution of citric acid and HF acid for a suitable time period to create the desired surface topography. [0041] The initial treatment may include etching the surface with HF acid. According to another method, the initial treatment includes grit blasting to remove substantially all of the native oxide. The initial treatment as used in this process is used to remove aesthetic surface irregularities (e.g., tooling marks, minor galling) caused during the machining. [0042] It is important to remove substantially all the native oxide from the implant surface (e.g., a dental implant surface) that is intended to interface with the living bone, so that the subsequent treatment of that surface produces a substantially uniform surface texture to promote uniform bonding to the living bone. Thus, the native oxide layer is desirably removed from substantially all of the bone-interfacing surface of the implant. [0043] In one method, the initial treatment includes exposing the Ti 6/4 alloy to HF acid for a time period of from about 45 seconds to a minute at ambient temperature. It is contemplated that the processing conditions of the initial treatment may vary. After this
initial treatment, the Ti 6/4 alloy may be exposed to the aqueous solutions of citric acid and
HF acid such as discussed above.
[0044] In one embodiment, the two step process of exposing the Ti 6/4 alloy results in a generally uniform roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. More specifically, the generally uniform roughened surface has irregularities with peak-to-valley heights of less than about 5 or less than about 3 microns. In one embodiment, the generally uniform roughened surface generally has irregularities with peak-to-peak distances of from about 1 to about 3 microns. The irregularities may be cone- shaped elements and it is contemplated that such irregularities may be of different shapes. It is contemplated that the irregularities may be in the form of a substantially uniform array. [0045] As with the one step process, the two step process using a Ti 6/4 alloy may be used on implant. One example of an implant is a dental implant such as shown in FIG. 1. [0046] Another two step process comprises exposing the bone-interfacing portion to an initial treatment and then exposure to an aqueous solution of citric acid and HF acid for a suitable time period. The initial treatment removes substantially all of the native oxide from the Ti 6/4 alloy and forms a modified surface. The modified surface generally has irregularities with peak-to-valley heights of less than about 10 microns. [0047] According to another method, the modified surface may be located only on a portion of the plurality of turns of the thread. In another method, the modified surface may be located only below a first turn of the plurality of turns that is adjacent to the gingival end. In yet another embodiment, the aqueous solution of citric acid and HF acid may be exposed to the gingival end.
[0048] Another method of preparing a dental implant involves using a blank of a Ti 6/4 alloy. The blank is machined to produce a desired structure of the dental implant. One example of a dental implant has been discussed and shown in FIG. 1. It is contemplated that other dental implants may be used instead of dental implant 110 shown in FIG. 1. A surface of the desired structure is exposed to oxygen to naturally form a native oxide layer thereon. After machining, at least a portion of the surface is exposed to an initial treatment and then is immersed in a aqueous solution of citric acid and HF acid to remove the native oxide and to produce surface irregularities having a peak-to-valley height less than about 10 microns and, more typically, less than about 5 microns or less than about 3 microns.
Titanium
[0049] Titanium has been generally used in implants such as, for example, dental implants. Commercially pure titanium typically includes trace amounts of carbon, iron, oxygen, hydrogen, and nitrogen. Types of commercial grade titanium that may be used in the processes of the present invention include commercial grade 3 or grade 4 titanium. It is contemplated that other grades of titanium maybe used.
[0050] One desirable characteristic of titanium is the rapid formation of tenacious titanium oxide films on the surface, which contributes to titanium's resistance to corrosion.
This oxide film is believed to be a combination of various oxides of titanium, including TiO,
TiO 2 , Ti 2 O 3 , and Ti 3 O 4 . This oxide film is referred to as "native oxide" film.
[0051] According to one method, a uniformly roughened surface may be obtained on titanium, which is to contact living bone. One method for obtaining such a uniform roughened surface may be performed in a single step. This method involves exposing titanium in an aqueous solution of citric acid and HF acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium metal surface and create the desired surface topography.
[0052] It is desirable to remove substantially all of the native oxide and even more desirable to remove all of the native oxide from the titanium during the exposure to the aqueous solution. It is understood by those of ordinary skill in the art, however, that some smaller bits of native oxide may still remain on the titanium alloy after exposure to the citric acid and HF acid. The method typically also includes rinsing the desired surface topography so as to remove the residual aqueous solution.
