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Heavy metal contamination, associated with the increase in industrial production and the development of the population in general, poses a significant risk in terms of the contamination of soil, water, and, consequently, industrial plants and human health. The presence of ecotoxic heavy metals (HMs) thus significantly limits the sustainable development of society and contributes to the deterioration of the quality of the environment as a whole. For this reason, the stabilization and immobilization of heavy metals is a very topical issue. This paper deals with the possibility of the simultaneous immobilization of heavy metals (Ba2+, Pb2+, and Zn2+) in mortar based on magnesium potassium phosphate cement (MKPC). The structural, mechanical, and hygric parameters of mortars artificially contaminated with heavy metals in the form of salt solutions were investigated together with the formed hydration products. In the leachates of the prepared samples, the content of HMs was measured and the immobilization ratio of each HM was determined. The immobilization rate of all the investigated HMs was >98.7%, which gave information about the effectiveness of the MKPC-based matrix for HM stabilization. Furthermore, the content of HMs in the leachates was below the prescribed limits for non-hazardous waste that can be safely treated without any environmental risks. Although the presence of heavy metals led to a reduction in the strength of the prepared mortar (46.5% and 57.3% in compressive and flexural strength, respectively), its mechanical resistance remained high enough for many construction applications. Moreover, the low values of the parameters characterizing the water transport (water absorption coefficient Aw = 4.26 × 10-3 kg·m-2·s-1/2 and sorptivity S = 4.0 × 10-6 m·s-1/2) clearly demonstrate the limited possibility of the leaching of heavy metals from the MKPC matrix structure.
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Composites consisting of iron aluminide and iron silicide phases were studied in this work. Powders of iron aluminide and iron silicide were prepared by mechanical alloying separately. Subsequently, they were blended in three different proportions and sintered by the SPS method under various conditions. After sintering, the composites are composed of FeAl and amounts of other silicides (Fe5Si3 and Fe3Si). Ternary Fe-Al-Si phases were not determined, even though their presence was predicted by DFT calculations. This disagreement was explained by steric factors, i.e., by differences in the space lattice of the present phases. Hardness and tribological properties were measured on composites with various weight ratios of iron aluminide and iron silicide. The results show that sintered silicides with the matrix composed of iron aluminide reach comparable hardness to tool steels. The composites with higher mass ratios of iron aluminide than silicide have higher hardness and better tribological properties.
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Three mechanically alloyed (MA) and spark plasma sintered (SPS) CoCrFeNiNbX (X = 5, 20, and 35 at.%) alloys with an addition of 5 at.% of SiC were investigated. The face-centered cubic (FCC) high-entropy solid solution, NbC carbides, and hexagonal Laves phase already developed during MA. In addition, the SPS compacting led to the formation of oxide particles in all alloys, and the Cr7C3 carbides in the Nb5 alloy. The fraction of the FCC solid solution decreased with increasing Nb concentration at the expense of the NbC carbide and the Laves phase. Long-term annealing at 800 °C led to the disappearance of the Cr7C3 carbide in the Nb5 alloy, and new oxides-Ni6Nb6O, Cr2O3, and CrNbO4-were formed. At laboratory temperature, the Nb5 alloy, containing only the FCC matrix and carbide particles, was relatively strong and very ductile. At a higher Nb content (Nb20 and Nb35), the alloys became brittle. After annealing for 100 h at 800 °C, the Nb5 alloy conserved its plasticity and the Nb20 and Nb35 alloys maintained or even increased their brittleness. When tested at 800 °C, the Nb5 and Nb20 alloys deformed almost identically (CYS ~450 MPa, UTS ~500 MPa, plasticity ~18%), whereas the Nb35 alloy was much stronger (CYS of 1695 MPa, UCS of 1817 MPa) and preserved comparable plasticity.
