Search Results (17)

One of the most effective methods of improving the properties of aluminium alloys is grain refining using Al-Ti-B master alloys. In contrast, zirconium is a key alloying element, used mainly in 2xxx and 7xxx series aluminium alloys, where it contributes to dispersion enhancement and reduces the rate of dynamic recrystallisation. However, even trace amounts of zirconium—just a few hundredths of ppm—significantly reduce the performance of Al-Ti-B grain refiners, a phenomenon known as ‘Zr poisoning’. This study investigates the impact of holding time and the level of Al-5Ti-1B addition on the microstructure and properties of an AlMgSi(Cu) alloy containing 0.15 wt.% Zr, cast as 7-inch DC billets. The structure and phase distribution were characterised using optical microscopy (OM), scanning electron microscopy (SEM) with energy-dispersive spectroscopy (EDS), and transmission electron microscopy (TEM). Grain size and morphology were evaluated through macrostructure analysis (etched cross-sections and polarised light microscopy), while chemical and elemental distributions were analysed via SEM-EDS and STEM-EDS mapping. Additionally, Brinell hardness measurements were conducted across the billet diameter to assess the correlation between grain size and mechanical properties. The results show that reducing holding time and increasing the Al-5Ti-1B addition improves grain refinement efficiency despite the presence of Zr. The finest grain structure (150–170 μm) and most homogeneous hardness distribution were achieved when the grain refiner was continuously fed during casting at 80 ppm B. These findings are supported by the literature and contribute to a deeper understanding of the Zr poisoning effect and its mitigation through optimized casting practice. Full article

In the present study, (Cr,Al)N nanolayer coatings with different Al/Cr atomic ratios were deposited by magnetron sputtering on different substrate materials (H11 and D2 tool steel, alumina). To prepare the (Cr,Al)N coatings with different Al/Cr atomic ratios in the same batch, we used two targets composed of two triangle-like segments together with two standard Al and Cr targets. This approach enabled us to study the evolution of structural and mechanical properties in dependence on composition. The elemental composition of the coatings was determined by energy-dispersive X-ray analysis (EDS). The phase composition of the (Cr,Al)N coatings was determined utilizing X-ray diffraction (XRD), while scanning electron microscopy (SEM) was employed to assess their morphology and microstructure. The coating surface topography was analyzed by atomic force microscopy (AFM). In order to evaluate the effect of the Al/Cr atomic ratio on the oxidation behavior, the (Cr,Al)N coatings were oxidized in ambient atmospheres at temperatures between 700 and 850 °C and subsequently analyzed by means of cross-sectional SEM and transmission electron microscopy (TEM). The oxidation rate, determined by weight gain over time, was utilized to quantify the oxidation process. The oxidation tests showed that the Al-rich (Cr,Al)N nanolayer coatings exhibit a considerably better oxidation resistance than the Cr-rich ones. We found that the oxide scale formed on the Al-rich coating is composed of double layers: a Cr-oxide top layer and an inner (Cr,Al) mixed oxide layer. In contrast, the oxide scale of the Cr-rich coating mainly consists of the Cr₂O₃ layer. In particular, we focused on the oxidation process occurring at the locations of growth defects. We noticed that the first oxidation products on the coated substrate occurred at a temperature that was much lower than the temperature for the (Cr,Al)N coating oxidation initiation. These products (iron oxides) formed only at the sites of those growth defects that extended through the entire coating thickness. Full article

