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The paper describes the effects of thermal, mechanical and chemical treatment of silicon carbide nanowires (SiCNWs) obtained via combustion synthesis from Si and PTFE micropowders. The bundles of the combustion product are contaminated with various fractions of SiC and impurities like carbon, silicon and silica. Attempts have been made to debundle the wires and to remove impurities from SiCNWs samples, in order to obtain pure and shape-controlled material. The morphology of SiCNWs was examined as the material was physically and chemically modified.

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.

Two-nanophase SiC-Zn composites were synthesized under pressure up to 8 GPa at up to 1000oC using an high-pressure infiltration method. The advantage of this technique is that in a single, continuous process the ceramic nanopowder is compressed to form the matrix with nanopores; the nanopores are filled with a liquid secondary phase, (here Zn), which crystallizes as nano-scale grains. The key limitation is that the pores in the infiltrated preform have to stay open during the entire process. For this reason only powders of very hard ceramic materials can be used as a matrix. Two types of SiC nanopowders with average crystallite size of 10 nm and 60 nm and average particle size of 30 nm and 100 nm, respectively were used. The measurements of porosity of the green compacts prepared from these powders, pressed at 2.5 GPa and 8 GPa at room temperature, indicated that open porosity was maintained. The nanocomposites obtained show a “nano-nano” type microstructure with a uniform mixture of SiC and Zn phases. The volume fraction of Zn is 20 % independent of the process conditions and initial powder morphology. The process parameters and powder granularity influenced the crystal size of the secondary phase. The average grain size of Zn varied from 20 to 85 nm and was smaller in the composites obtained with the finer matrix, under higher pressure and at lower temperature. The microhardness HV02 of SiCZn nanocomposites varied from 6 to 22 GPa and increased with an increase of pressure and temperature of the infiltration process, and was significantly larger for the finer grained composites.

A technique of preparation of novel nanocrystalline composites by infiltration of a liquid metal under high-pressure is presented. A porous nanocrystalline body is obtained by compacting nanosized powder of a high-hardness ceramic material under the pressure of 2-8 GPa. The molten metal penetrates into the open pores and crystallizes there upon cooling. As a result the second nano-phase is obtained. Practical aspects of the technique and some properties of the composites are discussed.

A method of analysis of disordering in α- and β-SiC polycrystals by numerical modeling, and a simulation of X-ray diffraction profiles are presented. The diffraction patterns of nonperiodic structures were simulated for models of 2000 layer fragments of the structure. Computer generation of the models was based on the Poisson function describing the size distribution of the domains of basic polytypes and faults. The models were quantified by a set of input probability parameters describing relative frequencies of the occurrence of the domains of polytypes and faults. Implementation of a correlation parameter that characterizes coherence of sequential domains of a given polytype assures a good reproducibility of the simulated diffraction profiles obtained for the same set of the model parameters. Based on this method, a quantitative analysis of disordering in polycrystals of SiC annealed in the temperature range 1100–2200 °C was performed.