Crystalline phase composition, Ca/P ratio, percent weight of Eu3+ in the samples, average particle dimensions (length, width) measured by SEM and/or TEM and average dimensions (length, width) of the crystalline domains determined by Rietveld refinement.
[Eu3+]0, M (x) | Crystalline phasesa | Ca/P ratiob | wt% Eub | L (nm) | W (nm) | L (nm) (Rietveld) | W (nm) (Rietveld) |
---|---|---|---|---|---|---|---|
0.001 4 h | Ap | 1.59 ± 0.14 | 1.72 ± 0.31 | 23.5 ± 5.4 | 23.5 ± 5.4 | 25.4 ± 6.9 | 7.9 ± 0.9 |
0.001 24 h | Ap | 1.65 ± 0.24 | 1.56 ± 0.37 | 38.7 ± 5.8 | 18.7 ± 6.2 | 32.9 ± 8.3 | 11.2 ± 1.2 |
0.001 96 h | Ap | 1.63 ± 0.09 | 2.04 ± 0.27 | 39.2 ± 5.3 | 9.6 ± 1.4 | 35.1 ± 0.5 | 11.7 ± 0.1 |
0.005 4 h | Ap + OCP | 1.34 ± 0.42 | 14.6 ± 2.1 | 65.3 ± 9.3 | 65.3 ± 9.3 | 26 ± 0.9 | 5.1 ± 0.1 |
0.005 24 h | Ap | 1.53 ± 0.12 | 6.40 ± 0.48 | 170.4 ± 6.5 | 52.5 ± 6.4 | 41.2 ± 0.7 | 9.1 ± 0.1 |
0.005 96 h | Ap | 1.48 ± 0.18 | 5.25 ± 0.68 | 127 ± 27 | 17.9 ± 7.2 | 39.7 ± 0.7 | 9.3 ± 0.1 |
0.010 4 h | Ap + OCP | 1.08 ± 0.54 | 23.8 ± 5.7 | 526 ± 235 | 134.5 ± 40.7 | 54.7 ± 6.4 | 31.2 ± 1.4 |
0.010 24 h | Ap | 1.08 ± 0.15 | 24.0 ± 7.7 | 325 ± 50 | 73 ± 7 | 79.7 ± 3.6 | 60.4 ± 1.4 |
0.010 96 h | Ap | 1.54 ± 0.14 | 11.5 ± 0.3 | 380 ± 65 | 92 ± 12 | 80.5 ± 2.2 | 53.5 ± 0.7 |
0.010 7 d | Ap | 1.53 ± 0.04 | 5.4 ± 1.2 | 90 ± 21 | 90 ± 21 | 30.6 ± 0.8 | 13.6 ± 0.1 |
0.020 4 h | Ap + OCP | 0.98 ± 0.02 | 13.0 ± 0.3 | 340 ± 50 | 75 ± 10 | 92.3 ± 2.3 | 62.3 ± 1.3 |
0.020 24 h | Ap + OCP | 1.05 ± 0.03 | 20.6 ± 0.4 | 1250 ± 15 | 225 ± 40 | 328 ± 5.6 d | 247 ± 4.1d |
0.020 96 h | Ap + OCP | 1.45 ± 0.01 | 13.3 ± 2.6 | 1870 ± 100 | 260 ± 45 | 567 ± 4.5d | 166 ± 3.2d |
0.030 96 hc | Ap + OCP | 1.56 ± 0.01 | 10.03 ± 0.3 | 1230 ± 50 | 210 ± 55 | 643 ± 10.2d | 128 ± 9.8d |
Ap = apatitic phase; OCP = octacalcium phosphate.
Measured by EDS technique averaging the composition of 6–10 different zones of the Ap phase.
At this timepoint the europium phosphate phase started to appear.
Calculated crystallite dimensions greater than 100–150 nm have to be considered only as an estimated trend. They are accurate only for dimensions below these sizes, because for bigger sizes the difference between the instrumental FWHM contribution and the FWHM contribution due to the size is negligible.