The characters of metal powder particles are depending on their size, shape and chemical surrounding. In sample preparation it is very important to control the particle size, particle shape and morphology. X-Ray Diffraction (XRD) (Model: Panalytical Empyrean) study is most important tool used in powder materials science. A discussion about simple and low cost preparation of iron powder by (Mini Mill 2 Panalytical) and preparation of the sample was rotating at 15 min and in the case of grinding of samples at high speed 659 rpm. The surface morphology of α-Fe metallic powder was determined with Scanning Tunneling Microscope (STM) (Model: NT-MDT Solver Nano.). X-ray fluorescence analysis is a powerful analytical tool for the determination of almost all the elements present in a sample. The spectra obtained were analyzed using a X-ray fluorescence (XRF) (Model: Rigaku-NEX CG). From the spectra obtained, there were some elements to be present in the sample were Iron (Fe) and Zirconium (Zr).