Extensive research in the area of optical sensing for medical diagnostics requires development of tissue phantoms with optical properties similar to those of living human tissues. Development and improvement of in vivo optical measurement systems requires the use of stable tissue phantoms with known characteristics, which are mainly used for calibration of such systems and testing their performance over time. Optical and mechanical properties of phantoms depend on their purpose. Nevertheless, they must accurately simulate specific tissues they are supposed to mimic. Many tissues and organs including head possess a multi-layered structure, with specific optical properties of each layer. However, such a structure is not always addressed in the presentday phantoms. In this paper, we focus on the development of a plain-parallel multi-layered phantom with optical properties (reduced scattering coefficient μ^'_s and absorption coefficient μ_a) corresponding to the human head layers, such as skin, skull, and gray and white matter of the brain tissue. The phantom is intended for use in noninvasive diffuse near-infrared spectroscopy (NIRS) of human brain. Optical parameters of the fabricated phantoms are reconstructed using spectrophotometry and inverse adding-doubling calculation method. The results show that polyvinyl chloride-plastisol (PVCP) and zinc oxide (ZnO) nanoparticles are suitable materials for fabrication of tissue mimicking phantoms with controlled scattering properties. Good matching was found between optical properties of phantoms and the corresponding values found in the literature.