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In this study a highly flexible microwave shielding material was fabricated by solution casting method utilizing Nickel and biocarbon particles in PVA matrix and characterized for mechanical, magnetic, and microwave shielding properties. The main aim of this study was to prove the significant role of magnetic particles in electromagnetic interference (EMI) shielding along with conductive particles. The results show that the addition of Ni‐biocarbon hybrid particle increases the shielding properties up to 56.5 dB at 20 GHz. The magnetic permeability increased gradually with the inclusion of Ni particles with a highest magnetization, coercivity, and retentivity of 1250 E⁻⁶ emu, −9000 G, and 1100 E⁻⁶ emu. Similarly the mechanical results show that adding biocarbon enhances the composite's mechanical properties. A highest tensile strength, tear strength, elongation, and hardness are noted as 38, 168 MPa, 18.4 …