Effect of coating thickness on the deformation behaviour of diamond-like carbon-silicon system

The effect of coating thickness on the deformation behaviour of diamond-like carbon (DLC) coatings on silicon substrates was investigated. Following nanoindentation of a 0.6 µm thick DLC coating, the subsurface microstructures were characterized and the data was compared to prior studies on a similar, but thicker coating. Indentation resulted in localized plastic compression in the coating without any through-thickness cracking. It was shown that the discontinuities in the load-displacement curves appeared at lower loads for the thinner coating. Accordingly, the silicon substrate exhibited cracking, plastic deformation and phase transformation at significantly lower loads than in the case of the thicker coating. Further, the widths, parallel to the interface, over which slip and the phase transformation zone are spread out in the substrate, was found to increase with the thickness of the coating. The mechanism responsible for the first pop-in was found to change from phase transformation in uncoated silicon to dislocation nucleation in the presence of the coating.     

Three dimensional imaging of deformation modes in TiN-based thin film coatings

A TiN thin film coating, approximately 4 μm in thickness, deposited on a ductile steel substrate, was subject to surface deformation via nanoindentation using a spherical indenter, 5 μm in radius, with loads up to 500 mN. Pop-ins were observed during loading, which are characteristic of the onset of cracking and the formation of shear steps at the coating-substrate interface. Focused ion beam microscopy was used to prepare cross-sections through the indentation that revealed the presence of both intercolumnar and inclined cracks. Three-dimensional reconstructions of the deformation zone beneath the indentation were performed using a dual-beam focus ion beam instrument. These constructions provided more detailed images of the morphology of cracks, which were observed to be consistent with theoretical models of plastic deformation of such brittle coatings.     

In-situ investigation on the deformation and damage behaviour of diamond-like carbon coated thin films under uniaxial loading

In the present work, the failure behaviour of diamond-like carbon (DLC) coatings on thin steel substrate under uniaxial tensile loading is analyzed in-situ in scanning electron microscopy as well as ex-situ using focused ion beam cross section and transmission electron microscopy. Aim of the work is to find correlations between the failure behaviour of the coating system, the adhesion and the stress-strain behaviour of a DLC coating system under tensile loadings conditions. Therefore thin amorphous DLC films were coated onto thin stainless steel foils using a plasma assisted chemical vapour deposition technique. It is found from the in-situ investigations that at increasing strains cracks were formed in the coating, with decreasing spacing at higher strains. By comparing uncoated steels foils with coated systems the stress-strain behaviour of a DLC coating was determined. The DLC coating, although already strongly cracked, bears loads up to a total strain of 15%. Cross section analyses with a focused ion beam and microscopy techniques supported these investigations. During straining the formation of two deformation bands adjacent to the Cr adhesion layer was observed. This deformation bands also indicate a high interfacial adhesion.     

Indentation-induced subsurface damage in silicon particles of Al–Si alloys

Damage microstructures generated beneath the Vickers indentation applied to the silicon particles in an Al–18.5 wt.%Si alloys were studied. Plastic deformation at low loads and volume expansion due to subsurface crack formation at high loads (>650 mN) were responsible for pile-up formations around the indentations. The probability of lateral cracks reaching the surface and causing particle fracture was shown to obey Weibull statistics with a low modulus. The indentation pressure estimated as 19.3 GPa induced the transformation of diamond cubic Si-I to bcc Si-III and rhombohedral Si-XII, as observed by Raman microspectroscopy. Cross-sectional FIB and TEM revealed a semi-circular plastic core and subsurface lateral crack pattern below the residual indents and a localized amorphous zone at the median crack boundary immediately below the plastic core.     

