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Metallic sample preparation process from cutting to polishing introduces defects into the subsurface layers by plastic deformation. Methods of bulk sample characterization are usually sensitive to the microstructure and presence of defects e.g. dislocations, grain boundaries, etc. near the surface. The X-ray diffraction technique (XRD) is a unique method used primarily for phase identification and quantification of crystalline materials. The extending of the method by the whole pattern fitting using Rietveld refinement analysis enables also utilisation for other purposes such as determination of the size of coherently diffracting domains (CDD). This property quantifies the degree of disorder in material and is usually correlated with mean crystallite size, i.e. subgrain size. However, since the penetration depth of the laboratory X-ray radiation is limited to the order of tens of micrometers (depending on the material), the observed result is highly affected by the density of defects such as dislocations in the surface area of the specimen and thus by their surface condition. The effect of the different final steps of grinding and polishing on the observed size of CDD was studied and discussed for two materials - aluminum Al7075 alloy and high entropy alloy HfNbTaTiZr. The reasonable finishing for the optimal results was found for both materials.

The aim of this work was investigation of hydrogen interaction with defects in Ti. Well-annealed Ti samples were loaded with hydrogen either electrochemically or using H2 gas phase. The hydrogen content and the phase composition of hydrogen loaded samples was determined by thermogravimetric analysis and by X-ray diffraction (XRD) respectively. Positron lifetime (LT) spectroscopy was employed for investigation of defects created by hydrogen loading. High-temperature H2 gas loading led to complete transformation of the whole sample into δ-TiH2 while low-temperature H2 gas loading and the electrochemical loading resulted in a non-uniform structure with most of the hydrogen absorbed in a sub-surface layer. All hydrogen-loaded samples exhibit positron lifetime component of ≈ 170 ps corresponding to positrons trapped at dislocations. Vacancy clusters were observed in the electrochemically loaded sample and the H2 gas phase loaded sample at low temperature.

A Pd-H system is a model system suitable for studying interactions of hydrogen with metals. In the present work, we studied hydrogen-induced buckling of thin Pd films deposited on various substrates with different bonding strengths (sapphire, glimmer) and also the effect of deposition temperature. Lattice expansion and phase transitions were investigated by X-ray diffraction of synchrotron radiation. The influence of the substrate and microstructure of the film on the buckling process and phase transformation to palladium hydride are discussed.

The Mg-Zn-Y system attracts interest of researchers due to the formation of quasicrystalline particles which are believed to improve mechanical properties of Mg-based alloys. In the Mg-Zn-Y-Nd-Zr alloy (WE43 modified by addition of Zn) studied here the formation of icosahedral phase (I-phase) with quasicrystalline structure competes with cubic W-phase. Grain boundary phases in Mg-Zn-Y-Nd-Zr alloys subjected to various heat treatments were characterized. It was found that the portion of the I-phase in Mg-Zn-Y-Nd-Zr alloy can be increased by a suitable heat treatment. Moreover, the solidification process is influenced by the cooling rate resulting in a striking difference in the morphology of grain boundary phases.

Nanocrystalline powders of iron aluminum alloy of the Fe82Al18 nominal composition were prepared under air, hydrogen and nitrogen atmospheres from the Fe and Al elemental powders by mechanical alloying and also from the conventionally cast Fe82Al18 alloy by the high-energy ball milling. The intensive plastic deformation during high-energy mechanical treatment has introduced high concentrations of open volume defects and contributed to a rapid decrease in the crystallite size down to a nanoscopic range.The hydrogen atmosphere was found to be the most efficient for the Fe-Al mechanical alloying since it has resulted into the fully alloyed Fe82Al18 after 30 h of milling. On the other hand, the nitrogen and air atmosphere have slightly prevented mechanical alloying and after the same milling time the pure iron particles were still detected in the powder mixtures. This partial suppression of the mechanical alloying process is explained by a formation of thin iron nitride and/or oxide layers on the surface of Fe particles preventing mutual inter-diffusion of Fe and Al atoms.

