We evaluated Triangular Voltage Sweep (TVS) measurements as a technique to characterize plasma damage in low-k films. Blanket wafers with low-k films of different porosity and k value were prepared. Our samples included an SiOC:H material with 7% porosity and k value of 3.0, deposited on 200mm wafers, and two SiOC:H materials with 25% porosity and k value of 2.5, deposited on 300mm wafers. Before deposition, a thin layer of dry thermal oxide (2 – 5 nm) was grown on the n-type wafers to stabilize the silicon interface. After deposition, low-k films were exposed to N2/H2 plasma for different times in order to induce different degree of plasma damage. Untreated low-k films were always included as a reference. For electrical measurements, metal dots were deposited on pieces to fabricate Metal-Insulator-Semiconductor capacitors.
TVS measurements were performed at 190°C on the different samples. On samples exposed to N2/H2 plasma, we detected a current peak in the TVS trace, whose magnitude increased with exposure time to plasma. No peaks were detected on untreated films. This indicates that TVS measurements are sensitive to plasma damage. Furthermore, TVS results correlated well with FTIR spectra that showed increasing damage and H2O uptake with increasing exposure time to plasma. We conclude that TVS measurements are suitable for characterizing the degree of plasma damage in low-k films and complement well materials analysis, because with the help of TVS a link to leakage properties can be made. As an application, we used TVS measurements for evaluating restoration of plasma damaged low-k films by long N2-bake at high temperature. Wafer pieces from each sample were baked at 350°C for 4h30min in N2 atmosphere. A few pieces were measured immediately after baking. The remaining pieces were either left exposed to ambient for a few days or dipped in deionized H2O for a few hours to evaluate recovery of hydrophobic properties. The different treatments (N2-bake, exposure to ambient, H2O dipping) were always performed on blanket wafer pieces. Metal dots for electrical measurements were only deposited after the treatment. CV and FTIR measurements were performed before and after treatments to evaluate change in k-value and material structure, respectively. Our data show that long N2-bake at high temperature can partially restore damaged low-k films. The magnitude of the damage-related TVS peak was significantly reduced after heat treatment and remained stable even after H2O dipping. CV measurements performed on baked pieces after 6 days of exposure to ambient showed a reduced k-value. Consistently, FTIR spectra showed a significant reduction of H2O content soon after baking. The materials remained stable over several days and only minor reincorporation of H2O occurred after exposure to ambient or H2O dipping. Therefore, long N2-bake at high temperature can partially restore leakage (TVS), k-value (CV) and hydrophobic properties (FTIR) of damaged low-k films.