[0053] The aqueous solution generally comprises from about 1 to about 50 wt.% citric acid. More specifically, the aqueous solution may comprise from about 22 to about 23 wt.% citric acid. The citric acid may be the same as described above in connection with the Ti 6/4 alloy.
[0054] The aqueous solution generally comprises from about 0.01 to about 1.0 wt.% HF acid. More specifically, the aqueous solution comprises from about 0.07 to about 0.08 wt.%
HF acid. Commercially available HF acid may be used in this processing.
[0055] The aqueous solution may also further include sulfuric acid. The aqueous solution may comprise from 0 to about 20 wt.% sulfuric acid (H 2 SO 4 ). More specifically, the aqueous
solution may comprise from about 5 to about 6 wt.% sulfuric acid. Commercially available sulfuric acid may be used in this invention.
[0056] The aqueous solution may comprise from about 1 to about 50 wt.% citric acid, 0 to about 20 wt.% sulfuric acid, and from about 0.01 to about 1.0 wt.% HF acid. More specifically, the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% HF acid, and from about 5 to about 6 wt.% sulfuric acid. [0057] The processing conditions for exposing the titanium in the aqueous solution of citric acid and HF acid may vary. One non-limiting example of processing conditions for exposing the titanium in the aqueous solution of citric acid and HF acid is a temperature of from about 55 to about 80 0 C for a time period of from about 7 to about 8 minutes. One specific example is a temperature of about 66°C and a time period of from about 7 minutes and 30 seconds. It is contemplated that other temperatures and times may be used for exposing the aqueous solution of citric acid and HF acid to the titanium alloy. [0058] In one embodiment, the one step process of exposing the titanium in an aqueous solution of citric acid and HF acid for a suitable time period results in a generally uniform roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. More specifically, the roughened surface has irregularities with peak-to-valley heights of less than about 5 or less than about 3 microns. In one embodiment, the roughened surface generally has irregularities with peak-to-peak distances of from about 1 to about 3 microns. The irregularities may be cone-shaped elements and it is contemplated that such irregularities may be of different shapes. It is contemplated that the irregularities may be in the form of a substantially uniform array.
[0059] As discussed above, the method for preparing a uniformly roughened surface may be done on an implant (e.g., a dental implant), which is surgically implanted in living bone. One non-limiting example of a dental implant (a screw-type dental implant) is depicted in FIG. 1. It is contemplated that other implants, including other dental implants, may be used. [0060] It is important to remove substantially all the native oxide from the implant surface (e.g., a dental implant surface) that is intended to interface with the living bone so that a substantially uniform surface texture is formed that promotes uniform bonding to the living bone. Thus, the native oxide layer is desirably removed from substantially all of the entire bone-interfacing surface of the implant.
[0061] One method comprises exposing the bone-interfacing portion to an aqueous solution of citric acid and HF acid for a suitable time period. The aqueous solution of citric acid and HF acid removes substantially all of the native oxide from the titanium and forms a modified surface. The modified surface generally has irregularities with peak-to-valley heights of less than about 10 microns.
[0062] According to another method, the modified surface may be located only on a portion of the plurality of turns of the thread. In another method, the modified surface may be located only below a first turn of the plurality of turns that is adjacent to the gingival end. In yet another embodiment, the aqueous solution of citric acid and HF acid may be exposed to the gingival end.
[0063] Another method of preparing a dental implant involves using a blank of titanium. The blank is machined to produce a desired structure of the dental implant. One example of a dental implant has been discussed and is shown in FIG. 1. It is contemplated that other dental implants may be used instead of the dental implant 110 shown in FIG. 1. A surface of the desired structure is exposed to oxygen to naturally form a native oxide layer thereon. After machining, at least a portion of the surface is immersed in a single solution of citric acid and HF acid to remove the native oxide and to produce surface irregularities having a peak-to- valley height less than about 10 microns and, more typically, less than about 5 microns or less than about 3 microns.
[0064] According to another method, a uniformly roughened surface on titanium for contact with living bone comprises (a) performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and (b) after performing the initial treatment, exposing the titanium in an aqueous solution of citric acid and HF acid for a suitable time period to create the desired surface topography.
