Search Results (85)

The Mixed-Conduction Model for oxide films is used to quantitatively interpret in situ electrochemical and ex situ surface analytical results on the corrosion of AISI 316L (an internal reactor material) and Alloy 690 (a steam generator tube material) in small modular reactor primary coolant with the addition of soluble Zn. The model parameters of alloy oxidation and corrosion release are estimated with the time of exposure up to 168 h and anodic polarization potential (up to −0.25 V vs. standard hydrogen electrode) using fitting of the transfer function to experimental impedance spectra. Model parameters of individual alloy constituents are estimated by fitting of the model equations to the atomic fraction profiles of respective elements in the formed oxide obtained by Glow-Discharge Optical Emission Spectroscopy (GDOES). Conclusions on the effect of Zn addition on film growth and cation release processes in boron-free SMR coolant are drawn and future research directions are outlined. Full article

Tool steels are critical for high-load applications, e.g., forging and metal-forming, where they face thermal cracking, fatigue, erosion, and wear. This study evaluates the impact of gas nitriding and S-phase PVD coatings on the mechanical and tribological properties of four tool steels: 40CrMnNiMo8-6-4, 60CrMoV18-5, X50CrMoV5-2, and X38CrMoV5-3. Samples were heat-treated (quenched and tempered at 600 °C), then gas-nitrided at 575 °C for 6 h with nitriding potentials (Kn) of 0.18, 0.79, or 2.18, or coated via reactive magnetron sputtering in Ar/N₂ or Ar/N₂/CH₄ atmospheres at 200 °C or 400 °C. Characterization involved XRD, LOM, FE-SEM, GDOES, Vickers hardness (HV0.1), and ball-on-disk wear testing with Al₂O₃_ counter-samples. Gas nitriding produced nitrogen diffusion layers (80–200 μm thick) and compound layers (ε-Fe_(2-3)N, γ’-Fe₄N) at higher Kn, increasing hardness by 80–100% (up to 1100 HV0.1 for steel X38CrMoV5-3). S-phase coatings (1.6–3.6 μm thick) formed expanded austenite with varying N content, achieving comparable hardness (up to 1100 HV0.1) in high-N₂ atmospheres, alongside substrate diffusion layers. Both types of treatment enhance load-bearing capacity, adhesion, and durability, offering superior wear resistance compared to conventional PVD coatings and addressing demands for extended tool life in industrial applications. Full article

This study systematically investigates the effect of hydrogen flow rate (100, 200, 300, and 400 sccm) on the properties of DC53 steel during a 4 h plasma nitriding process conducted at 400 °C in an asymmetric bipolar pulsed reactor. A comprehensive characterisation approach was employed. X-ray diffraction (XRD) was used to identify the phase composition, revealing the formation of a compound layer consisting of ε-Fe_2–3N (identified by its (100), (101), and (102) planes) and γ’-Fe₄N (identified by its (220) plane). Mechanical properties were assessed using Vickers microhardness for surface measurements and nanoindentation for depth profiling. Glow discharge optical emission spectroscopy (GD-OES) provided elemental depth analysis, while a ball-on-disk tribometer evaluated the tribological performance. The optimal treatment was achieved at a hydrogen flow rate of 200 sccm. This condition yielded a peak surface hardness of 1121.5 ± 69.2 HV_0.2. GD-OES analysis directly correlated this mechanical enhancement to a high surface nitrogen content of approximately 8.5% and an effective diffusion depth of about 50 µm. Full article

The effect of KOH concentration as a boron-free coolant for prospective use in Small Modular Reactors (SMRs) on the corrosion of Alloy 690 is studied by in situ impedance spectroscopy at 280 °C/9 MPa during 168 h exposure in a flow-through cell connected to a high-temperature/high-pressure loop. To follow further oxidation of the passive film, the samples were subsequently polarized up to potentials 0.5 V more positive than the corrosion potential. The formed oxides were analyzed ex situ by measuring the atomic concentration of the constituent elements via glow discharge optical emission spectroscopy (GDOES) depth profiling. The Mixed-Conduction Model for Oxide Films (MCM) was employed to quantitatively interpret the impedance results. The estimated parameters are used to quantify the influence of KOH concentration and anodic polarization on oxide formation and soluble product release rates. Results are compared to those obtained in the nominal primary chemistry of pressurized water reactors and indicate that Alloy 690 can also be successfully used as a steam generator tube material in SMRs. Full article

The impact of final surface preparation immediately prior to hydrogen content measurements in aluminum alloy samples was investigated using thermal desorption analysis (TDA). Samples ground in water showed an apparent hydrogen signal. Glow-discharge optical emission spectroscopy (GDOES) confirmed that the analyzed hydrogen originated from the subsurface layer. X-ray photoelectron spectroscopy (XPS) revealed the presence of a thin aluminum oxide/hydroxide layer on the surface. Formation of these compounds indicates that hydrogen was introduced into the material by the reaction of oxide-free aluminum with water molecules during the grinding, followed by its entrapment at near-surface interstitial lattice sites. Chemical pickling in concentrated nitric acid and combined grinding, chemical pickling, and electrochemical polishing approaches are proposed as proper surface-preparation techniques for samples without and with adherent corrosion products, respectively. Full article

