Search Results (16)

PVD hard coatings improve the wear and frictional properties in metal cutting and, therefore, extend the lives of cutting tools. Cutting fluids, including the novel use of liquid carbon dioxide (LCO₂), are crucial for reducing tool wear and enhancing machining efficiency. This experimental research is focused on ball-on-disc wear tests of TiAlN hard coatings in environmental, N₂ and CO₂ atmospheres. In the latter case, the experiments were also performed by adding LCO₂ directly into the contact zone. In order to achieve the same temperatures as real cutting conditions, tests were performed at 250 °C, 500 °C and 700 °C, in addition to room temperature. Results show that the TiAlN coating had the highest wear rate in room-temperature tests, regardless of the atmosphere. The wear significantly dropped with the test temperature. It was the lower in the CO₂ atmosphere at all temperatures than in all gas-only atmospheres. When LCO₂ was introduced to the contact, the wear was at its highest at 500 °C, which is the opposite of all other gas-only atmospheres, where it was at its lowest. In all tribological LCO₂ tests, we noticed increased friction coefficient fluctuations. In all gas-only atmospheres, adhered material was observed on the wear tracks, but in LCO₂, wear debris was not detected either on the disk or on the ball. Full article

In this study, we used the depth-sensing indentation technique to determine the cracking resistance of different PVD hard coatings deposited on tool steel substrates. By comparison, with the load–displacement curves, measured at the sites of carbide inclusion and a tempered martensite matrix in the D2 tool steel substrate surface, we observed different fracture mechanisms on TiAlN hard coating prepared by sputtering. Additional information about the deformation and fracture phenomena was obtained from the SEM images of FIB cross-sections of both types of indents. We found that the main deformation mechanism in the coating is the shear sliding along the columnar boundaries, which causes the formation of steps on the substrate surface under individual columns. Using nanoindentation test, we also analyzed the cracking resistance of a set of nl-(Cr,Al)N nanolayer coatings with different Cr/Al atomic ratios, which were sputter deposited in a single batch. From the indentation curves, we determined the loads (F_c) at which the first pop-in appears and compared them with the plasticity index H³/E². A good correlation of both parameters was found. We also compared the indentation curves of the TiAlN coating, which were prepared by cathodic arc evaporation using 1-fold, 2-fold and 3-fold rotation of the substrates. Additionally, on the same set of samples, the fracture toughness measurements were performed by micro-cantilever deflection test. The impact of growth defects on the cracking resistance of the hard coatings was also confirmed. Full article

Reports of the influence of surface roughness on the adhesion and tribological performance of contemporary nitride coatings with different layer designs are still scarce in the literature. Therefore, in this study, we evaluated the behavior of a single-layer TiAlN, a bilayer TiAlN/CN_x, and a nanolayer AlTiN/TiN coating. Coatings were deposited in an industrial magnetron sputtering unit on the substrates of EN 100Cr6 steel, prepared to four degrees of surface roughness (Sa = 10–550 nm). The coatings’ adhesion was determined by scratch tests performed perpendicular and parallel to the machining marks. Dry reciprocating sliding tests in air were employed to evaluate the coatings’ tribological behavior against an Al₂O₃ ball. Before and after the tests, coating properties were characterized by 3D profilometry, confocal microscopy, and energy dispersive spectroscopy. Deposition of all coatings significantly altered the surface topography and increased the roughness of the samples. No general rule could be established for the effect of surface roughness on tribological behavior and adhesion of different hard coatings. For very fine surface finishes the adhesion and tribological performance of TiAlN and TiAlN/CN_x coatings was independent of the surface roughness. For the roughest surfaces, a decrease in adhesion and an increase in the wear rate were observed. The AlTiN/TiN coating exhibited the largest sensitivity of adhesion to roughness and scratching direction. The coefficient of friction and wear rate increased when AlTiN/TiN roughness exceeded Sa ≈ 100 nm. Full article