Substrate dependent cracking behavior of CrAlN coatings

The present study investigated the effect of substrate deformation behavior on crack resistance of CrAlN coatings under quasi-static and cyclic loads using nanoindentation. (Cr₄₇Al₅₃)N coatings were deposited on cemented carbide WC-Co and high-speed steel HS652C substrates through physical vapor deposition (PVD) und characterized. In order to study the coating cracking behavior, the coated substrates were subjected to quasi-static nanoindentations with indentation force F_max = 1 N, F_max = 1.5 N and F_max = 2 N. Moreover, the crack resistance under cyclic loading with frequency f = 0.16 Hz was analyzed at F = 1 N and F = 1.5 N after n = 900 cycles. A conical diamond indenter was used for the tests. At the end, the indentation imprints were analyzed by scanning electron microscopy (SEM). The substrate dependency was apparent in cracking behavior of the coating. Albeit the lower indentation depth compared to the variant with HS6-5-2C substrate, the CrAlN coating on WC-Co substrate showed surface cracks under quasi-static and cyclic loading. These cracks on the coated surface were absent in the variant with HS6-5-2C substrate. This could be related to higher resistance of cemented carbide substrates against plastic deformation, prompting earlier crack initiation in CrAlN coating for effective energy dissipation during indentation.     

Assessment of the toughness of thin coatings using nanoindentation under displacement control

Various indentation models have been developed to measure the toughness of bulk materials and coatings. Most of them are based on the formation of well-developed cracks. However, in order to eliminate the influence of elastic–plastic deformation in the substrate, it is preferable to perform small indentations in thin coatings and thus the cracks may not be well-developed compared to the indentation size. Relatively little work has been done to investigate this kind of small cracks. The ultra small cracks (< 500 nm in length) in thin coatings (∼ 500 nm in thickness) confined to indentation zone are investigated here. A new method to assess the toughness of the main components of solar control coatings such as SnO₂, TiO_xN_y and ITO deposited on soda–lime glass is proposed here. This method is able to separate the energy contributions from other deformation mechanisms from that dissipated in the fracture event. The energy release rate of these ceramics coating are in the range 15–45 J/m² by this method.     

Tensile behaviour of as deposited and heat-treated electroless Ni-P deposits

Electroless Ni-P coatings were deposited on mild steel substrates and the effect of heat-treatment on their structure and tensile behaviour was studied, with the following conclusions. The as-deposited electroless Ni-P coating is amorphous and it remains amorphous up to 300 °C. At 400 °C the coating becomes crystalline and consists of a Ni₃P matrix containing areas of metallic nickel. For the selected coating/substrate thickness ratio, the contribution of the coating in the tensile properties of the coating-substrate system is negligible as expressed by the values of yield strength, ultimate tensile strength and fracture strain in mild steel substrates and coated as-deposited and heat-treated specimens. Extensive cracking of the coating accompanied by spalling was occurred during the tensile tests. The density of cracks was found to increase close to the fracture surface of the tensile specimen and with increasing heat-treatment temperature. The cracks observed on the surface of the coatings are believed to form due to the inability of the brittle coating to accommodate the strain generated in the ductile substrate. Their orientation to the tensile axis is in close relation to the structure of the coating and the failure mechanism that is dictated by this structure. The first cracks on the surface of the coatings were found to form after the yield strength of the tensile specimen has been reached and plastic deformation of the substrate takes place. Their density increases with the accumulation of strain up to fracture.     

A contribution to the mechanical characterization of polymeric coatings by depth-sensing indentation measurements

Coating-substrate systems consisting of polypropylene coatings with thicknesses of 6 and 9.8 m on silicon are investigated by depth-sensing indentation measurements with end loads between 20 and 1000 mN. Different effective load rates were applied. The results are correlated to an energy- and volume-related interpretation of the deformation processes. The proposed model permits to proof constant material behaviour over extended penetration depths. The potential on the quantification of the viscoelastic character as well as on the compound strength must be further verified.     

Improving fretting fatigue behaviour of Al 7075-T6 bolted plates using electroless Ni–P coatings

In this paper, the effect of electroless nickel–phosphorous coatings on the fatigue and fretting fatigue behaviour of Al 7075-T6 bolted plates has been investigated. A double-lap bolted joint specimen was designed and manufactured from the aluminium plates and subsequently coated with Ni–P coatings of 40 μm in thickness with a high phosphorous content of 10–13 wt.%. Then, different tightening torques were applied to clamp the plates together with the aim of studying the effect of clamping force on the fretting fatigue life of the joints. Ni–P coatings were found to protect Al 7075-T6 clamped plates against fretting fatigue damages even at low fatigue loads where the uncoated joints showed a large reduction in their fatigue life due to the fretting effects. Fretting fatigue life of moderately and firmly clamped plates was successfully improved by approximately 30–40% and 50–60% respectively after the application of Ni–P coatings. Furthermore, fatigue cracks were found at the outer surface of the aluminium substrate at the edge of the hole associated with nodular defects whose deleterious effect was more pronounced at high cyclic loads. The Ni–P deposit presented a very good adhesion to the substrate at low and moderate loads; however, considerable delaminations and fracture of the coating film at high cyclic loads was observed.     

