Abstract
Ordered mesoporous CMK-5 carbons with ultra-thin carbon pore walls and highly dispersed Ni nanoparticles have been successfully prepared by using two different SBA-15 silicas as hard templates and 2, 3-di-hydroxynaphtalene (DHN) as a carbon precursor. The nickel precursor was a concentrated nickel nitrate hexahydrate [Ni(NO3)2.6H2O] solution in isopropanol added to the carbon-silica nanocomposites prior to thermal treatments. The samples studied were analyzed by thermogravimetry (TG), nitrogen adsorption at -196�C, powder X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (STEM) and in situ electron diffraction X-ray spectroscopy (EDX). While TG revealed carbon contents lower than 30 wt%, nitrogen adsorption provided information about homogeneity of carbon thin film deposited onto mesopore walls of ordered silica templates, SBA-15. The templates, carbon-silica nanocomposites and carbon inverse replicas with nickel nanoparticles exhibited uniform pores, high surface areas and large pore volumes. Graphitic carbon was identified by the presence of a characteristic G band on Raman spectra, whereas the diffraction peak attributed to the stacking of graphene planes was not observed by powder XRD. The presence of ordered domains in the carbon materials studied was confirmed by small angle XRD and STEM imaging. In addition, the STEM images revealed that the nickel nanoparticles were uniform in size, ~3nm, and were homogeneously dispersed within ordered tubular carbon walls. A few larger clusters of nickel, ~60nm, present on the external surface, were identified by powder XRD as metallic Ni. The in situ EDX revealed that the small nanoparticles were largely composed of Ni with traces of NiO. Similar nanoparticles dispersions have been reported only for Ni-containing multi-walled carbon nanotubes (CNTs), whereas previously reported ordered mesoporous carbons possessed larger Ni/NiO nanoparticles within CMK-3 nanostructure.
