Deposition, Microstructure and Nanoindentation of Multilayer Zr Nitride and Carbonitride Nanostructured Coatings

Nitrides, carbides, and carbonitrides of transition metal elements like Zr, W, Ti, etc. are generally employed to produce hard coatings. Zirconium-based hard coatings have shown useful applications in the areas of tribology, biomedicine and electrical due to their high thermal stability, hardness, biocompatibility, good erosion, wear, and corrosion resistance. In this study, we created homogeneous and tenacious nanostructured hard coatings based on Zr with good mechanical properties. The magnetron sputter deposition technique was utilized to coat stainless steel 316L substrates with multilayers of Zr/ZrN and ZrN/ZrCN with individual layer thicknesses of 250 and 500 nm for each coating composition. The deposition conditions were adjusted to create two different coating thicknesses of 2 and 3 µm. The thickness of the coating was confirmed using Calotest and the coatings’ morphology and elemental composition were determined utilizing the atomic force microscope and scanning electron microscope equipped with energy dispersive x-ray spectrometer. Coating thickness and adhesion were measured using cross-sectional samples and XRD was utilized to analyze the coatings structure. Nanoindenter was employed to determine the instrumental nanoindentation hardness and elastic modulus. The influence of coating thickness on tribological behavior was further investigated using the ratio of nanohardness-to-elastic modulus (H/E). No evidence of decohesion was observed at the substrate/coatings interface, and the grains of all the coatings were observed to show columnar growth which were homogeneous, compact and dense. The grains of the ZrN/ZrCN coatings were observed to be denser, finer and more compact compared to those of the Zr/ZrN coatings. Correspondingly, higher hardness, modulus and H/E values were exhibited by ZrN/ZrCN than Zr/ZrN coatings. This suggests that the ZrN/ZrCN coatings are capable of exhibiting better wear resistance and fracture toughness. The coatings developed in this investigation are anticipated to be suitable for applications in tribology due to their excellent hardness and H/E properties.

Xe Ion Irradiation-Induced Microstructural Evolution and Hardening Effect of Nickel-Base Superalloy

The nickel-base superalloy Hastelloy N was irradiated using 1 MeV Xe20+ and 7 MeV Xe26+ ions with displacement damage ranging from 0.5 dPa to 10 dPa at room temperature (RT). The irradiated Ni-based superalloy was characterized with transmission electron microscopy (TEM), XRD, and nanoindenter to determine the changes in microstructural evolution and nanoindentation hardness. The TEM results showed that ion irradiation induced a large number of defects such as black spots and corrugated structures and the second phase was rapidly amorphized after being irradiated to a fluence of 0.5 dPa. The XRD results showed that the Hastelloy N alloy sample did not undergo lattice distortion after ion irradiation. An obvious irradiation hardening phenomenon was observed in this study, and the hardness increased with Xe ion fluence. The pinning effect in which the defects can become obstacles to the free movement of dislocation may be responsible for the irradiation-induced hardening.

The influence of the titanium Grade 2 thermoplastic deformation on the nanoindenation properties

Pure titanium is in biotechnology a desired material due to its excellent biocompatibility and the absence of toxic elements like a vandium or aluminium. Unfortunately, in comparison to widely used Ti6Al4V alloy it has low strenght properties. Therefore, the thermoplastic deformation was used as a means to improve its mechanical properties by the grain fragmentation. An experiment of samples compression in hightened temperature and various strain rates was conducted. The stress-strain curves and microstructure observations were made. Both indicated grain reduction. In the next step nanoindentation hardness and Young modulus measurments were made. The results indicate slight increase in hardness and stiffness in most cases. For the high strain rates a decrease in those values was observed.

Effect of Cold Rolling on the Evolution of Shear Bands and Nanoindentation Hardness in Zr41.2Ti13.8Cu12.5Ni10Be22.5 Bulk Metallic Glass

The effect of cold rolling on the evolution of hardness (H) and Young’s modulus (E) on the rolling-width (RW), normal-rolling (NR), and normal-width (NW) planes in Zr41.2Ti13.8Cu12.5Ni10Be22.5 (Vitreloy 1) bulk metallic glass (BMG) was investigated systematically using nanoindentation at peak loads in the range of 50 mN–500 mN. The hardness at specimen surface varied with cold rolling percentage (%) and the variation is similar on RW and NR planes at all the different peak loads, whereas the same is insignificant for the core region of the specimen on the NW plane. Three-dimensional (3D) optical surface profilometry studies on the NR plane suggest that the shear band spacing decreases and shear band offset height increases with the increase of cold rolling extent. Meanwhile, the number of the pop-in events during loading for all the planes reduces with the increase of cold rolling extent pointing to more homogeneous deformation upon rolling. Calorimetric studies were performed to correlate the net free volume content and hardness in the differently cold rolled specimens.

Nanoindentation Hardness and Practical Scratch Resistance in Mechanically Tunable Anti-Reflection Coatings

This work presents fundamental understanding of the correlation between nanoindentation hardness and practical scratch resistance for mechanically tunable anti-reflective (AR) hardcoatings. These coatings exhibit a unique design freedom, allowing quasi-continuous variation in the thickness of a central hardcoat layer in the multilayer design, with minimal impact on anti-reflective optical performance. This allows detailed study of anti-reflection coating durability based on variations in hardness vs. depth profiles, without the durability results being confounded by variations in optics. Finite element modeling is shown to be a useful tool for the design and analysis of hardness vs. depth profiles in these multilayer films. Using samples fabricated by reactive sputtering, nanoindentation hardness depth profiles were correlated with practical scratch resistance using three different scratch and abrasion test methods, simulating real world scratch events. Scratch depths from these experiments are shown to correlate to scratches observed in the field from consumer electronics devices with chemically strengthened glass covers. For high practical scratch resistance, coating designs with hardness >15 GPa maintained over depths of 200–800 nm were found to be particularly excellent, which is a substantially greater depth of high hardness than can be achieved using previously common AR coating designs.

Nanoindentation in multi-modal map combinations: a correlative approach to local mechanical property assessment

A method is presented for the registration and correlation of property maps of materials, including data from nanoindentation hardness, Electron Back-Scattered Diffraction (EBSD), and Electron Micro-Probe Analysis (EPMA). This highly spatially resolved method allows for the study of micron-scale microstructural features, and has the capability to rapidly extract correlations between multiple features of interest from datasets containing thousands of data points. Two case studies are presented in commercially pure (CP) titanium: in the first instance, the effect of crystal anisotropy on measured hardness and, in the second instance, the effect of an oxygen diffusion layer on hardness. The independently collected property maps are registered using affine geometric transformations and are interpolated to allow for direct correlation. The results show strong agreement with trends observed in the literature, as well as providing a large dataset to facilitate future statistical analysis of microstructure-dependent mechanisms. Graphical abstract