[0065] The initial treatment may include etching the surface with HF acid. According to another method, the initial treatment includes grit blasting to remove substantially all of the native oxide. The initial treatment as used in this process is used to remove aesthetic surface irregularities {e.g., tooling marks, minor galling) caused during the machining. [0066] It is important to remove substantially all the native oxide from the implant surface {e.g., a dental implant surface) that is intended to interface with the living bone, so that the subsequent treatment of that surface produces a substantially uniform surface texture
to promote uniform bonding to the living bone. Thus, the native oxide layer is desirably removed from substantially all of the entire bone-interfacing surface of the implant. [0067] In one method, the initial treatment includes exposing the titanium to HF acid for a time period of from about 45 seconds to a minute at ambient temperature. It is contemplated that the processing conditions of the initial treatment may vary. After this initial treatment, the titanium may be exposed to the aqueous solutions of citric acid and HF acid such as discussed above.
[0068] In one embodiment, the two step process of exposing the titanium results in a generally uniform roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. More specifically, the generally uniform roughened surface has irregularities with peak-to-valley heights of less than about 5 or less than about 3 microns, hi one embodiment, the generally uniform roughened surface generally has irregularities with peak-to-peak distances of from about 1 to about 3 microns. The irregularities may be cone- shaped elements and it is contemplated that such irregularities may be of different shapes. It is contemplated that the irregularities may be in the form of a substantially uniform array. [0069] As with the one step process, the two step process using titanium may be used on an implant. One example of an implant is a dental implant such as shown in FIG. 1. [0070] Another two step process comprises exposing the bone-interfacing portion to an initial treatment and then exposure to an aqueous solution of citric acid and HF acid for a suitable time period. The initial treatment removes substantially all of the native oxide from the titanium and forms a modified surface. The modified surface generally has irregularities with peak-to-valley heights of less than about 10 microns.
[0071] According to another method, the modified surface may be located only on a portion of the plurality of turns of the thread, hi another method, the modified surface may be located only below a first turn of the plurality of turns that is adjacent to the gingival end. In yet another embodiment, the aqueous solution of citric acid and HF acid may be exposed to the gingival end.
[0072] Another method of preparing a dental implant involves using a blank of titanium. The blank is machined to produce a desired structure of the dental implant. One example of a dental implant has been discussed and shown in FIG. 1. It is contemplated that other dental implants may be used instead of dental implant 110 shown in FIG. 1. A surface of the desired structure is exposed to oxygen to naturally form a native oxide layer thereon. After
machining, at least a portion of the surface is exposed to an initial treatment and then is immersed in a aqueous solution of citric acid and HF acid to remove the native oxide and to produce surface irregularities having a peak-to-valley height less than about 10 microns and, more typically, less than about 5 microns or less than about 3 microns.
EXAMPLES
Example No. 1
[0073] An example of a screw-type cylindrical implant made of 6/4 titanium alloy E.L.I.
(6 wt.% aluminum and 4 wt.% vanadium) is shown in FIGs. 2a-c.
[0074] The implant was exposed to an aqueous solution of 16.7 wt.% citric acid and 0.18 wt.% hydrofluoric (HF) acid with the remainder being water. The HF was 5% v/v HF (2.87% w/w). The aqueous solution was at a temperature of 30 0 C. The implant was exposed for 18 minutes and 30 seconds to remove the native oxide from the Ti 6/4 E.L.I, alloy. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C.
[0075] After this processing, SEMs of the implant were taken and are shown in FIGs. 2a- c. FIG. 2a is an SEM (scanning electron microscopy) photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 2b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG.
2c is an SEM photograph that shows a flute of the thread of the implant at a magnification of
2,000. FIG. 2d is a photograph of the implant using an interferometric surface profiler. It will be observed that the surface features over the areas shown are generally consistent and generally uniform, and resulted in an Osseotite® surface. The highest peak-to-valley measured on FIG. 2d was 3.5 microns.
Example No. 2
[0076] An example of a screw-type cylindrical implant made of 6/4 titanium alloy E.L.I.
(6 wt.% aluminum and 4 wt.% vanadium) is shown in FIGs. 3a-c.
[0077] In the first step, the implant was exposed to a 4.28 wt.% HF solution with the remainder being water. The HF was 50 ml of 15% v/v (8.44% w/w). The HF solution was at a temperature of 25°C. The implant was exposed to the HF solution for about 52 seconds and then rinsed with water.