In the present paper, impedance spectroscopy was employed to study the corrosion and anodic oxidation of stainless steel (AISI 316L at 280 °C/9 MPa) in contact with the boron-free primary coolant of a small modular reactor at two levels of KOH concentration. Analysis of impedance spectra with a distribution of relaxation times revealed contributions from the oxide layer and its interface with the coolant. Glow-Discharge Optical Emission Spectroscopy (GDOES) was used to estimate the thickness and elemental composition of the formed oxides. A quantitative interpretation of the impedance data using the Mixed-Conduction Model allowed us to estimate the kinetic and transport parameters of oxide growth and dissolution, as well as iron dissolution through oxide. The film thicknesses following exposure agreed with ex-situ analyses. The obtained corrosion and release rates were used for comparison with laboratory and industrial data in nominal pressurized water reactor primary coolants. Full article

Glow discharge optical emission spectroscopy (GDOES) is a powerful and well-established method of elemental analysis of metals, coatings and surface-modified materials. This review contains essential information needed to establish and successfully run a GDOES laboratory and perform accurate, quantitative GDOES analyses. The basics of the methodology, instrumentation and analytical interpretation of experimental data are presented, and examples of typical depth profiling applications are given. Special attention is paid to application-specific calibrations, their assumptions and prerequisites. The calibration model of GDOES is special; besides the composition of calibration samples, their sputter rates (sputter factors) need to be accounted for. Typical analytical performance of GDOES is discussed (precision, accuracy), as well as the depth quantification in depth-profiling applications. Links to some other methods, complementary to GDOES, are mentioned, including the type and the character of analytical information each method can deliver. Full article

The advancement of additive manufacturing (AM) technologies, particularly laser powder bed fusion (LPBF), has enabled the production of complex components with enhanced mechanical properties and shorter lead times compared to conventional manufacturing processes. This study focuses on the characterization of maraging steel (EOS MS1) fabricated by LPBF technology using an EOS M 290 system. Three material groups were investigated: a conventionally manufactured tool steel (95MnWCr5) serving as a reference, LPBF-produced maraging steel in the as-built condition, and LPBF-produced maraging steel subjected to post-processing heat treatment. The samples were thoroughly examined using optical microscopy, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), glow discharge optical emission spectroscopy (GDOES), electrochemical corrosion analyses in a 3.5% NaCl solution, and Vickers microhardness measurements. Electrochemical tests revealed that heat-treated LPBF maraging steel samples exhibited slightly increased corrosion current densities relative to their as-built counterparts, attributed to the formation of Ti-rich and Ni-rich precipitates during aging, creating localized microgalvanic cells. Despite the increased corrosion susceptibility, hardness measurements clearly demonstrated enhanced hardness and mechanical properties in heat-treated samples compared to the as-built state and conventional tool steel reference. The findings underscore the importance of optimized LPBF parameters and controlled post-processing heat treatments in balancing mechanical performance and corrosion resistance. Consequently, LPBF-produced maraging steels hold considerable promise for tooling and industrial applications where high strength, dimensional stability, and acceptable corrosion behavior are required. Full article

This paper reports on the successful preparation of a low absorption–emission thermal control coating on the surface of LAZ933 magnesium–lithium alloy using the micro-arc oxidation method. This study analyzed the microstructure, phase composition, and thermal control properties of the coating using Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), UV–visible near-infrared spectroscopy (UV-VIS-NIR) and infrared emissivity measurements. The results indicate that the hemispherical emissivity of the coating remains unaffected with an increase in temperature and holding time, while the solar absorption ratio gradually increases. The thermal control performance of the coating after a high-temperature experiment was found to be related to the diffusion of the Li metal element in the magnesium lithium alloy matrix, as determined by X-ray photoelectron spectroscopy (XPS), flame graphite furnace atomic absorption spectrometry (GFAAS) and Glow Discharge Optical Emission Spectroscopy (GD-OES). As the holding time is extended, the coating structure gradually loosens under thermal stress. The Li metal element in the substrate diffuses outward and reacts with O₂, H₂O and CO₂ in the air, forming LiO₂, LiOH, Li₂CO₃ and other products. This reaction affects the coating’s solar absorption ratio in the end. Full article

The use of low-carbon unalloyed steel with minimal silicon content is widespread in structural steel and automotive applications due to its ease of manipulation. The mechanical properties of this steel can be significantly enhanced through severe plastic deformation (SPD) techniques. Our study focuses on the practical benefits of the dual rolling equal channel extrusion (DRECE) method, which strengthens the steel and has implications for material hardness and the thickness of subsequently applied hot-dip zinc galvanizing. Furthermore, the steel’s corrosion potential and current are investigated as a function of material hardness and thickness. The findings show a 20% increase in hardness HV 30 after the first run through the forming machine, with an additional 10% increase after the second run. Subsequent galvanizing leads to a further 1–12% increase in HV 30 value. Notably, the DRECE hardening demonstrates no statistically significant effect on the corrosion potential and current; however, the impact of galvanizing is as anticipated. Full article

