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This invention discloses a walnut-shaped In2O3 / CuO material, its preparation method, and its applications, comprising the following steps: Step 1: solvothermal synthesis of a bimetallic coordination polymer precursor; Step 2: controllable pyrolysis of the precursor to convert it into a target oxide composite material; This invention addresses the difficulty of synergistic regulation of heterostructures and oxygen vacancies in existing methods by proposing a one-step solvothermal-programmed pyrolysis method to prepare a walnut-shaped In2O3 / CuO heterojunction composite material with a three-dimensional hierarchical porous structure and controllable oxygen vacancies, thereby achieving simultaneous optimization of material structure, composition, and defects to improve low-temperature Cl2 sensing performance.