Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 1

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Allyson Roberts
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1 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 1 INDEX A1. The reactants... 3 A2. XRD analysis... 5 A2.1. Qualitative analysis... 5 A2.2. Quantitative analysis... 11

2 Page 2 Master s thesis

3 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 3 A1. THE REACTANTS Here are the technical notices of both reactants: HA CalbioChem and Cab-O-Sperse 1030 K Fig A1: Product Data sheet of Hydroxylapatite CalbioChem High Resolution

4 Page 4 Master s thesis Fig A2: Product Data sheet of the silicon oxide Cab-O-Sperse

5 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 5 A2. XRD ANALYSIS As explained in the Materials and Methods section, the XRD analysis is made in two steps: first, a qualitative analysis through the Origin program using the spectra of known phases, and then the Rietveld refinement method, using the FullProf software. A2.1. QUALITATIVE ANALYSIS Here are the patterns used to create the template in order to analyze our results in the first step: α-tcp: Fig A3: Pattern of α-tcp phase

6 Page 6 Master s thesis β-tcp: Fig A4: Pattern of β-tcp phase

7 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 7 HA: Fig A5: Pattern of HA phase

8 Page 8 Master s thesis SiO2: Fig A6: Pattern of SiO2 phase

9 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 9 Here is the Origin analysis of the Si-α-TCP powders with the various ratio of silicon used: Absorption (a.u) HA + 0 SO β-tcp HA Wavenumber (cm -1 ) Fig. A7: XRD spectrum of α-tcp with 0SO/HA ratio Absorption (a.u) HA + 0,16 SO α TCP β-tcp HA Wavenumber (cm -1 ) Fig. A8: XRD spectrum of α-tcp with 0.16 SO/HA ratio

10 Page 10 Master s thesis Abosrption (a.u) HA SO α-tcp β-tcp HA Wavenumber (cm -1 ) Fig. A9: XRD spectrum of α-tcp with 0.32 SO/HA ratio Absorption (a.u) HA SO α-tcp β-tcp HA Wavenumber (cm -1 ) Fig. A10: XRD spectrum of α-tcp with 0.48 SO/HA ratio In the following table are summarized the results obtained from these spectra:

11 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 11 SiO 2/HA molar ratio % alpha % beta % HA Table A1: crystalline phase repartition according to Origin analysis A2.2. QUANTITATIVE ANALYSIS As referred in the report, the XRD quantitative analysis has been made using the Rietveld refinement method, through the FullProf program. The following parameters have been refined: Instrument displacement. Scale factors. Lattice parameters using a Thompson-Cox-Hastinge pseudo Voight*Axial divergence. FWHM/shape parameters. Preferred orientation. Background. Once the XRD results are refined, the program gives a spectrum such as the followings. In black appears the theoretical spectrum and the experimental one is displayed in red. The blue one below shows the difference between the two mentioned, and is expressed by χ². The spectra obtained for the different ratio of SO/HA are displayed below:

12 Page 12 Master s thesis Fig. A11: XRD Rietveld analysis spectrum of α-tcp with 0 SO/HA ratio Fig. A12: XRD Rietveld analysis spectrum of α-tcp with 0.16 SO/HA ratio

13 Development of bioactive silicon doped Calcium Phosphate cements for tissue engineering application Page 13 Fig. A13: XRD Rietveld analysis spectrum of α-tcp with 0.32 SO/HA ratio Fig. A14: XRD Rietveld analysis spectrum of α-tcp with 0.48 SO/HA ratio

14 Page 14 Master s thesis Here are the results obtained by the Rietveld method for the Si-α-TCP powder with the different SiO 2/HA ratio (a Rietveld refinement is considered valid according to the χ² value: the smaller it is. the more precise the result will be): SiO 2 /HA molar ratio % alpha % beta % HA χ² 0 10 ± ± ± ± ± ± ± ± ± ± ± ± Table A2: crystalline phase repartition according to Rietveld analysis

Supplementary Fig. 1.

Supplementary Fig. 1. (a,b,e,f) SEM and (c,d,g,h) TEM images of (a-d) TiO 2 mesocrystals and (e-h) NiO mesocrystals. The scale bars in the panel c, d, g, and h are 500, 2, 50, and 5 nm, respectively. SAED