Effects of Synthesis Conditions on the Formation of Si-Substituted Alpha Tricalcium Phosphates
Abstract
:1. Introduction
2. Results and Discussion
2.1. Scanning and Transmission Electron Microscopy
2.2. Powder X-ray Diffractometry
2.3. Quantitative Analysis of Silicon
2.4. Vibrational Spectroscopy
2.5. Solid-State 31P NMR MAS Spectroscopy
3. Materials and Methods
3.1. Preparation of Samples
3.2. Sample Sharacterization
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Acknowledgments
Conflicts of Interest
References
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Sample | Composition [wt%] | Si Content [wt%] | Lattice Parameters | |||||
---|---|---|---|---|---|---|---|---|
Si-α-TCP | SC | a [Å] | b [Å] | c [Å] | β [⁰] | |||
09Si-aTCP | 97.15 | 2.85 | 0.85 (1.05 *) | 12.909 | 27.268 | 15.211 | 125.80 | |
18Si-aTCP | 97.62 | 2.37 | 1.59 (1.91 *) | 12.875 | 27.341 | 15.239 | 125.76 | |
37Si-aTCP | 96.94 | 3.06 | 2.44 (3.74 *) | 12.900 | 27.356 | 15.224 | 125.66 | |
09Si-aTCPs | 96.60 | 3.40 | 1.06 (1.07 *) | 12.892 | 27.345 | 15.235 | 125.73 | |
18Si-aTCPs | 94.96 | 5.04 | 2.06 (2.11 *) | 12.911 | 27.564 | 15.189 | 125.77 | |
37Si-aTCPs | 92.64 | 7.33 | 3.78 (3.78 *) | 12.874 | 27.202 | 15.282 | 125.80 |
IR (cm−1) | Raman (cm−1) | Normal Modes (Assignments) |
---|---|---|
458 | 448 | symmetric P-O bending υ2 (α-TCP and SC) |
491–498 | υ2 SiO44− | |
556 596 613 | 567 583 609 | anti-symmetric P-O bending υ4 (α-TCP and SC) |
678 723 | υ1 SiO44− | |
791–793 | silica (SiO2) | |
868 898 | 844 | υ3 SiO44− silica (SiO2) |
935–938 959 | 969–954 | symmetric P–O stretching, υ1 (α-TCP and SC) symmetric P–O stretching, υ1 (α-TCP) |
1010–1013 1066–1068 | 1024 1060 1100 1136 | anti-symmetric P–O stretching, υ3 (α-TCP and SC) |
Sample | Synthesis Method | Silicon Source | Expected Chemical Formula | Expected Si Content [wt%] |
---|---|---|---|---|
09Si-aTCP | precipitation | silicon acetate | Ca3(P0.95Si0.05O3.975)2 | 0.9 |
18Si-aTCP | Ca3(P0.9Si0.1O3.95)2 | 1.8 | ||
37Si-aTCP | Ca3(P0.8Si0.2O3.9)2 | 3.7 | ||
09Si-aTCPs | solid state | fumed silica | Ca3(P0.95Si0.05O3.975)2 | 0.9 |
18Si-aTCPs | Ca3(P0.9Si0.1O3.95)2 | 1.8 | ||
37Si-aTCPs | Ca3(P0.8Si0.2O3.9)2 | 3.7 |
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Szurkowska, K.; Szeleszczuk, Ł.; Kolmas, J. Effects of Synthesis Conditions on the Formation of Si-Substituted Alpha Tricalcium Phosphates. Int. J. Mol. Sci. 2020, 21, 9164. https://doi.org/10.3390/ijms21239164
Szurkowska K, Szeleszczuk Ł, Kolmas J. Effects of Synthesis Conditions on the Formation of Si-Substituted Alpha Tricalcium Phosphates. International Journal of Molecular Sciences. 2020; 21(23):9164. https://doi.org/10.3390/ijms21239164
Chicago/Turabian StyleSzurkowska, Katarzyna, Łukasz Szeleszczuk, and Joanna Kolmas. 2020. "Effects of Synthesis Conditions on the Formation of Si-Substituted Alpha Tricalcium Phosphates" International Journal of Molecular Sciences 21, no. 23: 9164. https://doi.org/10.3390/ijms21239164