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Phase change of monoclinic hydroxyapatite prepared by wet method

机译:湿法制备单斜羟基磷灰石的相变

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Monoclinic hydroxyapatite was prepared by a wet method and followed by heating in air at 1473 K for 1 h, and its phase transition was investigated by high temperature X-ray powder diffractometry and differential scanning calorimetry. The prepared hydroxyapatite is 98percent monoclinic. The Rietveld refinement results revealed that the low temperature phase has monoclinic symmetry, space group P2_1/b and the high temperature phase has hexagonal symmetry, space group P6_3/m. In monoclinic hydroxyapatite, two different sizes of oxygen triangles exist. The rotation of phosphate tetrahedra at about 6 deg and the change of the hydroxyl order to disorder arrangement occurred due to the phase transition. The phase transition took place reversibly at 480.5(1) K in heating process and 477.5(1) K in cooling process with the enthalpy value of 130(1) Jmol~(-1). Further, a sintered monoclinic hydroxyapatite was prepared. Discontinuity of dielectric curves was observed at 483 K The discontinuity of dielectric curves was concluded to the change of hydroxyl order to disorder arrangement.
机译:采用湿法制备单斜基羟基磷灰石,然后在空气中于1473 K下加热1 h,并通过高温X射线粉末衍射法和差示扫描量热法研究其相变。制备的羟基磷灰石为98%的单斜晶。 Rietveld细化结果表明,低温相具有单斜对称性,空间群为P2_1 / b,高温相具有六边形对称性,空间群为P6_3 / m。在单斜羟基磷灰石中,存在两个不同大小的氧三角。磷酸四面体在大约6度旋转,并且由于相变而发生羟基顺序改变为无序排列。在加热过程中相变可逆地发生在480.5(1)K,在冷却过程中相变发生在477.5(1)K,其焓值为130(1)Jmol〜(-1)。此外,制备了烧结的单斜晶羟基磷灰石。介电曲线的不连续性在483 K处观察到。介电曲线的不连续性可以归结为羟基顺序改变为无序排列。

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