In this work, we studied the recovery of copper from AMD by cementation with iron powder. Aiming to control the size of copper particles within the nanoscale, we tested the use of the anionic surfactant sodium dodecyl sulfate (SDS). We tested three levels of concentration (0.2, 0.4 and 0.6 M) and temperature (25, 50 and 75°C). The activation energy of cementation was also assessed by fitting the experimental data with the Arrhenius equation. The concentration of dissolved metals was determined by inductively-coupled plasma spectrometry (ICP/AES). The cemented product was characterized by X-ray diffraction (XRD) and scansion electron microscopy (FE-SEM) to determine phase composition, particle size distribution and morphology. Under all investigated conditions, the cementation reaction was found to be a diffusion-controlled process. Without surfactant, the activation energy was 18 kJ/mol. In the presence of SDS the activation energy increased up to about 35 kJ/mol. Whether using SDS or not, the particle size of the copper product was strongly affected by the cementation temperature. Without SDS, the cemented product aggregated into micro-sized clusters of about 15 µm at 25°C, 2-3 µm at 50°C and 1 µm at 75°C. The addition of SDS determined a dramatic decrease of copper particle size up to the nanoscale. Under the best operating conditions, the particle size of copper was lower than 100 nm.