Search Results (13)

The impact of modulation periods on the microstructure, as well as the tribological and mechanical characteristics of the AlCrTiVNbN/TiSiN nano multilayer films, was investigated. The films were prepared with modulation periods ranging from 4 nm to 7 nm, and their properties were explored using X-ray diffraction (XRD), scanning electron microscope (SEM), nanoindentation, and a tribological tester. All nano multilayer films revealed a face-centered cubic (FCC) structure with a preferred planar direction of (200). As the modulation period increased, the XRD peak moved to higher angles, and the interplanar distance decreased. Also, the mechanical properties deteriorated, and the COF rose monotonically as a result. The nano multilayer film with a modulation period equal to 4 nm exhibited a smooth surface with minimal small particles, the highest hardness of 15.51 ± 0.16 GPa and elastic modulus of 182.89 ± 2.38 GPa, the highest values for the ratios of H/E and H³/E², the lowest average friction coefficient of 0.73, and a wear rate equal to (8.2 9 ± 0.18) × 10⁻⁸ mm³·N⁻¹·m⁻¹. The improvement in the properties of the film was ascribed to the coherent growth and alternating stress field between the AlCrTiVNbN and TiSiN layers. Full article

This study investigates the nanomechanical and tribological behavior of multilayered nitride/carbonitride nanostructured superlattice type coatings (NTCs) composed of alternating TiAlSiNb-N and TiCr-CN sublayers, deposited via high-power ion-plasma magnetron sputtering (HiPIPMS) technique. Reinforced with refractory elements Cr and Nb, the NTC samples exhibit high nanohardness (39–59 GPa), low friction, and excellent wear resistance. A novel analytical approach was introduced to extract stress–strain field (SSF) gradients and divergences from nanoindentation data, revealing alternating strain-hardening and strain-softening cycles beneath the incrementally loaded indenter. The discovered oscillatory behavior, consistent across all samples under the investigation, suggests a general deformation mechanism in thin films under incremental loading. Fourier analysis of the SSF gradient oscillatory pattern revealed a variety of characteristic dominant wavelengths within the length-scale interval (0.84–8.10) nm, indicating multi-scale nanomechanical responses. Additionally, the NTC samples display an anisotropic coating morphology exhibited as unidirectional undulating surface roughness waves, potentially attributed to atomic shadowing, strain-induced instabilities, and limited adatom diffusion. These findings deepen our understanding of nanoscale deformation in advanced PVD coatings and underscore the utility of SSF analysis for probing thin-film mechanics. Full article

In this study, as-cast ductile iron was austempered to produce austempered ductile iron (ADI). A CrAlSiN film was then deposited on the surface of ADI specimens using the cathodic arc deposition (CAD) method. The gas flow ratio of Ar/N₂ varied (2, 2.5, and 3) under different processing parameters, designated as S1, S2, and S3, respectively. The composition, structure, hardness, adhesion, and wear resistance of the coated specimens were analyzed to evaluate the effect of the gas flow ratio on surface hardness and abrasion resistance. The experimental results indicated that CrN/Al(Si)N nano-multilayered films were successfully synthesized using oppositely positioned dual targets (Cr and AlSi) reacting with N₂ gas during the CAD process. The coatings significantly enhanced the surface hardness and wear resistance of ADI. A comparison of the three coating conditions with varying gas flow ratios revealed that as the Ar/N₂ gas flow ratio decreased (i.e., N₂ gas flow increased), the surface hardness of the coated ADI specimens increased while the abrasion rate decreased. Among the tested conditions, S1 exhibited the highest hardness (1479 HV_0.1) and the lowest wear rate (1.6 × 10⁻⁶ g/m). Full article

This article discusses the micromechanical properties and true microhardness determination of nanostructured tribological coatings (NTCs) based on a multilayered alternating nitride/carbonitride bilayer substructure for transition metals. The constituent nitride/carbonitride bilayers in the superlattice structure of the NTC were alloyed with refractory metals, denoted as Me = Me₁ or Me₂= Cr, Hf, Nb, W, and Zr. The resulting NTC coatings were deposited onto 100Cr6 steel substrates using an advanced physical vapor deposition (PVD) technique, referred to here as high-power ion-plasma magnetron sputtering (HiPIPMS). The comprising crystalline nanometer-scale TiAlSiMe₁-N/TiMe₂-CN nanoparticles strengthened by Me additives significantly increased the NTC microhardness to over 3200 HV. The primary focus of this research was to determine the true microhardness of the NTC film samples. The apparent microhardness (H_a) of the film/substrate system for various NTC samples was measured during microindentation testing using the Vickers method. Nine NTC samples were tested, each generating a corresponding microindentation dataset containing between 430 and 640 imprints, depending on the specific NTC sample. These datasets were analyzed using three distinct empirical approaches: (i) the inverse power-law model (IPL-Model), (ii) the sigmoid-like decay model (SLD-Model), and (iii) the error function model (ERF-Model). The observed solid correlation between the proposed models and experiments suggests that the true microhardness estimates (H_f) obtained through the empirical mathematical modeling approach are reliable. Full article

