| The electro-synthesis of metal alkoxide used pure metal as sacrificial anode and inertia electrode as cathode. Current passed through the absolute alcohol solution with the electro-conductive additive, and metal anode was dissolved and reducing reaction occurred on cathode. The Sol-gel process, which was based on the hydrolysis and condensation of metal alkoxide, could synthesize nanometer material with a special structure , high purity and well-proportioned granularity at a low temperature.In this paper, the organic ammonium was used as electro-conductive additive. 3.5g lithium slice was added in the ethanol and acetyl-acetone solution, and then the precursor of the nano-LiTi2O4 powder was synthesized by anodic dissolution of titanium at the current of 0.2A for 4h. Nano-LiTi2O4 powder was prepared for by a direct sol-gel process of the electrolyte solution and calcining at the temperature of 4500C for 2h. IR. spectrum, TG-DTA, XRD, and TEM were used to investigate the structure of the precursor and the nano- LiTi2O4 powder. The result showed that the nano-sized LiTi2O4 with a narrow distribution of 10-15 nm was obtained by the electrochemical dissolution following hydrolysis. The measure, by which nano-NiAl2O4 was synthesized, is similar with that of LiTi2O4 . Nano-sized NiAl2O4 was prepared for by a direct sol-gel process of the electrolyte solution. The structures of the precursor and its nano-sized powder were investigated by IR. spectrum ,TG-DTA, XRD, and TEM. The experiment showed that nano-sized NiAl2O4 with a narrow distribution of 10-20 nm was obtained at a low temperature of 3500C, and it possessed a certain heat stability and a disperse structure. This process may be recommended as a promising method to synthesize other composite nano-powders. |