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The paper analyses the electromagnetic shielding measurements of carbon fiber composite structure. In particular the shielding effectiveness is measured applying the nested reverberation chamber method in the frequency range of 3.5 GHz–8.5 GHz. This method ensure a realistic electromagnetic excitation of the sample under test characterized by a random polarization and incoming direction. The paper also describes the material manufacturing procedure and gives important details about the sample mounting technique. Three material samples are considered which differ in carbon fiber orientation and stratification. Obtained results highlight the capability of such materials to behave as high-performance shields in the microwave region.