Investigation of Layered Structure Formation in MgB2 Wires Produced by the Internal Mg Coating Process under Low and High Isostatic Pressures.

Currently, MgB2 wires made by the powder-in-tube (PIT) method are most often used in the construction and design of superconducting devices. In this work, we investigated the impact of heat treatment under both low and high isostatic pressures on the formation of a layered structure in PIT MgB2 wires manufactured using the Mg coating method. The microstructure, chemical composition, and density of the obtained superconductive wires were investigated using scanning electron microscopy (SEM) with an energy-dispersive X-ray spectroscopy (EDS) analyzer and optical microscopy with Kameram CMOS software (version 2.11.5.6). Transport measurements of critical parameters were made by using the Physical Property Measurement System (PPMS) for 100 mA and 19 Hz in a perpendicular magnetic field. We observed that the Mg coating method can significantly reduce the reactions of B with the Fe sheath. Moreover, the shape, uniformity, and continuity of the layered structure (cracks, gaps) depend on the homogeneity of the B layer before the synthesis reaction. Additionally, the formation of a layered structure depends on the annealing temperature (for Mg in the liquid or solid-state), isostatic pressure, type of boron, and density of layer B before the synthesis reaction.

Comparison of the Microstructural, Mechanical and Corrosion Resistance Properties of Ti6Al4V Samples Manufactured by LENS and Subjected to Various Heat Treatments.

In this paper, the influences of two post-heat treatments on the structural, mechanical and corrosion resistance properties of additively manufactured Ti6Al4V alloys were discussed in detail. The materials were produced using the laser engineering net shaping (LENS) technique, and they were subjected to annealing without pressure and hot isostatic pressing (HIP) under a pressure of 300 MPa for 30 min at temperatures of 950 °C and 1050 °C. Annealing without pressure led to the formation of a thin plate structure, which was accompanied by decreasing mechanical properties and increasing elongation and corrosion resistance values. For the HIP process, the formation of a thick plate structure could be observed, resulting in the material exhibiting optimal mechanical properties and unusually high elongation. The best mechanical and corrosion resistance properties were obtained for the material subjected to HIP at 950 °C.

Effect of Low Annealing Temperature on the Critical-Current Density of 2% C-Doped MgB2 Wires Used in Superconducting Coils with the Wind-and-React (W&R) Method-High-Field and High-Temperature Pinning Centers.

The use of a low annealing temperature during the production of coils made from superconducting materials is very important because it reduces the production costs. In this study, the morphology, transport critical-current density (Jc), irreversible magnetic field (Birr), and critical temperature (Tc) of straight wires and small 2% C-doped MgB2 coils were investigated. The coils were made using the wind-and-react (W&R) method and annealed at various temperatures from 610 °C to 650 °C for 2-12 h. Critical-current measurements were made for both the coils and straight wires at the temperatures of 4.2 K, 20 K, 25 K, and 30 K. During our research study, we determined the process window that provides the best critical parameters of the coils (annealing at a temperature of 650 °C for 6 h). Moreover, we observed that small coils made with unreacted MgB2 wire and then annealed had morphology and critical parameters similar to those of straight 2% C-doped MgB2 wires. Moreover, small-diameter bending of 20 mm and 10 mm did not lead to transverse cracks, which can cause a large reduction in Jc in the coils. This indicates that the processes of optimization of thermal treatment parameters can be carried out on straight MgB2 wires for MgB2 superconducting coils.

High Critical Current Density in the Textured Nanofiber Structure in Multifilament MgB2 Wires Made by the Powder-In-Tube (PIT) Technique.

We show that the structure of multifilament MgB2 wires made by the powder-in-tube (PIT) method can be texturized by annealing the structure under high isostatic pressure. Our results show that we obtained continuous fibers with a uniform diameter of 250 nm in all 36 filaments, a small grain size of approximately 50 nm and a high density of the superconducting material. These results contribute to a significant improvement in the critical current density in high magnetic fields, e.g., 100 A/mm2 at 14 T and 4.2 K.