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The equiatomic CoCrFeNiMn alloy prepared by mechanical alloying and spark plasma sintering underwent partial substitution of Mn by Al (5, 10 and 15 at.%) to determine its influence on mechanical properties and thermal stability. It was discovered that the higher the Al content, the higher the volume fraction of the hard phase with primitive cubic (PC) crystallographic lattice, which increases the hardness and strength of the alloys. The most promising mechanical properties have been achieved in the CoCrFeNiMn5Al15 alloy reaching the compressive yield strength (CYS) of 2135 ± 21 MPa and the ultimate compressive strength (UCS) of 2496 ± 21 MPa. All the prepared alloys showed good thermal stability as they maintained or only slightly reduced their initial hardness during the 100 h annealing at 800 °C. Furthermore, the higher the Al content, the higher the resistance against high-temperature oxidation. The oxidic layer changed its composition from Mn-oxides (CoCrFeNiMn15Al15 alloy) to Al-based oxides with exceptional protective properties.
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Stainless steels are materials that could be used for constructing not only the bearing parts of fuel cells but also the functional ones, particularly the bipolar plates. The advantage of stainless steel is its valuable electrical and thermal conductivity, reasonably low cost, excellent mechanical properties, and good formability. Paradoxically, the self-protection effect resulting from passivation turns into the main disadvantage, which is unacceptable interfacial contact resistance. The aim of this study was to test a number of possible stainless steels in a simulated fuel cell environment, especially those alloyed with boron and manganese, which were found to improve the contact resistance properties of stainless steels. The primary focus of the study is to determine the corrosion resistance of the individual materials tested. Electrochemical tests and contact resistance measurements were performed following the DOE requirements. Manganese-alloyed LDX stainless steel achieved the best results in the electrochemical tests; the worst were achieved by boron-containing steels. Boron-containing stainless steels suffered from localized corrosion resulting from chromium-rich boride formation. All steels tested exceeded the DOE limit in the contact resistance measurement, with 316L reaching the lowest values.
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The present work describes the influence of different temperatures on mechanical properties and microstructure of additively manufactured high-strength 1.2709 maraging steel. For this purpose, samples produced by selective laser melting technology were used in their as-printed as well as their heat-treated state. Both samples were than exposed to temperatures ranging between 100 °C to 900 °C with a total dwell time of 2 h followed by water-cooling. The microhardness of the as-printed material reached its maximum (561 ± 6 HV0.1) at 500 °C, which corresponded to the microstructural changes. However, the heat-treated material retained its initial mechanical properties up to 500 °C. As the temperature increased, the microhardness of both the materials reduced, reaching their minimum at 900 °C. This phenomenon was accompanied by a change in the microstructure by forming coarse-grained martensite. This also resulted in a significant decrease in the ultimate tensile strength and an increase in the plasticity. TEM analysis confirmed the formation of Ni3Mo intermetallic phases in the as-printed material when exposed to a temperature of 500 °C. It was found that the same phase was present in the heat-treated sample and it remained stable up to a temperature of 500 °C.
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As the commercially most-used Ti-6Al-4V alloy has a different modulus of elasticity compared to the modulus of elasticity of bone and contains allergenic elements, ß-Ti alloy could be a suitable substitution in orthopedics. The spark plasma sintering (SPS) method is feasible for the preparation of materials, with very low porosity and fine-grained structure, leading to higher mechanical properties. In this study, we prepared quaternary Ti-25Nb-4Ta-8Sn alloy using the spark plasma sintering method. The material was also heat-treated in order to homogenize the structure and compare the microstructure and properties in as-sintered and annealed states. The SPS sample had a modulus of elasticity of about 63 ± 1 GPa, which, after annealing, increased to the value of 73 ± 1 GPa. The tensile yield strength (TYS) of the SPS sample was 730 ± 52 MPa, ultimate tensile strength (UTS) 764 ± 10 MPa, and ductility 22 ± 9%. Annealed samples reached higher values of TYS and UTS (831 ± 60 MPa and 954 ± 48 MPa), but the ductility decreased to the value of 3 ± 1%. The obtained results are discussed considering the observed microstructure of the alloy.
