The article is about the development of a new non-destructive microwave method for measuring the electrophysical properties of materials, based on the method of transmission and reflection of a plane monochromatic wave through layered materials. The method has been verified by the results of numerical and field experiments. A data processing technique is described for obtaining complex values of dielectric and magnetic permeability based on an original measurement scheme. Based on the results of mathematical calculations, the laboratory model was created using an ultra-wideband antenna and a parabolic mirror. The optimal distance of the antenna from the parabolic mirror for focusing the electromagnetic field has been determined based on the simulation. Testing was carried out in the frequency range 3–13 GHz on two samples of materials (plexiglass and textolite) with known electrophysical properties. The obtained results showed the reliability of the developed method and its applicability. The measurement error was less than 2%.