Effect of Heat Treatments under High Isostatic Pressure on the Transport Critical Current Density at 4.2 K and 20 K in Doped and Undoped MgB2 Wires.

Annealing undoped MgB2 wires under high isostatic pressure (HIP) increases transport critical current density (Jtc) by 10% at 4.2 K in range magnetic fields from 4 T to 12 T and significantly increases Jtc by 25% in range magnetic fields from 2 T to 4 T and does not increase Jtc above 4 T at 20 K. Further research shows that a large amount of 10% SiC admixture and thermal treatment under a high isostatic pressure of 1 GPa significantly increases the Jtc by 40% at 4.2 K in magnetic fields above 6 T and reduces Jtc by one order at 20 K in MgB2 wires. Additionally, our research showed that heat treatment under high isostatic pressure is more evident in wires with smaller diameters, as it greatly increases the density of MgB2 material and the number of connections between grains compared to MgB2 wires with larger diameters, but only during the Mg solid-state reaction. In addition, our study indicates that smaller wire diameters and high isostatic pressure do not lead to a higher density of MgB2 material and more connections between grains during the liquid-state Mg reaction.

Mechanical and Electrical Properties of Epoxy Composites Modified by Functionalized Multiwalled Carbon Nanotubes.

This paper investigates the effect of multiwalled carbon nanotubes on the mechanical and electrical properties of epoxy resins and epoxy composites. The research concerns multiwalled carbon nanotubes obtained by catalytic chemical vapor deposition, subjected to purification processes and covalent functionalization by depositing functional groups on their surfaces. The study included the analysis of the change in DC resistivity, tensile strength, strain, and Young's modulus with the addition of carbon nanotubes in the range of 0 to 2.5 wt.%. The effect of agents intended to increase the affinity of the nanomaterial to the polymer on the aforementioned properties was also investigated. The addition of functionalized multiwalled carbon nanotubes allowed us to obtain electrically conductive materials. For all materials, the percolation threshold was obtained with 1% addition of multiwalled carbon nanotubes, and filling the polymer with a higher content of carbon nanotubes increased its conductivity. The use of carbon nanotubes as polymer reinforcement allows higher values of tensile strength and a higher strain percentage to be achieved. In contrast, Young's modulus values did not increase significantly, and higher nanofiller percentages resulted in a drastic decrease in the values of the abovementioned properties.

Influence of Amorphous Boron Grain Size, High Isostatic Pressure, Annealing Temperature, and Filling Density of Unreacted Material on Structure, Critical Parameters, N-Value, and Engineering Critical Current Density in Mgb2 Wires.

Our results show that a lower density of unreacted Mg + B material during an Mg solid-state synthesis reaction leads to a significant reduction in the quantity of the superconducting phase and lowers the homogeneity of the superconducting material. It also significantly reduces the irreversible magnetic field (Birr), critical temperature (Tc), upper magnetic field (Bc2), engineered critical current density (Jec), and n-value, despite high isostatic pressure (HIP) treatment and the use of nanoboron in the sample. Our measurements show that samples with large boron grains with an 8% higher density of unreacted Mg + B material allow better critical parameters to be achieved. Studies have shown that the density of unreacted material has little effect on Birr, Tc, Bc2, Jec, and the n-value for an Mg liquid-state synthesis reaction. The results show that the critical parameters during an Mg liquid-state synthesis reaction depend mainly on grain size. Nanoboron grains allow for the highest Birr, Tc, Bc2, Jec, and n-values. Scanning electron microscopy (SEM) images taken from the longitudinal sections of the wires show that the samples annealed under low isostatic pressure have a highly heterogeneous structure. High isostatic pressure heat treatment greatly improves the homogeneity of MgB2.

Microstructure and Properties of Inconel 625 Fabricated Using Two Types of Laser Metal Deposition Methods.

