Papers by Author: Pavol Šajgalík

Abstract: The scratch resistance of the silicon nitride with the addition of 1 and 7 wt% of graphene multiplatelets prepared by hot press sintering has been studied. The scratch resistance behaviour of Si₃N₄-GNP composites were investigated using a Rockwell indenter for normal applied loads ranging from 1-150 N. Si₃N₄-7-wt%GNP composite behaved differently during the scratch test depending on the normal applied load. The coefficient of friction changed dramatically at higher load and extensive crack propagation resulting in the chipping is observed.

Abstract: The study deals with the development of highly porous undegradable ceramics based on silicon nitride as potential replacement of trabecular bone. These materials were produced using replication method with polyurethane foams as pore-forming agents to achieve similar porous structure to trabecular bone. Prepared porous ceramics had a bimodal pore structure with macro-pores larger than 200 μm and micro-pores smaller than 1 μm in diameter, which are necessary for tissue ingrowths, cell adhesion, adsorption of biological metabolites and nutrition delivery in organism. The microstructure and local mechanical properties (Young’s modulus and Yield strength) were evaluated and compared with human trabecular bone. Results showed that studied porous materials have satisfactory porosity and pore sizes for trabecular bone replacement. Young’s modulus of bone was 12.6 ± 2.23 GPa and porous silicon nitride samples ranged from 10.9 ± 3.38 GPa to 12.9 ± 1.13 GPa. The values of Yield strength of trabecular bone was determined as 493 ± 30.7 MPa and the values of porous samples varied from 250 ± 19.3 MPa to 558 ± 36.5 MPa. Young’s modulus and Yield strength increase with increasing of the pre-sintering temperature and multiple infiltrations.

Abstract: Local mechanical properties, particularly the hardness and Youngs modulus of highly porous silicon nitride based foams were studied in this work. Silicon nitride foams were prepared using polyurethane foam replication method to obtain appropriate cellular structure suitable for bio-application. Two types of the polyurethane foams were used (with average pore size 0.48 mm and 0.62 mm). Some of these samples were prepared by single or multiple infiltrations. The effects of structures, temperature of calcination, volume fraction of Si₃N₄ powder and number of the infiltrations on the local mechanical properties were investigated. The Youngs modulus of studied samples range from 12 to 46 GPa at the macroscopic scale measured by resonant frequency technique and from 10 to 28 GPa at the microscopic scale measured by instrumented indentation. Results showed increase of the hardness and Youngs modulus with increasing of the calcination temperature, with increasing of the number of infiltrations and also with increasing of volume fraction of Si₃N₄ powder in suspension. The results obtained from nanoindentation carry out lower values in comparison with the values measured by resonant frequency technique.

Abstract: The influence of microstructural variations on the macro/microhardness, nanohardness and Young`s modulus of liquid phase sintered silicon carbide (LPS SiC) has been observed. In order to modify the microstructures some samples were further heat treated at 1850°C for 5 hours to promote grain growth. The depth-sensing indentation tests of SiC materials were performed at several peak loads in the range 10-400 mN. For a better assessment, the indentation values of hardness and Young`s modulus modulus of SiC matrix were also compared to the hardness and Elastic modulus of individual SiC grains. The comparison of macro/micro and nanohardness showed that nanohardness was significantly higher, generally by 6-7 GPa. The nanohardness of individual plate-like SiC grains was around 2 GPa higher than nanohardness of SiC matrix.

Abstract: Mechanical properties of porous silicon nitride prepared by two different processing routes have been studied. Depth sensing methods was used to measure the hardness and elastic modulus of experimental materials. The results were compared with the hardness and elastic modulus of trabecular bone in order to find out porous ceramics with properties close to that of trabecular bone. Material prepared by infiltration of polyurethane sponge exhibited properties close to the properties of bone and it is the potential material for further investigation in the bioapplication field.

Abstract: The corrosion resistance of liquid phase sintered (LPS) alumina ceramics in aqueous environments strongly depends on composition and chemistry of grain boundary glass formed during sintering. The chemical durability of model alumino-silicate glasses with various contents of CaO in aqueous solutions was therefore evaluated. Prepared glasses were corroded under hydrothermal conditions in deionized water under static conditions. The examination of surface morphology of corroded specimens after the contact with deionized water, together with the analysis of corrosion solution provided information on mechanism of dissolution of grain boundary glasses in LPS aluminas and confirmed that dissolution process is hindered due to saturation of solution with respect to leached elements. The initial dissolution rates for studied glasses were determined. The results are applicable for optimization and enhancement of corrosion resistance of LPS alumina under hydrothermal conditions.

Abstract: Corrosion resistance of solid state (SSS) and liquid phase sintered (LPS) alumina under hydrothermal conditions (subcritical water and sodium chloride solution at temperatures up to 290 °C, and pressures up to 7 MPa) was evaluated. The influence of sintering additives as well as the conditions of the test (temperature, corrosion medium) on dissolution of ceramics was studied. For evaluation of the corrosion mechanisms special attention was paid to determination of the eluate chemistry combined with the chemical and phase analysis of corroded surfaces. Corrosion of LPS alumina in both media was controlled by dissolution of calcium aluminosilicate grain boundary glass. Corrosion rates of SSS ceramics were several times lower and were largely controlled by dissolution of highly resistant alumina matrix. Corrosion of the ceramics was moderately faster in sodium chloride solution. The data are supplemented by calculations of phase equilibria in the corrosion solutions.

Abstract: Microstructure and mechanical properties of Si3N4 and Si3N4 + SiC nanocomposites sintered with rare-earth oxide additives (La2O3, Y2O3, Yb2O3 and Lu2O3) have been investigated. The composites exhibited smaller grain diameter compared to that of monolithic materials. The aspect ratio of β-Si3N4 grains increased with a decreasing ionic radius of rare-earth elements in the Si3N4 monoliths as well as in the Si3N4-SiC nanocomposites. The hardness of both systems increased with a decreasing ionic radius of rare-earth element. The fracture toughness of the materials with coarser microstructure and higher aspect ratio was higher due to the more frequent toughening mechanisms. No significant difference between strength values of monoliths and composites was observed and the strength in the composites was determined mainly by the present processing flaws. Significantly improved creep resistance was observed in the case of composites and for materials with smaller ionic radius of RE3+.

Abstract: Fracture toughness of hot-pressed silicon nitride and Si3N4+SiC nanocomposites prepared with different rare-earth oxides (La2O3, Sm2O3, Y2O3, Yb2O3, Lu2O3) sintering additives have been investigated by Chevron Notched Beam, Indentation Strength and Indentation Fracture techniques. The fracture toughness values of composites were lower due to the finer microstructures and the lack of toughening mechanisms. In the Si3N4 with higher aspect ratio (Lu or Yb additives) crack deflection occurred more frequently compared to the Si3N4 doped with La or Y, which was responsible for the higher fracture toughness.

Abstract: The effect of the heat treatment on the fracture toughness and flexural strength of the silicon carbide – silicon nitride composites prepared by liquid-phase-sintering was investigated. The results were compared to those obtained for a reference silicon carbide material, prepared by the same fabrication route. The fracture toughness increased from 3.19 to 5.15 MPa.m1/2 due to the toughening mechanisms (crack deflection, mechanical interlocking, crack branching) occurring in the heat treated materials during the crack propagation. However, the flexural strength decreased after the heat treatment of the experimental materials. The strength of the investigated materials was degraded by the presence of processing flaws mainly in the form of pores, clusters of pores, and SiC agglomerates.