Papers by Author: János L. Lábár

Abstract: The effect of different plastic deformation methods on the phase composition, lattice defect structure and hardness in 316L stainless steel was studied. The initial coarse-grained γ-austenite was deformed by cold rolling (CR) or high-pressure torsion (HPT). It was found that the two methods yielded very different phase compositions and microstructures. Martensitic phase transformation was not observed during CR with a thickness reduction of 20%. In γ-austenite phase in addition to the high dislocation density (~10 × 10¹⁴ m^-2) a significant amount of twin-faults was detected due to the low stacking fault energy. On the other hand, γ-austenite was gradually transformed into ε and α’-martensites with transformation sequences γ→ε→α’ during HPT deformation. A large dislocation density (~133 × 10¹⁴ m^-2) was detected in the main phase (α’-martensite) at the periphery of the disk after 10 turns of HPT. The high defect density is accompanied by a very small grain size of ~45 nm in the HPT-processed sample, resulting in an very large hardness of 6130 MPa.

Abstract: The evolution of phase composition, microstructure and hardness in 316L austenitic stainless steel processed by high-pressure torsion (HPT) was studied up to 20 turns. It was revealed that simultaneous grain refinement and phase transformation occur during HPT-processing. The γ-austenite in the initial material transformed gradually to ɛ-and α’-martensites due to deformation. After 20 turns of HPT the main phase was α’-martensite. The initial grain size of ~42 μm was refined to ~48 nm while the dislocation density increased to ~143 × 10¹⁴ m^-2 in the α’-martensite phase at the disk periphery processed by 20 turns. The microstructure and hardness along the disk radius became more homogeneous with increasing numbers of turns. An approximately homogeneous hardness distribution with a saturation value of ~6140 MPa was achieved in 20 turns.

Abstract: The CrSi compacts containing 10, 20, 30 and 40 at. % Si sintered from mixed elemental powders were used as targets for reactively deposited magnetron (Cr,Si)N coatings. The silicon substrates were kept either at ambient temperature or heated up to 600 °C. The microstructure observations were performed using TECNAI FEG (200 kV) with EDAX X-ray Energy Dispersive Spectroscopy (EDS) system and JEOL 3010 (300 kV) with Gatan Energy Filtering (GIF) attachment microscopes. The thin foils were cut using QUANTA Focused Ion Beam (FIB) system. The performed investigations proved that increasing silicon content in coatings deposited at 600 °C using CrSi10, CrSi20 and CrSi30 targets caused a refining of their fully crystalline CrN-type columnar microstructure from ~ 40 to ~ 35 and ~ 25 nm. The deposition performed from the same targets, but at ambient temperatures, i.e. without resistive heating of the substrates, produced coatings of mixed crystalline-amorphous type. They were characterized by gradient microstructure, i.e. amorphous material was prevailing close to the substrate and decreasing close to coating surface. The rising of silicon content in the targets resulted in decreasing amount of crystalline phase. The coatings obtained from Cr40Si target were fully amorphous independently of substrate temperature during deposition. The measurements of local chemical compositions obtained using EDS technique indicated that the Cr:Si ratio in the coatings roughly reproduced that present in the targets used for their deposition. Additionally, these measurements indicated that all coatings are contaminated with oxygen. The mapping of chemical composition using GIF technique of mixed crystalline-amorphous coatings proved that they are enriched in Cr and Si, respectively. The present results showed, that relying on single CrSi target magnetron sputtering the crystalline-amorphous nano-composite could be obtain at silicon additions from 10 to 30 at %, i.e. well above were that type of microstructure is formed during deposition using double target magnetron systems. Additionally, for the first time, the measurements helped to prove that the crystallites and amorphous material are enriched in chromium and silicon respectively, i.e. confirmed presence of CrN/Si3N4 composite.

Abstract: A method is presented here for complete geometrical characterization of grain boundaries, based on measurement of thin films in the TEM. First, the three parameters, characterizing the misorientation of the two neighboring grains are determined from convergent beam electron diffraction (CBED). Next, the last two (of the total five macroscopic degrees of freedom) parameters are determined from bright field (BF) images to describe the orientation of the boundary plane between them. Ambiguity in the tilt direction of the plane is resolved from BF images recorded at two distinct goniometer settings. Application of the method is demonstrated in Silicon thin films. GB-plane distribution in a thin film is not necessarily identical to the distribution of similar planes in bulk materials. It was observed in low dimensional fcc metals (wires or thin films) that energy minimization of GBs can follow two (mainly alternative) routes. Either low energy planes (like {111}) are formed in 3 boundaries, or alternatively, it is observed that the GB plane has a general index (and high energy density) but it ends at both free surfaces of the sample, resulting in a GB, almost normal to the sample surface, minimizing the total area of the GB. We observed that this later type of planes is mainly characteristic of non-3 boundaries in thin Si films, crystallized from melt on glass substrates (separated by a thin SiN barrier layer). This observation is important for the expected recombination properties of the multicrystalline Si (m-Si) in planned solar cell (SC) applications.

Abstract: The evolution of the microstructure during processing by equal-channel angular pressing (ECAP) in silver having extremely low stacking fault energy was studied up to 16 passes. It was shown that at high strains the contribution of twinning to deformation increased at the expense of dislocation-controlled processes. It was also found that during storage at room temperature (i.e. at the temperature of ECAP) there was a self-annealing of the severely deformed microstructure after 1 month and its degree was revealed to have a strong dependence on the number of passes.

Abstract: This work describes atomic-scale, crystalline structure and size distribution for noble metal nanoparticles produced by water-based, environmental friendly technologies. The process was developed and implemented to produce noble metal nanoparticles to be used in water filters, sensors and cosmetics. The particles were investigated by TEM methods and particle size analysis. Growth process of the crystallites in sols made by chemical reduction in aqueous solutions is discussed. Comparison with growth models for vacuum deposited thin films is also identified.

Abstract: A method is presented to measure lattice and grain boundary diffusion coefficients using secondary ion mass spectroscopy and 2-dimensional diffusion simulations. SIMS is used to measure concentration profiles of implanted species before and after annealing. The as-implanted concentration profile is used as the initial condition for 2-dimensional diffusion simulations using the finite element method. The geometry of the simulation is based on the microstructure of the sample observed by transmission electron microscopy. Both lattice and grain boundary diffusion are simulated. The final 2-dimensional concentration distribution is projected on the depth axis to obtain a simulated depth profile. The diffusion coefficients are adjusted to fit the profiles measured after annealing. We find that this method allows to determine simultaneously and independently the lattice and grain boundary diffusion coefficients from the same profiles. This method is used to measure the diffusion coefficients of As in polycrystalline Ni2Si thin films. The simulations are found to fit the measured profiles with accuracy. The coefficients are measured between 550 and 700°C. An activation energy ratio Qgb/Qv is found greater than one. This result is corroborated by existing data in silicides and is compared to results in other materials for discussion.

Abstract: Ultrafine-grained titanium was processed by severe plastic deformation (SPD). The SPD was carried out by equal channel angular pressing (ECAP) at high temperature. The ECAPprocessed sample was further deformed by conventional techniques such as radial forging and drawing. The microstructure was characterized quantitatively by X-ray diffraction line profile analysis and transmission electron microscopy after each step of deformation. The effect of procesing routes on the mechanical behavior was also studied. It was found that the conventional deformation processes after ECAP result in further increment in dislocation density and strength at the expense of ductility.