The effect of PVD coatings on the corrosion behaviour of AZ91 magnesium alloy

In this study, multilayered AlN (AlN + AlN + AlN) and AlN + TiN were coated on AZ91 magnesium alloy using physical vapour deposition (PVD) technique of DC magnetron sputtering, and the influence of the coatings on the corrosion behaviour of the AZ91 alloy was examined. A PVD system for coating processes, a potentiostat for electrochemical corrosion tests, X-ray difractometer for compositional analysis of the coatings, and scanning electron microscopy for surface examinations were used. It was determined that PVD coatings deposited on AZ91 magnesium alloy increased the corrosion resistance of the alloy, and AlN + AlN + AlN coating increased the corrosion resistance much more than AlN + TiN coating. However, it was observed that, in the coating layers, small structural defects e.g., pores, pinholes, cracks that could arise from the coating process or substrate and get the ability of protection from corrosion worsened were present.     

Relative performance of hydrogenated, argon-incorporated and nitrogen-incorporated diamond-like carbon coated Ti-6Al-4V samples under fretting wear loading

Hydrogenated diamond-like carbon (DLC) (H-DLC), argon-incorporated DLC (Ar-DLC) and nitrogen-incorporated DLC (N-DLC) coatings were deposited on flat rectangular Ti-6Al-4V samples. The DLC coatings were characterised by Raman spectroscopy and nanoindentation. Fretting wear tests were conducted on uncoated and DLC coated samples with an alumina ball as the counterbody. As the Ar-DLC and N-DLC coatings had relatively more sp² network compared to the H-DLC coating, they exhibited lower values of hardness and elastic modulus. At both loads of 4.9 N and 14.7 N, all DLC coated specimens showed lower values of tangential force coefficient (TFC), wear volume and specific wear rate compared to the uncoated samples. While the Ar-DLC coated sample exhibited the lowest TFC, wear volume and specific wear rate at 4.9 N load, the N-DLC coated specimen exhibited the lowest TFC, wear volume and specific wear rate at 14.7 N load.     

Mechanical properties of in situ Al2O3 formed Al–Si composite coating via atmospheric plasma spraying

In this study, mechanically alloyed Al–12Si/SiO₂ composite powder was deposited onto an aluminum substrate by atmospheric plasma spraying. The composite coating consisting of in situ formed Al₂O₃ reinforced hypereutectic Al–18Si matrix alloy was achieved. The produced coatings were extensively analyzed with respect to X-ray diffraction (XRD). The XRD patterns of the coatings include Al, Si and Al₂O₃ phase formation. Mechanical properties of layers were examined by Dynamic Ultra-micro hardness test machine for estimating Young’s modulus due to load–unload sensing analysis. The hardness and Young’s modulus of the composite coatings sprayed at different plasma current and the distance were measured under 200, 400, 600, 800 and 1000 mN of applied peak loads by indentation technique. The effects of spray distance and arc current on the hardness and Young’s modulus have been investigated. Additionally, it was observed that the arc current and spray distance strongly influence the mechanical properties of the coatings.     

