The grain boundary area has a great influence on the polycrystalline material properties and in nano crystallized metals. It could be considered as a glass metal phase in addition to crystallites in a composite structure. In this research, a general procedure for directly quantifying the crystalline and amorphous phases is introduced by using an x-ray diffractometry technique.Nickel with a nano crystalline structure was deposited onto pure copper samples with grain sizes of between 17 to 124 nm by an electroplating technique. A combination of measuring the area of the XRD pattern characteristic peaks and x-ray background scattering were used for the estimation of the crystalline and amorphous volume percentages. The results show that there is a non-linear relationship between the percentage of the crystalline phase calculated by the geometrical method and the area of the selected XRD peak. An experimental formula is suggested for the calculation of the crystalline phase volume percentage of the nano structure nickel samples based on the (200) x-ray peak area.