The exceptional property of plasmonic materials to localize light into sub-wavelength regimes has significant importance in various applications, especially in photovoltaics. In this study, we report the localized surface plasmon-enhanced perovskite solar cell (PSC) performance of plasmonic gold nanoparticles (AuNPs) embedded into a titanium oxide (TiO₂) microdot array (MDA), which was deposited using the inkjet printing technique. The X-ray (XRD) analysis of MAPI (methyl ammonium lead iodide) perovskite films deposited on glass substrates with and without MDA revealed no destructive effect of MDA on the perovskite structure. Moreover, a 12% increase in the crystallite size of perovskite with MDA was registered. Scanning electron microscopy (SEM) and high-resolution transmission electron microscopy (HR-TEM) techniques revealed the morphology of the TiO₂_MDA and TiO₂-AuNPs_MDA. The finite-difference time-domain (FDTD) simulation was employed to evaluate the absorption cross-sections and local field enhancement of AuNPs in the TiO₂ and TiO₂/MAPI surrounding media. Reflectance UV-Vis spectra of the samples comprising glass/TiO₂ ETL/TiO₂_MDA (ETL—an electron transport layer) with and without AuNPs in TiO₂_MDA were studied, and the band gap (E_g) values of MAPI have been calculated using the Kubelka–Munk equation. The MDA introduction did not influence the band gap value, which remained at ~1.6 eV for all the samples. The photovoltaic performance of the fabricated PSC with and without MDA and the corresponding key parameters of the solar cells have also been studied and discussed in detail. The findings indicated a significant power conversion efficiency improvement of over 47% in the PSCs with the introduction of the TiO₂-AuNPs_MDA on the ETL/MAPI interface compared to the reference device. Our study demonstrates the significant enhancement achieved in halide PSC by utilizing AuNPs within a TiO₂_MDA. This approach holds great promise for advancing the efficiency and performance of photovoltaic devices. Full article

Equiatomic medium-entropy alloy (MEA) FeNiCr-B₄C (0, 1, and 3 wt.% B₄C) coatings were deposited onto an AISI 1040 steel substrate using pulsed laser cladding. Based on an SEM microstructural analysis, it was found that the cross-sections of all the obtained specimens were characterized by an average coating thickness of 400 ± 20 μm, a sufficiently narrow (100 ± 20 μm) “coating–substrate” transition zone, and the presence of a small number of defects, including cracks and pores. An XRD analysis showed that the formed coatings consisted of a single face-centered cubic (FCC) γ-phase and the space group Fm-3m, regardless of the B₄C content. However, additional TEM analysis of the FeNiCr coating with 3 wt.% B₄C revealed a two-phase FCC structure consisting of grains (FCC-1 phase, Fm-3m) up to 1 µm in size and banded interlayers (FCC-2 phase, Fm-3m) between the grains. The grains were clean with a low density of dislocations. Raman spectroscopy confirmed the presence of B₄C carbides inside the FeNiCr (1 and 3 wt.% B₄C) coatings, as evidenced by detected peaks corresponding to amorphous carbon and peaks indicating the stretching of C-B-C chains. The mechanical characterization of the FeNiCr-B₄C coatings specified that additions of 1 and 3 wt.% B₄C resulted in a notable increase in microhardness of 16% and 38%, respectively, with a slight decrease in ductility of 4% and 10%, respectively, compared to the B₄C-free FeNiCr coating. Thus, the B₄C addition can be considered a promising method for strengthening laser-cladded MEA FeNiCr-B₄C coatings. Full article

The microstructure and surface topography of PVD hard coatings are among the most important properties, as they significantly determine their mechanical, tribological and other properties. In this study, we systematically analyzed the microstructure and topography of a TiAlN/CrN nanolayer coating (NL-TiAlN/CrN), not only because such coatings possess better mechanical and tribological properties than TiAlN and CrN monolayer coatings, mainly because the contours of the individual layers, in the cross-sectional STEM or SEM images of such coatings, make it easier to follow topographic and microstructural changes that occurred during its growth. We investigated the effects of the substrate rotation modes on the microstructure and surface topography of the NL-TiAlN/CrN coating, as well as on the periodicity of the nanolayer structure. The influence of the substrate material and the ion etching methods were also studied, while special attention was given to the interlayer roughness and influence of non-metallic inclusions in the steel substrates on the growth of the coating. The topographical features of the NL-TiAlN/CrN coating surface are correlated with the observations from the cross-sectional TEM and FIB analysis. Selected non-metallic inclusions, covered by the NL-TiAlN/CrN coating, were prepared for SEM and STEM analyses by the focused ion beam. The same inclusions were analyzed prior to and after deposition. We found that substrate rotation modes substantially influence the microstructure, surface topography and periodicity of the NL-TiAlN/CrN layer. Non-metallic inclusions in the substrates cause the formation of shallow craters or protrusions, depending on their net removal rates during the substrate pretreatment (polishing and ion etching), as compared to the matrix. Full article

