用X射线衍射(XRD)、傅立叶变换红外光谱(FTIR)、热重-差热(TG-DTA)、扫面电子显微镜(SEM)等分析方法对水热改性前及改性不同阶段乌贼骨的矿物组成、表面形貌等进行了表征、分析, 并对水热反应机理进行了研究. 结果显示, 原始乌贼骨主要由棒状文石层堆砌而成, 外观呈多孔的房架式结构. 在磷酸盐溶液中水热处理后, 内部的文石经由固态局部规整离子交换反应(Solid-state topotactic ion exchange reaction)转变为羟基磷灰石, 原来文石结晶体的形貌及规则排列方式没有改变; 而外表面文石则通过溶解-重结晶(Dissolution-recrystallization)过程转变为鳞片
状的羟基磷灰石, 随着水热处理时间的延长, 鳞片状羟基磷灰石进一步自组装成5μm左右的规则圆球, 本文对自组装的机理也做了初步探讨.
The composition and morphology
of original cuttlebone and hydroxyapatite(HAP)-converted cuttlebone were
characterized by means of X-ray diffraction (XRD), Fourier transmission
infrared spectroscopy (FTIR), thermogravimetric-differential thermal analysis(TG-DTA) and scanning electron microscopy (SEM). The mechanism of self-assembly was also discussed. The results show that the mineral of original cuttlebone is rod-like aragonite polymorph of CaCO3 and the chamber-like macroporous architecture is its extrinsic feature. In phosphate solution, the interior aragonite
converts hydrothermally to HAP by a solid-state topotactic ion-exchange reaction in which the HAP retains the morphology and the orientation of the original aragonite. Meanwhile, the exterior aragonite converts hydrothermally to HAP via dissolution-recrystallization, with squama-like morphology. These squama-like HAP self-assemble to microspheres with hydrothermal reaction time prolonged.
参考文献
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