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Different shape Fe3O4 nanoparticles and its core/shell nanostructures are fabricated for the investigation into microwave absorption.The size,morphology, and various core/shell structure have great influence on the microwave properties of the particles.The complex permeability and complex permittivity are measured and for the further calculation of the reflection loss of the Fe3O4 composites in a range of 2-18 GHz.