This study investigates accelerated physical–chemical processes in a complex adaptive surface-engineered system represented by a nano-multilayer TiAlCrSiYN/TiAlCrN PVD coating under the extreme tribological conditions of ultra-high-performance dry machining of hardened H 13 tool steel. These processes are similar to the different catalyzing phenomena. Experimental results of tool life vs. wear rate, SEM/TEM data of the worn surfaces, XPS and EDS data of tribo-films formed on the friction surfaces, and chip surface morphology are presented in this study. The corresponding relationships between self-organization, self-organized criticality, and various catalyzing phenomena were evaluated on the basis of the accrued data. A method of enhancing these processes through the variation of machining conditions is also outlined, which resulted in the improvement of coated tool life by 35%. Full article

A nano-multilayer Ti_0.2Al_0.55Cr_0.2Si_0.03Y_0.02N/Ti_0.25Al_0.65Cr_0.1N PVD coating was deposited on Kennametal carbide K 313 inserts. These coatings are widely used to protect cutting tools under severe exploitation conditions. Under equilibrium conditions, it was found that the Al₂O₃ oxide possessed better adhesive properties than the TiO₂. The addition of chromium further enhanced the oxidation resistance of the coatings. Silicon significantly increased the oxidation resistance of this type of coating. The properties of the diffusion process in this coating have not been sufficiently investigated, despite the considerable number of articles published on this topic. For the purpose of this study, a multilayer ion-plasma (TiAlCrSiY)N/(TiAlCr)N coating was oxidized under equilibrium conditions; its chemical inhomogeneity was studied by time-of-flight mass spectroscopy using a TOF SIMS5-100 instrument. The data was collected from an area of 100 × 100 µ. A D-300 profilometer (KLA-Tencor Corp., Milpitas, California 95035, USA) was used to determine the rate of ion etching. It was found that oxidation commenced at the surface nanolayer of a TiAlCrN nitride, forming loose films of Cr₂O₃, TiO₂, and Al₂O₃ oxides. This passivating film had a thickness of around 140 nm. For the first time, the interlayer diffusion coefficients of Si and Y were determined in multilayer coatings based on Ti_0.2Al_0.55Cr_0.2Si_0.03Y_0.02N/Ti_0.25Al_0.65Cr_0.1N, under open air annealing at 700 °C. The physical nature of the differences in the diffusion of these elements is discussed. The diffusion rate in the near-surface volumes was lower than in the deep layers of the multilayer coating, most likely due to the formation of passivating oxide films on the surface. Full article

The impact wear property of hard coatings at elevated temperatures is of particular interest for applications in nuclear power plants. This study evaluated the impact wear behavior of two CrAlN/TiSiN coatings with and without sand. Alternately grown CrAlN and TiSiN films with modulation periods of 455 and 19 nm were formed in a columnar structure. The nanomultilayer shows better impact wear resistance than multilayer films with and without sand. The energy absorption rate has a similar trend to wear rate, leading to lower rebound velocity and peak impact force of the nanomultilayer compared with that of the multilayer. CrAlN/TiSiN coatings can protect the 308L substrate from oxidation. The dominant impact wear mechanism without sand is plastic deformation, and this wear region can be defined as the percussive zone. Peeling occurs on the multilayer surface without sand after 10⁴ percussions, leading to rapid oxidation of the 308L substrate at 500 °C. Due to the abrasion effect, the wear rate of the sample with sand increases by an order of magnitude compared to the sample without sand. The wear scar of the sample with sand can be divided into the mixing zone and the sand−affected zone from inside to outside. Fe oxides are formed beyond the unbroken coating, which may be related to the outward diffusion of Fe. Full article

