Glancing angle deposition (GLAD) of AlN nanostructures was performed at room temperature by reactive magnetron sputtering in a mixed gas atmosphere of Ar and N₂. The growth behavior of nanostructures shows strong dependence on the total working pressure and angle of incoming flux. In GLAD configuration, the morphology changed from coalesced, vertical nanocolumns with faceted terminations to highly inclined, fan-like, layered nanostructures (up to 38°); while column lengths decreased from around 1743 to 1068 nm with decreasing pressure from 10 to 1.5 mTorr, respectively. This indicates a change in the dominant growth mechanism from ambient flux dependent deposition to directional ballistic shadowing deposition with decreasing working pressures, which is associated with the change of energy and incident angle of incoming reactive species. These results were corroborated using simulation of metal transport (SiMTra) simulations performed at similar working pressures using Ar and N separately, which showed the average particle energy and average angle of incidence decreased while the total average scattering angle of the metal flux arriving at substrate increased with increasing working pressures. Observing the crystalline orientation of GLAD deposited wurtzite AlN nanocolumns using X-ray diffraction (XRD), pole-figure measurements revealed c-axis growth towards the direction of incoming flux and a transition from fiber-like to biaxial texture took place with increasing working pressures. Under normal deposition conditions, AlN layer morphology changed from {0001} to {10$\overline{1}$1} with increasing working pressure because of kinetic energy-driven growth.

The optical contrast and minimum layer thickness of Ni/Ti broadband neutron multilayer supermirrors is usually hampered by an interface width, typically 0.7 nm, caused by nanocrystallites, interdiffusion, and/or intermixing. We explore the elimination of nanocrystallites in combination with interface smoothening by modulation of ion assistance during magnetron sputter deposition of 0.8 to 6.4 nm thick Ni and Ti layers. The amorphization is achieved through incorporation of natural B₄C where B and C preferably bond to Ti. A two-stage substrate bias was applied to each layer; -30 V for the initial 1 nm followed by -100 V for the remaining part, generating multilayer mirrors with interface widths of 0.40-0.45 nm. The results predict that high performance supermirrors with m-values as high as 10 are feasible by using ¹¹B isotope-enriched B₄C combined with temporal control of the ion assistance.

The performance of multilayers in optical components, such as those used in neutron scattering instruments, is crucially dependent on the achievable interface width. We have shown how the interface width of Ni/Ti multilayers can be improved using the incorporation of B₄C to inhibit the formation of nanocrystals and limit interdiffusion and intermetallic reactions at the interfaces. A modulated ion-assistance scheme was used to prevent intermixing and roughness accumulation throughout the layer stack. In this work we investigate the incorporation of low-neutron-absorbing ¹¹B₄C for Ni/Ti neutron multilayers. Combined fitting of neutron reflectivity and X-ray reflectivity measurements shows an elimination of accumulated roughness for the ¹¹B₄C containing multilayers with a mean interface width of 4.5 Å, resulting in an increase in reflectivity at the first Bragg peak by a factor of 2.3 and 1.5 for neutron and X-ray measurements, respectively.

NiP (P > 10 wt.%) coatings are amorphous coatings whose structure can be transformed by heat treatment into a crystalline structure and hardened by precipitation of Ni₃P. In this study, NiP coatings and composite ones with SiC nanoparticles were produced by electrodeposition, and their structural transformation by heat treatment was studied using differential scanning calorimetry (DSC) and X-ray diffraction (XRD). The microhardness and the scratch and corrosion resistance of the coatings were evaluated and compared before and after different heat treatments. The results showed that in as-plated condition, the addition of SiC particles in the coatings did not modify the microstructure, microhardness, or electrochemical behavior. However, the SiC particles’ role was disclosed in combination with heat treatment. Composite coatings that were heat treated at 300 °C had higher microhardness and scratch resistance than the pure NiP one. In addition, composite coatings maintained their scratch resistance up to 400 °C, while in the case of the NiP ones, there was a reduction in scratch resistance by heating at 400 °C. It was also concluded that heating temperature has the main role in hardness and corrosion resistance of NiP and composite coatings, rather than heating time. The optimum heat-treatment protocol was found to be heating at 360 °C for 2 h, which resulted in a maximum microhardness of about 1500 HV_0.02 for NiP and its composite coating without sacrificing the corrosion resistance.

This study analysed the influence of the codeposition of SiC particles with different sizes: 50 nm, 500 nm and 5 μm, and the type of bath agitation (stirring or ultrasonic) on the electrocrystallisation of nickel coatings. The composites matrix microstructure was analysed by means of SEM, EBSD and XRD, to evaluate the grain size, crystal orientation, and internal stresses and was benchmarked against pure nickel samples electrodeposited in equivalent conditions. The codeposition of nano- and microsize particles with an approximate content of 0.8 and 4 vol.%, respectively, caused only a minor grain refinement and did not vary the dominant < 100 > crystal orientation observed in pure Ni. The internal stress was, however, increased by particles codeposition, up to 104 MPa by nanoparticles and 57 MPa by microparticles, compared to the values observed in pure nickel (41 MPa). The higher codeposition rate (11 vol.%) obtained by the addition of submicron-size particles caused a change in the grain growth from columnar to equiaxial, resulting in deposits with a fully random crystal orientation and pronounced grain refinement. The internal stress was also increased by 800% compared to pure nickel. The ultrasound (US) agitation during the deposition caused grain refinement and a selective particle inclusion prompting a decrease in the content of the particles with the larger particles. The deposits produced under US agitation showed an increase in the internal stresses, with double values compared to stirring. The increase in the deposits microhardness, from 280 HV in pure Ni to 560 HV in Ni/SiC submicron-US, was linked to the microstructural changes and particles content. Graphical abstract