A simple, rapid quantitative approach to determining attachment density on silica nanoparticles has been demonstrated using attenuated total reflectance Fourier transform infrared spectroscopy and verified by thermogravimetric analysis. A very high attachment of approximately 5 attachments per nm2 has been achieved through photoinduced thiol-ene click reaction of 11-bromo-1-undecene with a thiol functionalized silica nanoparticle formed from mercaptopropyltrimethoxysilane as the sole precursor. Attachment density with concentration of alkene and reaction time is shown to be highly nonlinear and appears to be limited by accessability of thiols on the surface of the particle. This method opens the opportunity to form nanoparticles with controlled functionality including multifunctional particles, which have been produced in this work.
Keywords: ATR-FTIR; Quantitative functionalization; Silica nanoparticles; Sol–gel; Thiol–ene click chemistry.