Porous tubular oxide precursors have been fabricated from the ZrO2 powder and its mixture with the Nb2O5 powder, and directly metallised to pure Zr or the Zr−2.5Nb Zircaloy tubes through electrochemical reduction and deoxygenation that induces in situ consolidation or sintering of the metallized tubes in molten CaCl2 at ∼900 °C. This new process is simple, fast, and low in energy consumption, promising a new technology for the fabrication of zirconium/Zircaloy tubes, which are the crucial materials in nuclear reactors and chemical plants. Also reported in this paper is the mechanism of the electrochemical process, correlating the cyclic voltammogram of ZrO2 powder in a metallic cavity electrode with the morphological and compositional analyses of the products from potentiostatic electrolysis of porous ZrO2 pellets.
Although, in the carbon family, graphite is the most thermodynamically stable allotrope, conversion of other carbon allotropes, even amorphous carbons, into graphite is extremely hard. We report a simple electrochemical route for the graphitization of amorphous carbons through cathodic polarization in molten CaCl at temperatures of about 1100 K, which generates porous graphite comprising petaloid nanoflakes. This nanostructured graphite allows fast and reversible intercalation/deintercalation of anions, promising a superior cathode material for batteries. In a Pyr TFSI ionic liquid, it exhibits a specific discharge capacity of 65 and 116 mAh g at a rate of 1800 mA g when charged to 5.0 and 5.25 V vs. Li/Li , respectively. The capacity remains fairly stable during cycling and decreases by only about 8 % when the charge/discharge rate is increased to 10000 mA g during cycling between 2.25 and 5.0 V.
Although, in the carbon family,graphite is the most thermodynamically stable allotrope,c onversion of other carbon allotropes,e ven amorphous carbons,i nto graphite is extremely hard. We report as imple electrochemical route for the graphitization of amorphous carbons through cathodic polarization in molten CaCl 2 at temperatures of about 1100 K, which generates porous graphite comprising petaloid nanoflakes.This nanostructured graphite allows fast and reversible intercalation/deintercalation of anions,p romising as uperior cathode material for batteries.I naPyr 14 TFSI ionic liquid, it exhibits aspecific discharge capacity of 65 and 116 mAh g À1 at ar ate of 1800 mA g À1 when charged to 5.0 and 5.25 Vv s. Li/ Li + ,r espectively.T he capacity remains fairly stable during cycling and decreases by only about 8% when the charge/ discharge rate is increased to 10000 mA g À1 during cycling between 2.25 and 5.0 V.Supportinginformation and the ORCID identification number(s) for the author(s) of this article can be found under http://dx.
Production of silicon film directly by electrodeposition from molten salt would have utility in the manufacturing of photovoltaic and optoelectronic devices owing to the simplicity of the process and the attendant low capital and operating costs. Here, dense and uniform polycrystalline silicon films (thickness up to 60 µm) are electrodeposited on graphite sheet substrates at 650 °C from molten KCl-KF-1 mol% K 2 SiF 6 salt containing 0.020-0.035 wt% tin. The growth of such high-quality tin-doped silicon films is attributable to the mediation effect of tin in the molten salt electrolyte. A four-step mechanism is proposed for the generation of the films: nucleation, island formation, island aggregation, and film formation. The electrodeposited tindoped silicon film exhibits n-type semiconductor behavior. In liquid junction photoelectrochemi cal measurement, this material generates a photocurrent about 38-44% that of a commercial n-type Si wafer.
The electrochemical reduction of the insulative
ZrO2
powder in molten
CaCl2
was investigated using the metallic cavity electrode (MCE) in molten
CaCl2
at
850°C
. Cyclic voltammograms (CVs) revealed two consecutive reduction peaks corresponding to (i)
ZrO2
to
ZrxO
(x≥1)
and (ii)
ZrxO
to Zr. The intermediate,
ZrxO
, was metastable and underwent disproportionation to
ZrO2
and Zr, which was responsible for the detection of Zr metal in the potentiostatic reduction at less negative potentials. In the anodic scan, four main oxidation processes were observed. The relevant reactions were rationalized as the reoxidation of (iii)
ZrxO
to
ZrO2
, (iv) Zr to
ZrO2
, (v) Zr to
ZrCl2
, and (vi) Zr to
ZrCl4
. The metastable intermediate also contributed to the unique current variations in the anodic potential scans under different conditions. Potentiostatic electrolysis of the
ZrO2
powder in the MCE at the feature potentials of the CVs and analyses of the electrolysis products by scanning electron microscopy and energy dispersive X-ray spectroscopy confirmed the electroreduction mechanism and revealed the localized conversion of the dense aggregates of the submicrometer particles of
ZrO2
to cauliflower-like aggregates of the nanoparticulates of Zr in the early stage of the electroreduction process.
Turing lead into gold: Hollow hybrid PbS(x)-Au nanostructures of about 10 nm in diameter were synthesized using a one-step reaction under mild experimental conditions. The redox reaction of gold precursors with PbS nanocrystals in the presence of dodecylamine leads to the hollow feature of hybrid nanostructures (see picture).
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