Hydrogen interaction with defects and structural development of Pd films with various microstructures were investigated. Nanocrystalline, polycrystalline and epitaxial Pd films were prepared and electrochemically loaded with hydrogen. Structural changes of Pd films caused by absorbed hydrogen were studied by in-situ X-ray diffraction combined with acoustic emission and measurement of electromotorical force. Development of defects during hydrogen loading was investigated by positron annihilation spectroscopy. It was found that hydrogen firstly fills open volume defects existing already in the films and subsequently it occupies also interstitial sites in Pd lattice. Absorbed hydrogen causes volume expansion, which is strongly anisotropic in thin films. This introduces high stress into the films loaded with hydrogen. Acoustic emission measurements revealed that when hydrogen-induced stress achieves a certain critical level rearrangement of misfit dislocations takes place. The stress which grows with increasing hydrogen concentration can be further released by plastic deformation and also by detachment of the film from the substrate.

Hydrogen absorption and diffusivity in high quality ZnO crystals were investigated in this work by X-ray diffraction combined with slow positron implantation spectroscopy and electrical resistometry. ZnO crystals were covered by a thin Pd over-layer and electrochemically charged with hydrogen. It was found that absorbed hydrogen causes plastic deformation in a sub-surface region. The depth profile of hydrogen concentration introduced into the crystal was determined by nuclear reaction analysis. Enhanced hydrogen concentration was found in the sub-surface region due to excess hydrogen atoms trapped at defects introduced by plastic deformation. Hydrogen diffusion in ZnO crystals with various orientations was studied by in-situ electrical resistometry. It was found that hydrogen diffusion in the c-direction is faster than hydrogen diffusion in the a-direction most probably due to open channels existing in the wurtzite structure along the c-axis.

In the present work hydrothermally grown ZnO single crystals were electrochemically charged with hydrogen. The influence of hydrogen on ZnO microstructure was investigated by positron annihilation spectroscopy (PAS) combined with X-ray diffraction (XRD) using synchrotron radiation. Hydrogen concentration in the samples was determined by nuclear reaction analysis (NRA). It was found that a high concentration of hydrogen can be introduced into ZnO by electrochemical loading. At low concentrations, absorbed hydrogen causes elastic volume expansion of ZnO crystal. At higher concentration, hydrogen-induced stresses exceed the yield stress in ZnO and plastic deformation of the crystal takes place leading to formation of a defected subsurface layer in the crystals.

Hydrogen absorption in Pd causes a significant volume expansion. In free-standing bulk Pd, the hydrogen-induced volume expansion is isotropic. However, the situation becomes more complicated in thin Pd films. Contrary to bulk samples, thin films are clamped to an elastically stiff substrate, which prevents in-plane expansion. Hence, the volume expansion of a thin film is strongly anisotropic because it expands in the out-of-plane direction only. Internal stresses introduced by absorbed hydrogen may become so high that detachment of a film from the substrate is energetically favorable and buckles of various morphologies are formed. In the present work, we studied hydrogen-induced buckling in a nanocrystalline thin Pd film deposited on a sapphire substrate. Slow positron implantation spectroscopy (SPIS) was employed as a principal tool for the characterization of defects and investigation of defect interactions with hydrogen. SPIS studies were combined with X-ray diffraction and direct observations of buckling by light microscopy. It was found that buckling of thin Pd film occurs at hydrogen concentrations xH > 0.1 and is accompanied by a strong increase of dislocation density.

A digital spectrometer for low background gamma ray spectroscopy equipped with two high purity Ge detectors and a 12-bit two channel digitizer was employed for the investigation of positron annihilation-in-flight. Measurements were performed for positrons emitted by 68Ge/68Ga and 22Na radioisotopes and annihilated in Cu and Mg targets. The contribution of the two-quantum positron annihilation-in-flight was clearly resolved in coincidence two-dimensional gamma ray energy spectra. The contribution of positrons annihilated in flight has a hyperbolic shape described well by the relativistic theory.

Hydrogen diffusivity in ZnO (0001) single crystal was investigated using electrical resistometry and nuclear reaction analysis (NRA). ZnO crystals were covered with a thin Pd over-layer and electrochemically charged with hydrogen. The net concentration of hydrogen determined by NRA was found to be in a reasonable agreement with the value estimated from the transported charge using the Faradays law. The hydrogen diffusion coefficient in ZnO was estimated from in-situ electrical resistivity measurements. Moreover, NRA investigations revealed existence of a subsurface layer with very high concentration of hydrogen (up to 40 at.%). Typical surface modification observed on hydrogen loaded crystal by light microscope indicates hydrogen-induced plastic deformation realized by a slip in the c-direction. Open-volume defects introduced by hydrogen-induced plastic deformation trap diffusing hydrogen and cause an enhancement of hydrogen concentration in the deformed subsurface layer.