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Morphological and optical properties of a multilayer film (CAZO/CZAO/ZACO) prepared by spin-coating method and deposited on a glass substrate were evaluated. The study was initially carried out for each layer, individually and then as a multilayer subsequently. Structural properties using X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS), infrared spectra (IR) and X-ray photoelectron Spectroscopy (XPS) showed the presence of three phases of zinc, copper and silver oxides at different levels. The CZAO sample observed with scanning electron microscope (SEM) showed an excellent porous surface with a large deformation in the multilayer configuration. Doping with zinc and copper in the silver crystal lattice improved the crystal structure and reduced the optical energy gap, thus increasing the optical absorbance and refractive index. The dielectric constants and showed an increase in the optical polarization values for lower photonic energies. The maximum degradation rate for photocatalysts of methylene blue was 89 % for a 5-h exposure period with CAZO/CZAO/ZACO while it reached 71 % for the CZAO sample during the same time period. The sensitivity of samples to light proved that the presence of ultraviolet radiation increases the number of holes trapped by oxygen ions and causes more free electrons and contribute to a better production of photocurrent than in darkness.
In order to create alloys with exceptional properties for orthopedic uses, this study focuses on the impact of zirconium (Zr) content on the structural, electrochemical, and tribological qualities of nanostructured Ti–25Nb-xZr [x = 5, 10, 15, 20, 25, and 30 atomic (at.) %] alloys. The structural evolution was investigated using XRD and SEM techniques. The mechanical characteristics of the produced alloys, including Vickers hardness and Young's modulus, were measured. In addition, the corrosion tests were performed using the OCP, EIS, and PD methods in Ringer's solution within the independent pH range at 37 °C. A ball-on-disc tribometer was used to investigate the tribological behavior of the alloys under various loads and wet conditions using the Ringer solution. It has been verified that Zr content (at. %) in the alloys had an impact on their morphologies, structural evolution, and mechanical characteristics. According to the morphological analysis, the particle and crystallite size decreases with increasing Zr content. Young's modulus and Vickers hardness show the same tendency. The EIS data demonstrated that a single passive film formed on the alloy surfaces, and the addition of Zr enhanced the corrosion resistance of the passive films. The polarization curves demonstrate that the alloys had low corrosion current densities and large passive areas without the passive films disintegrating. Likewise, the inclusion of Zr resulted in a reduction in the corrosion and passive current densities values. All of these results suggested that the titanium alloys exhibit a more noble electrochemical activity caused by Zr. From the tribological perspective, it was found that the friction coefficient of the alloys reduced with increasing Zr content.
This study investigates the in vitro biocompatibility, corrosion resistance, and adhesion strength of a gas abrasive-treated Ti6Al4V alloy, alongside microplasma-sprayed titanium and tantalum coatings. Employing a novel approach in selecting microplasma spray parameters, this study successfully engineers coatings with tailored porosity, roughness, and over 20% porosity with pore sizes up to 200 μm, aiming to enhance bone in-growth and implant integration. This study introduces an innovative methodology for quantifying surface roughness using laser electron microscopy and scanning electron microscopy, facilitating detailed morphological analysis of both the substrate and coatings. Extensive evaluations, including tests for in vitro biocompatibility, corrosion resistance, and adhesive strength, revealed that all three materials are biocompatible, with tantalum coatings exhibiting superior cell proliferation and osteogenic differentiation, as well as the highest corrosion resistance. Titanium coatings followed closely, demonstrating favorable osteogenic properties and enhanced roughness, which is crucial for cell behavior and attachment. These coatings also displayed superior tensile adhesive strengths (27.6 ± 0.9 MPa for Ti and 28.0 ± 4.9 MPa for Ta), surpassing the ISO 13179-1 standard and indicating a robust bond with the substrate. Our findings offer significant advancements in biomaterials for medical implants, introducing microplasma spraying as a versatile tool for customizing implant coatings, particularly emphasizing the superior performance of tantalum coatings in terms of biocompatibility, osteogenic potential, and corrosion resistance. This suggests that tantalum coatings are a promising alternative for enhancing the performance of metal implants, especially in applications demanding high biocompatibility and corrosion resistance.