Structure, mechanical and tribological properties of diamond-like carbon films on aluminum alloy by arc ion plating

The low hardness and poor tribological performance of aluminum alloys restrict their engineering applications. However, protective hard films deposited on aluminum alloys are believed to be effective for overcoming their poor wear properties. In this paper, diamond-like carbon (DLC) films as hard protective film were deposited on 2024 aluminum alloy by arc ion plating. The dependence of the chemical state and microstructure of the films on substrate bias voltage was analyzed by X-ray photoelectron spectroscopy and Raman spectroscopy. The mechanical and tribological properties of the DLC films deposited on aluminum alloy were investigated by nanoindentation and ball-on-disk tribotester, respectively. The results show that the deposited DLC films were very well-adhered to the aluminum alloy substrate, with no cracks or delamination being observed. A maximum sp³ content of about 37% was obtained at −100 V substrate bias, resulting in a hardness of 30 GPa and elastic modulus of 280 GPa. Thus, the surface hardness and wear resistance of 2024 aluminum alloy can be significantly improved by applying a protective DLC film coating. The DLC-coated aluminum alloy showed a stable and relatively low friction coefficient, as well as narrower and shallower wear tracks in comparison with the uncoated aluminum alloy.     

Wear behavior of aluminum-coated glass compared to uncoated glass investigated by cyclic wear tests in the micrometer scale

Micro wear tests have been conducted on soda lime glass covered with a 4.5 μm aluminum film and on an uncoated glass substrate. High resolution lateral force-displacement measurements were carried out with a spherical diamond indenter of 6 μm radius while the normal force was kept constant. The wear behavior was investigated for different normal loads (100 mN, 200 mN), different scratch lengths (10 μm, 40 μm) and different lateral sliding speed (5 μm/s, 10 μm/s, 20 μm/s). These conditions were used as a model for the characterization of surface damage by hard wear particles. The average friction coefficient and the average normal displacement per cycle were calculated and their change was used for the characterization of the wear behavior. Significant changes could be observed in the dependence on the wear parameters and the cycle number. Thus, wear dominated by plastic deformation and fracture-dominated wear could be distinguished. The soft aluminum coating on the brittle glass prevents fracture-dominated wear of the glass even after the failure of the coating. The wear rate of the glass is considerably decreased if only wear by plastic deformation occurs.     

Mechanical properties of conventional and nanostructured plasma sprayed alumina coatings

The hardness and the elastic modulus measured by microindentation of three different types of plasma sprayed alumina coatings have been compared. Usually, such coatings present porosity and heterogeneity which affect the measurement of the mechanical properties. To take such effects into account along with the indentation size effect which is relevant to all hardness studies, the Proportional Specimen Resistance model is applied. The three alumina coatings show closely similar mechanical properties at indentation loads exceeding 1 N, i.e., macrohardness around 5.7 GPa, indentation size effect parameter around 5.5 MPa mm and elastic modulus around 160 GPa. For loads below 1 N, the extrapolated values of the macrohardness of crushed and agglomerated alumina coatings increased to 8.5 GPa, while the indentation size effect parameter has the same value, and the elastic modulus increased to 320 GPa. However, no significant change in the measured values of hardness and the elastic modulus of the nanostructured alumina coating has been observed. This result is attributed to porosity and the bimodal microstructure of the nanostructured coating where a semimolten phase coexists along with the fully molten phases.     

Contact damage evolution in a diamond-like carbon (DLC) coating on a stainless steel substrate

A diamond-like carbon thin film was coated onto a stainless steel substrate using plasma assisted chemical vapour deposition (PACVD). Instrumented indentation and scratching were used, supported by focused ion beam (FIB) microscopy, to explore deformation and fracture behaviours of this coating system. The formation and growth of ring and radial cracks in the coating, as well as plastic flow in the ductile substrate, were observed to be the predominant deformation processes for this coating system. Lateral cracking occurred at the interface of the coating/substrate following indentation, but in the middle of the coating following scratching. No evidence of plastic flow within the coating was observed. Coating deformation is, therefore, controlled by its fracture energy. An indentation-energy-based model was applied to evaluate the fracture toughness of the coating.     

Element Analysis of Ceramic Coatings under Spherical Indentation with Metallic Interlayer:Part Ⅱ Ring Crack

Spherical indentation of ceramic coatings with metallic interlayer was performed by means of axisymmetric finite element analysis(FEA). Two typical ceramic coatings with relatively high and low elastic modulus deposited on aluminum alloy and carbon steel were considered. The fracture mechanics of the ceramic coatings mechanisms due to occurrence of surface ring cracks extending traverse the coating thickness under spherical indentation are investigated within the framework of linear fracture mechanics. The J-integral associated to such cracks was computed. The evolution of J-integral vs the crack length and the indentation depth was studied. The effects of the interlayer, the coating and the substrate on the J-integral evolution were discussed. The results show that a suitable metallic interlayer can improve the fracture resistance of the coating systems under the same indentation conditions through reducing the J-integral.     

