The
cheap stainless commodity steel AISI 304, which basically consists
of Fe, Ni, and Cr, was surface-oxidized by exposure to Cl2 gas. This treatment turned AISI 304 steel into an efficient electrocatalyst
for water splitting at pH 7 and pH 13. The overpotential of the anodic
oxygen evolution reaction (OER), which typically limits the efficiency
of the overall water-splitting process, could be reduced to 260 mV
at 1.5 mA/cm2 in 0.1 M KOH. At pH 7, overpotentials of
500–550 mV at current densities of 0.65 mA/cm2 were
achieved. These values represent a surprisingly good activity taking
into account the simplicity of the procedure and the fact that the
starting material is virtually omnipresent. Surface-oxidized AISI
304 steel exhibited outstanding long-term stability of its electrocatalytic
properties in the alkaline as well as in the neutral regime, which
did not deteriorate even after chronopoteniometry for 150 000
s. XPS analysis revealed that surface oxidation resulted in the formation
of Fe oxide and Cr oxide surface layers with a thickness in the range
of a few nanometers accompanied by enrichment of Cr in the surface
layer. Depending on the duration of the Cl2 treatment,
the purity of the Fe oxide/Cr oxide mixture lies between 95% and 98%.
Surface oxidation of AISI 304 steel by chlorination is an easy and
scalable access to nontoxic, cheap, stable, and efficient electrocatalysts
for water splitting.
The synthesis of 3D self-assembled plasmonic superstructures of gold nanospheres as well as the characterization of their structural and optical properties at the single-particle level is presented. This experimental work is complemented by FEM (finite element method) simulations of elastic scattering spectra and the spatial |E|(4) distribution for establishing structure-activity correlations in these complex 3D nanoclusters.
"Quat-primer" polymers bearing cationic groups were investigated as a surface modifier for Tb-doped cerium phosphate green-emitting fluorescent nanorods (NRs). The NRs were synthesized by a microwave process without using any complex agents or ligands and were characterized with different analytical tools such as X-ray diffraction, transmission electron microscopy, and fluorescence spectroscopy. Poly(ethyleneimine) partially quarternized with glycidyltrimethylammonium chloride was synthesized separately and characterized in detail. (1)H and (13)C NMR spectroscopic studies revealed that the quaternary ammonium group was covalently attached to the polymer. UV-vis spectroscopy was used to examine the stability of the colloidal dispersions of the bare NRs as well as the modified NRs. ζ potential, thermogravimetric analysis, and atomic force microscopy studies were carried out to confirm that the positively charged Quat-primer polymer is adsorbed on the negatively charged surface of the NRs, which results in high dispersion stability. Emission spectra of the modified NRs indicated that there was no interference of the Quat-primer polymer with the fluorescence behavior.
A top-down approach, i.e., creating small particles by mechanical force starting from bulk materials, probably presents the most logical approach to particle size reduction and, therefore, top-down techniques are among the first to achieve small particles. A new solvent-free, amazingly simple approach is reported, suitable to achieve nanoparticles and sub-micro particles.
This contribution aims at evaluating different synthesis procedures leading to zirconia-based aerogels. A series of undoped and yttrium-doped zirconia aerogels have been prepared via hydrolysis and condensation reaction of different alkoxy- and different inorganic salt-based precursors followed by supercritical drying. Well-established but deleterious zirconium n-propoxide (TPOZ) or zirconium n-butoxide (TBOZ) were used as metal precursors in combination with acids like nitric acid and acetic acid as auxiliary agent for the generation of non-yttrium stabilized zirconia aerogels. Yttrium-stabilized zirconia aerogels as well as pure zirconia aerogels were obtained by the salt route starting from ZrCl4 and crosslinking agents like propylene oxide or acetylacetone. The characteristics of the products were analyzed by nitrogen adsorption measurements, electron microscopy, and X-ray scattering. It turned out that with respect to all relevant properties of the aerogels as well as the practicability of the synthesis procedures, approaches based on inexpensive non-toxic salt precursors are the methods of choice. The salt-based approaches allow not only for low-cost, easy-to-handle synthesis procedures with realizable gelation times of less than 60 seconds, but also delivered the products with the highest surface area (449 m(2) g(-1) for ZrCl4) within this series of syntheses.
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