On the film density using high power impulse magnetron sputtering, 2010, SURFACE and COATINGS TECHNOLOGY, (205) AbstractThe influence on thin film density using high power impulse magnetron sputtering (HiPIMS) has been investigated for eight different target materials (Al, Ti, Cr, Cu, Zr, Ag, Ta, and Pt).The density values as well as deposition rates have been compared to results obtained from thin films grown by direct current magnetron sputtering (DCMS) under the same experimental conditions. Overall, it was found that the HiPIMS deposited coatings were approximately 5-15 % denser compared to the DCMS deposited coatings. This could be attributed to the increased metal ion bombardment commonly seen in HiPIMS discharges, which also was verified using a global plasma model to assess the degree of ionization of 2 sputtered metal. One key feature is that the momentum transfer between the growing film and the incoming metal ions is very efficient due to the equal mass of film and bombarding species, leading to a less pronounced columnar microstructure. As expected the deposition rates were found to be lower for HiPIMS compared to DCMS. For several materials this decrease is not as pronounced as previously reported in the literature, which is shown in the case of Ta, Pt, and Ag with rate HiPIMS /rate DCMS ~ 70-85 %, while still achieving denser coatings.

Due to the very limited availability of B 4 C targets in an Ar discharge, using an industrial deposition system. The films were characterized with scanning electron microscopy, elastic recoil detection analysis, x-ray reflectivity, and neutron radiography. We show that the film-substrate adhesion and film purity are improved by increased substrate temperature and deposition rate. A deposition rate of 3.8 Å /s and substrate temperature of 400 C result in films with a density close to bulk values and good adhesion to film thickness above 3 lm. Boron-10 contents of almost 80 at. % are obtained in 6.3 m 2 of 1 lm thick 10 B 4 C thin films coated on Al-blades. Initial neutron absorption measurements agree with Monte Carlo simulations and show that the layer thickness, number of layers, neutron wavelength, and amount of impurities are determining factors. The study also shows the importance of having uniform layer thicknesses over large areas, which for a full-scale detector could be in total $1000 m

Epitaxial growth of sp 2 -hybridized boron nitride (sp 2 BN) films on sapphire substrates is demonstrated in a hot wall chemical vapor deposition reactor at the temperature of 1500 °C, using triethyl boron and ammonia as precursors. The influence of the main important process parameters, temperature, N/B ratio, B/H 2 ratio, and carrier gas composition on the quality of the grown layers is investigated in detail. X-ray diffraction shows that epitaxial rhombohedral BN (r-BN) film can be deposited only in a narrow process parameter window; outside this window either turbostratic-BN or amorphous BN is favored if BN is formed. In addition, a thin strained AlN buffer layer is needed to support epitaxial growth of r-BN film on sapphire since only turbostratic BN is formed on sapphire substrate. The quality of the grown film is also affected by the B/H 2 ratio as seen from a change of the spacing between the basal planes as revealed by X-ray diffraction. Time-of-flight elastic recoil detection analysis shows an enhancement of the C and O impurities incorporation at lower growth temperatures. The gas phase chemistry for the deposition is discussed as well as the impact of the growth rate on the quality of the BN film.

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Piezoelectric wurtzite ScxAl1−xN (x = 0, 0.1, 0.2, 0.3) thin films were epitaxially grown by reactive magnetron co-sputtering from elemental Sc and Al targets. Al2O3(0001) wafers with TiN(111) seed and electrode layers were used as substrates. X-ray diffraction shows that an increase in the Sc content results in the degradation of the crystalline quality. Samples grown at 400 °C possess true dielectric behavior with quite low dielectric losses and the leakage current is negligible. For ScAlN samples grown at 800 °C, the crystal structure is poor and leakage current is high. Transmission electron microscopy with energy dispersive x-ray spectroscopy mapping shows a mass separation into ScN-rich and AlN-rich domains for x ≥ 0.2 when substrate temperature is increased from 400 to 800 °C. The piezoelectric response of epitaxial ScxAl1−xN films measured by piezoresponse force microscopy and double beam interferometry shows up to 180% increase by the addition of Sc up to x = 0.2 independent of substrate temperature, in good agreement with previous theoretical predictions based on density-functional theory.

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Epitaxial growth of sp2‐hybridized boron nitride (BN) using chemical vapour deposition, with ammonia and triethyl boron as precursors, is enabled on sapphire by introducing an aluminium nitride (AlN) buffer layer. This buffer layer is formed by initial nitridation of the substrate. Epitaxial growth is verified by X‐ray diffraction measurements in Bragg–Brentano configuration, pole figure measurements and transmission electron microscopy. The in‐plane stretching vibration of sp2‐hybridized BN is observed at 1366 cm–1 from Raman spectroscopy. Time‐of‐flight elastic recoil detection analysis confirms almost perfect stoichiometric BN with low concentration of carbon, oxygen and hydrogen contaminations. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)

Metastable Ti 1-x Al x N (0.4 ≤ x ≤ 0.76) films are grown using a hybrid approach in which high-power pulsed magnetron sputtering (HIPIMS) is combined with dc magnetron sputtering (DCMS). Elemental Al and Ti metal targets are co-sputtered with one operated in HIPIMS mode and the other target in DCMS; the positions of the targets are then switched for the next set of experiments. In both cases, the AlN concentration in the co-sputtered films, deposited at T s = 500 °C with R = 1.5-5.3 Å/s, is controlled by adjusting the average DCMS target power. Resulting films are analyzed by x-ray diffraction, scanning electron microscopy, transmission electron microscopy, atomic force microscopy, elastic recoil detection analysis, and nanoindentation.Mass spectroscopy is used to determine ion energy distribution functions at the substrate. The distinctly different flux distributions obtained from targets driven in HIPIMS vs. DCMS modes allow the effects of Al n+ and Ti n+ (n = 1, 2) ion irradiation on film growth kinetics, and resulting properties, to be investigated separately. Bombardment with Al n+ ions (primarily Al + in the Al-HIPIMS/Ti-DCMS configuration) during film growth leads to NaCl-structure Ti 1-x Al x N (0.53 ≤ x ≤ 0.60) films which exhibit high hardness (> 30 GPa) with low stress (0.2 -0.7 GPa tensile). In contrast, films with corresponding AlN concentrations grown under Ti n+ metal ion irradiation (with a significant Ti 2+ component) in the Ti-HIPIMS/Al-DCMS mode have much lower hardness, 18-19 GPa, and high compressive stress ranging up to 2.7 GPa. The surprisingly large variation in mechanical properties results from the fact that the kinetic AlN solubility limit x max in 2 Ti 1-x Al x N depends strongly on, in addition to T s and R, the target power configuration during growth and hence the composition of the ion flux. AlN with x max  64 mol% can be accommodated in the NaCl structure under Al n+ ion flux, compared with  40 mol% for growth with Ti n+ flux. The strong asymmetry in film growth reaction paths is due primarily to the fact that the doubly-ionized metal ion flux is approximately two orders of magnitude higher from the Ti target, than from Al, powered with HIPIMS. This asymmetry becomes decisive upon application of a moderate substrate bias voltage, -60 V, applied synchronously with HIPIMS pulses, during growth.