Dr. M. N. Dastur School of Materials Science and Engineering, Indian Institute of Engineering Science and Technology, Shibpur, Howrah 711103, India; Bioceramics and Coating Division, CSIR-Central Glass & Ceramic Research Institute, 196 Raja S.C. Mullick Road, Kolkata 700032, India.
Advanced Mechanical and Materials Characterization Division, CSIR-Central Glass and Ceramic Research Institute, Kolkata 700032, India.
J Mech Behav Biomed Mater. 2019 Jul;95:136-142. doi: 10.1016/j.jmbbm.2019.03.032. Epub 2019 Apr 9.
Fluorine substituted hydroxyapatite (FAp) with different degree of fluorine (F) substitution, has been synthesized using hydrothermal synthesis method. In the present work, as synthesized powders were consolidated by sintering at 1200 °C in air for 1 h. The sintered specimens were characterized using Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD) for phase analysis. Further, fluorine intake in the sintered specimens was evaluated using ion chromatography (IC). XRD peaks clearly showed biphasic nature of the sintered specimen. However, the sintered samples containing more than ∼60% fluorine substitution showed no β-tricalcium phosphate (β-TCP) phase formation. The IC results revealed that the degree of fluoridation decreased significantly in the sintered specimen compare to the respective as synthesized powders. The effect of actual fluorine content in the sintered specimens was further evaluated in terms of sinterability, surface energy, mechanical properties and in vitro cytocompatibility study. The surface energy of the sintered specimen decreased from 51.8 mN/m to 42.5 mN/m, in which degree of fluoridation varies from 0% to 110%. The in vitro cytocompatibility of the sintered specimen were carried out against mouse osteoblast cell line (MC3T3-E1). In vitro study showed that all the samples were nontoxic but cell proliferation for the samples containing more than 40% fluorine substitution became significantly low.
采用水热合成法合成了不同氟取代度的氟取代羟基磷灰石（FAp）。在本工作中，将合成的粉末在空气中于 1200°C 下烧结 1 h 进行固结。采用傅里叶变换红外光谱（FTIR）和 X 射线衍射（XRD）对相分析进行了烧结试样的表征。此外，还采用离子色谱（IC）法评价了烧结试样中氟的摄入量。XRD 峰清楚地显示出烧结试样的双相性质。然而，氟取代度大于约 60%的烧结样品没有形成β-磷酸三钙（β-TCP）相。IC 结果表明，与相应的合成粉末相比，烧结试样中的氟化程度显著降低。进一步根据烧结性、表面能、力学性能和体外细胞相容性研究来评估烧结试样中实际氟含量的影响。烧结试样的表面能从 51.8 mN/m 降低到 42.5 mN/m，其中氟取代度从 0%变化到 110%。对烧结试样进行了体外细胞相容性测试，采用小鼠成骨细胞系（MC3T3-E1）。体外研究表明，所有样品均无毒，但含有 40%以上氟取代的样品的细胞增殖显著降低。
