Precipitation of secondary intermetallic phases in aluminium alloy Al7075 sintered by spark plasma sintering method from powders milled at room and cryogenic temperature was studied by X-ray powder diffraction. Deformation energy stored during cryogenic milling influences the precipitation in Al7075 alloy. High temperature X-ray diffraction experiment revealed the potential for further precipitation strengthening of samples prepared by spark plasma sintering of milled powders. It was established that the correction of absorption edge of metal Kβ-line filter used for laboratory sources greatly enhances the precision of quantitative Rietveld analysis as well as the determination of precipitates’ crystallite sizes.