Phase-pure Cu4O3 microspheres were
synthesized
for the first time via a facile solvothermal method, using Cu(NO3)2·3H2O as the precursor. A formation
mechanism was proposed based on the observation of a series of reaction
intermediates. The samples were characterized by X-ray diffraction,
scanning electron microscopy, transmission electron microscopy, thermogravimetric
analysis, temperature-programmed
reduction and oxidation, X-ray photoelectron spectroscopy, and nitrogen
adsorption. It was found that the composition of the prepared products
were highly dependent on the synthesis conditions, particularly the
hydrate water content in the copper precursor of Cu(NO3)2. Pure Cu4O3 microspheres with
a diameter of 2–10 μm could be obtained via the symproportionation
reaction (2CuO + Cu2O → Cu4O3), which was regarded not being feasible in aqueous media under mild
synthesis conditions. The electrochemical properties of the Cu4O3 microspheres as anode materials for Li-ion batteries
were also investigated. Compared to the simple physical mixture of
CuO and Cu2O with an equivalent atomic ratio of 2:1, the
as-prepared Cu4O3 exhibited unique lithium storage
behaviors at a low voltage range and superior electrochemical performances
as an anode material for Li-ion batteries. The successful preparation
of pure Cu4O3 material could provide opportunities
to further explore its physicochemical properties and potential applications.
Mesoporous Cu 2 O (MP-Cu 2 O) microspheres were prepared via a facile template-free hydrothermal synthesis in the open system, in which copper acetate was used as the copper precursor and glucose as a reducing agent. The synthesis conditions and catalytic property of MP-Cu 2 O for dimethyldichlorosilane synthesis via the Rochow reaction were investigated, and the formation mechanism of MP-Cu 2 O microspheres was proposed. The samples were characterized by nitrogen adsorption, X-ray diffraction, temperature-programmed reduction, thermogravimetric analysis, transmission electron microscopy, and scanning electron microscopy. It was found that the synthesis conditions such as reaction temperature, time, and reactant amount added have a significant effect on the morphology and pore structure of MP-Cu 2 O microspheres, and MP-Cu 2 O microspheres were formed through assembly of Cu 2 O nanoparticles. MP-Cu 2 O microspheres with a surface area of 65.8 m 2 /g, pore size of 26.7 nm, and a diameter of 400À700 nm were obtained under the optimized condition. As compared to the nonporous Cu 2 O microspheres, MP-Cu 2 O microspheres showed a better catalytic performance in dimethyldichlorosilane synthesis due to their developed pore structure and high surface area, which allow larger contact interface among the reaction gas, solid catalyst, and the solid reactant, together with enhanced mass transport. The work would be helpful for developing novel structured copper catalysts for organosilane synthesis and for understanding the catalytic mechanism.
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