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Characterization of electrodeposited calcium phosphate coatings by complementary scanning electron microscopy and sanning-transmission electron microscopy associated to X-ray microanalysis

Abstract : Calcium phosphate (CAP) coatings on Ti6A14V substrate were elaborated by electrodeposition at different current densities (2,5 and 10 mA/cm2). The surface morphology and the chemical composition of the coatings were characterized by scanning electron microscopy associated to X-ray microanalysis (SEM-EDXS). However, these CAP coatings are irregular specimens (rough surface, porosity, variable thickness), so the SEM-EDX analysis becomes limited. Therefore, we carried out an experimental procedure to minimize these effects which is based on global analysis by SEM-EDXS confirmed by a nanometer scale analysis using scanning transmission electron microscopy associed to X-ray microanalysis. Moreover, phase analysis was performed by X-ray diffraction in order to corroborate the chemical characterization and to identify the different calcium phosphate phases as a function of current density. The results showed that at 2 m/cm2 current density, the coating is composed of an octacalcium phosphate: Ca8H2(PO4)6 and its amorphous phase called OCPam. At 5 mA/cm2, the coating is a mix of calcium deficient hydroxyapatite (Ca-def HAP): Ca10-x(HPO4)x(PO4)6-X(OH)2-x with 0< x <2 and its amorphous phase called Ca-def HAPam. And, at 10 mA/cm2, the coating is mainly composed of an amorphous phase of Ca-def HAPam. Furthermore, cathodic reaction mechanisms of electrolytic CaP coatings on Ti6A14V are proposed to explain the different kinds of calcium phosphate obtained.
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https://www.hal.inserm.fr/inserm-00069610
Contributor : Dominique Laurent-Maquin <>
Submitted on : Thursday, May 18, 2006 - 4:16:24 PM
Last modification on : Wednesday, November 6, 2019 - 6:26:11 PM

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Nicolas Dumelié, Hicham Benhayoune, Céline Rousse-Bertrand, Sylvie Bouthors, Alain Perchet, et al.. Characterization of electrodeposited calcium phosphate coatings by complementary scanning electron microscopy and sanning-transmission electron microscopy associated to X-ray microanalysis. Thin Solid Films, Elsevier, 2005, 492 (1-2), pp.131-139. ⟨10.1016/j.tsf.2005.07.209⟩. ⟨inserm-00069610⟩

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