The atomic layer deposition (ALD) synthesis of copper-tin sulfide thin films using low-cost precursors.

In this work we demonstrated the process of co-deposition of copper-tin sulfide species by the atomic layer deposition (ALD) technique using all-low-cost precursors. For the deposition of tin species, the tin(IV) chloride SnCl4was used successfully for the first time in the ALD process. Moreover, we showed that the successful deposition of the tin sulfide component was conditioned by the pre-deposition of CuSxlayer. The co-deposition of copper and tin sulfides components at 150 °C resulted in the in-process formation of the film containing Cu2SnS3, Cu3SnS4andπ-SnS phases. The process involving only tin precursor and H2S did not produce the SnSxspecies. The spectroscopic characteristic of the obtained materials were confronted with the literature survey, allowing us to discuss the methodology of the determination of ternary and quaternary sulfides purity by Raman spectroscopy. Moreover, the material characterisation with respect to the morphology (SEM), phase composition (XRD), surface chemical states (XPS), optical properties (UV-vis-NIR spectroscopy) and electric (Hall measurements) properties were provided. Finally, the obtained material was used for the formation of the p-n junction revealing the rectifyingI-Vcharacteristics.

Influence of Magnetron Sputtering-Deposited Niobium Nitride Coating and Its Thermal Oxidation on the Properties of AISI 316L Steel in Terms of Its Medical Applications.

An NbN coating was produced on AISI 316L steel using reactive DC magnetron sputtering. The effects of oxidation of the NbN coating in air on the microstructure, mechanical properties, corrosion resistance, contact angle and bioactivity were investigated. Phase composition was determined using X-ray diffraction (XRD), the coatings' cross-sectional microstructure and thickness including surface morphology using a scanning electron microscope (SEM), microhardness via the Vickers method, corrosion by means of a potentiodynamic polarisation test in Ringer's solution and bioactivity by observation in an SBF solution, while the contact angle was studied using a goniometer. The NbN coating and the oxidised coating were shown to demonstrate a Ca/P ratio close to that of hydroxyapatite, as well as increased microhardness and corrosion resistance. The best combination of mechanical, corrosion, bioactivity and hydrophilic properties was demonstrated by the air oxidised NbN coating, which featured an orthorhombic Nb2O5 structure in the top, surface layer.

Synthesis of Ti3SiC2 Phases and Consolidation of MAX/SiC Composites-Microstructure and Mechanical Properties.

The article describes the Ti3SiC2 powder synthesis process. The influence of the molar ratio and two forms of carbon on the phase composition of the obtained powders was investigated. The synthesis was carried out using a spark plasma sintering (SPS) furnace. In addition, using the obtained powders, composites reinforced with SiC particles were produced. The obtained results showed no effect of the carbon form and a significant impact of annealing on the purity of the powders after synthesis. The composites were also consolidated using an SPS furnace at two temperatures of 1300 and 1400 °C. The tests showed low density and hardness for sinters from 1300 °C (maximum 3.97 g/cm3 and 447 HV5, respectively, for composite reinforced with 10% SiC). These parameters significantly increase for composites sintered at 1400 °C (maximum density 4.43 g/cm3 and hardness 1153 HV5, for Ti3AlC2-10% SiC). In addition, the crack propagation analysis showed mechanisms typical for granular materials and laminates.

Impact of an Aluminization Process on the Microstructure and Texture of Samples of Haynes 282 Nickel Alloy Produced Using the Direct Metal Laser Sintering (DMLS) Technique.

In this study, we examined the effects of an aluminization process on the microstructure and texture of Haynes 282 nickel samples fabricated using the direct metal laser sintering technique. The aluminization process involved the use of chemical vapor deposition with AlCl3 vapors in a hydrogen atmosphere at a temperature of 1040 °C for 8 h. Following the 3D printing and aluminization steps, we analyzed the microstructure of the Haynes 282 nickel alloy samples using light microscopy and scanning electron microscopy. Additionally, we investigated the texture using X-ray diffractometry. A texture analysis revealed that after the process of direct laser sintering of metals, the texture of the Haynes 282 nickel alloy samples developed a texture typical of cast materials. Then, in the aluminization process, the texture was transformed-from foundry-type components to a texture characteristic of recrystallization.

Polymer-Nickel Composite Filaments for 3D Printing of Open Porous Materials.

