Instytut Podstawowych Problemów Techniki

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The interest in the Spark Plasma Sintering (SPS) technique has continuously increased over the last few years. This article shows the possibility of the development of an SPS device used for material processing and synthesis in both scientific and industrial applications and aims to present manufacturing methods and the versatility of an SPS device, presenting examples of processing Arc-Melted- (half-Heusler, cobalt triantimonide) and Self-propagating High-temperature Synthesis (SHS)-synthesized semiconductor (bismuth telluride) materials. The SPS system functionality development is presented, the purpose of which was to broaden the knowledge of the nature of SPS processes. This approach enabled the precise design of material sintering processes and also contributed to increasing the repeatability and accuracy of sintering conditions.

Słowa kluczowe:

spark plasma sintering, arc melting, semiconductor materials, half-Heusler, bismuth telluride, cobalt triantimonide, SHS, SPS

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Oxide Dispersion Strengthened (ODS) ferritic steels are promising materials for the nuclear power sector. This paper presents the results of a study on the sintering process using the Spark Plasma Sintering (SPS) technique, focusing on ODS ferritic steel powders with different contents (0.3 and 0.6 vol.%) of Y2O3. The novelty lies in the analysis of the effect of pre-annealing treatment on powders previously prepared by mechanical alloying on the microstructure, mechanical, and thermal properties of the sinters. Using the SPS method, it was possible to obtain well-densified sinters with a relative density above 98%. Pre-annealing the powders resulted in an increase in the relative density of the sinters and a slight increase in their thermal conductivity. The use of low electron energies during SEM analysis allowed for a fairly good visualization of the reinforcing oxides uniformly dispersed in the matrix. Analysis of the Mössbauer spectroscopy results revealed that pre-annealing induces local atomic rearrangements within the solid solution. In addition, there was an additional spectral component, indicating the formation of a Cr-based paramagnetic phase. The ODS material with a higher Y2O3 content showed increased Vickers hardness values, as well as increased Young’s modulus and nanohardness, as determined by nanoindentation tests.

Słowa kluczowe:

spark plasma sintering, ODS ferritic steel, mechanical alloying, Mössbauer spectroscopy, nanoindentation

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A novel metal matrix composites (MMC) with Mg matrix reinforced with natural filler in the form of Didymosphenia geminata frustules (algae with distinctive siliceous shells) are presented in this work. Pulse plasma sintering (PPS) was used to manufacture Mg-based composites with 1, 5 and 10 vol.% ceramic filler. As a reference, pure Mg was sintered. The results show that the addition of 1 vol.% Didymosphenia geminata frustules to the Mg matrix increases its corrosion resistance by supporting passivation reactions, and do not affect the morphology of L929 fibroblasts. Addition of 5 vol.% the filler does not cause cytotoxic effects, but it supports microgalvanic reactions leading to the greater corrosion rate. Higher content than 5 vol.% the filler causes significant microgalvanic corrosion, as well as increases cytotoxicity due to the greater micro-galvanic effect of the composites containing 10 and 15 vol.% diatoms. The results of contact angle measurements show the hydrophilic character of the investigated materials, with slightly increase in numerical values with addition of amount of ceramic reinforcement. The addition of Didymosphenia geminata frustules causes changes in a thermo-elastic properties such as mean apparent value of coefficient of thermal expansion (CTE) and thermal conductivity (λ). The addition of siliceous reinforcement resulted in a linear decrease of CTE and reduction in thermal conductivity over the entire temperature range. With the increasing addition of Didymosphenia geminata frustules, an increase in strength with a decrease in compressive strain is observed. In all composites an increase in microhardness was attained.
The results clearly indicate that filler in the form of Didymosphenia geminata frustules may significantly change the most important properties of pure Mg, indicating its wide potential in the application of Mg-based composites with a special focus on biomedical use.

Słowa kluczowe:

Metal-matrix composites (MMCs),Pulse plasma sintering (PPS),Ceramic filler,Microstructure,Properties

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This article discusses the morphology and thermomechanical properties of graphene oxide (GO) paper sheets and GO paper composites reinforced with carbon fibers. GO paper was fabricated using GO paste obtained by the condensation of GO aqueous solution synthesized using the Hummers' method. Carbon fibers were implemented to improve the mechanical properties of the pristine GO paper. All the investigated papers were subjected to thermal treatment to check thermo-related morphological and mechanical properties. The results presented in this study allowed for the deeper insight into morphological, structural, and mechanical volume and surface-related properties of pristine GO and GO-based composite materials reinforced with carbon fibers. We showed that there are two important factors that should be taken into consideration for the design and fabrication of GO-based papers. These factors were the concentration of the reinforcing agent and the thermal reduction of the papers. Both factors have influenced the final properties of the resulting GO-based papers. For the first time, it was revealed how the addition of the reinforcing material affects the GO paper thermal expansion coefficient.

