A new process to synthesize polycrystalline samples of Sr(14)Cu(14)O(41) was presented. Firstly, dry gel powder of Sr(14)Cu(21)O(41) was synthesized by the citrates sol-gel method, using Sr(NO(3))(2), Cu(NO(3))(2), ethylene glycol and citrate acid as raw materials. Then, polycrystalline samples of Sr(14)Cu(24)O(4)1 were prepared by solid-state reaction. Thermal Gravimetric and Differential Thermal Analysis(TG-DTA) showed that the temperature for solid-state reaction is at 942 degrees C. The samples are,identified to be single phase by X-ray Diffraction(XRD) and Scanning Electron Microscopy(SEM). The SEM pictures showed that the first-step particles were at even size of about 100 nm by this technique. The electronic transport measurements showed that the doping compound were semiconductor with a crossover temperature T(rho) in the Arrhenius plot of the resistivity versus temprature.
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