Catalysis has been a key way of improving the efficiency-to-cost ratio of chemical and electrochemical processes. There have been recent developments in catalyst materials that enable the development of novel and more sophisticated devices that, for example, can be used in applications, such as membranes, batteries or fuel cells. Since catalytic reactions occur on the surface, most catalyst materials are based on open porous structures, which facilitates the transport of fluids (gas or liquid) and chemical (or electrochemical) specific surface activity, thus determining the overall efficiency of the device. Noble metals are typically used for low temperature catalysis, whereas lower cost materials, such as nickel, are used for catalysis at elevated temperatures. 3D printing has the potential to produce a more sophisticated fit for purpose catalyst material. This article presents the development, fabrication and performance comparison of three thermoplastic composites where PLA (polylactic acid), PVB (polyvinyl butyral) or ABS (acrylonitrile butadiene styrene) were used as the matrix, and nickel particles were used as filler with various volume fractions, from 5 to 25 vol%. The polymer-metal composites were extruded in the form of filaments and then used for 3D FDM (Fused Deposition Modeling) printing. The 3D printed composites were heat treated to remove the polymer and sinter the nickel particles. 3D printed composites were also prepared using nickel foam as a substrate to increase the final porosity and mechanical strength of the material. The result of the study demonstrates the ability of the optimized filament materials to be used in the fabrication of high open porosity (over 60%) structures that could be used in high-temperature catalysis and/or electrocatalysis.

Comparison of Microstructure, Texture, and Mechanical Properties of TZ61 and AZ61 Mg Alloys Processed by Differential Speed Rolling.

In this work, the comparison of microstructure, texture, and mechanical properties of the newly developed TZ61 (Mg-6Sn-1Zn) alloy with the commercially available AZ61 (Mg-6Al-1Zn) has been presented. Both analyzed Mg alloys were processed by conventional symmetric and asymmetric rolling (i.e., Differential Speed Rolling-DSR). The microstructure and texture were examined by EBSD and XRD, whereas the mechanical behavior was investigated by uniaxial tensile tests. DSR processing led to more effective grain refinement of both TZ61 and AZ61 sheets. However, a high fraction of Mg2Sn phase precipitates in the TZ61 sheets hindered grain growth what resulted in their smaller grain size as compared to AZ61 sheets. DSR processing lowered also the basal texture intensity in the TZ61 and AZ61 sheets. A unique basal poles splitting was observed for the as-rolled TZ61 alloy, while AZ61 alloy exhibited a typical single-peak basal texture. Finally, the reduced grain size and weakened basal texture by DSR processing caused increase of plasticity of the annealed TZ61 and AZ61 sheets. Nevertheless, the annealed AZ61 sheets showed higher uniform elongation and strength (as compared to TZ61 ones), which has been attributed to their significantly lower texture intensity and greater ability to strain hardening.

The Influence of Heat Treatment on the Mechanical Properties and Corrosion Resistance of the Ultrafine-Grained AA7075 Obtained by Hydrostatic Extrusion.

In this paper, the corrosion resistance and mechanical properties of the 7075 aluminum alloy are studied. The alloy was deformed by hydrostatic extrusion and then aged both naturally and artificially. Results are compared with those of coarse-grained material subjected to T6 heat treatment. The aim of the research is to find the optimal correlation between the mechanical properties and the corrosion resistance of the alloy. To this end, static tensile tests with subsequent fractography, open circuit potential, and potentiodynamic polarization tests in 0.05 M NaCl were conducted. Obtained results show that a combination of precipitate hardening and a deformed microstructure leads to increased mechanical strength with high anisotropy due to the presence of fibrous grains. Plastic deformation increases susceptibility to corrosion due to the increased number of grain boundaries, which act as paths along that corrosion propagates. However, further artificial aging incurs a positive effect on corrosion resistance due to changes in the chemical composition of the matrix as a result of the precipitation process.

Increasing the Mechanical Strength and Corrosion Resistance of Aluminum Alloy 7075 via Hydrostatic Extrusion and Aging.

