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Herein, a uniform spherical shaped Gd(III) doped Yb2O3 (Gd@Yb2O3) nanoparticles (NPs) was successfully synthesized via hydrothermal method for electrochemical detection of H2O2. The calcination effect and porosity of the materials well elaborated in the present work. The optical properties, size, morphological, thermal, sensing, surface and crystalline properties of synthesized materials were examined by several techniques. The enhanced electrocatalytic performance of Gd@Yb2O3 make the present sensor excellent towards the determination of H2O2.The a