[0078] In the second step, the implant was exposed to an aqueous solution of 16.7 wt.% citric acid and 0.18 wt.% HF acid with the remainder being water. The HF was 5% v/v HF (2.87% w/w). The aqueous solution was at a temperature of 3O 0 C. The implant was exposed for 18 minutes and 30 seconds to remove the native oxide from the Ti 6/4 E.L.I, alloy. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C. [0079] After this processing, SEMs of the implant were taken and are shown in FIGs. 3 a- c. FIG. 3 a is an SEM photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 3b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG. 3c is an SEM photograph that shows a flute of the thread of the implant at a magnification of 2,000. FIG. 3d is a photograph of the implant using an interferometric surface profiler. It will be observed that the surface features over the areas shown are generally consistent and generally uniform, and resulted in an Osseotite® surface. The highest peak-to- valley measured on FIG. 3d was 3.81 microns.
Example No. 3
[0080] An example of a screw-type cylindrical implant made of grade 3 titanium is shown in FIGs. 4a-c.
[0081] The implant was exposed to an aqueous solution of 22.4 wt.% citric acid, 0.08 wt.% HF acid, and 5.58 wt.% sulfuric acid with the remainder being water. The HF was 5% v/v (2.87 % w/w). The sulfuric acid was 4.4% v/v (7.45% w/w). The aqueous solution was at a temperature of 66°C. The implant was exposed for 7 minutes and 30 seconds to remove the native oxide from the grade 3 Ti implant. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C.
[0082] After this processing, SEMs of the implant were taken and are shown in FIGs. 4a- c. FIG. 4a is an SEM photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 4b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG. 4c is an SEM photograph that shows a flute of the thread of the implant at a magnification of 2,000. FIG. 4d is a photograph of the implant using an interferometric surface profiler. As shown in FIGs. 4a-d, the surface features over
the areas shown were generally consistent and generally uniform, and resulted in an
Osseotite® surface. The highest peak-to-valley measured on FIG. 4d was 4.38 microns.
Example No. 4
[0083] An example of a screw-type cylindrical implant made of grade 4 titanium is shown in FIGs. 5a-c.
[0084] The implant was exposed to an aqueous solution of 22.4 wt.% citric acid, 0.08 wt.% HF acid and 5.58 wt.% sulfuric acid with the remainder being water. The HF was 5% v/v (2.87 % w/w). The sulfuric acid was 4.4% v/v (7.45% w/w). The aqueous solution was at a temperature of 66°C. The implant was exposed for 7 minutes and 30 seconds to remove the native oxide from the grade 4 Ti implant. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C.
[0085] After this processing, SEMs of the implant were taken and are shown in FIGs. 5 a- c. FIG. 5 a is an SEM photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 5b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG. 5c is an SEM photograph that shows a flute of the thread of the implant at a magnification of 2,000. FIG. 5d is a photograph of the implant using an interferometric surface profiler. As shown in FIGs. 5a-d, the surface features over the areas shown were generally consistent and generally uniform, and resulted in an Osseotite® surface. The highest peak-to-valley measured on FIG. 5d was 4.44 microns.
Example No. 5
[0086] An example of a screw-type cylindrical implant made of grade 3 titanium is shown in FIGs. 6a-c.
[0087] hi the first step, the implant was exposed to a 4.28 wt.% HF solution with the remainder being water. The HF was 50 ml of 15% v/v (8.44% w/w). The HF solution was at a temperature of 25°C. The implant was exposed to the HF solution for about 52 seconds and then rinsed with water.
[0100] In the second step, the implant was exposed to an aqueous solution of 22.4 wt.% citric acid, 0.08 wt.% HF acid, and 5.58 wt.% sulfuric acid with the remainder being water.
The HF was 5% v/v (2.87 % w/w). The sulfuric acid was 4.4% v/v (7.45% w/w). The
aqueous solution was at a temperature of 66 0 C. The implant was exposed for 7 minutes and
30 seconds to remove the native oxide from the grade 3 Ti implant. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C. [0101] After this processing, SEMs of the implant were taken and are shown in FIGs. 6a- c. FIG. 6a is an SEM photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 6b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG. 6c is an SEM photograph that shows a flute of the thread of the implant at a magnification of 2,000. FIG. 6d is a photograph of the implant using an interferometric surface profiler. As shown in FIGs. 6a-d, the surface features over the areas shown were generally consistent and generally uniform, and resulted in an Osseotite® surface. The highest peak-to-valley measured on FIG. 6d was 4.05 microns.
