Journal of The Electrochemical Society · 2011 · 15 citations · 17 references
Natural SciencesChemistryMaterials ScienceElectrochemistryElemental AnalysisMaterials ChemistryCathode MaterialsElectrochemical CellsElectrode KineticsElectrode MaterialsElectrode-electrolyte InterfacesMetalsElectrochemical CharacterizationEnergy Dispersive X-ray SpectroscopyEnergy-dispersive X-ray SpectroscopyHydrogen EvolutionPowder DiffractionPowder Diffraction AnalysisPowder X-ray DiffractionX-ray Absorption Spectroscopy
The reduction and electrodeposition of on a smooth gold foil electrode with an exposed area of was performed in supporting electrolyte using bulk electrolysis with a constant current density of at a potential of . Significant hydrogen evolution accompanied the formation of Tc deposits. Tc concentrations consisted of and and were electrodeposited over various times. Deposited fractions of Tc were characterized by powder x-ray diffraction, x-ray absorption fine structure spectroscopy, and scanning electron microscopy with the capability to measure semiquantitative elemental compositions by energy-dispersive x-ray emission spectroscopy. Results indicate the presence of Tc metal on all samples as the primary electrodeposited constituent for all deposition times and Tc concentrations. Thin films of Tc have been observed followed by the formation of beads that are removable by scratching. After , the quantity of Tc removed from solution and deposited was . The solution, after electrodeposition, showed characteristic absorbances near corresponding to hydrolyzed Tc(IV) produced during deposition of Tc metal. No detectable Tc(IV) was deposited to the cathode.
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Theoretical approaches to x-ray absorption fine structure
J. J. Rehr, R. C. Albers · Reviews of Modern Physics · 2000 · 3.2K citations