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SiC-Zn nanocomposites with about 20% volume fraction of metal were fabricated by infiltration process under the pressure of 2-8 GPa and at the temperature of 400_1000oC. SiC nanopowders used in the experiments formed loosely agglomerated chains of single crystal nanoparticles. The dimension of the agglomerates was in the micrometer range, the mean grain size was up to tens of nanometers. Microstructural investigations of the nanocomposites were performed at a different resolution levels using scanning, transmission electron microscopy and atomic force microscopy techniques (SEM, TEM, AFM, respectively). SEM observations indicate a presence of nano-dispersed, uniform (on the micrometer scale) mixture of two phases. TEM observations show that distribution of SiC and Zn nanocrystallites is uniform on the nanometer scale. High-resolution TEM images demonstrate an existence of thin (on the order of tens of Angstroms) Zn layers separating SiC grains. AFM images of the mechanically polished samples show a smooth surface with the roughness on the order of the SiC grain size (10-30 nm). After ion etching of some samples the AFM topographs show surface irregularities: periodically spaced hillocks 50-100 nm in height. The size of the SiC grains remains equal to that of the initial powder crystallites. The size of the Zn grains varies in the range of 20-100 nm depending on the initial SiC grain size and the composite fabrication conditions.

Thermal surface purification in an inert gas flow and densification processes of SiC and diamond nanocrystalline powders with specific surface in the range of 60 – 300 m2/g and average grain sizes from 5 to 15 nm in diameter were examined. Termogravimetric Analysis (TGA) linked with mass spectrometry of outgassing products show that surface impurities desorb at up to 450°C. Further heating above 450°C leads to oxidation of the powder surface. Small Angle X-Ray Scattering (SAXS) and gas porosimetry (ASAP) was applied to investigate densification of the nanocrystalline powders. Compaction under 1GPa or higher pressure was found necessary for obtaining the ceramic matrix with porosity in the nanometer range.

A considerable fraction of atoms in nanosize particles is at the grain surface (due to the small size of the crystals). We assume that the surface atoms form a separate structural phase relative to the bulk of the grain (the core). Therefore, one set of the lattice parameters characterizing a nanocrystal may be inadequate for a unique description of its structure. An alternative evaluation of diffraction data of nanocparticles, based on the 'apparent lattice parameter' is proposed. Based on this new methodology it is shown that real nano-crystals constitiute a complex, more than a one-uniform-phase structure.

Two methods of the analysis of powder diffraction patterns of diamond and SiC nanocrystals are presented: (a) examination of changes of the lattice parameters with diffraction vector Q ('apparent lattice parameter', alp) which refers to Bragg scattering, and (b), examination of changes of inter-atomic distances based on the analysis of the atomic Pair Distribution Function, PDF. Application of these methods was studied based on the theoretical diffraction patterns computed for models of nanocrystals having (i) a perfect crystal lattice, and (ii), a core-shell structure, i.e. constituting a two-phase system. The models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the shell. X-ray and neutron experimental diffraction data of nanocrystalline SiC and diamond powders of the grain diameter from 4 nm up to micrometers were used. The effects of the internal pressure and strain at the grain surface on the structure are discussed based on the experimentally determined dependence of the alp values on the Q-vector, and changes of the interatomic distances with the grain size determined experimentally by the atomic Pair Distribution Function (PDF) analysis. The experimental results lend a strong support to the concept of a two-phase, core and the surface shell structure of nanocrystalline diamond and SiC.