Ti0.5Al0.5N alloy films, typically 1.5 μm thick, were grown on MgO(001) at temperatures Ts between 400 and 850 °C by ultra-high-vacuum reactive magnetron sputtering in pure N2. Films grown at Ts between ≂480 and 560 °C were single crystals in which the lattice misfit strain was partially relieved by glide of 〈001〉 misfit dislocations, with Burgers vector =a0/2〈011〉, on {011̄} planes. Cross-sectional transmission electron microscopy investigation showed no evidence of residual extended defects in the films until thicknesses of ≂150 nm at which point threading dislocations, oriented along the [001] growth direction, were observed. Surface-initiated spinodal decomposition, resulting in the formation of compositionally modulated NaCl-structure platelets along [001] with width ≂1 nm, occurred over a narrow growth temperature range between 540 and 560 °C as a precursor to bulk phase separation of wurtzite-structure AlN at Ts≥560 °C. The alloy was continuously depleted of AlN at higher growth temperatures until the equilibrium two-phase structure, cubic TiN and wurtzite AlN, was obtained at Ts≥750 °C.

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Abstract.A simple and cost effective approach to stabilize the sputtering process in the transition zone during reactive high-power impulse magnetron sputtering (HiPIMS) is proposed. The method is based on real-time monitoring and control of the discharge current waveforms. To stabilize the process conditions at a given set point, a feedback control system was implemented that automatically regulates the pulse frequency, and thereby the average sputtering power, to maintain a constant maximum discharge current. In the present study, the variation of the pulse current waveforms over a wide range of reactive gas flows and pulse frequencies during a reactive HiPIMS process of Hf-N in an Ar-N 2 atmosphere illustrates that the discharge current waveform is a an excellent indicator of the process conditions. Activating the reactive HiPIMS peak current regulation, stable process conditions were maintained when varying the N 2 flow from 2.1 to 3.5 sccm by an automatic adjustment of the pulse frequency from 600 Hz to 1150 Hz and consequently an increase of the average power from 110 to 270 W. Hf-N films deposited using peak current regulation exhibited a stable stoichiometry, a nearly constant power-normalized deposition rate, and a polycrystalline cubic phase Hf-N with (111)-preferred orientation over the entire reactive gas flow range investigated. The physical reasons for the change in the current pulse waveform for different process conditions are discussed in some detail.

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High power impulse magnetron sputtering (HiPIMS) is an ionized physical vapor deposition technique, providing a high flux of metal ions to the substrate. However, one of the disadvantages for industrial use of this technique is a reduced deposition rate compared to direct current magnetron sputtering (dcMS) at equal average power. This is mainly due to a high target back-attraction probability of the metal ions with typical values in the range 70%–90% during the pulse. In order to reduce this effect, we focused on the contribution of ion fluxes available immediately after each HiPIMS pulse; a time also known as afterglow. Without a negative potential on the target at this stage of the HiPIMS process, the back-attracting electric field disappears allowing remaining ions to escape the magnetic trap and travel toward the substrate. To quantify the proposed mechanism, we studied the effect of HiPIMS pulse duration on the outward flux of film-forming species in titanium discharges, which are known to exhibit more than 50% reduction in deposition rate compared to dcMS. By shortening the HiPIMS pulse length, it was found that the contribution to the outward flux of film-forming species from the afterglow increases significantly. For example, HiPIMS discharges at a constant peak current density of about 1.10 A cm−2 showed a 45% increase of the deposition rate, by shortening the pulse duration from 200 to 50 μs. Ionized flux fraction measurements, using a gridless quartz crystal micro-balance-based ion meter, showed that this increase of the deposition rate could be achieved without compromising the ionized flux fraction, which remained approximately constant. The key to the achieved optimization of HiPIMS discharges lies in maintaining a high peak discharge current also for short pulse lengths to ensure sufficient ionization of the sputtered species.

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Low-temperature epitaxial growth of refractory transition-metal nitride thin films by means of physical vapor deposition has been a recurring theme in advanced thin-film technology for several years. In the present study, 150-nm-thick epitaxial HfN layers are grown on MgO(001) by reactive high-power impulse magnetron sputtering (HiPIMS) with no external substrate heating. Maximum film-growth temperatures T s due to plasma heating range from 70 to 150 °C, corresponding to T s /T m = 0.10-0.12 (in which T m is the HfN melting point in K). During HiPIMS, gas and sputtered metal-ion fluxes incident at the growing film surface are separated in time due to strong gas rarefaction and the transition to a metal-ion-dominated plasma. In the present experiments, a negative bias of 100 V is applied to the substrate, either continuously during the entire deposition or synchronized with the metal-rich portion of the ion flux. Two different sputtering-gas mixtures, Ar/N 2 and Kr/N 2 , are employed in order to probe effects associated with the noble-gas mass and ionization potential. The combination of x-ray diffraction, high-resolution reciprocal-lattice maps, and high-resolution cross-sectional transmission electron microscopy analyses establishes that all HfN films have a cube-on-cube orientational relationship with the substrate, i.e., [001] HfN ||[001] MgO and (100) HfN ||(100) MgO . Layers grown with a continuous substrate bias, in either Ar/N 2 or Kr/N 2 , exhibit a relatively high mosaicity and a high concentration of trapped inert gas. In distinct contrast, layers grown in Kr/N 2 with the substrate bias synchronized to the metal-ion-rich portion of HiPIMS pulses have much lower mosaicity, no measurable inert-gas incorporation, and a hardness of 25.7 GPa, in good agreement with the results for epitaxial HfN(001) layers grown at T s = 650 °C (T s /T m = 0.26). The room-temperature film resistivity is 70 μΩ cm, which is 3.2-10 times lower than reported values for polycrystalline-HfN layers grown at T s = 400 °C.