Witold Lojkowski

The mechanism of formation of nanostructure and dissolution of cementite in a pearlitic steel during high pressure torsion

The nanostructure and the phase composition in UIC 860V pearlitic steel, deformed by high pressure torsion in the shear stress range from 62 to 430, were studied. The refinement of ferrite up to a grain size of 10 nm is accompanied by the total dissolution of the cementite and an increase in hardness of up to 11 GPa. The strain-induced cementite dissolution was found to be a three-stage process corresponding to the stages of nanostructure formation. The mechanism of the dissolution due to wear of cementite at the ferrite/cementite interface, followed by drag of the carbon atoms by the ferrite matrix, is discussed. The flow of carbon atoms with the ferrite phase can be considered as a mechanically driven mass transport process, quantitatively described by the mechanical diffusion parameter.

The mechanical properties of the nanocrystalline layer on the surface of railway tracks

Abstract The mechanical properties of the nanocrystalline layer on the surface of railroad tracks were investigated using the indentation technique. It was found that its hardness reaches 14 GPa. The ultimate compression stress is in the range of 4–5 GPa, and the elastic limit is in the range of 2–3 GPa. The hot hardness decreases to 1 GPa at 630°C. An already existing nanocrystalline layer is unlikely to be plastically deformed as long as the rail–wheel contact temperature is below 150°C. If friction causes an increase in temperature above 500°C, plastic deformation of the surface layer accompanied by dynamic recovery is plausible. It is unlikely that the growth of the nanocrystalline layer is a consequence of a high temperature process.

Mechanical Properties and Microstructure of Diamond–SiC Nanocomposites

A bulk composite material close in hardness to diamond was fabricated from nanocrystalline diamond and SiC. The mechanical properties and microstructure of the composite were studied. Youngs modulus of the composite is found to be notably lower than the one following from the additivity rule, which is attributable to the influence of structural defects present in the interfacial zone between SiC and diamond. SiC consists of nanometer-scale grains near the interface and submicron grains in the “pores.”

Highly biocompatible, nanocrystalline hydroxyapatite synthesized in a solvothermal process driven by high energy density microwave radiation.

A microwave, solvothermal synthesis of highly biocompatible hydroxyapatite (HAp) nanopowder was developed. The process was conducted in a microwave radiation field having a high energy density of 5 W/mL and over a time less than 2 minutes. The sample measurements included: powder X-ray diffraction, density, specific surface area, and chemical composition. The morphology and structure were investigated by scanning electron microscopy as well as transmission electron microscopy (TEM). The thermal behavior analysis was conducted using a simultaneous thermal analysis technique coupled with quadruple mass spectrometry. Additionally, Fourier transform infrared spectroscopy tests of heated samples were performed. A degradation test and a biocompatibility study in vitro using human osteoblast cells were also conducted. The developed method enables the synthesis of pure, fully crystalline hexagonal HAp nanopowder with a specific surface area close to 240 m2/g and a Ca/P molar ratio equal to 1.57. TEM measurements showed that this method results in particles with an average grain size below 6 nm. A 28-day degradation test conducted according to the ISO standard indicated a 22% loss of initial weight and a calcium ion concentration at 200 μmol/dm3 in the tris(hydroxymethyl)aminomethane hydrochloride test solution. The cytocompatibility of the obtained material was confirmed in a culture of human bone derived cells, both in an indirect test using the material extract, and in direct contact. A quantitative analysis was based on the 2,3-bis-(2-methoxy-4-nitro-5-sulfophenyl)-2H-tetrazolium-5-carboxanilide. Viability assay as well as on DNA content measurements in the PicoGreen test. Indirect observations were performed at one point in time according to the ISO standard for in vitro cytotoxicity (ie, after 24 hours of cell exposure to the extracts). The direct contact tests were completed at three time points: after 24 hours, on day 7, and on day 14 of a culture in an osteogenic medium. All of the tests revealed good tolerance of cells toward the material; this was also shown by means of live/dead fluorescent staining. Both quantitative results and morphological observations revealed much better cell tolerance toward the obtained HAp compared to commercially available HAp NanoXIM, which was used as a reference material.

Microstructure and mechanical properties of nano-Y2O3 dispersed ferritic steel synthesized by mechanical alloying and consolidated by pulse plasma sintering

Ferritic steel with compositions 83.0Fe–13.5Cr–2.0Al–0.5Ti (alloy A), 79.0Fe–17.5Cr–2.0Al–0.5Ti (alloy B), 75.0Fe–21.5Cr–2.0Al–0.5Ti (alloy C) and 71.0Fe–25.5Cr–2.0Al–0.5Ti (alloy D) (all in wt%) each with a 1.0 wt% nano-Y2O3 dispersion were synthesized by mechanical alloying and consolidated by pulse plasma sintering at 600, 800 and 1000°C using a 75-MPa uniaxial pressure applied for 5 min and a 70-kA pulse current at 3 Hz pulse frequency. X-ray diffraction, scanning and transmission electron microscopy and energy disperse spectroscopy techniques have been used to characterize the microstructural and phase evolution of all the alloys at different stages of mechano-chemical synthesis and consolidation. Mechanical properties in terms of hardness, compressive strength, yield strength and Youngs modulus were determined using a micro/nano-indenter and universal testing machine. All ferritic alloys recorded very high levels of compressive strength (850–2850 MPa), yield strength (500–1556 MPa), Youngs modulus (175–250 GPa) and nanoindentation hardness (9.5–15.5 GPa), with up to 1–1.5 times greater strength than other oxide dispersion-strengthened ferritic steels (<1200 MPa). These extraordinary levels of mechanical properties can be attributed to the typical microstructure of uniform dispersion of 10–20-nm Y2Ti2O7 or Y2O3 particles in a high-alloy ferritic matrix.