The effect of heat treatment at various temperatures (650, 850, 1050, and 1100°C) and dwell times (10 min and 1 h) on the metallurgical and microstructural evolution as well as on the related tensile properties of stainless steel 316L processed by selective laser melting (SLM) has been systematically evaluated. The metallurgical and microstructural features such as defects, stability of the columnar–cellular structure and substructure, second phase particles, and phase transformation imparted by SLM and heat treatment have been discussed. It has been shown that the processing conditions specific to SLM significantly alter the kinetics of phase evolution compared to standard welding techniques which affects the accuracy of the prediction. The influence of these characteristics on tensile properties and hardness was elucidated. It was disclosed that with increasing heat treatment temperature there was a gradual increase in elongation but a decrease in strength related to the dislocation density and the development of the microstructure.
Chromium carbonitride coatings were deposited by cathodic arc physical vapor deposition technology at a temperature of 300 °C, as were used the reactive gasses CH4 and N2. The structural analysis of the CrN coating showed a polycrystalline structure with mixed CrN and Cr2N phases. All studied coatings, including the CrC exhibits fcc structure. The phases were confirmed by X-ray photoelectron spectroscopy measurements where a surface oxidation was also detected. The increase of the CH4 gas flow during the deposition process leads to a parabolic trend with the highest hardness of 33.5 GPa for the coating deposited at CH4 / N2 = 0.53. At the same time the lowest coefficient of friction for both counterparts Al2O3 and ZrO2 (0.28 and 0.26, respectively) were measured at CH4 / N2 = 1.86. The tribological tests reveal that the wear of the coatings increases with an increasing CH4 flow rate, whereas the coefficient of friction decreases. This observed contradiction is explained by a phenomenon described as the effect of Rebinder.
In this study, heat-treated and multisurface engineered DIN 1.2367 tool steel was subjected to room and elevated temperature wear tests, and the effect of nitriding on its tribological behavior was investigated. CrN, AlTiN, and CrN/AlTiN coatings with a total thickness of 2 µm were obtained by arc cathodic physical vapor deposition on conventional heat-treated and gas-nitrided steels. The white layer formed during nitriding was removed, and a diffusion layer (100 µm) was achieved in the cross section of the steel having a tempered martensitic matrix. The highest surface hardness was attained with an integral coating (CrN/AlTiN), and surface hardness increased even more after nitriding due to the formation of a multicomponent ceramic layer on top of the diffusion layer. The room temperature wear tests performed against an alumina counterpart revealed that (i) CrN/AlTiN-coated steel had the highest friction coefficient of 0.26, which further increased to 0.33 by nitriding due to the increase in shear strength, and that (ii) with increasing surface hardness, the specific wear rates (W) of the heat-treated and coated steels could be ranked as follows: WCrN/AlTiN < WAlTiN < WCrN. The wear rates decreased when nitriding was carried out prior to coating. In order to simulate the aluminum extrusion conditions, hot wear behavior of the surfaces against AA6080 alloy at 450 °C was investigated. The hot wear tests revealed that (i) high friction coefficients were reached due to the adhesive characteristic of aluminum to the surfaces, (ii) the nitrided and CrN/AlTiN-coated sample exhibited the lowest wear rate among all studied surfaces, and (iii) the film damage on the worn surfaces mostly occurred in the form of droplet delamination.
A necklace structure composed of fine grains formed by dynamic recrystallization was uncommonly observed at the pre-existing grain boundaries during the hot compression of a BCC Fe-25Al-1.5Ta alloy containing C14 - (Fe, Al)2Ta Laves phase precipitates. Two possible mechanisms for necklace formation were proposed; particle-stimulated nucleation and grain boundary bulging, depending on whether the original grain boundaries are occupied by C14 particles, or they are free of them. Recrystallization was initiated preferentially around the clusters of large particles at the boundaries containing particles. In contrast, the bulging of the original grain boundaries by strain-induced boundary migration was observed as a preliminary stage for necklace formation at the particle-free boundaries. The necklace structure expanded into the deformed volume in such a way that low-angle subgrain boundaries decorating the necklace layers transformed into grains with increasing deformation strain.
