Ultraprecision machining of metal matrix composites (MMCs) is observed as a scientific challenge, due to their hard-to-machine property and often the poor surface finish. This paper presents an experimental investigation on surface generation in ultraprecision machining of Al/B4C/50p MMCs. The machining trials using straight flute polycrystalline diamond (PCD) tools are conducted on a high precision micro milling machine. Side milling is adopted under varied cutting conditions. Metrology assessments on the workpiece surface roughness, topography, texture and defects/features are undertaken using a ZYGO 3D surface profiler and a scanning electron microscope (SEM). Experimental results indicate that process parameters and their contributions play essential roles in the machining process. By applying the optimal process parameters, e.g. cutting speed of 188.496 m/min, feed rate of 10 μm/rev and axial depth of cut of 150 μm, a better surface generation with surface roughness Ra < 20 nm can be obtained in ultraprecision machining of Al/B4C/50p particulate MMCs.