P
USRE39196EExpiredUtilityPatentIndex 99

Nanocrystalline apatites and composites, prostheses incorporating them, and method for their production

Assignee: MASSACHUSETTS INST TECHNOLOGYPriority: Jan 16, 1997Filed: Jan 11, 2002Granted: Jul 18, 2006
Est. expiryJan 16, 2017(expired)· nominal 20-yr term from priority
Inventors:YING JACKIE YAHN EDWARD SNAKAHIRA ATSUSHI
C04B 35/6262A61F 2310/00293C04B 2235/5409C04B 2235/3225C04B 2235/549C04B 2235/785A61L 27/32F16C 2240/64C04B 2235/77A61L 2400/12A61F 2310/00796C04B 2235/3246C04B 2235/668C04B 35/645C04B 2235/656B82Y 30/00C04B 35/62675C04B 2235/6567C04B 2235/5445C04B 2235/3244A61L 27/12C04B 2235/3212C04B 2235/96C04B 2235/3217C04B 35/447C04B 35/488C04B 35/46Y10S977/776A61F 2/30767C04B 2235/80C03C 14/00C03C 4/0007C04B 2235/3232C04B 2235/6562A61F 2310/00239C01B 25/32C04B 2235/608C04B 35/117C04B 2235/5454C04B 2235/9653C03C 4/0021
99
PatentIndex Score
75
Cited by
49
References
105
Claims

Abstract

Methods for synthesis of nanocyrstalline apatites are presented, as well as a series of specific reaction parameters that can be adjusted to tailor, in specific ways, properties in the recovered product. Particulate apatite compositions having aveage crystal size of less than 150 nm are provided. Products also can have a surface area of at least 40 m 2 /g and can be of high density. Hydroxyapatite material is investigated in particular detail. Compositions of the invention can be used as prosthetic implants and coatings for prosthetic implants.

Claims

exact text as granted — not AI-modified
1. A composition, comprising particulate apatate having an aveage apatite crystal size of less than 100 nm, wherein the crystal is a spherical. 
     
     
       2. The composition of  claim 1  comprising particulate apatite having an average apatite crystal size of less than 50 nm. 
     
     
       3. The composition of  claim 1  comprising partiuclate apatite having an average apatite crystal size of less than 30 nm. 
     
     
       4. The composition of  claim 1  comprising partiuclate apatite having an average apatite crystal size of less than 30 nm. 
     
     
       5. The composition of  claim 1  wherien the partiuclate apatite is densified. 
     
     
       6. The composition of  claim 1  comprising apatite having an average particle size of less than 1 μm. 
     
     
       7. The composition of  claim 1  comprising apatite having an aveage particle size of less than 0.5 μm. 
     
     
       8. The composition of  claim 1  comprising apatite having an average particle size of less than 0.25 μm. 
     
     
       9. A composition comprising particulate apatite having a surface area of at least 40 m 2 /g and a spherical crystal. 
     
     
       10. The composition of  claim 7  comprising particulate apatite having a surface area of at least 100 m 2 /g. 
     
     
       11. The composition of  claim 9  comprising particulate apatite having a surface area of at least 150 m 2 g. 
     
     
       12. The composition of  claim 9  that undergoes apatite phase decomposition of less than 10% when exposed to conditions of at least 1000° C. for at least 2 hours. 
     
     
       13. The composition of  claim 12  that undergoes apatite phase decomposition of less than 5% when exposed to conditions of at least 1000° C. for at least 2 hours. 
     
     
       14. The composition of  claim 12  that undergoes apatite phase decomposition of less than 3% when exposed to conditions of at least 1000° C. for at least 2 hours. 
     
     
       15. The composition of  claim 12  that undergoes apatite phase decomposition of less than 10% when exposed to conditions of at least 1100° C. for at least 2 hours. 
     
     
       16. The composition of  claim 12  that undergoes apatite phase decomposition of less than 5% when exposed to conditions of at least 1100° C. for at least 2 hours. 
     
     
       17. The composition of  claim 12  that undergoes apatite phase decomposition of less than 3% when exposed to conditions of at least 1100° C. for at least 2 hours. 
     
     
       18. The composition of  claim 12  that undergoes apatite phase decomposition of less than 10% when exposed to conditions of at least 1200° C. for at least 2 hours. 
     
     
       19. The composition of  claim 12  that undergoes apatite phase decomposition of less than 5% when exposed to conditions of at least 1200° C. for at least 2 hours. 
     
     
       20. The composition of  claim 12  that undergoes apatite phase decomposition of less than 3% when exposed to conditions of at least 1200° C. for at least 2 hours. 
     
     
       21. The composition of  claim 12  that undergoes apatite phase decomposition of less than 10% when exposed to conditions of at least 1300° C. for at least 2 hours. 
     