The aim of the present study was the development of Nb-doped ITO thin films for carbon monoxide (CO) sensing applications. The detection of CO is imperious because of its high toxicity, with long-term exposure having a negative impact on human health. Using a feasible sol–gel method, the doped ITO thin films were prepared at room temperature and deposited onto various substrates (Si, SiO₂/glass, and glass). The structural, morphological, and optical characterization was performed by the following techniques: X-ray diffractometry (XRD), atomic force microscopy (AFM), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV/Vis/NIR spectroscopic ellipsometry (SE). The analysis revealed a crystalline structure and a low surface roughness of the doped ITO-based thin films. XTEM analysis (cross-sectional transmission electron microscopy) showed that the film has crystallites of the order of 5–10 nm and relatively large pores (around 3–5 nm in diameter). A transmittance value of 80% in the visible region and an optical band-gap energy of around 3.7 eV were found for dip-coated ITO/Nb films on SiO₂/glass and glass supports. The EDX measurements proved the presence of Nb in the ITO film in a molar ratio of 3.7%, close to the intended one (4%). Gas testing measurements were carried out on the ITO undoped and doped thin films deposited on glass substrate. The presence of Nb in the ITO matrix increases the electrical signal and the sensitivity to CO detection, leading to the highest response for 2000 ppm CO concentration at working temperature of 300 °C. Full article

Nickel tungsten alloy tapes (Ni—5 at% W, 10 mm wide, 80 µm thick, biaxially textured) used in second-generation high temperature superconductor (2G-HTS) technology were laser-processed in air with ultraviolet ps-laser pulses (355 nm wavelength, 300 ps pulse duration, 250–800 kHz pulse repetition frequency). By employing optimized surface scan-processing strategies, various laser-generated periodic surface structures were generated on the tapes. Particularly, distinct surface microstructures and nanostructures were formed. These included sub-wavelength-sized highly-regular hexagonally-arranged nano-protrusions, wavelength-sized line-grating-like laser-induced periodic surface structures (LIPSS, ripples), and larger irregular pyramidal microstructures. The induced surface morphology was characterized in depth by electron-based techniques, including scanning electron microscopy (SEM), electron back scatter diffraction (EBSD), cross-sectional transmission electron microscopy (STEM/TEM) and energy dispersive X-ray spectrometry (EDS). The in-depth EBSD crystallographic analyses indicated a significant impact of the material initial grain orientation on the type of surface nanostructure and microstructure formed upon laser irradiation. Special emphasis was laid on high-resolution material analysis of the hexagonally-arranged nano-protrusions. Their formation mechanism is discussed on the basis of the interplay between electromagnetic scattering effects followed by hydrodynamic matter re-organization after the laser exposure. The temperature stability of the hexagonally-arranged nano-protrusion was explored in post-irradiation thermal annealing experiments, in order to qualify their suitability in 2G-HTS fabrication technology with initial steps deposition temperatures in the range of 773–873 K. Full article

A series of Zeolitic imidazole framework-8 (ZIF-8) clusters supported on graphene oxide (ZIF-8@GO) nanocomposites were prepared by varying the ratios of ZIF-8 to GO. The resultant nanocomposites were characterized using various techniques, such as Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET), thermogravimetric analysis (TGA), Fourier Transform Infrared (FTIR) and Raman spectroscopy. These nanocomposites were incorporated into the thin film layer during interfacial polymerisation process of m-phenylenediamine (aqueous phase which contained the dispersed nanocomposites) and trimesoyl chloride (TMC, organic phase) at room temperature onto polyethersulfone (PES) ultrafiltration (UF) support membrane. The membrane surface morphology, cross section and surface roughness were characterized using SEM and AFM, respectively. Compared to the baseline membranes, the thin film nanofiltration (TFN) membranes exhibited improved pure water flux (from 1.66 up to 7.9 L.m⁻²h⁻¹), salt rejection (from 40 to 98%) and fouling resistance (33 to 88%). Optimum ZIF-8 to GO ratio was established as indicated in observed pure water flux, salt rejection and BSA fouling resistance. Therefore, a balance in hydrophilic and porous effect of the filler was observed to lead to this observed membrane behaviour suggesting that careful filler design can result in performance gain for thin film composite (TFC) membranes for water treatment application. Full article

