The direct electrochemical synthesis of metal alkoxides [Ti(OEt)4, Ti(OPr-i)4, Ti(OBu)4, Ti(OEt)2(acac), Cu(OEt)2, Cu(OBu)2, Mg(OEt)2 and Ni(OEt)2] were studied by anode dissolution of metals in abso...The direct electrochemical synthesis of metal alkoxides [Ti(OEt)4, Ti(OPr-i)4, Ti(OBu)4, Ti(OEt)2(acac), Cu(OEt)2, Cu(OBu)2, Mg(OEt)2 and Ni(OEt)2] were studied by anode dissolution of metals in absolute ethanol in the presence of a conductive additives. The anodic behaviour of Ti electrode in ethanol was investigated by using cyclic voltammetry(CV). These metal alkoxides were characterized by FTIR spectra. The results show that direct electrochemical synthesis of metal alkoxides have a high current efficiency and electrolysis yield. These alkoxides have a high purity and can be directly used as the precursor of nanosize oxides prepared by sol-gel procedure. The anodic behaviour of Ti electrode in alcohol is markedly the feature of the pitting corrosion. The passivation of Ti anode would occur in the presence of trace water.展开更多
Metallic titanium was electrochemically dissoluted in absolute ethanol in the presence of Et4N· Br(as electro conductive additive),The electrolyte solution was then directly hydrolysized to obtain nanocrystalline...Metallic titanium was electrochemically dissoluted in absolute ethanol in the presence of Et4N· Br(as electro conductive additive),The electrolyte solution was then directly hydrolysized to obtain nanocrystalline TiO2.The powder obtained was calcined at 720℃ for 1 h.FT IR,Raman spectra,XRD and TEM were used to investigate the structure and particle size of the powder.Studies showed that the nanocrystalline TiO2 prepared by this method was of monocline structure with high textural stability and narrow size distribution of 10- 20 nm,and its Raman spectra showed a shift of about 25 cm- 1.The experiments also showed that the product yield could be improved by controlling the temperature under 50- 60℃ ,selecting R4N· Br as conductive additive and preventing titanium anode from being passivated.The electrochemical dissolution of metal anode may be recommanded as a promising technique for the synthesis of nanomaterials.展开更多
文摘The direct electrochemical synthesis of metal alkoxides [Ti(OEt)4, Ti(OPr-i)4, Ti(OBu)4, Ti(OEt)2(acac), Cu(OEt)2, Cu(OBu)2, Mg(OEt)2 and Ni(OEt)2] were studied by anode dissolution of metals in absolute ethanol in the presence of a conductive additives. The anodic behaviour of Ti electrode in ethanol was investigated by using cyclic voltammetry(CV). These metal alkoxides were characterized by FTIR spectra. The results show that direct electrochemical synthesis of metal alkoxides have a high current efficiency and electrolysis yield. These alkoxides have a high purity and can be directly used as the precursor of nanosize oxides prepared by sol-gel procedure. The anodic behaviour of Ti electrode in alcohol is markedly the feature of the pitting corrosion. The passivation of Ti anode would occur in the presence of trace water.
文摘Metallic titanium was electrochemically dissoluted in absolute ethanol in the presence of Et4N· Br(as electro conductive additive),The electrolyte solution was then directly hydrolysized to obtain nanocrystalline TiO2.The powder obtained was calcined at 720℃ for 1 h.FT IR,Raman spectra,XRD and TEM were used to investigate the structure and particle size of the powder.Studies showed that the nanocrystalline TiO2 prepared by this method was of monocline structure with high textural stability and narrow size distribution of 10- 20 nm,and its Raman spectra showed a shift of about 25 cm- 1.The experiments also showed that the product yield could be improved by controlling the temperature under 50- 60℃ ,selecting R4N· Br as conductive additive and preventing titanium anode from being passivated.The electrochemical dissolution of metal anode may be recommanded as a promising technique for the synthesis of nanomaterials.