     
       22. The composition of  claim 12  that undergoes apatite phase decomposition of less than 5% when exposed to conditions of at least 1300° C. for at least 2 hours. 
     
     
       23. The composition of  claim 12  that undergoes apatite phase decomposition of less than 3% when exposed to conditions of at least 1300° C. for at least 2 hours. 
     
     
       24. An article having a dimension of at least 0.5 cm made up of the composition of  claim 1 . 
     
     
       25. The article of  claim 24  wherein the particulate apatite is consolidated. 
     
     
       26. The article of  claim 24 , formed into the shape of a prosthesis. 
     
     
       27. The article of  claim 24  that is a prosthesis. 
     
     
       28. The article of  claim 24  comprising an exterior coating on a prosthesis. 
     
     
       29. The article of  claim 28  comprising an exterior coating, on a prosthesis, of at least 0.5 micron in thickness. 
     
     
       30. The article of  claim 24  wherein a theoretical density of at least 90%. 
     
     
       31. The article of  claim 24  having a theoretical density of at least 95%. 
     
     
       32. The article of  claim 24  having a theoretical density of at least 98%. 
     
     
       33. An article having a dimension of at least 0.5 cm made up of the composition of  claim 9 . 
     
     
       34. The article of  claim 33  having a porosity of at least 20%. 
     
     
       35. The article of  claim 33  having a porosity of at least 50%. 
     
     
       36. The article of  claim 33  having a porosity of at least 50%.  
     
     
       37. The article of  claim 33  having a porosity of at least 75%. 
     
     
       38. The densified article of  claim 33  having compressive strength of at least about 150 MPa. 
     
     
       39. The densified article of  claim 38 , having a density of at least about  98 %. 
     
     
       40. The densified article of  claim 33  having compressive strength of at least about 500 MPa. 
     
     
       41. The densified article of  claim 33  having compressive strength of at least about 700 MPa. 
     
     
       42. The densified article of  claim 38 , having a density of at least about 90%. 
     
     
       43. The densified article of  claim 38 , having a density of at least about 95%. 
     
     
       44. The article of  claim 24  that is a part of a prosthesis. 
     
     
       45. An article comprising a densified apatite structure having a dimension of at least  0 . 5  cm and an average XRD crystal size of less than  250  nm, wherein the apatite structure undergoes phase decomposition of less than  10 %  when exposed to conditions of at least  1300 ° C. for at least  2  hours and has a compressive strength of at least  150  MPa.    
     
     
       46. The article of  claim 45 , wherein the densified apatite structure has a density of at least about  90 % .    
     
     
       47. The article of  claim 46 , wherein the densified apatite structure has a density of at least about  98 % .    
     
     
       48. The article of  claim 45 , wherein the densified apatite structure has a compressive strength of at least about  500  MPa.  
     
     
       49. The article of  claim 48 , wherein the densified apatite structure has a compressive strength of at least about  700  MPa.  
     
     
       50. The article of  claim 45 , wherein the phase decomposition is less than  5 % .    
     
     
       51. The article of  claim 45 , wherein the densified apatite structure has an average XRD crystal size of less than  150  nm.  
     
     
       52. The article of  claim 45 , wherein the densified apatite structure comprises an auxiliary strcutural additive.  
     
     
       53. The article of  claim 52 , wherein the auxiliary structure additive comprises a ceramic additive.  
     
     
       54. The article of  claim 53 , wherein the ceramic additive comprises a metal oxide.  
     
     
       55. The article of  claim 54 , wherein the metal oxide comprises zirzonia.  
     
     
       56. The article of  claim 52 , wherein the auxiliary structural additive is nanocrystalline.  
     
     
       57. The article of  claim 52 , wherein the auxiliary structural additive is a metal or alloy.  
     
     
       58. The article of  claim 52 , wherein the auxiliary structural additive is present in an amount of between about  1 %  and about  50   %  by volume.    
     
     
       59. The article of  claim 45 , wherein the densified apatite structure comprises carbonated apatite.  
     
     
       60. The article of  claim 45 , wherein the article is at least part of a prosthesis.  
     
     
       61. The article of  claim 60 , wherein the article is a prosthesis.  
     
     
       62. The article of  claim 45 , wherein the article comprises an exterior coating on a prosthesis.  
     
     
       63. The article of  claim 45 , wherein the article is a bioactive implant.  
     
     
       64. The article of  claim 63 , wherein the bioactive implant is an orthopedic or dental implant.  
     
     
       65. The article of  claim 59 , wherein the carbonated apatite is a reactive layer on a bioceramic capable of enhancing bioactivity for bone growth.  
     
