The thermal atomic layer deposition of TiO2 from Cp*Ti(OMe)3 and ozone was studied in a 300 mm wafer reactor by quadrupole mass spectrometry (QMS). The deposited thin films were analyzed by X-ray reflectivity (XRR), X-ray photoelectron spectroscopy (XPS), grazing incident X-ray diffraction, and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The XRR and XPS measurements revealed that nearly stoichiometric TiO2 films were grown in a self-limiting growth mode. The growth per cycle increased from 0.22 Å at 235 °C to 0.29 Å at 330 °C. Films deposited on titanium nitride showed an anatase crystal structure, while films deposited on ruthenium crystallized in the rutile phase. The ToF-SIMS analysis indicated that the carbon contamination reduced to very low levels at a deposition temperature of 295 °C. The QMS studies revealed the release of MeOH during the precursor pulse. CO2 and H2O were released during the ozone pulse at a process pressure of 7 mbar. At a pressure of 3 × 10−3 mbar, the release of the Cp* ligand and the remaining OMe ligands during the ozone pulse could be observed. It was demonstrated that QMS studies can be used in a 300 mm reactor at very low pressures to study the process chemistry.

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The mechanisms of technologically important atomic layer deposition (ALD) processes, trimethylaluminium (TMA)/ozone and tetrakis(ethylmethylamino)hafnium (TEMAH)/ozone, for the growth of Al(2)O(3) and HfO(2) thin films are studied in situ by a quadrupole mass spectrometer coupled with a 300 mm ALD reactor. In addition to released CH(4) and CO(2), water was detected as one of the reaction byproduct in the TMA/O(3) process. In the TEMAH/O(3) process, the surface after the ozone pulse consisted of chemisorpted active oxygen and -OH groups, leading to the release of H(2)O, CO(2), and HNEtMe during the metal precursor pulse.

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