Silicon nanoparticles (SiNPs) can be synthesized by a variety of methods. In many cases these routines are non-scalable with low product yields or employ toxic reagents. One way to overcome these drawbacks is to use one-pot synthesis based on the chemical reduction of micelles. In the following study trichloroalkylsilanes of differing chain lengths were used as a surfactant, and the level of capping, surface bonding and size of the nanoparticles formed has been investigated. FTIR results show that the degree of alkyl capping for SiNPs with different capping layers was constant, although SiNPs bound with shorter chains display a much higher level of Si-O owing to the reaction of the ethanol used in the method with uncapped sites on the particle. SiNPs with longer chain length capping show a sharp Si-H peak on the FTIR, these were heated at reflux with the corresponding 1-alkene to fully cap these particles, resulting in a reduction/disappearance of this peak with a minimal change in the intensity of the Si-O peak. Other techniques used to analyze the surface bonding and composition, XPS, H-NMR, and TEM/EDX, show that alkyl-capped SiNPs have been produced using this method. The optical properties showed no significant changes between the different capped SiNPs.