This study presents research into the unique method of depositing carbon layers onto processed surfaces, during finishing with abrasive films, on a global basis. The authors of this article are holders of the patent for this method. What makes this technology outstanding is that it integrates processes, whereby micro-finishing and the deposition of a carbon layer onto freshly exposed surface fragments is achieved simultaneously, in a single process. Among the main advantages accruable from this process is the reduction of surface irregularities, while the deposition of a carbon layer is achieved simultaneously. Ultrathin graphite layers can be widely used in conditions where other methods of reducing the coefficient of friction are not possible, such as in regard to micromechanisms. This article illustrates the application of carbon coating, end on, on a surface processed with abrasive film, containing intergranular spaces, saturated with graphite. Thin carbon layers were obtained on two substrates that did not contain carbon in their initial composition: soda–lime glass and a tin–bronze alloy. It was performed through microscopic examinations of the produced surface, roughness analyses of these surfaces, and analysis of the chemical compositions determined by two methods, namely EDS and GDOES, proving the existence of the coatings. The aim of this paper is to prove the possibility and efficiency of using graphite-impregnated lapping films in the deposition process of carbon films, with improved surface smoothness, durability, and wear resistance. The produced coatings will be tested in regard to their operational properties in further research. The authors underline the potential of this method to revolutionize surface treatment processes, due to the significant advantages it offers across various industries. Full article

Electrolytic capacitors store larger amounts of energy thanks to their thin dielectric layers and enlarged surface area. However, the benefits of using a liquid electrolyte are at the expense of the possibility of leakage, evaporation, or rupture of the device over time. As a solution, solid electrolytes, such as conductive polymers, substitute the liquid ones decreasing the internal resistance and enlarging the lifetime of these devices. PEDOT:PSS is a widely used conductive polymer in the formation of solid electrolytic capacitors. However, using the enlarged surface of the porous electrodes efficiently requires industrial processes, the efficacy of which has not been explored. In this work, porous aluminium electrodes with dielectric layers of different thicknesses were coated with PEDOT:PSS at different levels of doping in order to study the efficiency of the production of solid electrolytic capacitors in industry. The combination of odd random phase electrochemical impedance spectroscopy (ORP-EIS) with surface characterization techniques (SEM-EDX, GDOES) formed a methodology that allowed the study of both the electrical properties and the level of impregnation for these model systems. All samples consisting of a porous aluminium electrode with an amount of PEDOT:PSS deposited on top resulted in an inefficient degree of penetration between the two electrodes. However, the electrochemical analysis proved that the use of dopants produces systems with the highest capacitive properties. Consequently, the evolution towards better solid electrolytic capacitors does not rely solely on the proper coverage of the porous electrodes, but on the proper electrical properties of the PEDOT:PSS within the pores. Full article

Low friction and high wear resistance are critical properties for sliding bearings. In this research, advanced Cu/GO nanocomposite coatings have been developed by a brush plating method to improve the tribological performance of brass-based sliding bearings. A series of brush plating studies under voltages from 2 to 6 V with different GO concentrations (0.2–0.8 g/L) was conducted, and the coating microstructures were characterised by SEM, EDX, GDOES and XRD and the tribological behaviour of the Cu/GO composite coatings were evaluated using dry ball-on-plane tribological tests The experimental results have demonstrated that GO can be successfully introduced into the whole composite coating layer; the Cu/GO composite coatings can reduce the friction of brass and increase its wear resistance by two orders of magnitude, mainly due to the self-lubricating GO added into the coatings. Full article

This paper deals with the evaluation of the surface of structural steel whose samples were deliberately contaminated with transparent spray primer, adhesive label glue, and welding sprays prior to hot-dip galvanizing. The galvanized samples were studied by optical microscopy, GDOES, adhesion tests, and condensation humidity tests. The effect of surface contamination on the quality of the zinc coating was found to be significant. In some cases, the zinc coating is damaged (after contamination with welding sprays), in others, it is completely absent (after contamination with spray primer or adhesive label glue). Full article

In the present paper, the effect of the evolution of primary water chemistry during power operation on the corrosion rate and conduction mechanism of oxide films on stainless steel is studied by in situ impedance spectroscopy at 300 °C/9 MPa during 1-week exposure periods in an autoclave connected to a recirculation loop. At the end of the exposure period, the samples were anodically polarized in a wide range of potentials to evaluate the stability of the passive oxide. Separate samples of the same steel were simultaneously exposed to the coolant and subsequently analyzed by glow discharge optical emission spectroscopy (GDOES) in order to estimate the thickness and the in-depth composition of the formed oxides. Impedance data were quantitatively interpreted using the mixed-conduction model for oxide films (MCM) to estimate the rates of metal oxidation at the alloy/oxide interface, oxide dissolution and restructuring at the film/coolant interface, and ion transport in the protective corrosion layer. Full article