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Ultrastructural Observation of Hydroxyapatite Ceramics with Preferred Orientation to a-plane Using High-resolution Transmission Electron Microscopy

机译:使用高分辨率透射电子显微镜具有优选取向对羟基磷灰石陶瓷的超微结构观察

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The dense hydroxyapatite (HAp) ceramics with preferred orientation to a-plahe were fabricated using composite powders of single-crystal apatite fibers (AF) and wet-synthesized apatite gels (AG). AF was synthesized by homogeneous precipitation method. The composites of AF and AG were prepared as the following process. Aqueous (NH4)2HPO4 solutions were added into the AF slurry with the amount of 1 mass%. In addition, aqueous Ca(NO3)2 solutions were added dropwise to the slurry to precipitate the AG on the AF at room temperature, and then aged at room temperature for 24 h with stirring. The dried powders were uniaxially pressed at 200 MPa of compaction pressure and then fired at 1300 °C for 5 h. All the resulting ceramics were identified with HAp single phases. The (100), (200) and (300) reflections which correspond to a-plane were more intense than those of a standard HAp ceramics. With increasing the additive amount of AG, the orientation degree of a-plane decreased, and the relative density increased. Furthermore, the ultrastructure of the resulting ceramics was examined by high-resolution transmission electron microscopy. The selected area electron diffraction patterns showed clear spots corresponding to [110] zone axis direction of HAp crystal with high crystallinity. The lattice spacings of crystal grains were determined to be 0.34 nm or 0.68 nm which corresponds to the lattice constant of (002) or (001) plane of HAp crystal. Therefore, the resulting ceramics were HAp single phases with preferred orientation to a-plane.
机译:使用单晶磷灰石纤维(AF)和湿合成的磷灰石凝胶(Ag)的复合粉末制备具有优选取向的致密羟基磷灰石(HAP)陶瓷与A-PlaHe的优选取向。通过均匀降水法合成AF。制备AF和AG的复合材料作为以下过程。将(NH 4)2HPO 4溶液加入到AF浆料中,其量为1质量%。此外,将Ca水溶液(NO 3)2溶液滴加到浆料中,以在室温下沉淀到AF上的Ag,然后在室温下在搅拌下在室温下老化24小时。将干燥的粉末在200MPa的压实压力下压制,然后在1300℃下烧制5小时。用Hap单相鉴定所有得到的陶瓷。对应于A平面的(100),(200)和(300)反射比标准HAP陶瓷更强烈。随着AG的增加量,A平面的取向度降低,相对密度增加。此外,通过高分辨率透射电子显微镜检查所得陶瓷的超微结构。所选择的区域电子衍射图案显示出对应于Hap晶体的[110]区域轴方向的透明点,具有高结晶度。将晶粒的晶格间隔物测定为0.34nm或0.68nm,其对应于Hap晶体的(002)或(001)平面的晶格常数。因此,所得陶瓷是具有优选取向的HAP单相。

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