Thermo-mechanical behavior of the Al–Si alloy coated hot stamping boron steel

Hot tensile tests of boron steels with and without an Al–Si coating were performed using a Gleeble 3500 test system, at temperatures of 700–850 °C and strain rates of 0.01–1/s. The phase and microstructure of the coating in as-coated and press-hardened conditions were observed under scanning electron microscopy (SEM) equipped with energy dispersive X-ray analysis and X-ray diffraction (XRD). Experimental results indicate that the Al–Si coating gave an unignorable influence on the thermo-mechanical properties of the boron steels. The ultimate tensile strength (UTS) of the Al–Si coated boron steel was almost equal to that of the uncoated under the lower strain rate at the same deformation temperature. At a higher strain rate, the UTS value appeared to be lower than that of the uncoated. Moreover, the UTS difference increased with the decreasing deformation temperature. The ductility of the Al–Si coated steel was lower than that of the uncoated under the described test conditions. Following the tensile tests, extensive cracks were visible in the Al–Si coating layer. SEM observation showed that microcracks and voids appeared after austenization, which may act as nucleation sites for the cracks. The cracks first propagated in the direction perpendicular to the coating/substrate interface and were identified as Type I cracks. The propagation was hindered by the substrate when these cracks reached the coating/substrate interface. This occurred because the interfacial bonding strength between the coating and the substrate was lower than the substrate strength. Following this initial failure, the cracks turned to propagate paralleled to the coating/substrate interface. In addition with the shear stress resulting from the substrate yielding, Type II cracks formed. Eventually, the cracked coatings were accompanied by interface decohesion from the substrate. The width and density of the cracks were found to increase with the decreasing deformation temperature and rising stain rate.     

Element Analysis of Ceramic Coatings under Spherical Indentation with Metallic Interlayer：Part Ⅱ Ring Crack

Spherical indentation of ceramic coatings with metallic interlayer was performed by means of axisymmetric finite element analysis （FEA）. Two typical ceramic coatings with relatively high and low elastic modulus deposited on aluminum alloy and carbon steel were considered. The fracture mechanics of the ceramic coatings mechanisms due to occurrence of surface ring cracks extending traverse the coating thickness under spherical indentation are investigated within the framework of linear fracture mechanics. The J-integral associated to such cracks was computed. The evolution of J-integral vs the crack length and the indentation depth was studied. The effects of the interlayer, the coating and the substrate on the J-integral evolution were discussed. The results show that a suitable metallic interlayer can improve the fracture resistance of the coating systems under the same indentation conditions through reducing the J-integral.     

Corrosion behaviour and galvanic coupling with steel of Al-based coating alternatives to electroplated cadmium

The galvanic corrosion behaviour of bare steel coupled to steel with an Al–Zn flake inorganic spin coating, an Al-based slurry sprayed coating, an arc sprayed Al coating and electroplated cadmium has been investigated. The sacrificial and galvanic behaviour of the coatings was studied in 3.5 wt. % NaCl solution using open-circuit potential, potentiodynamic polarisation and electrochemical noise measurements. The coatings were characterised by scanning electron microscopy, energy dispersive X-ray spectroscopy and X-ray diffraction. Experimental results showed that the Al-based slurry sprayed coating exhibited an open-circuit potential closer to the steel substrate than other coatings, as well as a low corrosion current density and a more positive corrosion potential. In terms of the galvanic suitability of the investigated coatings for the steel substrate, both the Al–Zn flake inorganic spin coating and the Al-based slurry sprayed coating show low galvanic current, in comparison with the arc sprayed Al coating and electroplated cadmium. This behaviour confirms their superior cathodic protection capability and galvanic compatibility over other coatings tested. Electrochemical noise measurements provide accurate information on the coatings' galvanic behaviour, which can be complimented by the data obtained from superposition of potentiodynamic corrosion scans of the coating and bare steel, provided that the corrosion potential difference between the two materials does not exceed 300 mV.