This paper reports the sliding wear properties and wear mechanisms of Hadfield high-Mn austenitic steel in a dry-sliding reciprocal tribotest against a WC counterpart. The associated wear mechanisms were studied through extensive characterisation of the obtained worn surface using analytical SEM, TEM, XRD and micro-hardness test. The tribotest revealed a coefficient of wear in the scale of 10⁻¹⁴ m³·N⁻¹·m⁻¹ and a coefficient of friction of 0.5–0.6. The steel encountered severe plastic deformation beneath the worn surface leading to a gradient of hardness profile, including the extreme hardening of the worn surface up to HV_0.1 8.2 GPa. Despite the severe deformation and significant strain hardening, the steel still retained its austenitic structure without any detectable martensite. The combined surface and cross-sectional microscopic observations and extensive analysis of XRD peak breadth revealed the formation of nano-heterogeneous microstructure including nano-laminate, nanotwins and nanocrystalline beneath the worn surface. Spalling wear was found as the predominant wear mechanism. The spalling wear was caused by the embrittlement of the extremely hardened and nanocrystallised worn surface. Tribo-oxidation was also observed in the resultant wear debris. Full article

Wafer direct bonding is an attractive approach to manufacture future micro-electro-mechanical system (MEMS) and microelectronic and optoelectronic devices. In this paper, a combined hydrophilic activated Si/Si wafer direct bonding process based on wet chemical activation and O₂ plasma activation is explored. Additionally, the effect on bonding interface characteristics is comprehensively investigated. The mechanism is proposed to better understand the nature of hydrophilic bonding. The water molecule management is controlled by O₂ plasma activation process. According to the contact angle measurement and FTIR spectrum analysis, it can be concluded that water molecules play an important role in the type and density of chemical bonds at the bonding interface, which influence both bonding strength and voids’ characteristics. When annealed at 350 °C, a high bonding strength of more than 18.58 MPa is obtained by tensile pulling test. Cross sectional SEM and TEM images show a defect-free and tightly bonded interface with an amorphous SiO_x layer of 3.58 nm. This amorphous SiO_x layer will induce an additional energy state, resulting in a lager resistance. These results can facilitate a better understanding of low-temperature hydrophilicity wafer direct bonding and provide possible guidance for achieving good performance of homogenous and heterogenous wafer direct bonding. Full article

Plasma nitridation was conducted to modify the surfaces of Zircaloy-4. Scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Raman analysis were used to characterize microstructures and phases. Surface indentation and cross-sectional indentation were performed to evaluate mechanical property changes. Nitridation forms a thin layer of ZrN phase, followed by a much deeper layer affected by nitrogen diffusion. The ZrN phase is confirmed by both TEM and Raman characterization. The Raman peaks of ZrN phase show a temperature dependence. The intensity increases with increasing nitridation temperatures, reaches a maximum at 700 °C, and then decreases at higher temperatures. The ZrN layer appears as continuous small columnar grains. The surface polycrystalline ZrN phase is harder than the bulk by a factor of ~8, and the nitrogen diffusion layer is harder by a factor of ~2–5. The activation energy of nitrogen diffusion was measured to be 2.88 eV. The thickness of the nitrogen-hardened layer is controllable by changing the nitridation temperature and duration. Full article

A novel, high throughput method to characterize the chemistry of ultra-thin diamond-like carbon films is discussed. The method uses surface sensitive SEM/EDX to provide substrate-specific, semi-quantitative silicon nitride/DLC stack composition of protective films extensively used in the hard disk drives industry and at Angstrom-level. SEM/EDX output is correlated to TEM to provide direct, gauge-capable film thickness information using multiple regression models that make predictions based on film constituents. The best model uses the N/Si ratio in the films, instead of separate Si and N contributions. Topography of substrate/film after undergoing wear is correlatively and compositionally described based on chemical changes detected via the SEM/EDX method without the need for tedious cross-sectional workflows. Wear track regions of the substrate have a film depleted of carbon, as well as Si and N in the most severe cases, also revealing iron oxide formation. Analysis of film composition variations around industry-level thicknesses reveals a complex interplay between oxygen, silicon and nitrogen, which has been reflected mathematically in the regression models, as well as used to provide valuable insights into the as-deposited physics of the film. Full article