The influence of milling time on the tribological behavior of a Co–Cr–Mo alloy designed for biomedical applications, synthesized via mechanical alloying is investigated. Elemental Co, Cr and Mo powders are milled using different milling times (2, 6, 12 and 18 h) in a high-energy ball mill. The resulting powders were subjected to cold uniaxial and hot isostatic pressing respectively, followed by sintering to obtain cylindrical samples, which were evaluated for their structural, mechanical and the wear behavior. Results showed that the grain and crystallite sizes of the powders decreased with increasing milling time, reaching low values of <10 μm and 32 μm respectively, at higher milling times. Furthermore, the wear rates and the coefficients of friction were lower, at higher milling times due to high densities (96%), and higher elasto-plastic resistance, as presented by the H/E and H3/E2 values of 0.026 and 0.0021 GPa, respectively. Increased milling time enables the refinement of grains and reduction in porosity in the Co–Cr–Mo alloy, which in turn increases the alloy's elasto-plastic resistance and enhances its wear resistance.
In the present work, a combined process of laser powder bed fusion (LPBF) and hot working in terms of microstructure refinement was investigated for Fe-25Al-1.5Ta alloy samples. Uniaxial compression tests were carried out parallel and perpendicular to the building direction (BD) at 1000 °C, where BCC A2-phase was stable, at a strain rate of 0.0013 s−1. The true stress–true strain curves indicated a broad flow stress peak followed by a slight decrease, which is typical for dynamic recrystallization (DRX) of conventional BCC metals such as ferritic iron. A negligible dependence in the flow stress behavior on the compression direction was observed. DRX initiated at a stress of 18.7 MPa for the sample compressed parallel to the BD, corresponding to a true strain of 0.011, and at 18.1 MPa for the samples compressed normal to the BD, which corresponded to a true strain of 0.010. The microstructural investigations by electron backscatter diffraction (EBSD) showed that the relatively coarse and elongated grains of the as-LPBF builds were significantly refined after hot working. The microstructure of the compressed samples mainly consisted deformed grains. These were fragmented by sub-grains bounded by low-angle boundaries independent of the compression axis, indicating the occurrence of dynamic recovery (DRV) during hot working. In addition, a few equiaxed, small grains were observed in the pre-existing grain boundaries, which formed due to DRX. Most pores in the as-LPBF builds were closed after hot compression, particularly in the central region of the deformed specimens where the compressive stress state is dominant. In summary, hot compression reveals a practical thermomechanical post-processing treatment for Fe-Al-Ta iron aluminides built by LPBF. The hot working refines the epitaxially elongated microstructure of the as-LPBF builds by DRV/DRX and reduces the porosity.
Nowadays, the recycled fine aggregate sourced from construction and demolition waste is not frequently used in manufacturing of epoxy resin coatings. Therefore, the main novelty of the article is to prepare green epoxy resin coatings modified with recycled fine aggregate in a replacement ratio of natural fine aggregate ranged from 20 to 100%. The microstructural properties of the aggregates and epoxy resin were analyzed using micro-computed tomography, scanning electron microscopy and nanoindentation. The macroscopic mechanical properties were examined using pull-off strength tests. The highest improvement of the mechanical properties was observed for epoxy resin coatings modified with 20% of natural fine aggregate and 80% of recycled fine aggregate. It has been found that even 100% of natural fine aggregate can be successfully replaced using the recycled fine aggregate with consequent improvement of the pull-off strength of analyzed epoxy resin coatings. In order to confirm the assumptions resulting from the conducted research, an original analytical and numerical failure model proved the superior behavior of modified coating was developed.