The present study investigates the correlation between mechanical properties and resistance to corrosion of hydrostatically extruded aluminum alloy 7075. Supersaturated solid solutionized samples undergo a plastic deformation process, followed by both natural and artificial aging. Furthermore, two types of hydrostatic extrusion are applied to the samples: single-stepped and double-stepped. This process is shown to influence grain refinement and the precipitation process, resulting in changes in the electrochemical properties of the samples. Hydrostatic extrusion combined with aging is shown to cause an increase in mechanical strength ranging from 50 MPa to 135 MPa in comparison to coarse-grained sample subjected to T6 heat treatment. The highest value of tensile strength is obtained for a sample subjected to single-step hydrostatic extrusion followed by natural aging. This strength increase is caused by refinement of the microstructure, in addition to the small size and number of precipitates at the grain boundaries, which are coarsened by artificial aging. Hydrostatic extrusion is also shown to increase resistance to corrosion, with the T6-treated coarse-grained sample being most susceptible to corrosion attack.

Heat Treatment of NiTi Alloys Fabricated Using Laser Powder Bed Fusion (LPBF) from Elementally Blended Powders.

The use of elemental metallic powders and in situ alloying in additive manufacturing (AM) is of industrial relevance as it offers the required flexibility to tailor the batch powder composition. This solution has been applied to the AM manufacturing of nickel-titanium (NiTi) shape memory alloy components. In this work, we show that laser powder bed fusion (LPBF) can be used to create a Ni55.7Ti44.3 alloyed component, but that the chemical composition of the build has a large heterogeneity. To solve this problem three different annealing heat treatments were designed, and the resulting porosity, microstructural homogeneity, and phase formation was investigated. The heat treatments were found to improve the alloy's chemical and phase homogeneity, but the brittle NiTi2 phase was found to be stabilized by the 0.54 wt.% of oxygen present in all fabricated samples. As a consequence, a Ni2Ti4O phase was formed and was confirmed by transmission electron microscopy (TEM) observation. This study showed that pore formation in in situ alloyed NiTi can be controlled via heat treatment. Moreover, we have shown that the two-step heat treatment is a promising method to homogenise the chemical and phase composition of in situ alloyed NiTi powder fabricated by LPBF.

Modelling and Characterisation of Residual Stress of SiC-Ti3C2Tx MXene Composites Sintered via Spark Plasma Sintering Method.

This article presents an attempt to determine the effect of the MXene phase addition and its decomposition during sintering with the use of the spark plasma sintering method on mechanical properties and residual stress of silicon carbide based composites. For this purpose, the unreinforced silicon carbide sinter and the silicon carbide composite with the addition of 2 wt.% of Ti3C2Tx were tested. The results showed a significant increase of fracture toughness and hardness for composite, respectively 36% and 13%. The numerical study involving this novel method of modelling shows the presence of a complex state of stress in the material, which is related to the anisotropic properties of graphitic carbon structures formed during sintering. An attempt to determine the actual values of residual stress in the tested materials using Raman spectroscopy was also made. These tests showed a good correlation with the constructed numerical model and confirmed the presence of a complex state of residual stress.

Influence of Ti3C2Tx MXene and Surface-Modified Ti3C2Tx MXene Addition on Microstructure and Mechanical Properties of Silicon Carbide Composites Sintered via Spark Plasma Sintering Method.

This article presents new findings related to the problem of the introduction of MXene phases into the silicon carbide matrix. The addition of MXene phases, as shown by the latest research, can significantly improve the mechanical properties of silicon carbide, including fracture toughness. Low fracture toughness is one of the main disadvantages that significantly limit its use. As a part of the experiment, two series of composites were produced with the addition of 2D-Ti3C2Tx MXene and 2D-Ti3C2Tx surface-modified MXene with the use of the sol-gel method with a mixture of Y2O3/Al2O3 oxides. The composites were obtained with the powder metallurgy technique and sintered with the Spark Plasma Sintering method at 1900 °C. The effect adding MXene phases had on the mechanical properties and microstructure of the produced sinters was investigated. Moreover, the influence of the performed surface modification on changes in the properties of the produced composites was determined. The analysis of the obtained results showed that during sintering, the MXene phases oxidize with the formation of carbon flakes playing the role of reinforcement. The influence of the Y2O3/Al2O3 layer on the structure of carbon flakes and the higher quality of the interface was also demonstrated. This was reflected in the higher mechanical properties of composites with the addition of modified Ti3C2Tx. Composites with 1 wt.% addition of Ti3C2Tx M are characterized with a fracture toughness of 5 MPa × m0.5, which is over 50% higher than in the case of the reference sample and over 15% higher than for the composite with 2.5 wt.% addition of Ti3C2Tx, which showed the highest fracture toughness in this series.

