In this project, Ti13Zr13Nb alloy was investigated in term of surface pre-treatment using two different types of acids, i.e. H2SO4 and Kroll’s etchant solutions. Prior to etching, all substrates were cut, polished and blasted at identical conditions. Al2O3 abrasive particles of 150 µm mean grain size were used to blast. Consequently, substrates were etched using two different acid solution (H2SO4 66% and Kroll’s etchant) at three different temperatures (25ºC, 45ºC, 60ºC) and varied times (10 s, 20 s, 30 s). Surface morphologies of etched substrates were evaluated under Field Emission-Scanning Electron Microscope equipped with Energy Dispersive Analysis X-ray (EDAX) and Atomic Force Microscopy (AFM). Surface roughness of treated samples were measured using the surface roughness machine. Finally, Kroll’s etchant with 30 seconds and 45ºC considers the best condition for providing surface roughness, at 400 nanometer (Ra) which is believed as good surface prior to PVD coating.