Abstract

Alumina powders, pure and doped with nickel, were synthetized by sol-gel method and calcined at 500, 900 and 1100?C in order to obtain mesoporous structures with a high specific surface area, well adapTab. to catalytic application. The characterization of samples was performed by XRD, EPR spectroscopy and electrochemical impedance spectroscopy (EIS). XRD analysis showed that the addition of Ni2+, as well as the annealing temperature, affects the structural properties of the obtained composites. EPR analysis revealed the traces of Fe3+ impurities, the presence of oxy defects in alumina and Ni2+ in tetrahedral position for samples calcined at 1100?C. The impedance of the Nafion/alumina modified GCE depended on combined effect of porous structure and surface properties of alumina samples. The electrochemical behavior of a glassy carbon electrode modified with Ni (II)-doped aluminas was studied in 0.5 M NaOH solution, with and without methanol. The electrochemical activity of nickel-doped alumina composites was dictated by the amount of present NiO impurity.

Highlights

  • There is an increasingly growing interest in the electrochemistry of ordered solids based on zeolites, clays, layered double hydroxides with common a nanostructured porous inorganic matrix able to be permeated with organic and inorganic species [1]

  • With further increase of Ni content in alumina samples A20-500 and A40-500, positions of diffraction reflections keep moving to the left, which means that a greater amount of nickel is incorporated into the spinel structure and for sample A40-500 a spinel NiAl2O4 phase (PDF No 73-0239) is stabilized

  • Alumina samples dopped with different amount of nickel were synthetized by sol-gel method and annealed at 500, 900 and 1100 oC

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Summary

Introduction

There is an increasingly growing interest in the electrochemistry of ordered solids based on zeolites, clays, layered double hydroxides with common a nanostructured porous inorganic matrix able to be permeated with organic and inorganic species [1]. Such materials comprise a variety of nanoarchitectures in relation to the shape and size of the crystals and their cavities, pores, channels, etc., from microporous to mesoporous, and a variety of guest’s species. Transition aluminas are important in the field of various catalytic processes because of their high specific surface areas, surface property and crystalline structure [2,3,4,5,6,7]. The aim of electrochemical investigation was to establish connection between electrochemical activity of investigated aluminas and data obtained by other characterization techniques

Materials and Experimental Procedures
X-ray diffraction
Electrochemical impedance spectroscopy
Cyclic voltammetry
Conclusion
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