Ultrasonic probes for high-temperature applications are provided with metallic wedges, which can withstand the contact with the high temperature of the inspected structure. The ultrasonic signal travels within the wedge and gets reflected from its boundaries, causing interference signals called “ghost echoes”. The current work presents an investigation of the additional damping effect provided by porous sintered metal plates applied onto the surface of the wedge. In particular, the study evaluates the effect of damping plate thickness on the interference signal level at different transmission frequencies. Damping plates made of sintered metal SIKA-R 15 AX were attached to a wedge prototype made of steel 1.4301. The study revealed, that the most effective thickness of damping plates in the selected frequency interval of 1 to 4 MHz is equal to 4 mm. The evaluation of the interference signal has shown that the application of such damping plates to the wedge surface contributes to an additional attenuation of an interference signal of 10 to 30 dB after 500 µs of signal propagation.
The paper presents the characteristics of Ti-Mo-xTiC composites manufactured under experimentally selected conditions using the upgraded field-assisted sintering technique (U-FAST). Mixtures of microstructural titanium powders and nc-Ti0.9Mo0.1C/C carbide powders protected from oxidation by a carbon shell were subjected to sintering. The powders with nc-Ti0.9Mo0.1C/C contents of 10 and 20 wt% were used. The content of carbon forming the carbon shell was approximately 3 or 40 wt%. Composites with near full density were reinforced with titanium carbides in a Ti-Mo matrix. The composites with the highest content of reinforcing phase are characterized by the highest values of hardness, Young's modulus and wear resistance. Although the hardness of these composites is similar to that of ceramics, their nature is not brittle. Despite the high value of the Young's modulus, the addition of hard particles of the reinforcing phase to the titanium matrix significantly increases the values of the H/E ratio of the composites compared to the reference samples of cp-Ti and Ti6Al4V. A comparison of the research results for the composites with the highest share of titanium carbides showed that lowering the sintering temperature from 1300 to 1150 °C resulted in the inhibition of grain growth, a reduction in composite heterogeneity, composite roughness and hardness as well as a rise in the Young's modulus. An increase in the sintering temperature from 1150 to 1300 °C contributed to the higher high angle grain boundaries (HAGB) content.
Microhardness variations across the friction stir welded (FSW) and impulse friction stir welded (IFSW) AA2024–T351 joints have been elucidated by the transformations of the S–Al2CuMg phase with a special focus on a distinguished hardness peak within the heat-affected zone (HAZ) of the impulse welds. The increase in hardness within the stir zone (SZ) originated from the partial re-precipitation of the initial Guinier-Preston-Bagaryatsky zones (GPB) and metastable S needles, previously dissolved.) Formation and growth of stable S precipitates via coalescence accounted for the softening through the thermo-mechanically affected zone (TMAZ). The peak strengthening within the HAZ of the IFSW joints was mainly caused by the dense needle-shaped S particles, which can be explained by a mutual influence of the process specific temperature and strain cycles. Dislocations and subgrain boundaries introduced to the material due to plastic deformation facilitated the nucleation of strengthening S precipitates in the HAZ. It demonstrates that the impact of deformation should be considered by the characterization of the precipitation development in the HAZ.
CrNx coatings were deposited at high rates (100–130 nm/min) using hot Cr target magnetron sputtering enhanced by a radio-frequency inductively coupled plasma (RF-ICP) source in an Ar + N2 atmosphere. Besides separation of inert and reactive atmosphere, the RF-ICP source can be an effective tool for ion assistance in case of coating growth and to tailor film parameters. The effects of nitrogen flow rate and substrate bias potential on microstructure and functional properties of the CrNx coatings were investigated. An increase in nitrogen flow rate favored the formation of a looser microstructure of the coatings, while substrate biasing had the opposite effect. The functional properties were strongly dependent on the phase composition of the CrNx coatings. The change in coating microstructure significantly affected hardness, elastic modulus, adhesion, friction coefficients and corrosion resistance. The results indicated that ion assistance can be a key feature for regulating functional properties in the considered type of coating deposition. Cr2N and CrN compound coatings with high hardness (∼20 GPa) and low corrosion current density (icorr ∼ 3–5·10−9 A/cm2) in a 3.5 wt% NaCl solution were obtained by high-rate deposition.