Optimization of the composition of a new generation of bi-nano-multilayered TiAlCrSiN/TiAlCrN-based coatings is outlined in this study for the machining of direct aged (DA) Inconel 718 alloy. Three types of TiAlCrSiN/TiAlCrN-based bi-nano-multi-layer coatings with varying chemical compositions were investigated: (1) a previous state-of-the-art Ti_0.2Al_0.55Cr_0.2Si_0.03Y_0.02N/Ti_0.25Al_0.65Cr_0.1N (coating A); (2) Ti_0.2Al_0.52Cr_0.2Si_0.08N/Ti_0.25Al_0.65Cr_0.1N with increased amount of Si (up to 8 at.%; coating B); (3) a new Ti_0.18Al_0.55Cr_0.17Si_0.05Y_0.05N/Ti_0.25Al_0.65Cr_0.1N coating (coating C) with an increased amount of both Si and Y (up to 5 at.% each). The structure of each coating was evaluated by XRD analysis. Micro-mechanical characteristics were investigated using a MicroMaterials NanoTest system and an Anton Paar-RST3 tester. The wear performance of nano-multilayered TiAlCrSiN/TiAlCrN-based coatings was evaluated during the finish turning of direct aged (DA) Inconel 718 alloy. The wear patterns were assessed using optical microscopy imaging. The tribological performance was evaluated through (a) a detailed chip characteristic study and (b) XPS studies of the worn surface of the coated cutting tool. The difference in tribological performance was found to correspond with the type and amount of tribo-films formed on the friction surface under operation. Simultaneous formation of various thermal barrier tribo-films, such as sapphire, mullite, and garnet, was observed. The overall amount of beneficial tribo-films was found to be greater in the new Ti_0.18Al_0.55Cr_0.17Si _0.05Y_0.05N/Ti_0.25Al_0.65Cr_0.1N nano-bi-multilayer coating (coating C) than in the previous state-of-the-art coatings (A and B). This resulted in over two-fold improvement of this coating’s tool life compared with those of the commercial benchmark AlTiN coating and coating B, as well as a 40% improvement of the tool life of the previous state-of-the-art coating A. Multi-scale self-organization processes were observed: nano-scale tribo-film formation on the cutting tool surface combined with micro-scale generation of strain-induced martensite zones as a result of intensive metal flow during chip formation. Both of these processes are strongly enhanced in the newly developed coating C. Full article

This paper discusses the surface-engineered nanomaterials (adaptive nano-structured physical vapor deposition (PVD) thin-film coatings) that can effectively perform under severely non-equilibrium tribological conditions. The typical features of these nanomaterials are: (a) Dynamically interacting elements present in sufficient amounts to account for its compositional/structural complexity; (b) an initial non-equilibrium state; (c) optimized micro-mechanical characteristics, and (d) intensive adaptation to the external stimuli. These could be considered as functionally graded nanomaterials that consist of two major layers: an underlying (2–3 microns) thin-film PVD coating, the surface on which an outer nanoscale layer of dynamically re-generating tribo-films is produced as a result of self-organization during friction. This tribo-film nanolayer (dissipative structures) was discovered to represent complex matter, which exhibits characteristic properties and functions common to naturally occurring systems. These include adaptive interaction with a severely non-equilibrium environment; formation of compounds such as sapphire, mullite, and garnet, similar to those that arise during metamorphism; ability to evolve with time; as well as complexity and multifunctional, synergistic behavior. Due to several nanoscale effects, this nanolayer is capable of protecting the surface with unprecedented efficiency, enabling extensive control over the performance of the entire surface-engineered system. These surface-engineered nanomaterials can achieve a range (speed and level) of adaptability to the changing environment that is not found in naturally occurring materials. Therefore, these materials could be classified as metamaterials. The second major characteristic of these materials is the structure and properties of the coating layer, which mostly functions as a catalytic medium for tribo-film generation and replenishment. A functioning example of this type of material is represented by an adaptive hard thin-film TiAlCrSiYN/TiAlCrN nano-multilayer PVD coating, which can efficiently work in an extreme environment, typical for the dry machining of hard-to-cut materials. Full article

We investigated the effects of substrate rotation speed on the structural and mechanical properties of CrN/CrAlSiN multilayer coatings produced using high-power impulse magnetron sputtering (HiPIMS) on silicon and high-speed steel (HSS) substrates. Structural analysis and characterization of the multilayer coatings were performed using an X-ray diffractometer (XRD), field emission scanning electron microscopy (FE-SEM), an electron probe microanalyzer (EPMA), and a transmission electron microscope (TEM). The thickness of the bi-layer film depended on the substrate rotation speed, as follows: 12 (1.5 rpm), 9.5 (2 rpm), 6 (3 rpm), 4 (4 rpm), and 3.2 nm (5 rpm). The results revealed that the hardness and coating–substrate adhesion strength increased inversely with the thickness of the bi-layer. TEM analysis revealed smaller columnar structures in thinner CrN/CrAlSiN multilayer coatings. The highest results for hardness (20.1 GPa), elastic modulus (336 GPa), and adhesion strength (77 N) were obtained at a substrate rotation speed of 5 rpm. We also investigated the adhesion properties of the multilayer structures and formulated a hypothesis to explain adhesion strength. Full article