Morphology and luminescence properties of zinc oxide nanopowders doped with aluminum ions obtained by hydrothermal and vapor condensation methods

In this paper, we analyze the influence of Al doping on microstructure and light emission efficiency of ZnO nanoparticles obtained by the hydrothermal method and after vapor condensation method, where vaporization of the precursor powders was caused by high solar energy and subsequent deposition. We report an increase of lattice parameters with increasing level of doping as well as large emission enhancement, which we relate to surface passivation of recombination mechanisms and/or plasmon mechanism of photoluminescence stimulation.

Effect of pressure on synthesis of Pr-doped zirconia powders produced by microwave-driven hydrothermal reaction

A high-pressure microwave reactor was used to study the hydrothermal synthesis of zirconia powders doped with 1 mol % Pr. The synthesis was performed in the pressure range from 2 to 8 MPa corresponding to a temperature range from 215°C to 305°C. This technology permits a synthesis of nanopowders in short time not limited by thermal inertia of the vessel. Microwave heating permits to avoid contact of the reactants with heating elements, and is thus particularly well suited for synthesis of doped nanopowders in high purity conditions. A mixture of ZrO2 particles with tetragonal and monoclinic crystalline phases, about 15nm in size, was obtained. The p/T threshold of about 5-6MPa/265-280°C was necessary to obtain good quality of zirconia powder. A new method for quantitative description of grain-size distribution was applied, which is based on analysis of the fine structure of the X-ray diffraction line profiles. It permitted to follow separately the effect of synthesis conditions on the grain-size distribution of the monoclinic and tetragonal phases.

Paramagnetism of cobalt-doped ZnO nanoparticles obtained by microwave solvothermal synthesis.

Summary Zinc oxide nanopowders doped with 1–15 mol % cobalt were produced by the microwave solvothermal synthesis (MSS) technique. The obtained nanoparticles were annealed at 800 °C in nitrogen (99.999%) and in synthetic air. The material nanostructure was investigated by means of the following techniques: X-ray diffraction (XRD), helium pycnometry density, specific surface area (SSA), inductively coupled plasma optical emission spectrometry (ICP-OES), extended X-ray absorption fine structure (EXAFS) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and with magnetometry using superconducting quantum interference device (SQUID). Irrespective of the Co content, nanoparticles in their initial state present a similar morphology. They are composed of loosely agglomerated spherical particles with wurtzite-type crystal structure with crystallites of a mean size of 30 nm. Annealing to temperatures of up to 800 °C induced the growth of crystallites up to a maximum of 2 μm in diameter. For samples annealed in high purity nitrogen, the precipitation of metallic α-Co was detected for a Co content of 5 mol % or more. For samples annealed in synthetic air, no change of phase structure was detected, except for precipitation of Co3O4 for a Co content of 15 mol %. The results of the magentometry investigation indicated that all as-synthesized samples displayed paramagnetic properties with a contribution of anti-ferromagnetic coupling of Co–Co pairs. After annealing in synthetic air, the samples remained paramagnetic and samples annealed under nitrogen flow showed a magnetic response under the influences of a magnetic field, likely related to the precipitation of metallic Co in nanoparticles.

Size-dependent density of zirconia nanoparticles

Summary The correlation between density and specific surface area of ZrO2 nanoparticles (NPs) was studied. The NPs were produced using a hydrothermal process involving microwave heating. The material was annealed at 1100 °C which resulted in an increase in the average grain size of the ZrO2 NPs from 11 to 78 nm and a decrease in the specific surface area from 97 to 15 m2/g. At the same time, the density increased from 5.22 g/m3 to 5.87 g/m3. This effect was interpreted to be the result of the presence of a hydroxide monolayer on the NP surface. A smaller ZrO2 grain size was correlated with a larger contribution of the low density surface layer to the average density. To prove the existence of such a layer, the material was synthesized using 50% heavy water. Fourier transform infrared spectroscopy (FTIR) permitted the identification of the –OD groups created during synthesis. It was found that the –OD groups persisted on the ZrO2 surface even after annealing at 1100 °C. This hydroxide layer is responsible for the decrease in the average density of the NPs as their size decreases. This study of the correlation between particle size and density may be used to assess the quality of the NPs. In most cases, the technological aim is to avoid an amorphous layer and to obtain fully crystalline nanoparticles with the highest density possible. However, due to the effect of the surface layers, there is a maximum density which can be achieved for a given average NP diameter. The effect of the surface layer on the NP density becomes particularly evident for NPs smaller than 50 nm, and thus, the density of nanoparticles is size dependent.

Luminescence Properties of ZnO Nanocrystals and Ceramics

The luminescence excitation spectra, luminescence spectra and the nanosecond-scale decay kinetics were studied. The ZnO and ZnO:Al nanopowders were prepared by vaporization-condensation in a solar furnace using different raw powders: commercial, hydrothermal and those obtained by plasma synthesis. Exciton-phonon as well as exciton-exciton interaction processes in nanopowders, a bulk crystal and ZnO ceramics were studied and compared. The fast decay and low afterglow intensity of ZnO nanopowders and ceramics support these materials for scintillators.