The objective of this work is to investigate the strain localization
and slip activation of the microstructure of oligo-crystalline 316LVM steel struts evolving during different cyclic bending deformation stages (number of cycles) and loading conditions (maximum stress and neutral). A micro-scale three-point bending fixture was designed and incorporated into a micro tensile/compression machine inside a scanning electron microscope (SEM) to perform in-situ electron backscatter diffraction (EBSD) measurements during different phases of cyclic fatigue testing. The following results were obtained:
1) The quantitative strain could be compared after each stage of
deformation.
2) The rotation of the grains orientations is observed during the cyclic deformation while the morphology did not change significantly. The results contribute to the understanding of the evolution of the microstructure at low strain variations under bending fatigue conditions, and can support the prediction of the fatigue life of 316LVM stainless steel oligocrystalline microdevices like coronary artery stents.
Impulse Friction Stir Welding (IFSW) was utilized to join 6082–T6 alloy plates at various impulse frequencies. A distinctive feature of IFSW is the generation of mechanical impulses that enhances the forging action of the tool, and thereby, alters the weld microstructure. The microstructural evolution in the Stir Zone (SZ) with special focus on the strengthening precipitation behavior, and overall mechanical properties of the IFSW joints have been investigated. It was demonstrated that the strengthening β″ precipitates reprecipitated in the SZ of the IFSW joints during natural aging. In contrast, no precipitates were found in the SZ of the Friction Stir Welding (FSW) weld. Partial reversion of β″ after IFSW is supposed to occur due to more developed subgrain network and higher dislocation density introduced by impulses that accelerated precipitation kinetics. Dynamic recrystallisation was facilitated by impulses resulting in a fine, homogeneous structure. There was no significant difference between the microhardness in the SZ, tensile and yield strength of the FSW and IFSW joints. However, the application of impulses demonstrated the smoothing of the hardness reduction in the transition region at the advancing side. The shift of the fracture location from the Heat-Affected Zone (HAZ) by FSW to the SZ as well as higher elongation of the joints by IFSW of lower frequencies could be related to the grain refinement and the change of the grain orientation.
The effect of milling time on the microstructure and mechanical properties of Ti-6Al-4Fe alloys
(2021)
Replacement of toxic and expensive vanadium (V) in medical grade titanium alloys with cheaper and non-toxic elements such as iron (Fe) or niobium (Nb), is an important step forward in developing safer and less expensive biomaterials. Evaluating the effect of different process parameters such as the milling time on the properties of these newly developed alloys helps in understanding and controlling their behavior. Hence, in this study, the influence of ball-milling duration (2, 6, 8, 12 and 18 h) on crystalline structure, phase evolution, densification, and mechanical characteristics of biomedical nanocrystalline Ti-6Al-4Fe (wt. %) alloys is investigated. X-ray diffraction (XRD) confirmed that after 6 h of milling, aluminum (Al) and Fe completely dissolved into Ti matrix to form a solid solution of Ti (Al, Fe). XRD further revealed that the crystallite size decreased from 56 to 30 nm and the micro-strain increased with an increase in milling time. A decrease in porosity along with an increase in density is also observed for the alloys with increasing milling time. Moreover, the values of porosity obtained for the developed Ti-6Al-4Fe alloys ranged from 1 to 12 %, which is comparable to the porosity of one of the cortical bones making it a potential candidate for bone replacements. Microhardness measurements showed that the hardness of the Ti-6Al-4Fe alloys was greater than the hardness of the conventional Ti-6Al-4V alloys. It was observed that the Ti-6Al-4Fe alloy fabricated with the powders milled for 2 h showed the lowest value of Young’s Modulus. Milling time also had a significant effect on the surface roughness of the alloy samples, which showed a decreasing trend with increasing milling times.