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High entropy alloys (HEAs) are materials of great application potential and which have been extensively studied during the last two decades. As the number of possible element combinations is enormous, model materials representing certain groups of HEAs are used for the description of microstructure, properties, and deformation mechanisms. In this study, the microstructure and mechanical properties of the so-called Cantor alloy composed of Co, Cr, Fe, Mn, and Ni in equiatomic ratios prepared by various techniques (casting, melt-spinning, spark plasma sintering) were examined. The research focused on the indentation measurements, namely, the indentation size effect describing the evolution of the hardness with penetration depth. It was found that the standard Nix-Gao model can be used for this type of alloy at higher penetration depths and its parameters correlate well with microstructural observations. The Nix-Gao model deviates from the measured data at the submicrometer range and the applied modification affords additional information on the deformation mechanism.
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Due to the high affinity of ceria (CeO2) towards carbon dioxide (CO2) and the high thermal and mechanical properties of cellulose triacetate (CTA) polymer, mixed-matrix CTA-CeO2 membranes were fabricated. A facile solution-casting method was used for the fabrication process. CeO2 nanoparticles at concentrations of 0.32, 0.64 and 0.9 wt.% were incorporated into the CTA matrix. The physico-chemical properties of the membranes were evaluated by SEM-EDS, XRD, FTIR, TGA, DSC and strain-stress analysis. Gas sorption and permeation affinity were evaluated using different single gases. The CTA-CeO2 (0.64) membrane matrix showed a high affinity towards CO2 sorption. Almost complete saturation of CeO2 nanoparticles with CO2 was observed, even at low pressure. Embedding CeO2 nanoparticles led to increased gas permeability compared to pristine CTA. The highest gas permeabilities were achieved with 0.64 wt.%, with a threefold increase in CO2 permeability as compared to pristine CTA membranes. Unwanted aggregation of the filler nanoparticles was observed at a 0.9 wt.% concentration of CeO2 and was reflected in decreased gas permeability compared to lower filler loadings with homogenous filler distributions. The determined gas selectivity was in the order CO2/CH4 > CO2/N2 > O2/N2 > H2/CO2 and suggests the potential of CTA-CeO2 membranes for CO2 separation in flue/biogas applications.
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The chemical and phase composition of the coating and the coating/substrate interface of an Al-Si-coated 22MnB5 hot stamped steel was investigated by means of SEM-EDS, XRD, micro-XRD and electron diffraction. Moreover, the surface profile was analyzed by XPS and roughness measurements. The XPS measurements showed that the thickness of the Si and Al oxide layers increased from 14 to 76 nm after die-quenching, and that the surface roughness increased as well as a result of volume changes caused by phase transformations. In addition to the FeAl(Si) and Fe2Al5 phases and the interdiffusion layer forming complex structures in the coating, electron diffraction confirmed the presence of an Fe2Al5 phase, and also revealed very thin layers of Fe3(Al,Si)C, Fe2(Al,Si)5 and Al-bearing rod-shaped particles in the immediate vicinity of the steel interface. Moreover, the scattered nonuniform layer of the Fe2Al8Si phase was identified in the outermost layer of the coating. Despite numerous studies devoted to researching the phase composition of the Al-Si coating applied to hot stamped steel, electron diffraction revealed very thin layers and particles on the coating/substrate interface and outermost layer, which have not been analyzed in detail.
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The aim of this study was to prepare a low porosity bulk sample with a fine-grained structure from an AlZrTi alloy. Nanostructured powder particles were prepared by mechanical milling of gas atomized powder. The mechanically milled powder was consolidated using spark plasma sintering technology at 475 °C for 6 min using a pressure of 100 MPa. Sintering led to a low porosity sintered sample with a bimodal microstructure. The sintered sample was revealed to be composed of non-recrystallized grains with an approximate size of about 100 nm encompassed by distinct clusters of coarser, micrometer-sized grains. Whereas the larger grains were found to be lean on second phase particles, a high density of second phase particles was found in the areas of fine grains. The microhardness of the milled powder particles was established to be 163 ± 15 HV0.01, which decreased to a slightly lower value of 137 ± 25 HV0.01 after sintering.
