A new process to synthesize polycrystailine samples of Sr14Cu24O41 was presented. Firstly, dry gel powder of Sr14Cu24O41 was synthesized by the citrates sol-gel method, using Sr(NO3)2, Cu(NO3)2, ethylene glycol and citrate acid as raw materials. Then, polycrystalline samples of Sr14Cu24O41 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 ℃. 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 Tρin the Arrhenius plot of the resistivity versus temprature.
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