The effect of using two different deposition systems on the microstructure and mechanical properties was studied in this paper. For this purpose, laser-engineered net shaping (LENS) and high-power CO2 laser deposition processes were applied to fabricate Inconel 625 samples. The microstructure of the Inconel 625 produced by both additive techniques was characterized using light microscopy (LM), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and transmission electron microscopy (TEM). The mechanical properties were characterized by tensile tests and microhardness measurements. High-power laser application resulted in a strong <100> build texture, while, at low powers, the {011} <100> Goss component increased. Both types of deposited materials showed dendritic microstructures with Ti-, Mo-, and Nb-rich zones at the cell boundaries, where numerous precipitates (Nb2C, NbC, titanium carbides, Nb3Ni, and NbNiCr) were also observed. It was also noted that both variants were characterized by the same slope with a proportional length, but the Inconel 625 fabricated via LENS showed a higher average yield strength (YS; 524 MPa vs. 472 MPa) and ultimate tensile strength (UTS; 944 MPa vs. 868 MPa) and lower elongation (35% vs. 42%) than samples obtained with the high-power CO2 laser deposition process.

New Aspects of MgH2 Morphological and Structural Changes during High-Energy Ball Milling.

Magnesium hydride, despite the decomposition temperature being incompatible with the operating temperature of a typical PEM cell, is still considered a prospective material for hydrogen storage. Hence, this paper presents new aspects of the influence of milling time on the structural changes and temperature of MgH2 decomposition, with particular emphasis on the changes taking place in the first few seconds of the milling process. This paper presents qualitative and quantitative changes in the powder particle morphology determined using scanning electron microscopy (SEM) and infrared particle size analysis (IPS) systems. The crystallographic structure of the powders in the initial state and after mechanical milling was characterized by X-ray diffraction. The decomposition temperature and activation energy were determined by the differential scanning calorimetry (DSC). Changes in the activation energy and decomposition temperature were observed after only 1-2 min of the milling process. Two basic stages of the milling process were distinguished that impacted the MgH2 decomposition temperature, i.e., mechanical activation and a nanostructuring process. The activation was associated with the initial stage of particle size reduction and an increase in the fraction of fresh chemically active powder particle surfaces. On the other hand, the nanostructuring process was related to an additional decrease in the MgH2 decomposition temperature.

Nanoporous Anodic Aluminum-Iron Oxide with a Tunable Band Gap Formed on the FeAl3 Intermetallic Phase.

Nanostructured anodic oxide layers on an FeAl3 intermetallic alloy was prepared by two-step anodization in 20 wt.% H2SO4 at 0 °C. The obtained anodic oxide coating was subjected to phase and chemical composition analysis using XPS and XRD techniques. An analysis of the band gap of individual coatings was also performed. The applied parameters of the anodization process were determined, enabling the formation of a nanostructured coating on the FeAl3 intermetallic alloy. Tests were carried out on samples produced at a voltage between 10 V and 22.5 V in 2.5 V steps. The produced coatings were subjected to an annealing process at 900 °C for 2 h in an argon protective atmosphere. Moreover, the influence of the substrate chemical composition on the chemical and phase composition of the anodic oxide are discussed. Band gaps of 2.37 eV at 22.5 V and 2.64 eV at 10 V were obtained directly after the anodizing process. After applying the heat treatment, band gap values of 2.10 eV at 22.5 Vand 2.48 eV for the coating produced at 10 V were obtained.

Superelastic Behavior of Ti-Nb Alloys Obtained by the Laser Engineered Net Shaping (LENS) Technique.