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Zinc and its alloys belong to a group of biodegradable materials, which can be potentially used for the preparation of temporary orthopedic implants. The research of biodegradable zinc materials revealed a lot of limitations; however, the new processing approaches of those materials can enhance their properties, which are insufficient for now. In this study, the zinc composite with 8 wt.% of hydroxyapatite (Zn/HA8) prepared for the first time by extrusion process was characterized from the point of view of the structural, mechanical and corrosion properties. The extrusion process led to good integrity of the interfaces between the zinc and hydroxyapatite particles. Mechanical behavior confirmed the role of hydroxyapatite as a defect in the material structure, which led to a decrease of the Zn/HA8 mechanical properties by approximately 30% (compressive yield strength (CYS) = 154 MPa Zn, 113 MPa Zn/HA8). Despite that, the Zn/HA8 composite showed sufficient mechanical properties for cancellous bone replacement and reached the lower limit for cortical bone. Additionally, the presence of hydroxyapatite caused the preferential precipitation of hydroxyapatite (HA) from the solution and can lead to a significant enhancement of the tissue/implant interface interactions.
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This paper describes the structure and properties of an innovative Fe-Al-Si alloy with a reduced amount of silicon (5 wt. %) in order to avoid excessive brittleness. The alloy was produced by a combination of mechanical alloying and spark plasma sintering. Nickel and titanium were independently tested as the alloying elements for this alloy. It was found that wear resistance, which reached values comparable with tool steels, could be further improved by the addition of nickel. Nickel also improved the high-temperature oxidation behavior, because it lowers the liability of the oxide layers to spallation. Both nickel and titanium increased the hardness of the alloy. Titanium negatively influenced oxidation behavior and wear resistance because of the presence of titanium dioxide in the oxide layer and the brittle silicides that caused chipping wear, respectively.
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Short-term mechanical alloying and compaction by spark plasma sintering was used for the production of FeAl20Si20Mo20-XNiX (X corresponds to 5-15 wt %) alloy, which showed an ultrafine-grained microstructure with dimensions of phases around 200 nm or smaller. It was found that the addition of Mo and Ni to the FeAl20Si20 alloy results in the formation of the AlMoSi phase compared to the three-phase FeAl20Si20 alloy, which initially contained FeSi, Fe3Si, and Fe3Al2Si3 phases. All the investigated alloys increased their hardness, reaching up to 1401 HV 1 for the FeAl20Si20Mo5Ni15 alloy, which contained in total 58.5% of the FeSi and Fe3Al2Si3 phases. As a result, all the prepared alloys showed one order magnitude lower wear rates ranging from 3.14 to 5.97·10-6 mm3·N-1·m-1 as well as significantly lower friction coefficients compared to two reference tool steels. The alloys achieved high compressive strengths (up to 2200 MPa); however, they also exhibited high brittleness even after long-term annealing, which reduced the strengths of all the alloys below approximately 1600 MPa. Furthermore, the alloys were showing ductile behavior when compressively tested at elevated temperature of 800 °C. The oxidation resistance of the alloys was superior due to the formation of a compact Al2O3 protective layer that did not delaminate.
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Ni-Ti alloys are considered to be very important shape memory alloys with a wide application area including, e.g., biomaterials, actuators, couplings, and components in automotive, aerospace, and robotics industries. In this study, the NiTi46 (wt.%) alloy was prepared by a combination of self-propagating high-temperature synthesis, milling, and spark plasma sintering consolidation at three various temperatures. The compacted samples were subsequently heat-treated at temperatures between 400 °C and 900 °C with the following quenching in water or slow cooling in a closed furnace. The influence of the consolidation temperature and regime of heat treatment on the microstructure, mechanical properties, and temperatures of phase transformation was evaluated. The results demonstrate the brittle behaviour of the samples directly after spark plasma sintering at all temperatures by the compressive test and no transformation temperatures at differential scanning calorimetry curves. The biggest improvement of mechanical properties, which was mainly a ductility enhancement, was achieved by heat treatment at 700 °C. Slow cooling has to be recommended in order to obtain the shape memory properties.
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Maraging steels are generally characterized by excellent mechanical properties, which make them ideal for various industrial applications. The application field can be further extended by using selective laser melting (SLM) for additive manufacturing of shape complicated products. However, the final mechanical properties are strongly related to the microstructure conditions. The present work studies the effect of heat treatment on the microstructure and mechanical properties of 3D printed samples prepared from powder of high-strength X3NiCoMoTi 18-9-5 maraging steel. It was found that the as-printed material had quite low mechanical properties. After sufficient heat treatment, the hardness of the material increased from 350 to 620 HV0.1 and the tensile yield strength increased from 1000 MPa up to 2000 MPa. In addition, 3% ductility was maintained. This behavior was primarily affected by strong precipitation during processing.
