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BaZr0.9Y0.1O2.95 powders were synthesized using both gel‐casting process and solid‐state reaction. The gel‐casting process with citric acid as the complexing agent could result in nanoparticles with a single perovskite phase. Lower calcining temperature and shorter holding time were required to synthesize the BaZr0.9Y0.1O2.95 powders than the traditional solid‐state reaction method. The work demonstrates that the gel‐casting process is a simple, fast, and convenient method for preparing a high‐temperature proton conductor BaZr0.9Y0.1O2.95 powder.