Tricalcium phosphates, their composites, implants incorporating them, and methods for their production
View Patent ↗Methods for the synthesis of tricalcium phosphates are presented, as well as a series of specific reaction parameters that can be adjusted to tailor, in specific ways, properties in the tricalcium phosphate precursor precipitate. Particulate tricalcium phosphate compositions having an average crystal size of about 250 nm or less are provided. Compositions of the invention can be used as prosthetic implants and coatings for prosthetic implants.
1. A method for preparing particulate TCP comprising:
(i) precipitating a TCP precursor from a solution containing a calcium source to a phosphate source, wherein the pH of the mixture is about 5 to about 11,
(ii) aging the precipitated TCP precursor,
(iii) controlling the conditions of steps (i) and (ii) so as to produce a TCP precursor precipitate having an average crystal size of 250 nm or less,
(iv) collecting the TCP precursor precipitate,
(v) drying the TCP precursor,
(vi) milling the TCP precursor, and
(vii) calcining the TCP precursor to obtain a particulate TCP having an average crystal size of 250 nm or less, a surface area of about 20 m 2 /g and particle size of 5 μm or less.
2. The method of claim 1 , wherein step (i) involves adding the calcium source to the phosphate source.
3. The method of claim 1 , wherein the calcium source is calcium nitrate and the phosphorus source is selected from the group consisting of ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, or a combination thereof.
4. The method of claim 1 , wherein the calcium source and phosphate source has an atomic ratio (Ca/P) of about 1.4 to about 1.6.
5. The method of claim 1 , wherein the mixture has a pH of between about 7 and about 10.
6. The method of claim 1 , wherein the precipitated apatite is aged at a temperature of about 0° C. to about 90° C.
7. The method of claim 1 , wherein the precipitated apatite is aged at a temperature of about 10° C. to about 30° C.
8. The method of claim 1 , wherein the precipitated apatite is aged for at least 2 hours.
9. The method of claim 1 , wherein the precipitated TCP precursor is further calcined at a temperature of about 1000° C. to about 1400° C.
10. The method of claim 1 , wherein the precipitated TCP precursor is further calcined at a temperature of about 400° C. to about 900° C.