We report a new fullerenelike material consisting of cross-linked nano-onions of C and N. Growth of the onion shells takes place atom by atom on a substrate surface and yields thin solid films during magnetron sputter deposition. Electron microscopy and energy loss spectroscopy show that the core shell contains up to $20\mathrm{at}.\mathrm{}\%$ N corresponding to ${\mathrm{C}}_{48}{\mathrm{N}}_{12}$ aza-fullerene composition. Nanoindentation of this nanostructured material gives high resilience with hardness 7 GPa, Young's modulus 37 GPa, and complete elastic recovery after loading with 0.5 mN to a depth of 75 nm. Total energy calculations show the stability of ${\mathrm{C}}_{60-2n}{\mathrm{N}}_{2n}$ aza-fullerenes and suggest the existence of a novel ${\mathrm{C}}_{48}{\mathrm{N}}_{12}$ molecule.

AlN(0001) was alloyed with ScN with molar fractions up to $\sim 22\mathrm{\%}$ , while retaining a single-crystal wurtzite (w-) structure and with lattice parameters matching calculated values. Material synthesis was realized by magnetron sputter epitaxy of thin films starting from optimal conditions for the formation of w-AlN onto lattice-matched w-AlN seed layers on ${\text{Al}}_2{\text{O}}_3\left(0001\right)$ and MgO(111) substrates. Films with ScN contents between 23% and $\sim 50\mathrm{\%}$ exhibit phase separation into nanocrystalline ScN and AlN, while ScN-rich growth conditions yield a transformation to rocksalt structure ${\text{Sc}}_{1-\text{x}}{\text{Al}}_{\text{x}}\text{N}\left(111\right)$ films. The experimental results are analyzed with ion beam analysis, x-ray diffraction, and transmission electron microscopy, together with ab initio calculations of mixing enthalpies and lattice parameters of solid solutions in wurtzite, rocksalt, and layered hexagonal phases.

Epitaxial ${\mathrm{Ti}}_3{\mathrm{SiC}}_2\left(0001\right)$ thin films have been deposited by dc magnetron sputtering from three elemental targets of $\mathrm{Ti}$ , $\mathrm{C}$ , and $\mathrm{Si}$ onto $\mathrm{MgO}\left(111\right)$ and ${\mathrm{Al}}_2{\mathrm{O}}_3\left(0001\right)$ substrates at temperatures of $800–900°\mathrm{C}$ . This process allows composition control to synthesize ${\mathrm{M}}_{n+1}{\mathrm{AX}}_n$ (MAX) phases ($\mathrm{M}$ : early transition metal; $\mathrm{A}$ : $\mathrm{A}$ -group element; $\mathrm{X}$ : $\mathrm{C}$ and∕or $\mathrm{N}$ ; $n=1–3$ ) including ${\mathrm{Ti}}_4{\mathrm{SiC}}_3$ . Depositions on $\mathrm{MgO}\left(100\right)$ substrates yielding the $\mathrm{Ti}–\mathrm{Si}–\mathrm{C}$ MAX phases with $\left(10\overline{1}5\right)$ , as the preferred orientation. Samples grown at different substrate temperatures, studied by means of transmission electron microscopy and x-ray diffraction investigations, revealed the constraints of ${\mathrm{Ti}}_3{\mathrm{SiC}}_2$ nucleation due to kinetic limitations at substrate temperatures below $700°\mathrm{C}$ . Instead, there is a competitive ${\mathrm{TiC}}_x$ growth with $\mathrm{Si}$ segregation to form twin boundaries or $\mathrm{Si}$ substitutional incorporation in ${\mathrm{TiC}}_x$ . Physical properties of the as-deposited single-crystal ${\mathrm{Ti}}_3{\mathrm{SiC}}_2$ films were determined. A low resistivity of $25\mu \Omega \mathrm{cm}$ was measured. The Young’s modulus, ascertained by nanoindentation, yielded a value of $343–370\mathrm{GPa}$ . For the mechanical deformation response of the material, probing with cube corner and Berkovich indenters showed an initial high hardness of almost $30\mathrm{GPa}$ . With increased maximum indentation loads, the hardness was observed to decrease toward bulk values as the characteristic kink formation sets in with dislocation ordering and delamination at basal planes.

Radio frequency sputtering has been used to deposit α-alumina (α-Al2O3) thin films at substrate temperatures of 280–560 °C. The films are shown to be single phased and hard. Nanoindentation gives values of 306±31 and 27±3 GPa for elastic modulus and hardness, respectively, for a substrate temperature of 280 °C. Growth of the α phase was achieved by in situ predeposition of a chromia template layer. Chromia crystallizes in the same hexagonal structure as α-alumina, with a lattice mismatch of 4.1% in the a- and 4.6% in the c-parameter, and is shown to nucleate readily on the amorphous substrates (silicon with a natural oxide layer). This results in local epitaxy of α-alumina on the chromia layer, as is shown by transmission electron microscopy. The alumina grains are columnar with grain widths increasing from 22±7 to 41±9 nm, as the temperature increases from 280 to 560 °C. This is consistent with a surface diffusion dominated growth mode and suggests that α-alumina deposition at low temperatures is possible once initial grain nucleation has occurred. Results are also presented demonstrating chromia/α-alumina growth on a technological substrate (Haynes230 Ni-based super alloy, Haynes International, Inc.).

In this series of articles, a method is presented that performs (semi)quantitative phase analysis for nanocrystalline transmission electron microscope samples from selected area electron diffraction (SAED) patterns. Volume fractions and degree of fiber texture are determined for the nanocrystalline components. The effect of the amorphous component is minimized by empirical background interpolation. First, the two-dimensional SAED pattern is converted into a one-dimensional distribution similar to X-ray diffraction. Volume fractions of the nanocrystalline components are determined by fitting the spectral components, calculated for the previously identified phases with a priori known structures. These Markers are calculated not only for kinematic conditions, but the Blackwell correction is also applied to take into account dynamic effects for medium thicknesses. Peak shapes and experimental parameters (camera length, etc.) are refined during the fitting iterations. Parameter space is explored with the help of the Downhill-SIMPLEX. The method is implemented in a computer program that runs under the Windows operating system. Part I presented the principles, while part II elaborated current implementation. The present part III demonstrates the usage and efficiency of the computer program by numerous examples. The suggested experimental protocol should be of benefit in experiments aimed at phase analysis using electron diffraction methods.