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FeAlSi intermetallics are materials with promising high-temperature mechanical properties and oxidation resistance. Nevertheless, their production by standard metallurgical processes is complicated. In this study, preparation of powders by mechanical alloying and properties of the samples compacted by spark plasma sintering was studied. Various initial feedstock materials were mixed to prepare the material with the same chemical composition. Time of mechanical alloying leading to complete homogenization of powders was estimated based on the microstructure observations, results of XRD and indentation tests. Microstructure, phase composition, hardness and fracture toughness of sintered samples was studied and compared with the properties of powders before the sintering process. It was found that independently of initial feedstock powder, the resulting phase composition was the same (Fe3Si + FeSi). The combination of hard initial powders required the longest milling time, but it led to the highest values of fracture toughness.
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Melting metallurgy is still the most frequently used and simplest method for the processing of metallic materials. Some of the materials (especially intermetallics) are very difficult to prepare by this method due to the high melting points, poor fluidity, or formation of cracks and pores after casting. This article describes the processing of Ti-Al-Si alloys by arc melting, and shows the microstructure, phase composition, hardness, fracture toughness, and compression tests of these alloys. These results are compared with the same alloys prepared by powder metallurgy by the means of a combination of mechanical alloying and spark plasma sintering. Ti-Al-Si alloys processed by melting metallurgy are characterized by a very coarse structure with central porosity. The phase composition is formed by titanium aluminides and titanium silicides, which are full of cracks. Ti-Al-Si alloys processed by the powder metallurgy route have a relatively homogeneous fine-grained structure with higher hardness. However, these alloys are very brittle. On the other hand, the fracture toughness of arc-melted samples is immeasurable using Palmqvist's method because the crack is stopped by a large area of titanium aluminide matrix.
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Fe-Al-Si alloys have been previously reported as an interesting alternative to common high-temperature materials. This work aimed to improve the properties of FeAl20Si20 alloy (in wt.%) by the application of powder metallurgy process consisting of ultrahigh-energy mechanical alloying and spark plasma sintering. The material consisted of Fe3Si, FeSi, and Fe3Al2Si3 phases. It was found that the alloy exhibits an anomalous behaviour of yield strength and ultimate compressive strength around 500 °C, reaching approximately 1100 and 1500 MPa, respectively. The results also demonstrated exceptional wear resistance, oxidation resistance, and corrosion resistance in water-based electrolytes. The tested manufacturing process enabled the fracture toughness to be increased ca. 10 times compared to the cast alloy of the same composition. Due to its unique properties, the material could be applicable in the automotive industry for the manufacture of exhaust valves, for wear parts, and probably as a material for selected aggressive chemical environments.
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The compact samples of an Al7075 alloy were prepared by a combination of gas atomization, high energy milling, and spark plasma sintering. The predominantly cellular morphology observed in gas atomized powder particles was completely changed by mechanical milling. The continuous-like intermetallic phases present along intercellular boundaries were destroyed; nevertheless, a small amount of Mg(Zn,Cu,Al)2 phase was observed also in the milled powder. Milling resulted in a severe plastic deformation of the material and led to a reduction of grain size from several µm into the nanocrystalline region. The combination of these microstructural characteristics resulted in abnormally high microhardness values exceeding 300 HV. Consolidation through spark plasma sintering (SPS) resulted in bulk samples with negligible porosity. The heat exposition during SPS led to precipitation of intermetallic phases from the non-equilibrium microstructure of both gas atomized and milled powders. SPS of the milled powder resulted in a recrystallization of the severely deformed structure. An ultra-fine grained structure (grain size close to 500 nm) with grains divided primarily by high-angle boundaries was formed. A simultaneous release of stored deformation energy and an increase in the grain size caused a drop of microhardness to values close to 150 HV. This value was retained even after annealing at 425 °C.