Słowa kluczowe:

Flake graphene, Graphene oxide, Graphene oxide paper, Carbon fibers, Mechanical properties

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Additive manufacturing (AM) has seen remarkable development in recent years due to relatively high efficiency of the process. Cold spraying (CS) is a particular method of AM, in which titanium and titanium alloy powders are used. CS is a very competitive technology enabling the deposition of coatings, repairing machine parts, and manufacturing new components. For specific applications, the surface of cold-sprayed materials may require further processing. This paper reports an attempt to employ laser surface treatment (LST) of cold-sprayed coatings on an aluminium alloy substrate. The influence of laser beam interaction time on the coatings’ properties was analysed. The microstructure was investigated and observed employing scanning electron microscopy (SEM). To evaluate residual stress after CS and LST, the sin2ψ technique was used. Investigations were also performed on Vickers hardness, contact angle, and surface roughness. Significant changes in the surface morphology of the coatings and elevated residual stress levels dependent on the laser beam interaction time were observed. Increased Vickers hardness was recorded for titanium alloy Ti6Al4V. LST also led to increased surface hydrophilicity of the modified materials Ti and Ti6Al4V.

Słowa kluczowe:

cold spray, laser surface treatment, titanium coating, Ti6Al4V, residual stresses

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Doping is one of the possible ways to significantly increase the thermoelectric properties of many different materials. It has been confirmed that by introducing bismuth atoms into Mg sites in the Mg2Si compound, it is possible to increase career concentration and intensify the effect of phonon scattering, which results in remarkable enhancement in the figure of merit (ZT) value. Magnesium silicide has gained scientists’ attention due to its nontoxicity, low density, and inexpensiveness. This paper reports on our latest attempt to employ ultrafast selfpropagating high-temperature synthesis (SHS) followed by the spark plasma sintering (SPS) as a synthesis process of doped Mg2Si. Materials with varied bismuth doping were fabricated and then thoroughly analyzed with the laser flash method (LFA), X-ray diffraction (XRD), scanning electron microscopy (SEM) with an integrated energy-dispersive spectrometer (EDS). For density measurement, the Archimedes method was used. The electrical conductivity was measured using a standard four-probe method. The Seebeck coefficient was calculated from measured Seebeck voltage in the sample subjected to a temperature gradient. The structural analyses showed the Mg2Si phase as dominant and Bi2Mg3 located at grain boundaries. Bismuth doping enhanced ZT for every dopant concentration. ZT = 0:44 and ZT=0.38 were obtained for 3wt% and 2wt% at 770 K, respectively.

Słowa kluczowe:

thermoelectric materials, magnesium silicide, bismuth doping, SHS, spark plasma sintering

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This article presents the results of the cross-linking of oxidized flake graphene (GO) using hydrazine at room temperature. Conducting the process at temperatures up to 30 °C allowed to eliminate the phenomenon of thermal GO reduction to its non-oxidized form. In addition, based on the Infrared and Raman spectroscopy as well as X-ray photoelectron spectroscopy (XPS) analysis, the cross-linking ability of GO was observed depending on its size and degree of oxidation. These parameters were associated with selected physicochemical and electrical properties of obtained 3D structures. Three GO flakes sizes were tested in three different oxidation degrees. It was shown that, regardless of the size of GO, it is crucial to achieve a specific oxidation degree threshold which for the conducted tests was a >20% share of oxygen atoms in the whole structure. This value determines the ability to cross-link with hydrazine thanks to which it is possible to synthesize the spatial structure in which the π–π interactions among individual flakes are significantly reduced. This directly translates into the fact that the 3D structure shows an electrical resistance value in the range of 4–103 Ω, depending on the size and oxidation degree of the used material. The explanation of this phenomenon related to the electrical conductivity of 3D structures was confirmed based on the molecular modeling of the chemical structures.

Słowa kluczowe:

graphene, graphene oxide, cross-linking, 3D structures

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This article discusses the effect of hydrogenation of graphene (one-sided and two-side hydrogenation) in relation to the change in the physicochemical properties of graphane as a material capable of reversible H2 storage. Therefore, the change of the system's energy was determined, differences in HOMO-LUMO molecular levels and the distribution of electrostatic potential as a function of its hydrogenation were simulated. At the same time, the mechanism of graphane reduction to graphene was discussed as a result of interaction with steam from the air. It has been shown that along with the increase in the degree of hydrogenation, the graphane changes its electrostatic potential from negative to positive, simultaneously pushing the negative charge to the edge of the graphene flake. This fact may have an impact on its further chemical reactions, which may significantly limit the sorption properties of graphene. Areas rich in negative charge will prefer chemical reactions with molecules of electrophilic properties, while positive areas with molecules of nucleophilic properties. This determines the elimination of the storage environment of graphene structures used as reversible sources of chemical bonding of hydrogen in order to increase their lifetime as well as sorption capacity.

Słowa kluczowe:

Graphene, Hydrogen, Hydrogen storage, Graphane, Molecular simulation

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