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X-ray photoemission spectra of reactively sputtered TiN1.0 films are recorded without interference from adsorbed contaminants or ion sputter cleaning damage. In this way, the transition from hcp TiN0.3 to fcc TiN1.0 is characterized by a discontinuity in film stoichiometry, Ti 2p splitting energy, and Ti 2p3/2 binding energy as a function of the Ar/N2 ratio during sputtering. The line shapes of the N 1s and 2s transitions experience only an asymmetric broadening on forming fcc TiN. The core-level N 1s transition of fcc TiN is modeled as two components peaks with binding energies at 396.8 and 396.0 eV. Similarly, the valence band N 2s transition has corresponding component peaks at 16.8 and 16.2 eV. These high and low binding energy pairs are interpreted as on-site Ns and interstitial site Ni populations of nitrogen in a fcc TiN lattice, respectively. The ratio of N/Ti is 1.0 and the Ns/Ni ratio is approximately 6. Both ratios are independent of the composition of the sputtering gas mixture and the substrate temperature once fcc TiN is formed. The core level Ti 2p transition in fcc TiN is characteristic of a single Ti3+ oxidation state with a line shape that is also insensitive to the gas composition and the substrate temperature during sputtering.

The electrical resistivity of reactively sputtered TiN films was measured as a function of film thickness. The effect of directionality of the sputtered atoms, substrate temperature, bias voltage, deposition rate, and film morphology on the electron conductivity in TiN films was studied. The combination of rapid deposition rate and high substrate temperature with bias-collimated sputtering results in TiN films with the lowest resistivity, 45 μΩ cm, the largest temperature coefficient of resistance, 1355 ppm, and the highest superconducting transition temperature, 5.04 K. These films are characterized by small grains with mixed <111≳ and <200≳ orientation and reduced electron scattering with an estimated electron mean-free path of 96 nm.

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Silicon surfaces are cleaned in an electron cyclotron resonance excited hydrogen plasma and characterized by in situ x-ray photoelectron spectroscopy and in situ static secondary ion-mass spectrometry. Emission spectroscopy and actinometry are used to characterize the hydrogen plasma. Exposure to the plasma for 3 to 4 minutes without applying heat or bias to the substrate completely removes the native silicon oxide resulting in a hydrogen terminated surface that is resistant to reoxidation. Adventitious hydrocarbon, when present on the surface, is also completely removed by the plasma. A shift in the isotope ratios of silicon suggests that a clean 〈100〉 silicon surface is monohydride terminated, whereas a 〈111〉 silicon surface appears largely dihydride terminated. A depth profile of the silicon isotope ratios shows a temporal instability, which with the assignment of a H 1s state in the valence-band spectra provides evidence that the hydrogen is concentrated at the surface and has not diffused deep into the silicon lattice. The oxygen removal rate has the following characteristics: two distinct microwave operating regimes separated by a discontinuity in power around 600 W; a singularity corresponding to rapid oxygen removal at 2.5 mTorr; an abrupt and near monotonic decrease in oxygen removal above 14 mTorr; and an invariance of the removal rate to ion-energy from about 10 to 100 eV. The density of hydrogen excited species and the ground state hydrogen atom density are correlated with the oxygen removal rate under all conditions except high pressure, where the density of hydrogen ions is low. This suggests an ion-induced etching mechanism whereby the native silicon oxide removal is enhanced with low-energy hydrogen ion bombardment.