Microstructure and Mechanical Properties of Alumina Composites with Addition of Structurally Modified 2D Ti3C2 (MXene) Phase.

This study presents new findings related to the incorporation of MXene phases into ceramic. Aluminium oxide and synthesised Ti3C2 were utilised as starting materials. Knowing the tendency of MXenes to oxidation and degradation, particularly at higher temperatures, structural modifications were proposed. They consisted of creating the metallic layer on the Ti3C2, by sputtering the titanium or molybdenum. To prepare the composites, powder metallurgy and spark plasma sintering (SPS) techniques were adopted. In order to evaluate the effectiveness of the applied modifications, the emphasis of the research was placed on microstructural analysis. In addition, the mechanical properties of the obtained sinters were examined. Observations revealed significant changes in the MXenes degradation process, from porous areas with TiC particles (for unmodified Ti3C2), to in situ creation of graphitic carbon (in the case of Ti3C2-Ti/Mo). Moreover, the fracture changed from purely intergranular to cracking with high participation of transgranular mode, analogously. In addition, the results obtained showed an improvement in the mechanical properties for composites with Ti/Mo modifications (an increase of 10% and 15% in hardness and fracture toughness respectively, for specimens with 0.5 wt.% Ti3C2-Mo). For unmodified Ti3C2, enormously cracked areas with spatters emerged during tests, making the measurements impossible to perform.

Microstructure, Texture and Mechanical Properties of Mg-6Sn Alloy Processed by Differential Speed Rolling.

The effect of shear deformation introduced by differential speed rolling (DSR) on the microstructure, texture and mechanical properties of Mg-6Sn alloy was investigated. Mg-6Sn sheets were obtained by DSR at speed ratio between upper and lower rolls of R = 1, 1.25, 2 and 3 (R = 1 refers to symmetric rolling). The microstructural and textural changes were investigated by electron backscattered diffraction (EBSD) and XRD, while the mechanical performance was evaluated based on tensile tests and calculated Lankford parameters. DSR resulted in the pronounced grain refinement of Mg-6Sn sheets and spreading of basal texture as compared to conventionally rolled one. The average grain size and basal texture intensity gradually decreased with increasing speed ratio. The basal poles splitting to transverse direction (TD) or rolling direction (RD) was observed for all Mg-6Sn sheets. For the as-rolled sheets, YS and UTS increased with increasing speed ratio, but a significant anisotropy of strength and ductility between RD and TD has been observed. After annealing at 300 °C, Mg-6Sn sheets became more homogeneous, and the elongation to failure was increased with higher speed ratios. Moreover, the annealed Mg-6Sn sheets were characterized by a very low normal anisotropy (0.91-1.16), which is normally not achieved for the most common Mg-Al-Zn alloys.

Influence of MXene (Ti3C2) Phase Addition on the Microstructure and Mechanical Properties of Silicon Nitride Ceramics.

This paper discusses the influence of Ti3C2 (MXene) addition on silicon nitride and its impact on the microstructure and mechanical properties of the latter. Composites were prepared through powder processing and sintered using the spark plasma sintering (SPS) technic. Relative density, hardness and fracture toughness, were analyzed. The highest fracture toughness at 5.3 MPa·m1/2 and the highest hardness at HV5 2217 were achieved for 0.7 and 2 wt.% Ti3C2, respectively. Moreover, the formation of the Si2N2O phase was observed as a result of both the MXene addition and the preservation of the α-Si3N4→ß-Si3N4 phase transformation during the sintering process.

A Study of Second-Phase Precipitates and Dispersoid Particles in 2024 Aluminum Alloy after Different Aging Treatments.

Aluminum alloys such as AA2024 are popular in the automotive and aircraft industries. The application of artificial aging significantly improves their mechanical properties by precipitation hardening. However, commercial alloys very often contain different amounts of elements such as Si and Fe that make the evolution of the microstructure harder to control. Large intermetallic particles can influence the overall results of heat treatment and cause deterioration of material properties. The authors decided to examine changes in the microstructure of three commercial 2024 alloys with varying chemical compositions by applying three different types of aging treatments. The results show considerable differences in the amount, size and morphologies of the precipitates. Second-phase Al2Cu and Al2CuMg precipitates were identified in one of the alloys. Other interesting types of multiphase particles were discovered in alloys with higher Si contents. The results show that even small variations in the composition can lead to a completely different microstructure.