Example No. 6
[0102] An example of a screw-type cylindrical implant made of grade 4 titanium is shown in FIGs. 7a-c.
[0103] In the first step, the implant was exposed to a 4.28 wt.% HF solution with the remainder being water. The HF was 50 ml of 15% v/v (8.44% w/w). The HF solution was at a temperature of 25°C. The implant was exposed to the HF solution for about 52 seconds and then rinsed with water.
[0104] In the second step, the implant was exposed to an aqueous solution of 22.4 wt.% citric acid, 0.08 wt.% HF acid and 5.58 wt.% sulfuric acid with the remainder being water.
The HF was 5% v/v (2.87 % w/w). The sulfuric acid was 4.4% v/v (7.45% w/w). The aqueous solution was at a temperature of 66 0 C. The implant was exposed for 7 minutes and
30 seconds to remove the native oxide from the grade 4 Ti implant. The implant was then rinsed to remove the residual acids from the surfaces of the implant. One of the rinses included using water that was heated to a temperature of at least 65°C.
[0105] After this processing, SEMs of the implant were taken and are shown in FIGs. 7a- c. FIG. 7a is an SEM photograph that shows a minor diameter of a thread of the implant at a magnification of 2,000. FIG. 7b is an SEM photograph that shows a flank of the thread of the implant at a magnification of 2,000. FIG. 7c is an SEM photograph that shows a flute of the thread of the implant at a magnification of 2,000. FIG. 7d is a photograph of the implant
using an interferometric surface profiler. As shown in FIGs. 7a-d, the surface features over the areas shown were generally consistent and generally uniform, and resulted in an Osseotite® surface. The highest peak-to-valley measured on FIG. 7d was 3.88 microns. [0106] Alternative Process A
A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone comprising the act of exposing the Ti 6/4 alloy in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and create the desired surface topography. [0107] Alternative Process B
The method of Alternative Process A further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0108] Alternative Process C
The method of Alternative Process A wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid. [0109] Alternative Process D
The method of Alternative Process C wherein the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid. [0110] Alternative Process E
The method of Alternative Process A wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid. [0111] Alternative Process F
The method of Alternative Process E wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0112] Alternative Process G
The method of Alternative Process A wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid and from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0113] Alternative Process H
The method of Alternative Process A wherein all of the native oxide is removed from the Ti 6/4 alloy.
[0114] Alternative Process I
The method of Alternative Process A wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0115] Alternative Process J
A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone comprising the act of exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the Ti 6/4 alloy so as to expose the Ti 6/4 metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0116] Alternative Process K
The method of Alternative Process J wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0117] Alternative Process L
The method of Alternative Process J wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0118] Alternative Process M
The method of Alternative Process K wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0119] Alternative Process N
The method of Alternative Process J wherein the irregularities are cone-shapes. [0120] Alternative Process O
The method of Alternative Process J further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0121] Alternative Process P
The method of Alternative Process J wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid. [0122] Alternative Process O
The method of Alternative Process P wherein the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid. [0123] Alternative Process R
The method of Alternative Process J wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid.
[0124] Alternative Process S
The method of Alternative Process R wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0125] Alternative Process T
The method of Alternative Process J wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid and from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0126] Alternative Process U
The method of Alternative Process J wherein all of the native oxide is removed from the Ti 6/4 alloy. [0127] Alternative Process V
The method of Alternative Process J wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0128] Alternative Process W
A method of preparing a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the act of: exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period, wherein the aqueous solution of citric acid and hydrofluoric acid removes substantially all of the native oxide from the Ti 6/4 alloy and forms a modified surface with substantially uniform array of irregularities having peak-to-valley heights less than about 10 microns. [0129] Alternative Process X
The method of Alternative Process W wherein the implant is a dental implant. [0130] Alternative Process Y
The method of Alternative Process X wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components. [0131] Alternative Process Z
The method of Alternative Process X wherein the exposing of the Ti 6/4 alloy is conducted only on a region of the dental implant located outside the gingival end.
