This chapter measures surface mechanical properties of hybrid-treated layers at low temperature using nanoindentation method. The tools to characterize the treated layers including its roughness were performed by FESEM (Field Emission Scanning Electron Microscope) and USPM (Universal Scanning Probe Microscope). These hybrid-treated samples have shown an increase in hardness and elastic modulus compared to the untreated sample. Moreover, all treated samples have improvement on E/H ratio which shows a decrement to plastic deformation and degrade the disparity of properties, while maintaining the elastic range of deformation. © 2014, Springer International Publishing Switzerland.