The effect of Nb content on microstructure, mechanical properties and superelasticity was investigated for a series of Ti-xNb alloys, fabricated by the laser engineered net shaping method, using elemental Ti and Nb powders. The microstructure of as-deposited materials consisted of columnar ß-phase grains, elongated in the built direction. However, due to the presence of undissolved Nb particles during the deposition process, an additional heat treatment was necessary. The observed changes in mechanical properties were explained in relation to the phase constituents and deformation mechanisms. Due to the elevated oxygen content in the investigated materials (2 at.%), the specific deformation mechanisms were observed at lower Nb content in comparison to the conventionally fabricated materials. This made it possible to conclude that oxygen increases the stability of the ß phase in ß-Ti alloys. For the first time, superelasticity was observed in Ti-Nb-based alloys fabricated by the additive manufacturing method. The highest recoverable strain of 3% was observed in Ti-19Nb alloy as a result of high elasticity and reverse martensitic transformation stress-induced during the loading.

The Characterization of Stress Corrosion Cracking in the AE44 Magnesium Casting Alloy Using Quantitative Fractography Methods.

In this work an assessment of the susceptibility of the AE44 magnesium alloy to stress corrosion cracking in a 0.1M Na2SO4 environment is presented. The basic assumed criterion for assessing the alloy behavior under complex mechanical and corrosive loads is deterioration in mechanical properties (elongation, reduction in area, tensile strength and time to failure). The AE44 magnesium alloy was subjected to the slow strain rate test (SSR) in air and in a corrosive environment under open circuit potential (OCP) conditions. In each variant, the content of hydrogen in the alloy was determined. The obtained fractures were subjected to a quantitative evaluation by original fractography methods. It was found that under stress corrosion cracking (SCC) conditions and in the presence of hydrogen the mechanical properties of AE44 deteriorated. The change in the mechanical properties under SCC conditions in a corrosive environment was accompanied by the presence of numerous cracks, both on fracture surfaces and in the alloy microstructure. The developed method for the quantitative evaluation of cracks on the fracture surface turned out to be a more sensitive method, enabling the assessment of the susceptibility of AE44 under complex mechanical and corrosive loads in comparison with deterioration in mechanical properties. Mechanical tests showed a decrease in properties after SSRT tests in corrosive environments (UTS ≈ 153 MPa, ε = 11.2%, Z = 4.0%) compared to the properties after air tests (UTS ≈ 166 MPa, ε = 11.9%, Z = 7.8%) but it was not as visible as the results of quantitative assessment of cracks at fractures (number of cracks, length of cracks): after tests in corrosive environment (900; 21.3 µm), after tests in air (141; 34.5 µm). These results indicate that the proposed new proprietary test methodology can be used to quantify the SSC phenomenon in cases of slight changes in mechanical properties after SSRT tests in a corrosive environment in relation to the test results in air.

Formation of Nanoporous Mixed Aluminum-Iron Oxides by Self-Organized Anodizing of FeAl3 Intermetallic Alloy.

Nanostructured anodic oxide layers on an FeAl3 intermetallic alloy were prepared by two-step anodization in 20 wt% H2SO4 at 0 °C. The voltage range was 10.0-22.5 V with a step of 2.5 V. The structural and morphological characterizations of the received anodic oxide layers were performed by field emission scanning electron microscopy (FE-SEM). Therefore, the formed anodic oxide was found to be highly porous with a high surface area, as indicated by the FE-SEM studies. It has been shown that the morphology of fabricated nanoporous oxide layers is strongly affected by the anodization potential. The oxide growth rate first increased slowly (from 0.010 µm/s for 10 V to 0.02 µm/s for 15 V) and then very rapidly (from 0.04 µm/s for 17.5 V up to 0.13 µm/s for 22.5 V). The same trend was observed for the change in the oxide thickness. Moreover, for all investigated anodizing voltages, the structural features of the anodic oxide layers, such as the pore diameter and interpore distance, increased with increasing anodizing potential. The obtained anodic oxide layer was identified as a crystalline FeAl2O4, Fe2O3 and Al2O3 oxide mixture.

The Tribaloy T-800 Coatings Deposited by Laser Engineered Net Shaping (LENSTM).