[0132] Alternative Process AA
27. The method of Alternative Process X wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end. [0133] Alternative Process BB
The method of Alternative Process W wherein the exposing of the Ti 6/4 alloy is conducted only on the bone-contacting surface. [0134] Alternative Process CC
The method of Alternative Process W wherein the irregularities include cone-shaped elements. [0135] Alternative Process DD
The method of Alternative Process W wherein the substantially uniform array of irregularities has peak-to-peak distances of from about 1 to about 3 microns. [0136] Alternative Process EE
The method of Alternative Process W wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 5 microns. [0137] Alternative Process FF
The method of Alternative Process EE wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 3 microns. [0138] Alternative Process GG
The method of Alternative Process W further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0139] Alternative Process HH
The method of Alternative Process W wherein the aqueous solution comprises from about 16.0 to about 17.3 wt.% citric acid. [0140] Alternative Process II
The method of Alternative Process HH wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0141] Alternative Process JJ
The method of Alternative Process W wherein the aqueous solution comprises from about 0.16 to about 0.20 wt.% hydrofluoric acid.
[0142] Alternative Process KIC
The method of Alternative Process W wherein all of the native oxide is removed from the Ti 6/4 alloy. [0143] Alternative Process LL
The method of Alternative Process W wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0144] Alternative Process MM
A method of producing a uniformly roughened surface on Ti 6/4 alloy for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography. [0145] Alternative Process NN
The method of Alternative Process MM wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0146] Alternative Process OO
The method of Alternative Process MM wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0147] Alternative Process PP
The method of Alternative Process MM further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0148] Alternative Process OO
The method of Alternative Process MM wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid. [0149] Alternative Process RR
The method of Alternative Process MM wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0150] Alternative Process SS
The method of Alternative Process MM wherein all of the native oxide is removed from the Ti 6/4 alloy.
[0151] Alternative Process TT
The method of Alternative Process MM wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0152] Alternative Process ULJ
A method of producing a generally uniformly roughened surface on Ti 6/4 alloy for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0153] Alternative Process VV
The method of Alternative Process UU wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0154] Alternative Process WW
The method of Alternative Process UU wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0155] Alternative Process XX
The method of Alternative Process UU wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0156] Alternative Process YY
The method of Alternative Process UU wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0157] Alternative Process ZZ
The method of Alternative Process YY wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0158] Alternative Process AAA
The method of Alternative Process UU wherein the irregularities are cone-shapes. [0159] Alternative Process BBB
The method of Alternative Process UU further including rinsing the desired surface topography so as to remove the residual aqueous solution.
[0160] Alternative Process CCC
The method of Alternative Process UU wherein the aqueous solution comprises from about 0.1 to about 1.0 wt.% hydrofluoric acid. [0161] Alternative Process DDD
The method of Alternative Process UU wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0162] Alternative Process EEE
The method of Alternative Process UU wherein all of the native oxide is removed from the Ti 6/4 alloy. [0163] Alternative Process FFF
The method of Alternative Process UU wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0164] Alternative Process GGG
A method of preparing a surface of a Ti 6/4 alloy implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the Ti 6/4 alloy; and after performing the initial treatment, exposing the Ti 6/4 alloy to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0165] Alternative Process HHH
The method of Alternative Process GGG wherein the implant is a dental implant. [0166] Alternative Process HI
The method of Alternative Process HHH wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components. [0167] Alternative Process JJJ
The method of Alternative Process HI wherein the exposing of the Ti 6/4 alloy is conducted only on a region of the dental implant located outside the gingival end.
[0168] Alternative Process KKK
The method of Alternative Process in wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end. [0169] Alternative Process LLL
The method of Alternative Process GGG wherein the exposing of the Ti 6/4 alloy is conducted only on the bone-contacting surface. [0170] Alternative Process MMM
The method of Alternative Process GGG wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0171] Alternative Process NNN
The method of Alternative Process GGG wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0172] Alternative Process QOO
The method of Alternative Process GGG wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0173] Alternative Process PPP
The method of Alternative Process GGG wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0174] Alternative Process OQQ
The method of Alternative Process PPP wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0175] Alternative Process RPJR.
The method of Alternative Process GGG wherein the aqueous solution comprises from about 16 to about 17.3 wt.% citric acid, and from about 0.16 to about 0.20 wt.% hydrofluoric acid. [0176] Alternative Process SSS
The method of Alternative Process GGG wherein the Ti 6/4 alloy is a Ti 6/4 E.L.I, alloy. [0177] Alternative Process TTT
A method of producing a generally uniformly roughened surface on titanium for contact with living bone comprising the act of exposing the titanium in an aqueous solution of
citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from the titanium so as to expose the titanium metal surface and create the desired surface topography.
