(562a) In-Situ Ftir Analysis Of Porous Low-K Film Repair

In-situ FTIR analyses were performed to study the mechanism of silylation reactions on porous methylsilsesquioxane (p-MSQ) films with hexamethyldisilazane (HMDS) and different chlorosilanes dissolved in carbon dioxide at supercritical conditions. Ellipsometry and goniometry analysis were used to measure the formation of layers over the film and the recovery of hydrophobicity of the surface by the different treatments performed. Three levels of temperature (40°C, 45°C, and 50°C), and three levels of concentrations (0.5 mL, 1 mL, and 2 mL of chlorosilane injected) at 8.0 MPa were used to measure the kinetic response of the reaction using a new system setup created with characteristic of a semibatch reactor. Besides this semibatch reactor, the apparatus had an ISCO syringe pump to supply the CO₂ to the reactor, temperature control loops (heating tape, PID controller, and a K-thermocouple), and actuated valves. The reactor had two chambers. One of them was used to mix the chlorosilane with the CO₂; the other was equipped with two IR-transparent windows (ZnSe) and was used to perform transmission analyses. The IR beam used was guided by two mirrors and went through a Thermonicolet FTIR spectrometer and an MCTA detector used to analyze the 4000-650 wavenumber IR range.