A Tribaloy family of alloys (CoMoCrSi) are characterized by a substantial resistance to wear and corrosion within a wide range of temperatures. These properties are a direct result of their microstructure including the presence of Laves phase in varying proportions. Tribaloy T-800 exhibits the highest content of Laves phase of all other commercial Tribaloy alloys, which provides high hardness and wear resistance. On the other hand, a large content of the Laves phase brings about a high sensitivity to brittle fracture of this alloy. The main objective of this work was a development of the Tribaloy T-800 coatings on the Ni-based superalloy substrate (RENE 77), which employs a Laser Engineered Net Shaping (LENSTM) technique. Technological limitations in this process are susceptibility of T-800 to brittle fracture as well as significant thermal stresses due to rapid cooling, which is an inherent attribute of laser techniques. Therefore, in this work, a number of steps that optimized the LENSTM process and improved the metallurgical soundness of coatings are presented. Employing volume and local substrate pre-heating resulted in the formation of high quality coatings devoid of cracks and flaws.

Static and Dynamic Loading Behavior of Ti6Al4V Honeycomb Structures Manufactured by Laser Engineered Net Shaping (LENSTM) Technology.

Laser Engineered Net Shaping (LENSTM) is currently a promising and developing technique. It allows for shortening the time between the design stage and the manufacturing process. LENS is an alternative to classic metal manufacturing methods, such as casting and plastic working. Moreover, it enables the production of finished spatial structures using different types of metallic powders as starting materials. Using this technology, thin-walled honeycomb structures with four different cell sizes were obtained. The technological parameters of the manufacturing process were selected experimentally, and the initial powder was a spherical Ti6Al4V powder with a particle size of 45-105 µm. The dimensions of the specimens were approximately 40 × 40 × 10 mm, and the wall thickness was approximately 0.7 mm. The geometrical quality and the surface roughness of the manufactured structures were investigated. Due to the high cooling rates occurring during the LENS process, the microstructure for this alloy consists only of the martensitic α' phase. In order to increase the mechanical parameters, it was necessary to apply post processing heat treatment leading to the creation of a two-phase α + ß structure. The main aim of this investigation was to study the energy absorption of additively manufactured regular cellular structures with a honeycomb topology under static and dynamic loading conditions.

Identification of Mechanical Properties for Titanium Alloy Ti-6Al-4V Produced Using LENS Technology.

This paper presents a characterization study of specimens manufactured from Ti-6Al-4V powder with the use of laser engineered net shaping technology (LENS). Two different orientations of the specimens were considered to analyze the loading direction influence on the material mechanical properties. Moreover, two sets of specimens, as-built (without heat treatment) and after heat treatment, were used. An optical measurement system was also adopted for determining deformation of the specimen, areas of minimum and the maximum principal strain, and an effective plastic strain value at failure. The loading direction dependence on the material properties was observed with a significant influence of the orientation on the stress and strain level. Microstructure characterization was examined with the use of optical and scanning electron microscopes (SEM); in addition, the electron backscatter diffraction (EBSD) was also used. The fracture mechanism was discussed based on the fractography analysis. The presented comprehensive methodology proved to be effective and it could be implemented for different materials in additive technologies. The material data was used to obtain parameters for the selected constitutive model to simulate the energy absorbing structures manufactured with LENS technology. Therefore, a brief discussion related to numerical modelling of the LENS Ti-6Al-4V alloy was also included in the paper. The numerical modelling confirmed the correctness of the acquired material data resulting in a reasonable reproduction of the material behavior during the cellular structure deformation process.

Severe Plastic Deformation of Fe-22Al-5Cr Alloy by Cross-Channel Extrusion with Back Pressure.