[0178] Alternative Process UUU
The method of Alternative Process TTT further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0179] Alternative Process VVV
The method of Alternative Process TTT wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid. [0180] Alternative Process WWW
The method of Alternative Process VVV wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid. [0181] Alternative Process XXX
The method of Alternative Process TTT wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid. [0182] Alternative Process YYY
The method of Alternative Process XXX wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid. [0183] Alternative Process ZZZ
The method of Alternative Process TTT wherein the aqueous solution further includes sulfuric acid. [0184] Alternative Process AAAA
The method of Alternative Process TTT wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt.% sulfuric acid. [0185] Alternative Process BBBB
The method of Alternative Process TTT wherein all of the native oxide is removed from the titanium. [0186] Alternative Process CCCC
A method of producing a generally uniformly roughened surface on titanium for contact with living bone comprising the act of exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to remove the native oxide from
the titanium so as to expose the titanium metal surface and etch the exposed metal to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns.
[0187] Alternative Process DDDD
The method of Alternative Process CCCC wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0188] Alternative Process EEEE
The method of Alternative Process CCCC wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0189] Alternative Process FFFF
The method of Alternative Process EEEE wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0190] Alternative Process GGGG
The method of Alternative Process CCCC wherein the irregularities are cone-shapes. [0191] Alternative Process HHHH
The method of Alternative Process CCCC further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0192] Alternative Process IHI
The method of Alternative Process CCCC wherein the aqueous solution comprises from about 1 to about 50 wt.% citric acid. [0193] Alternative Process JJJJ
The method of Alternative Process CCCC wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid. [0194] Alternative Process KKKX
The method of Alternative Process CCCC wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid. [0195] Alternative Process LLLL
The method of Alternative Process KXBCK wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid. [0196] Alternative Process MMMM
The method of Alternative Process CCCC wherein the aqueous solution further includes sulfuric acid.
[0197] Alternative Process NNNN
The method of Alternative Process CCCC wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20% sulfuric acid. [0198] Alternative Process OQOO
The method of Alternative Process CCCC wherein all of the native oxide is removed from the titanium. [0199] Alternative Process PPPP
A method of preparing a surface of a titanium implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the act of: exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period, wherein the aqueous solution of citric acid and hydrofluoric acid removes substantially all of the native oxide from the titanium and forms a modified surface with substantially uniform array of irregularities having peak-to-valley heights less than about 10 microns. [0200] Alternative Process QQOQ
The method of Alternative Process PPPP wherein the implant is a dental implant. [0201] Alternative Process RRRR
The method of Alternative Process QQQQ wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components. [0202] Alternative Process SSSS
The method of Alternative Process RRRR wherein the exposing of the titanium is conducted only on a region of the dental implant located outside the gingival end. [0203] Alternative Process TTTT
The method of Alternative Process RRRR wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
[0204] Alternative Process UUUU
The method of Alternative Process PPPP wherein the exposing of the titanium is conducted only on the bone-contacting surface. [0205] Alternative Process VVVV
The method of Alternative Process PPPP wherein the irregularities include cone- shaped elements. [0206] Alternative Process WWWW
The method of Alternative Process PPPP wherein the substantially uniform array of irregularities has peak-to-peak distances of from about 1 to about 3 microns. [0207] Alternative Process XXXX
The method of Alternative Process PPPP wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 5 microns. [0208] Alternative Process YYYY
The method of Alternative Process XXXX wherein the substantially uniform array of irregularities has peak-to-valley heights of less than about 3 microns. [0209] Alternative Process ZZZZ
The method of Alternative Process PPPP further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0210] Alternative Process AAAAA
The method of Alternative Process PPPP wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid. [0211] Alternative Process BBBBB
The method of Alternative Process AAAAA wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid. [0212] Alternative Process CCCCC
The method of Alternative Process PPPP wherein the aqueous solution comprises from about 0.07 to about 0.09 wt.% hydrofluoric acid. [0213] Alternative Process DDDDD
The method of Alternative Process PPPP wherein all of the native oxide is removed from the titanium.
