Synthesis, structural model and vibrational spectroscopy of lutetium tricalcium phosphate Ca9Lu(PO4)7  

作　　者：Francesco Capitelli Manuela Rossi Asmaa EIKhouri Mohammed Elaatmani Nicola Corrierot Armida Sodo Giancarlo Della Ventura 

机构地区：[1]Istituto di Cristallografia - CNR, Via Salaria Km 29.300, 00016 Monterotondo (Rome), Italy [2]Dipartimento di Scienze Della Terra Dell'Ambiente e Delle Risorse, University di Napoli FedericoⅡ, Via Mezzocannone 8, 80134 Naples, Italy [3]Faculte des Sciences Semlalia, BP 2390, Universite Cadi Ayyad, Marrakech, Morocco [4]Istituto di Cristallografia CNR, Via G. Amendola, 122/O, 70126 Bari, Italy [5]Dipartimento di Scienze, Universita Roma Tre, Largo S. L. Murialdo 1, 00146 Rome, Italy

出　　处：《Journal of Rare Earths》2018年第11期1162-1168,共7页稀土学报（英文版）

基　　金：Project partially supported by CNR(Italy)-CNRST(Morocco) Bilateral Project "Novel Ca_9RE(PO_4)_7 biomaterials:synthesis and multi-methodological characterization via X-ray techniques" reference CNR 1588/16

摘　　要：Lutetium β-tricalcium phosphate Ca9Lu（PO4）7 was synthesized by solid-state reaction at 1200 ℃, and investigated by means of a combination of scanning electron microscopy （SEM） equipped with energy dispersive X-ray spectroscopy （EDS）, X-ray diffraction （XRD）, Fourier transform infrared （FTIR） and Raman spectroscopies. SEM morphological analysis reveals the presence of sub spherical and prismatic micro crystalline aggregates, while EDS semi-quantitative analysis confirms the nominal Lu/Ca compo- sition. The unit cell and the space group were determined by X-ray powder diffraction data showing that the compound crystallizes in the rhombohedral R3c wfiitlockite-type structure, with unit cell constants a - b 1.04164（1） nm, c 3.7302（1） nm and cell volume V 3.5051（1） nm^3. The investigation was completed with the structural refinement by the Rietveld method, and discussion of the distribution of Lu within cationic sites according to the results of the Rietveld refinement. The FIIR and Raman spectra, correlated to isostructural rare earth phosphates from literature, show slight band shifts of the phosphate modes correlated to the evolving size of the rare earth elements.Lutetium β-tricalcium phosphate Ca9Lu（PO4）7 was synthesized by solid-state reaction at 1200 ℃, and investigated by means of a combination of scanning electron microscopy （SEM） equipped with energy dispersive X-ray spectroscopy （EDS）, X-ray diffraction （XRD）, Fourier transform infrared （FTIR） and Raman spectroscopies. SEM morphological analysis reveals the presence of sub spherical and prismatic micro crystalline aggregates, while EDS semi-quantitative analysis confirms the nominal Lu/Ca compo- sition. The unit cell and the space group were determined by X-ray powder diffraction data showing that the compound crystallizes in the rhombohedral R3c wfiitlockite-type structure, with unit cell constants a - b 1.04164（1） nm, c 3.7302（1） nm and cell volume V 3.5051（1） nm^3. The investigation was completed with the structural refinement by the Rietveld method, and discussion of the distribution of Lu within cationic sites according to the results of the Rietveld refinement. The FIIR and Raman spectra, correlated to isostructural rare earth phosphates from literature, show slight band shifts of the phosphate modes correlated to the evolving size of the rare earth elements.

关 键 词：TCP LUTETIUM SEM-EDS XRD FTIR RAMAN 

分 类 号：TQ132.32[化学工程—无机化工]