A new concept of the cross-channel extrusion (CCE) process under back pressure (BP) was proposed and tested experimentally. The obtained by finite element method (FEM) results showed that a triaxial compression occurred in the central zone, whereas the material was deformed by shearing in the outer zone. This led to the presence of a relatively uniformly deformed outer zone at 1 per pass and a strong deformation of the paraxial zone (3⁻5/pass). An increase in the BP did not substantially affect the accumulated strain but made it more uniform. The FEM results were verified using the physical modeling technique (PMT) by the extrusion of clay billet. The formation of the plane of the strongly flattened, and elongated grains were observed in the extrusion directions. With the increase in the number of passes, the shape of the resulting patterns expanded, indicating an increase in the deformation homogeneity. Finally, these investigations were verified experimentally for Fe-22Al-5Cr (at. %) alloy using of the purposely designed tooling. The effect of the CCE process is the fragmentation of the original material structure by dividing the primary grains. The complexity of the stress state leads to the rapid growth of microshear bands (MSB), grain defragmentation and the nucleation of new dynamically recrystallized grains about 200⁻400 nm size.

The Application of Globular Water-Atomized Iron Powders for Additive Manufacturing by a LENS Technique.

The water-atomized ATOMET 28, 1001, 4701, and 4801 powders, manufactured by Rio Tinto Metal Powders, were used for additive manufacturing by a laser engineered net shaping (LENS) technique. Their overall morphology was globular and rounded with a size distribution from about 20 to 200 µm. Only the ATOMET 28 powder was characterized by a strong inhomogeneity of particle size and irregular polyhedral shape of powder particles with sharp edges. The powders were pre-sieved to a size distribution from 40 to 150 µm before LENS processing. One particular sample-LENS-fabricated from the ATOMET 28 powder-was characterized by the largest cross-sectional (2D) porosity of 4.2% and bulk porosity of 3.9%, the latter determined by microtomography measurements. In contrast, the cross-sectional porosities of bulk, solid, nearly cubic LENS-fabricated samples from the other ATOMET powders exhibited very low porosities within the range 0.03⁻0.1%. Unexpectedly, the solid sample-LENS-fabricated from the reference, a purely spherical Fe 99.8 powder-exhibited a porosity of 1.1%, the second largest after that of the pre-sieved, nonspherical ATOMET 28 powder. Vibrations incorporated mechanically into the LENS powder feeding system substantially improved the flow rate vs. feeding rate dependence, making it completely linear with an excellent coefficient of fit, R² = 0.99. In comparison, the reference powder Fe 99.8 always exhibited a linear dependence of the powder flow rate vs. feeding rate, regardless of vibrations.

The Effect of the Traverse Feed Rate on the Microstructure and Mechanical Properties of Laser Deposited Fe3Al (Zr,B) Intermetallic Alloy.

The results of the fabrication of components made with Fe-30%Al-0.35%Zr-0.1%B alloy powder using the Laser Engineered Net Shaping (LENSTM) system operated at different traverse feed rates are described in this paper. The temperature of the molten metal pool was recorded during this process. Depending on the assumed feed rate, the formation of Zr⁻based precipitates with various morphologies and distributions was observed in the structure of the investigated material. It was found that as the traverse speed increased, spheroidization, refinement, and a more homogeneous distribution of these precipitates occurred.

The Microstructure Evolution of a Fe3Al Alloy during the LENS Process.

A Fe3Al intermetallic alloy has been successfully prepared by the laser-engineered net shaping (LENS) process. The applied process parameters were selected to provide various cooling rates during the solidification of the laser-melted material. The macro- and microstructure and the micro- and macrotexture of Fe3Al samples were investigated. The influence of the cooling rate on grain morphology and texture is discussed. For the applied cooling rate range of 0.64 × 104 K/s-2.6 × 104 K/s, the structure is characterized by the presence of columnar grains for which the growth is directed upwards from the substrate. The intensity of the microtexture varies with the height of the sample and the cooling rate. The intensity of the texture increases with the decrease in the cooling rate. The samples that were obtained with low and medium cooling rates are characterized by the well-developed <100> and <111> macrotextures. The Fe3Al alloy that was produced with a high cooling rate did not show a specific texture, which is reflected in the fairly uniform distribution of the normalized density intensity. Only a very weak texture with a <100> type component was observed.