[0214] Alternative Process EEEEE
A method of producing a generally uniformly roughened surface on titanium for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and after performing the initial treatment, exposing the titanium in an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to create the desired surface topography. [0215] Alternative Process FFFFF
The method of Alternative Process EEEEE wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0216] Alternative Process GGGGG
The method of Alternative Process EEEEE wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0217] Alternative Process HHHHH
The method of Alternative Process EEEEE further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0218] Alternative Process mil
The method of Alternative Process EEEEE wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid. [0219] Alternative Process JJJJJ
The method of Alternative Process EEEEE wherein the aqueous solution further includes sulfuric acid. [0220] Alternative Process KKXKK
The method of Alternative Process EEEEE wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt. % sulfuric acid. [0221] Alternative Process LLLLL
The method of Alternative Process EEEEE wherein all of the native oxide is removed from the titanium.
[0222] Alternative Process MMMMM
A method of producing a generally uniformly roughened surface on titanium for contact with living bone, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and after performing the initial treatment, exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0223] Alternative Process NNNNN
The method of Alternative Process MMMMM wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0224] Alternative Process QOOOO
The method of Alternative Process MMMMM wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0225] Alternative Process PPPPP
The method of Alternative Process MMMMM wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0226] Alternative Process OQQQO
The method of Alternative Process MMMMM wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0227] Alternative Process RRKRR
The method of Alternative Process QQQQQ wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0228] Alternative Process SSSSS
The method of Alternative Process MMMMM wherein the irregularities are cone- shapes. [0229] Alternative Process TTTTT
The method of Alternative Process MMMMM further including rinsing the desired surface topography so as to remove the residual aqueous solution. [0230] Alternative Process UUUUU
The method of Alternative Process MMMMM wherein the aqueous solution comprises from about 0.01 to about 1.0 wt.% hydrofluoric acid.
[0231] Alternative Process VVVVV
The method of Alternative Process MMMMM wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt. % sulfuric acid. [0232] Alternative Process WWWWW
The method of Alternative Process MMMMM wherein all of the native oxide is removed from the titanium. [0233] Alternative Process XXXXX
A method of preparing a surface of a titanium implant that is surgically implantable in living bone, the surface having a native oxide layer thereon, the method comprising the acts of: performing an initial treatment that removes substantially all of the native oxide from the surface of the titanium; and after performing the initial treatment, exposing the titanium to an aqueous solution of citric acid and hydrofluoric acid for a suitable time period to achieve a roughened surface having irregularities with peak-to-valley heights of less than about 10 microns. [0234] Alternative Process YYYYY
The method of Alternative Process XXXXX wherein the implant is a dental implant. [0235] Alternative Process ZZZZZ
The method of Alternative Process YYYYY wherein the surface of the dental implant has a threaded portion with a thread making a plurality of turns around the threaded portion, and a gingival end adjacent to the threaded portion, the gingival end adapted to mate with abutting components. [0236] Alternative Process AAAAAA
The method of Alternative Process ZZZZZ wherein the exposing of the titanium is conducted only on a region of the dental implant located outside the gingival end. [0237] Alternative Process BBBBBB
The method of Alternative Process ZZZZZ wherein the exposing is conducted only on a region of the dental implant located below a first turn of the plurality of turns that is located below the gingival end.
[0238] Alternative Process CCCCCC
The method of Alternative Process ZZZZZ wherein the exposing of the titanium is conducted only on the bone-contacting surface. [0239] Alternative Process DDDDDD
The method of Alternative Process ZZZZZ wherein performing the initial treatment includes etching the surface with hydrofluoric acid. [0240] Alternative Process EEEEEE
The method of Alternative Process ZZZZZ wherein performing the initial treatment includes grit blasting to remove substantially all of the native oxide. [0241] Alternative Process FFFFFF
The method of Alternative Process ZZZZZ wherein the roughened surface has irregularities with peak-to-peak distances of from about 1 to about 3 microns. [0242] Alternative Process GGGGGG
The method of Alternative Process ZZZZZ wherein the roughened surface has irregularities with peak-to-valley heights of less than about 5 microns. [0243] Alternative Process HHHHHH
The method of Alternative Process GGGGGG wherein the roughened surface has irregularities with peak-to-valley heights of less than about 3 microns. [0244] Alternative Process HIHI
The method of Alternative Process XXXXX wherein the aqueous solution comprises from about 22 to about 23 wt.% citric acid, from about 0.07 to about 0.09 wt.% hydrofluoric acid, and from 0 to about 20 wt.% sulfuric acid.
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