This paper presents a study and comparison of surface effects induced by picosecond and nanosecond laser modification of a Ti6Al4V alloy surface under different ambient conditions: air and argon- and nitrogen-rich atmospheres. Detailed surface characterization was performed for all experimental conditions. Damage threshold fluences for picosecond and nanosecond laser irradiation in all three ambient conditions were determined. The observed surface features were a resolidified pool of molten material, craters, hydrodynamic effects and parallel periodic surface structures. Laser-induced periodic surface structures are formed by multi-mode-beam nanosecond laser action and picosecond laser action. Crown-like structures at crater rims are specific features for picosecond Nd:YAG laser action in argon-rich ambient conditions. Elemental analysis of the surfaces indicated nitride compound formation only in the nitrogen-rich ambient conditions. The constituents of the formed plasma were also investigated. Exploring the impact of process control parameters on output responses has been undertaken within the context of laser modification under different environmental conditions. Parametric optimization of the nanosecond laser modification was carried out by implementing an advanced method based on Taguchi’s parametric design and multivariate statistical techniques, and optimal settings are proposed for each atmosphere. 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 energy of the sputtered atoms is important to control the microstructure and physical properties of thin films. In this work, we used the SRIM program to simulate the energy of sputtered atoms. We analyzed the energy distribution functions (EDFs) and the average energies of the atoms in different spatial directions for a range of target materials and Ar ion energies. The results were compared to the analytical equations for EDFs derived by Sigmund and Thompson and with experimental data from the literature. The SRIM simulations give realistic EDFs for transition metals, but not for elements lighter than Si. All EDFs show a low-energy peak positioned close to one-half of the surface binding energy and a high-energy tail decreasing as approximately E⁻². We analyzed the characteristics of EDFs, specifically, the position of low- and high-energy peaks, FWHM, and the energy tail, with respect to the ion energy and position of the element in the periodic table. The low-energy peak increases with atomic number for elements within each group in the periodic table. Similar changes were observed for FWHM. For the period 5 and 6 elements, additional broad high-energy peaks were observed at emission angles above 45° when sputtered by Ar ions with 300 eV and also in some heavier elements when bombarded by 600 eV and 1200 eV ions. The transition metals in groups 4, 5, and 6 in periods 5 and 6 have the highest average energies, while the lowest average energies have elements in group 11. The results of simulations show that the average energies of sputtered atoms were inversely proportional to the sputtering yield, i.e., the higher the sputtering yield, the lower the average energy of sputtered atoms. We established an empirical equation for transition metals to estimate the average energy of sputtered atoms from the sputtering yield. The angular distribution of the average atom energy depends on the atomic number. Transition metals with 22 < Z < 72 have an anisotropic energy distribution, with the highest average energies in the 40°–70° range. For the elements in group 11, the angular distribution of the average energies is more isotropic. Full article

In this experimental study, picosecond laser treatment was performed on a nickel-based superalloy Nimonic 263, aiming to investigate the surface effects induced by irradiation in different atmospheric conditions and, concerning changes in surface composition, regarding the possibility for improvement of its functionality. Besides the varying laser parameters, such as a number of pulses and pulse energy, environmental conditions are also varied. All surface modifications were carried out in standard laboratory conditions and a nitrogen- and argon-rich atmosphere. The resulting topography effects depend on the specific laser treatment and could be categorized as increased roughness, crater formation, and formation of the laser-induced periodic surface structures (LIPSS). Changes in the chemical surface composition are distinguished as the potential formation of the protective oxides/nitrides on the sample surface. Numerous characterization techniques analyse the resulting effects on the topography and surface parameters. The multi-response parametric optimization of the picosecond laser process was performed using an advanced statistical method based on Taguchi’s robust parameter design. Finally, the optimal parameter conditions for Nimonic 263 modification are suggested. 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

