ABSTRACT
The incorporation of various cations such as Zn (2+) into the structure of fluorapatite, Ca 5(PO 4) 3F, is governed by the effectiveness of the cations to substitute for Ca (2+) ions. In this work different concentrations of zinc were used to substitute for calcium. Microscopic characterization was done by observing the nanostructural variations induced by these zinc substitutions and by relating these observations to thermal behavior of the zinc-substituted fluorapatite. Random incorporation of zinc into the fluorapatite structure and the zinc induced amorphization effects oriented in the nanostructure of fluorapatite led to phase impurities of zinc-substituted fluorapatites when the amount of zinc used was greater than 25 mol % of the total cation concentration. It also was observed that the thermal stability of the samples decreased with increasing zinc concentration. Among the zinc-incorporated samples, the most similar chemical and physical properties to the single-phased fluorapatite were identified in the sample containing the lowest amount of zinc (25 mol %). After calcination, however, this sample showed to contain some defects in the atomic arrangement of the nanostructure which led to a thermal instability of the fluorapatite.
ABSTRACT
Fluorapatite is a naturally occurring mineral of the apatite group and it is well known for its high physical and chemical stability. There is a recent interest in this ceramic to be used as a radioactive waste form material due to its intriguing chemical and physical properties. In this study, the nano-sized fluorapatite particles were synthesized using a precipitation method and the material was characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Two well-known methods, called solution-drop and the microtome cutting, were used to prepare the sample for TEM analysis. It was found that the microtome cutting technique is advantageous for examining the particle shape and cross-sectional morphology as well as for obtaining ultra-thin samples. However, this method introduces artifacts and strong background contrast for high-resolution transmission electron microscopy (HRTEM) observation. On the other hand, phase image simulations showed that the solution-drop method is reliable and stable for HRTEM analysis. Therefore, in order to comprehensively analyze the microstructure and morphology of the nano-material, it is necessary to combine both solution-drop and microtome cutting techniques for TEM sample preparation.
