Coconut Shell (CS) as agricultural lignocellulosic biomaterial and agro-waste is predominantly available in India, Malaysia, Nigeria, Thailand, Sri Lanka, and Indonesia. It has proven to have effective durability characteristic, good abstractive resistance, high toughness, and good adsorption properties, and is most suitable for long standing use in many applications such as reinforcement, source of energy, fillers as well as activated carbon and its performance, efficiency and effectiveness depend wholly on whether is in form of nano-, micro-, and macro- particles. In this data, effects of milling time on morphological characteristics was experimented using Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX), and X-Ray Fluorescence (XRF) analyses. The SEM images were taken at magnifications of 1.00kx, 2.00kx and 5.00kx which gives respective 50 µm, 20 µm and 10 µm in different milling time of 0, 20, 40 and 60 mins. Digital Vibratory Disc Milling Machine (VDMM) rated 380 V/50 Hz at 940 rpm was employed for the grinding and the morphology of the milled nanoparticles were characterised. It was revealed from the data collected that 0 min (i.e. 75 µm sieved) has the highest mean area value of 16.105 µm2 and area standard deviation of 200.738 µm2 with least value of a number of particle size distribution of 809 µm. In contrast, 60 mins milled has the lowest values for mean area and area standard deviation of 8.945 µm2 and 115.851 µm2 respectively with the highest number of particle size distribution of 2032 µm. It was observed that milling time increases the number of particle sizes distributions and reduces the area of particle size.