In the present work, the structure, stress state and phase composition of MeN/SiN_x (Me = Zr, Cr, Al) multilayered films with the thickness of elementary layers in nanoscale range, as well as their stability to high temperature oxidation, were studied. Monolithic (reference) and multilayered films were deposited on Si substrates at the temperatures of 300 °C (ZrN/SiN_x and AlN/SiN_x systems) or 450 °C (CrN/SiN_x) by reactive magnetron sputtering. The thickness ratios of MeN to SiN_x were 5 nm/2 nm, 5 nm/5 nm, 5 nm/10 nm and 2 nm/5 nm. Transmission electron microscopy (TEM), X-ray Reflectivity (XRR) and X-ray Diffraction (XRD) testified to the uniform alternation of MeN and SiN_x layers with sharp interlayer boundaries. It was observed that MeN sublayers have a nanocrystalline structure with (001) preferred orientation at 5 nm, but are X-ray amorphous at 2 nm, while SiN_x sublayers are always X-ray amorphous. The stability of the coatings to oxidation was investigated by in situ XRD analysis (at the temperature range of 400–950 °C) along with the methods of wavelength-dispersive X-ray spectroscopy (WDS) and scanning electron microscopy (SEM) after air annealing procedure. Reference ZrN and CrN films started to oxidize at the temperatures of 550 and 700 °C, respectively, while the AlN reference film was thermally stable up to 950 °C. Compared to reference monolithic films, MeN/SiN_x multilayers have an improved oxidation resistance (onset of oxidation is shifted by more than 200 °C), and the performance is enhanced with increasing fraction of SiN_x layer thickness. Overall, CrN/SiN_x and AlN/SiN_x multilayered films are characterized by noticeably higher resistance to oxidation as compared to ZrN/SiN_x multilayers, the best performance being obtained for CrN/SiN_x and AlN/SiN_x with 5 nm/5 nm and 5 nm/10 nm periods, which remain stable at least up to 950 °C. Full article

Experimental investigations of nano-scale spatio-temporal effects that occur on the friction surface under extreme tribological stimuli, in combination with thermodynamic modeling of the self-organization process, are presented in this paper. The study was performed on adaptive PVD (physical vapor deposited) coatings represented by the TiAlCrSiYN/TiAlCrN nano-multilayer PVD coating. A detailed analysis of the worn surface was conducted using scanning electron microscopy and energy dispersive spectroscopy (SEM/EDS), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and Auger electron spectroscopy (AES) methods. It was demonstrated that the coating studied exhibits a very fast adaptive response to the extreme external stimuli through the formation of an increased amount of protective surface tribo-films at the very beginning of the running-in stage of wear. Analysis performed on the friction surface indicates that all of the tribo-film formation processes occur in the nanoscopic scale. The tribo-films form as thermal barrier tribo-ceramics with a complex composition and very low thermal conductivity under high operating temperatures, thus demonstrating reduced friction which results in low cutting forces and wear values. This process presents an opportunity for the surface layer to attain a strong non-equilibrium state. This leads to the stabilization of the exchanging interactions between the tool and environment at a low wear level. This effect is the consequence of the synergistic behavior of complex matter represented by the dynamically formed nano-scale tribo-film layer. Full article

In this paper, we will develop a strategy for controlling the self-organized critical process using the example of extreme tribological conditions caused by intensive build-up edge (BUE) formation that take place during machining of hard-to-cut austentic superduplex stainless steel SDSS UNS32750. From a tribological viewpoint, machining of this material involves intensive seizure and build-up edge formation at the tool/chip interface, which can result in catastrophic tool failure. Built-up edge is considered to be a very damaging process in the system. The periodical breakage of the build-ups may eventually result in tool tip breakage and, thereby, lead to a catastrophe (complete loss of workability) in the system. The dynamic process of build-up edge formation is similar to an avalanche. It is governed by stick-slip phenomenon during friction and associated with the self-organized critical process. Investigation of wear patterns on the frictional surfaces of cutting tools using Scanning Electron Microscope (SEM), combined with chip undersurface characterization and frictional (cutting) force analyses, confirms this hypothesis. The control of self-organized criticality is accomplished through application of a nano-multilayer TiAl60CrSiYN/TiAlCrN thin film Physical Vapor Deposition (PVD) coating containing elevated aluminum content on a cemented carbide tool. The suggested coating enhanced the formation of protective nano-scale tribo-films on the friction surface under operation. Moreover, machining process optimization contributed to further enhancement of this beneficial process, as evidenced by X-ray Photoelectron Spectroscopy (XPS) studies of tribo-films. This resulted in a reduction of the scale of the build ups leading to overall wear performance improvement. A new thermodynamic analysis is proposed concerning entropy production during friction in machining with buildup edge formation. This model is able to predict various phenomena and shows a good agreement with experimental results. In the presented research we demonstrated a novel experimental approach for controlling self-organized criticality using an example of the machining with buildup edge formation, which is similar to avalanches. This was done through enhanced adaptive performance of the surface engineered tribo-system, in the aim of reducing the scale and frequency of the avalanches. Full article