This paper presents results from the production of copper oxide layers on a Cu sheet substrate using diode and Yb:YAG disc lasers operating in the wavelength ranges of 808–940 nm and 1030 nm. The parameters of these layers were compared with the layer obtained in the thermal process of copper oxidation at 300 °C in an infrared (IR) furnace in a natural atmosphere. Investigations into the layers mentioned above, concerning their topography, chemical composition and roughness, were made using scanning electron microscopy (SEM) and atomic force microscopy (AFM). A hot-point probe was used to determine and check the type of conductivity of the copper oxide layers formed. The optical band gap energy was estimated by applying the Kubelka–Munk method based on spectrophotometric data. Cross-sections and the element distribution maps were made using transmission electron microscopy (TEM). The phase analysis was investigated by the X-ray diffraction method (XRD). In sum, controlled laser oxidations of copper sheets allow for the formation of a mixture of Cu₂O and CuO phases. The diode laser allows the production of a layer of copper oxides with a phase composition comparable to the oxides produced by the thermal oxidation method, while the distribution of high phase uniformity in the cross-section of the layer enables the process using a Yb:YAG disc laser. Full article

Molecular scale modifications were achieved by spontaneous polarization which is favored in enhancements of β-crystallization phase inside polyvinylidene fluoride (PVDF) nanofibers (NFs). These improvements were much more effective in nano and submicron fibers compared to fibers with relatively larger diameters. Metallic nanoparticles (NPs) supported by nanofibrous membranes opened new vistas in filtration, catalysis, and serving as most reliable resources in numerous other industrial applications. In this research, hydrogenation of phenol was studied as a model to test the effectiveness of polarized PVDF nanofiber support embedded with agglomerated palladium (Pd) metallic nanoparticle diameters ranging from 5–50 nm supported on polymeric PVDF NFs with ~200 nm in cross-sectional diameters. Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Atomic Force Microscopy (AFM), Energy Dispersive X-Ray Spectroscopy (EDX), Fourier Transform Infrared Spectroscopy (FTIR) and other analytical analysis revealed both molecular and surface morphological changes associated with polarization treatment. The results showed that the fibers mats heated to their curie temperature (150 °C) increased the catalytic activity and decreased the selectivity by yielding substantial amounts of undesired product (cyclohexanol) alongside with the desired product (cyclohexanone). Over 95% phenol conversion with excellent cyclohexanone selectivity was obtained less than nine hours of reaction using the polarized PVDF nanofibers as catalytic support structures. Full article

In this study, the effects of the microstructural properties on the deformation and damage mechanism of CrN/TiN multilayer coatings deposited on Custom 450 steel using the unbalanced reactive magnetron sputtering PVD process were studied. All coatings were fabricated with an overall thickness of 1.5 µm, but different bilayer periods (Λ). Structural and mechanical properties of coatings were investigated by XRD analysis and nanoindentation experiment, respectively. Indentation tests at three loads of 100, 300, and 450 mN were performed on the coatings’ surface and then, cross-sections of fractured imprints were analyzed with SEM and TEM. Measuring the length of the cracks induced by indentation loads and analyzing the load-displacement curves, apparent fracture energy values of multilayer coatings were calculated. We observed that multilayer systems with bilayer periods of 4.5–15 nm possess superlattice structure, which also results in higher values for Young’s modulus and hardness as well as higher fracture energy. Comparison of cross-sectional SEM and TEM observations showed that coatings with smaller bilayer periods tend to deform by shear sliding mechanism due to the existence of the long-grown columns, while short dispersed grains—growing in the coatings with a larger bilayer period—led to deformation via local grain boundary sliding and grain rotation. Full article