Amorphous citrate process has been used to synthesize the complex perovskite SrYb0.5Nb0.5O3 (SYN) powder. Citrate-nitrate gels were produced at room temperature by first reacting NbCl5 with aqueous solution of NH4OH to produce Nb(OH)(5) and then mixing the filtered Nb(OH)(5) with strontium nitrate and yitterbium nitrate in citric acid aqueous solution. The precursor ash was produced by auto ignition of the dehydrated precursor gel at 200degreesC. Finely crystallized SYN powder could be obtained by thermal decomposition of the citrate precursors ash at temperature as low as 1000degreesC. X-ray diffraction, Infra-red transmittance spectroscopy and electron microscopy have been used to characterize the precursors and annealed materials synthesized by citrate process. The citrate process is very promising and simple for preparing complex perovskite SrYb0.5Nb0.5O3.