František Lukáč

Microhardness and In Vitro Corrosion of Heat-Treated Mg–Y–Ag Biodegradable Alloy

Magnesium alloys are promising candidates for biodegradable medical implants which reduce the necessity of second surgery to remove the implants. Yttrium in solid solution is an attractive alloying element because it improves mechanical properties and exhibits suitable corrosion properties. Silver was shown to have an antibacterial effect and can also enhance the mechanical properties of magnesium alloys. Measurements of microhardness and electrical resistivity were used to study the response of Mg–4Y and Mg–4Y–1Ag alloys to isochronal or isothermal heat treatments. Hardening response and electrical resistivity annealing curves in these alloys were compared in order to investigate the effect of silver addition. Procedures for solid solution annealing and artificial aging of the Mg–4Y–1Ag alloy were developed. The corrosion rate of the as-cast and heat-treated Mg–4Y–1Ag alloy was measured by the mass loss method. It was found out that solid solution heat treatment, as well artificial aging to peak hardness, lead to substantial improvement in the corrosion properties of the Mg–4Y–1Ag alloy.

Vacancy-induced hardening in Fe-Al alloys

Hardness of Fe-Al alloys shows a non-trivial dependence on chemical composition and thermal treatment of samples and cannot be fully explained by consideration of intermetallic phases formed according to the equilibrium phase diagram of Fe-Al system. Hardening in Fe-Al alloys caused by quenched-in non-equilibrium vacancies was studied in this work. Non-equilibrium vacancies introduced into the alloys by quenching from 1000 °C were detected by means of positron annihilation spectroscopy. The concentration of quenched-in vacancies was found to strongly increase with increasing Al content from ≈ 10−5 at.−1 in the alloy with cAl = 18 at. % up to ≈ 10−1 at.−1 in the alloy with cAl = 45 at. %. Comparison of the vacancy concentration and the Vickers microhardness revealed that hardening is proportional to square root of concentration of quenched-in vacancies.

Spark Plasma Sintering of a Gas Atomized Al7075 Alloy: Microstructure and Properties

The powder of an Al7075 alloy was prepared by gas atomization. A combination of cellular, columnar, and equiaxed dendritic-like morphology was observed in individual powder particles with continuous layers of intermetallic phases along boundaries. The cells are separated predominantly by high-angle boundaries, the areas with dendritic-like morphology usually have a similar crystallographic orientation. Spark plasma sintering resulted in a fully dense material with a microstructure similar to that of the powder material. The continuous layers of intermetallic phases are replaced by individual particles located along internal boundaries, coarse particles are formed at the surface of original powder particles. Microhardness measurements revealed both artificial and natural ageing behavior similar to that observed in ingot metallurgy material. The minimum microhardness of 81 HV, observed in the sample annealed at 300 °C, reflects the presence of coarse particles. The peak microhardness of 160 HV was observed in the sample annealed at 500 °C and then aged at room temperature. Compression tests confirmed high strength combined with sufficient plasticity. Annealing even at 500 °C does not significantly influence the distribution of grain sizes—about 45% of the area is occupied by grains with the size below 10 µm.

Effect of Hydrogen on Formation of Fe-Al Nanoparticles by Mechanical Milling

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 in Nanocrystalline, Polycrystalline and Epitaxial Pd Films

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 Interaction with Defects in ZnO

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.

Diffusivity of Hydrogen in ZnO Single Crystal

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.

Influence of the Surface Condition of Specimens on the Size of Coherently Diffracting Domains

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.

Nanocrystalline Al7075 + 1 wt % Zr Alloy Prepared Using Mechanical Milling and Spark Plasma Sintering

The microstructure, phase composition, and microhardness of both gas-atomized and mechanically milled powders of the Al7075 + 1 wt % Zr alloy were investigated. The gas-atomized powder exhibited a cellular microstructure (grain size of a few µm) with layers of intermetallic phases along the cell boundaries. Mechanical milling (400 revolutions per minute (RPM)/8 h) resulted in a grain size reduction to the nanocrystalline range (20 to 100 nm) along with the dissolution of the intermetallic phases. Milling led to an increase in the powder’s microhardness from 97 to 343 HV. Compacts prepared by spark plasma sintering (SPS) exhibited negligible porosity. The grain size of the originally gas-atomized material was retained, but the continuous layers of intermetallic phases were replaced by individual particles. Recrystallization led to a grain size increase to 365 nm in the SPS compact prepared from the originally milled powder. Small precipitates of the Al3Zr phase were observed in the SPS compacts, and they are believed to be responsible for the retainment of the sub-microcrystalline microstructure during SPS. A more intensive precipitation in this SPS compact can be attributed to a faster diffusion due to a high density of dislocations and grain boundaries in the milled powder.

Hydrogen-Induced Defects in Titanium

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.