     
       66. An article comprising an apatite structure having a dimension of at least  0 . 5  cm, a density of at least about  98 % , a compressive strength of at least about  500  MPa, an average XRD crystal size of less than  250  nm, and wherein the apatite structure undergoes phase decomposition of less than  10   %  when exposed to conditions of at least  1300 ° C. for at least  2  hours.    
     
     
       67. The article of  claim 66 , wherein the apatite structure has a compressive strength of at least about  700  MPa.  
     
     
       68. The article of  claim 66 , wherein the phase decomposition is less than  5 % .    
     
     
       69. The article of  claim 66 , wherein the apatite structure has an average XRD crystal size of less than  150  nm.  
     
     
       70. The article of  claim 66 , wherein the article is a prosthesis.  
     
     
       71. The article of  claim 66 , wherein the article is at least part of a prosthesis.  
     
     
       72. The article of  claim 66 , wherein the article comprises an exterior coating on a prosthesis.  
     
     
       73. The article of  claim 66 , wherein the article is a bioactive implant.  
     
     
       74. The article of  claim 73 , wherein the bioactive implant is an orthopedic or dental implant.  
     
     
       75. The article of  claim 66 , wherein the apatite structure comprises an auxiliary structural additive.  
     
     
       76. The article of  claim 75 , wherein the auxiliary structural additive comprises a ceramic additive.  
     
     
       77. The article of  claim 76 , wherein the ceramic additive comprises a metal oxide.  
     
     
       78. The article of  claim 77 , wherein the metal oxide comprises zirconia.  
     
     
       79. The article of  claim 75 , wherein the auxiliary structural additive is nanocrystalline.  
     
     
       80. The article of  claim 75 , wherein the auxiliary structural additive is a metal or alloy.  
     
     
       81. The article of  claim 75 , wherein the auxiliary structural additive is added in an amount of between about  1 %  and about  50   %  by volume.    
     
     
       82. The article of  claim 66 , wherein the apatite structure comprises carbonated apatite.  
     
     
       83. The article of  claim 82 , wherein the carbonated apatite is a reactive layer on a bioceramic capable of enhancing bioactivity for bone growth.  
     
     
       84. An article comprising a consolidated apatite structure having a dimension of at least  0 . 5  cm, an average XRD crystal size of less than  250  nm, and a porosity of at least  20 % , wherein the apatite structure undergoes phase decomposition of less than  10   %  when exposed to conditions of at least  1300 ° C. for at least  2  hours.    
     
     
       85. The article of  claim 84 , wherein the consolidated apatite structure has a porosity of at least  50 % .    
     
     
       86. The article of  claim 85 , wherein the consolidated apatite sturcture has a porosity of at least  75 % .    
     
     
       87. The article of  claim 84 , wherein the consolidated apatite structure has a compressive strength of at least about  150  MPa.  
     
     
       88. The article of  claim 84 , wherein the phase decomposition is less than  5 % .    
     
     
       89. The article of  claim 84 , wherein the consolidated apatite structure has an average XRD crystal size of less than  150  nm.  
     
     
       90. The article of  claim 84 , wherein the consolidated apatite structure comprises an auxiliary structural additive.  
     
     
       91. The article of  claim 90 , wherein the auxiliary structural additive comprises a ceramic additive.  
     
     
       92. The article of  claim 91 , wherein the ceramic additive comprises a metal oxide.  
     
     
       93. The article of  claim 92 , where in the metal oxide comprises zirconia.  
     
     
       94. The article of  claim 90 , wherein the auxiliary structural additive is nanocrystalline.  
     
     
       95. The article of  claim 90 , wherein the auxiliary structural additive is a metal or alloy.  
     
     
       96. The article of  claim 90 , wherein the auxiliary structural additve is present in an amount of between about  1 %  and about  50   %  by volume.    
     
     
       97. The article of  claim 84 , wherein the consolidated apatite structure comprises carbonated apatite.  
     
     
       98. The article of  claim 97 , wherein the carbonated apatite is a reactive layer on a bioceramic capable of enhancing bioactivity for bone growth.  
     
     
       99. The article of  claim 84 , wherein the consolidated apatite structure is formed from an admixture of particulate apatite with an organic species.  
     
     
       100. The article of  claim 99 , wherein the organic species is a self- assembling surfactant or a polymer.    
     
     
       101. The article of  claim 84 , wherein the article is at least part of a prosthesis.  
     
     
       102. The article of  claim 101 , wherein the article is a prosthesis.  
     
     
       103. The article of  claim 101 , wherein the article comprises an exterior coating on a prosthesis.  
     
     
       104. The article of  claim 84 , wherein the article is a bioactive implant.  
     
     
       105. The article of  claim 104 , wherein the bioactive implant is an orthopedic or dental implant.

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