A combinatorial material adhesion study was used to optimize the composition of an adhesion promoting layer for a nanocrystalline diamond (NCD) coating on silicon. Three different adhesion promoting metals, namely W, Cr, and Ta, were selected to fabricate arrays of co-sputtered binary alloy films, with patches of seven different, distinct alloy compositions for each combination, and single element reference films on a single Si wafer (three wafers in total; W–Cr, Cr–Ta, Ta–W). Scratch testing was used to determine the critical failure load and practical work of adhesion for the NCD coatings as a function of adhesion layer chemistry. All tested samples eventually exhibit delamination of the NCD coating, with buckles radiating perpendicularly away from the scratch track. Application of any of the presented adhesion layers yields an increase of the critical failure load for delamination as compared to NCD on Si. While the influence of adhesion layers on the maximum buckle length is less pronounced, shorter buckles are obtained with pure W and Cr–Ta alloy layers. As a general rule, the addition of an adhesion layer showed a 75% improvement in the measured adhesion energies of the NCD films compared to the NCD coating without an adhesion layer, with specific alloys and compositions showing up to 125% increase in calculated practical work of adhesion.

The fabrication of high-hardness non-hydrogenated diamond-like carbon (DLC) via standard magnetron sputtering (MS) is often hindered by the low sputtering yields and ionisation rates of carbon, therefore investigations into pulsed alternatives of MS, else sputtered species post-ionisation methods, are of particular interest. This work focuses on investigating the influence of pulsed-direct current MS (pDCMS), high power impulse magnetron sputtering (HiPIMS) and their microwave plasma-assisted (MA-pDCMS, MA-HiPIMS) variants on the properties of the fabricated DLC films. Two setups were used for the pDCMS- and HiPIMS-based methods, respectively. The films were characterised using Raman spectroscopy, nanoindentation, X-ray reflectometry and scanning electron microscopy, where the pDCMS-produced films were additionally characterised by film-stress measurements. Moreover, in situ time-resolved Langmuir probe plasma analysis was performed under HiPIMS and MA-HiPIMS conditions to analyse the influence of the magnetron and microwave plasmas on one another. For both DCMS- and HiPIMS-based procedures, it was found that the addition of microwave plasma did not facilitate attaining hardnesses beyond 30 GPa, however, it did enable modifying the morphology of the films. Furthermore, this study shows the potential of synchronised sputtering with substrate biasing, as well as the importance of microwave plasma source positioning in relation to the substrate.

In this work, the influence of different pulse widths (25, 50 and 100 μs) during high power impulse magnetron sputtering (HiPIMS) of copper, silver and zirconium was investigated in terms of plasma properties and properties of combinatorial composition gradient CuAgZr film libraries. In situ plasma diagnostics via optical emission spectroscopy (OES), time-of-flight mass spectrometry (TOFMS), and modified quartz crystal microbalance (m-QCM), followed by film ex situ X-ray diffraction (XRD) and scanning electron microscopy (SEM) investigations allowed to determine the effect of deposition parameters on the thin films' microstructural changes. Changing the pulse width, while keeping the duty cycle constant, modified the discharge composition in the target region and the ionised fraction of the sputtered species in the substrate region. The maximum Cu ionised fraction (19 %) was found for 50 μs, resulting in compact and smooth morphology for Cu-rich films, whereas short 25 μs pulses provided porous columnar films with rough surfaces, as the result from Ar+ bombardment. For Ag-rich films, Ag segregation allowed the deposition of dense layers, regardless of the used pulse width. Furthermore, low Ag (<10 at.%) CuAgZr films produced via HiPIMS and direct-current magnetron sputtering (DCMS) were compared in terms of structural and mechanical property changes as a function of Zr contents. For the studied chemical composition range, a linear relationship between Zr content, XRD phase shift and mechanical properties was observed for HiPIMS films, in contrast to DCMS's more abrupt transitions. An increase in hardness and elastic modulus (up to 44 % and 22 %, respectively) was found for the HiPIMS films compared to DCMS ones. The obtained results highlight HiPIMS's flexibility in providing a wide range of tailoring possibilities to meet specific application requirements, such as crystalline microstructure, density and associated mechanical properties.

This work focuses on the low temperature fabrication process of InN thin films via microwave plasma-assisted reactive high power impulse magnetron sputtering (MAR-HiPIMS). The influence of microwave plasma on the HiPIMS discharge process at various nitrogen flows and microwave powers was monitored and characterised through in situ diagnostics, including following HiPIMS I(V,t) curves, optical emission spectroscopy (OES), as well as performing time-resolved Langmuir probe and time-of-flight mass spectroscopy (ToF-MS) measurements. This was followed by the deposition of InN films via standard reactive HiPIMS (reference sample) and MAR-HiPIMS and their characterisation via X-ray diffraction (XRD), reflectometry (XRR), as well as scanning and transmission electron microscopy (SEM, TEM). It was found that the microwave plasma facilitates the dissociation/activation of nitrogen species and supplies seed electrons to the magnetron discharge plasma. Furthermore, the energy of the incoming ions was determined via ToF-MS, and it was possible to identify their plasma origin and temporal behaviour. The produced R-HiPIMS sample was highly metallic, with no nitride phase detected. The MAR-HiPMS film, however, was stoichiometric and exhibited (0002) direction texturing, with an optical bandgap of approx. 1.5 eV, electron concentration of 2.72 × 1020 cm−3 and electron mobility of 7.16 cm2V−1 s−1 (in the range for polycrystalline InN).

Resist-based lithographic tools, such as electron beam (e-beam) and photolithography, drive today’s state-of-the-art nanoscale fabrication. However, the multistep nature of these processes, expensive resists, and multiple other consumables limit their potential for cost-effective nanotechnology. Here, we report a one-step, resist-free, and scalable methodology for directly structuring thin metallic films on flexible polymeric substrates via e-beam patterning. Controlling e-beam dose results in nanostructures as small as 5 nm in height with a sub-micrometer lateral resolution. We structure nanoscale thick films (100 nm) of Al, TiN, and Au on standard Kapton tape to highlight the universal use of our nanopatterning methodology. Further, we utilize direct e-beam writing to create various high-resolution biomimetic surfaces directly onto ceramic thin films. In addition, we assemble architectured mechanical metamaterials comprising crack “traps”, which confine cracks and prevent overall material/device failure. Such a resist-free lithographic tool can reduce fabrication cost dramatically and may be used for different applications varying from biomimetic and architectured metamaterials to strain-resilient flexible electronics and wearable devices.