Total sputtering yield and spatial distributions of sputtered atoms are important for numerous deposition techniques. We performed SRIM (Stopping and Range of Ions in Matter) simulations to analyze the total sputtering yield and angular distribution of sputtered atoms for a range of single-element target materials. The simulations were conducted for normal argon ion incidence in the 300–1200 eV range and at an oblique angle for selected ion energies. We examined the total and differential sputtering yields for the transition metals in the periods 4–6 and groups 4–6 (Ti, V, Cr; Zr, Nb, Mo; Hf, Ta, and W) and group 11 (Cu, Ag, and Au) of the periodic table, and other materials that are relevant to sputtering (B and C; Al and Si). For the transition metals, the total sputtering yield increases with the group of the periodic table. The elements in group 4 (i.e., Ti, Zr, and Hf) have the lowest sputtering yield, while the elements in group 11 (i.e., Cu, Ag, and Au) exhibit the highest sputtering yield. The angular distribution of the sputtered atoms shows a cosine distribution for the transition metal atoms. The angular distribution of the sputtered atoms for the oblique ion incidence is more asymmetric for the lower ion energies, while for the higher ion energies, the atoms are sputtered more symmetrically. The symmetry also depends on the group of the periodic table and the atomic mass of the target material. The elements in group 11 show the most symmetric distribution, while the elements in group 4 experience the most asymmetric distribution. Furthermore, in an individual group, the distribution becomes more symmetric with heavier target elements. We also examined in detail the influence of the surface binding energy, atomic mass, and ion energy on the total sputtering yield. These parameters were analyzed with regard to the simplified analytical formula for the total sputtering yield, which was derived by Sigmund. This formula was modified by introducing a power fitting parameter, which accounts for the non-linear sputtering yield dependence on the ion energy. The equation provided good estimates for the total sputtering yield of the transition metals that were sputtered by argon ions with energies up to 1200 eV. Full article

In–situ cleaning of the substrate surface by ion etching is an integral part of all physical vapor deposition (PVD) processes. However, in industrial deposition systems, some side effects occur during the ion etching process that can cause re-contamination. For example, in a magnetron sputtering system with several sputter sources and with a substrate holder located centered between them, the ion etching causes the contamination of the unshielded target surfaces with the batching material. In the initial stage of deposition, this material is redeposited back on the substrate surface. The identification of the contamination layer at the substrate–coating interface is difficult because it contains both substrate and coating elements. To avoid this problem, we prepared a TiAlN double coating in two separate production batches on the same substrate. In such a double-layer TiAlN hard coating, the contamination layer, formed during the ion etching before the second deposition, is readily identifiable, and analysis of its chemical composition is easy. Contamination of the batching material was observed also on seed particles that caused the formation of nodular defects. We explain the origin of these particles and the mechanism of their transfer from the target surface to the substrate surface. By comparison of the same coating surface area after deposition of the first and second TiAlN layers, the changes in coating topography were analyzed. We also found that after the deposition of the second TiAlN coating, the surface roughness slightly decreased, which we explain by the planarization effect. Full article

In this paper, we present a comparative study of tribological properties of TiN coatings deposited by low-voltage electron beam evaporation, magnetron sputtering and cathodic arc deposition. The correlation of tribological behavior of these coatings with their intrinsic properties and friction condition was studied. The influence of surface topography and the surrounding atmosphere was analyzed in more detail. We limited ourselves to the investigation of tribological processes that take place in the initial phase of the sliding test (the first 1000 cycles). A significant difference in the initial phase of the sliding test of three types of TiN coatings was observed. We found that nodular defects on the coating surface have an important role in this stage of the sliding test. The tribological response of TiN coatings, prepared by cathodic arc deposition, is also affected by the metal droplets on the coating surface, as well as those incorporated in the coating itself. Namely, the soft metal droplets increase the adhesion component of friction. The wear rates increased with the surface roughness of TiN coatings, the most for coatings prepared by cathodic arc deposition. The influences of post-polishing of the coating and the surrounding atmosphere were also investigated. The sliding tests on different types of TiN coatings were conducted in ambient air, oxygen and nitrogen. While oxygen promotes tribo-chemical reactions at the contact surface of the coating, nitrogen suppresses them. We found that the wear rate measured in ambient air, compared with that in an oxygen atmosphere, was lower. The difference is probably due to the influence of humidity in the ambient air. On the other hand, wear rates measured in a nitrogen atmosphere were much lower in comparison with those measured in an oxygen or ambient air atmosphere. Full article

