α-tricalcium phosphate (α-TCP) was prepared by a wet precipitation reaction between calcium hydroxide and orthophosphoric acid solutions. The as-synthesised powder was then characterised using a Scanning Electron Microscope (SEM) equipped with Energy Dispersive Spectroscope (EDS), X-ray Diffraction (XRD) and Fourier Transform Infrared Spectroscope (FTIR). Analyses revealed that a phase-pure powder with a Ca/P ratio of 1.5 was produced. In addition, nanosized α-TCP particles of diameter ~ 70 nm were agglomerated to form larger particles of 10μm in diameter. It was found that by the combination of attritor milling and solution evaporation, the agglomerates of α-TCP nanoparticles could be broken down, and distributed evenly within the poly(D,L-lactic-co-glycolic acid) (PLGA) matrix. Thus, a α-TCP/PLGA nanocomposite was successfully produced by a modified solution evaporation method at room temperature followed by hot pressing at 150 °C. The achievable ceramic loading was approximately 38 wt.%, which was confirmed by thermal gravimetric analysis (TGA).