The primary objective of this study was to investigate and compare the surface topography of hard coatings deposited by three different physical vapor deposition methods (PVD): low-voltage electron beam evaporation, unbalanced magnetron sputtering and cathodic arc evaporation. In these deposition systems, various ion etching techniques were applied for substrate cleaning. The paper summarizes our experience and the expertise gained during many years of development of PVD hard coatings for the protection of tools and machine components. Surface topography was investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM), scanning transmission electron microscopy (STEM) and 3D stylus profilometry. Observed similarities and differences among samples deposited by various deposition methods are discussed and correlated with substrate material selection, substrate pretreatment and deposition conditions. Large variations in the surface topography were observed between selected deposition techniques, both after ion etching and deposition processes. The main features and implications of surface cleaning by ion etching are discussed and the physical phenomena involved in this process are reviewed. During a given deposition run as well as from one run to another, a large spatial variation of etching rates was observed due to the difference in substrate geometry and batching configurations. Variations related to the specific substrate rotation (i.e., temporal variations in the etching and deposition) were also observed. The etching efficiency can be explained by the influence of different process parameters, such as substrate-to-source orientation and distance, shadowing and electric field effects. The surface roughness of PVD coatings mainly originates from growth defects (droplets, nodular defects, pinholes, craters, etc.). We briefly describe the causes of their formation. Full article

During the high pressure die casting (HPDC) process the die material is exposed to thermal fatigue, erosion, and corrosion. Corrosion leads to the soldering of cast alloy to tool surfaces which consequently bonds the casting with die material. Besides wear, such a process reduces the casting quality and production efficiency and endangers the tool integrity. Application of thin ceramic coatings on die surfaces reduces the soldering effects and improves the die performance. However, the development of ceramic coatings for these purposes still requires detailed information on the phenomena involved in these processes. In this study, the soldering performance of a complex nanolayer CrAlN coating, with three chemical compositions (high-Cr, balanced Cr:Al, and high-Al content) were evaluated. The cast alloy soldering was evaluated by the detachment test in three configurations. In this test, a simple casting is formed in contact with flat coated surfaces. Upon casting solidification, the formed joint is dismantled, and a force required for this process was recorded. To characterize and quantify the exhibited wear, after the detachment test, surfaces of the coated samples were analyzed by different microscopy techniques. Two forms of wear were detected on investigated samples. Cast alloy soldering processes induced the formation of thin layers of cast alloy on the surfaces of all investigated coatings. Additionally, substrate corrosion through the coating growth defects caused coating layer delamination during the detachment test. The evaluated coatings displayed different behaviors regarding the extent of wear and values of the detachment force. The coating with a balanced CrAlN composition exhibited the best soldering and corrosion resistance and displayed the lowest ejection force. In terms of soldering and corrosion resistance, the high-Al coating outperformed the high-Cr content coating. However, high-Al and high-Cr coating exhibited significantly higher and quite comparable values of detachment force. Based on the quantitative results it was postulated that, besides soldering and substrate corrosion, the casting-coating bonding strength depends also on “pure” sticking effects of cast alloy to coated surfaces. Full article

The paper summarizes current knowledge of growth defects in physical vapor deposition (PVD) coatings. A detailed historical overview is followed by a description of the types and evolution of growth defects. Growth defects are microscopic imperfections in the coating microstructure. They are most commonly formed by overgrowing of the topographical imperfections (pits, asperities) on the substrate surface or the foreign particles of different origins (dust, debris, flakes). Such foreign particles are not only those that remain on the substrate surface after wet cleaning procedure, but also the ones that are generated during ion etching and deposition processes. Although the origin of seed particles from external pretreatment of substrate is similar to all PVD coatings, the influence of ion etching and deposition techniques is rather different. Therefore, special emphasis is given on the description of the processes that take place during ion etching of substrates and the deposition of coating. The effect of growth defects on the functional properties of PVD coatings is described in the last section. How defects affect the quality of optical coatings, thin layers for semiconductor devices, as well as wear, corrosion, and oxidation resistant coatings is explained. The effect of growth defects on the permeation and wettability of the coatings is also shortly described. Full article