Failure assessment of a hard brittle coating on a ductile substrate subjected to cyclic contact loading

Hard brittle films and coatings are often employed as a protective coating for metallic ductile substrates. In use, such coatings are generally subjected to cyclic/repeated contact loading and sliding over long periods of time. This study investigated the monotonic and cyclic contact fracture mechanism of hard coatings on ductile substrates (an electroplated Ni–P coating on a stainless steel substrate, SUS304) in order to evaluate their mechanical durability. In the experiment, both monotonic and cyclic indentation tests using a ball indenter with large contact force were performed. The fracture nucleation process was identified using the acoustic emission method. For monotonic contact loading (single indentation), coating cracks are produced by the excessive plastic deformation of the substrate, itself caused by contact loading, which makes the bending curvature of a coating a critical moment. Subsequently, cyclic contact loading (cyclic indentation) was applied to the coating in order to investigate the cycle number of film cracking. It was found that the critical contact force for coating fracture decreases, compared with that of monotonic loading. This critical force is dependent on the number of loading cycles. This may be due to the fact that cyclic contact loading encourages large plastic deformation of the SUS304 substrate owing to cyclic plasticity. Therefore, the cyclic plastic deformation behavior of the substrate was investigated using cyclic microindentation tests and the finite element method. In the computation, the Chaboche model was employed to compute the cyclic plastic deformation of the substrate, since it simulates cyclic plasticity. We clarified the cyclic contact fracture mechanism of electroplated Ni–P coating on an SUS304 substrate. Based on this, we finally predicted the coating lifetime (i.e., mechanical durability) under cyclic contact loading. Therefore, the present study is useful for obtaining information about film/coating fracture properties under both monotonic and cyclic contact loadings.     

Finite Element Analysis of Ceramic Coatings under Spherical Indentation with Metallic Interlayer： Part Ⅰ Uncracked Coatings

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. Various combinations of indenter radius-coating thickness ratios and interlayer thickness-coating thickness ratios were used in the modeling. The effects of the interlayer, the coating and the substrate on the indentation behavior, such as the radial stress distribution along the coating surface as well as the coating interface, and the plastic deformation zone evolution in the substrate were investigated in connection with the above mentioned ratios. The coating cracking dominant modes were also discussed within the context of the peak tensile stresses on the coating surface and on the coating interface.     

Finite Element Analysis of Ceramic Coatings under Spherical Indentation with Metallic Interlayer: Part Ⅰ Uncracked Coatings

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. Various combinations of indenter radius-coating thickness ratios and interlayer thickness-coating thickness ratios were used in the modeling. The effects of the interlayer, the coating and the substrate on the indentation behavior, such as the radial stress distribution along the coating surface as well as the coating interface, and the plastic deformation zone evolution in the substrate were investigated in connection with the above mentioned ratios. The coating cracking dominant modes were also discussed within the context of the peak tensile stresses on the coating surface and on the coating interface.     

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.     

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.     

钼铜合金表面金镀层的制备及耐高温与焊接性能

为提高钼铜合金表面金镀层的耐高温性与焊接性能,采用置换镀及化学粗化及化学镀镍、最后氰化镀金的方式,在钼铜合金表面制备了金镀层。采用扫描电镜能谱仪分析了镀层形貌及成分,采用金锡焊接的方式测试其焊接性能,按GJB 1941-94考察了其耐高温性能。结果表明:置换镀方式实现了钼铜合金基材界面处元素Mo及元素Cu化学性质的均一性,避免了因化学活性不同所导致的沉积晶体内应力过大的问题;化学粗化增大了钼铜合金基材界面处的比表面积,增加了镀层与钼铜合金基材界面处"机械咬合点"数量,提高了镀层与钼铜合金基材的结合强度。钼铜合金基材表面所得金镀层耐高温性能≥350℃,焊接后空洞率≤30%,满足焊接技术指标要求。     

Mechanical integrity of thin inorganic coatings on polymer substrates under quasi-static, thermal and fatigue loadings

The interplay between residual stress state, cohesive and adhesive properties of coatings on substrates is reviewed in this article. Attention is paid to thin inorganic coatings on polymers, characterized by a very high hygro-thermo-mechanical contrast between the brittle and stiff coating and the compliant and soft substrate. An approach to determine the intrinsic, thermal and hygroscopic contributions to the coating residual stress is detailed. The critical strain for coating failure, coating toughness and coating/substrate interface shear strength are derived from the analysis of progressive coating cracking under strain. Electro-fragmentation and electro-fatigue tests in situ in a microscope are described. These methods enable reproducing the thermo-mechanical loads present during processing and service life, hence identifying and modeling the critical conditions for failure. Several case studies relevant to food and pharmaceutical packaging, flexible electronics and thin film photovoltaic devices are discussed to illustrate the benefits and limits of the present methods and models.     

Numerical interpretation of cone crack initiation trends in a brittle coating on a compliant substrate

Finite element analysis is used to interpret trends in experimentally observed critical loads for contact damage in a brittle (porcelain) coating on a compliant (polymeric) substrate. Different forms of cracking in the brittle layer—both “cone” cracking initiating at the surface, and “radial” cracking at the layer/substrate interface—are considered, with varying coating thicknesses.

The resulting predicted critical loads agree qualitatively with the experimentally observed figures. It is postulated that a previously unexplained peak in critical loads for the onset of cone cracking is caused by a transition between differing modes of cone cracking.     

用涂层压入仪测定薄膜与基体结合强度的探讨

用新颖的能连续加载、卸载并配有声发射监测的涂层压入仪 ,对薄膜与基体的结合强度进行了探讨。实验结果表明 ,膜或膜 /基破坏的声发射信号各有特点 ,可区分压入过程中 (含卸载 )开裂和剥落及其对应的载荷值。压入法的临界载荷 pc 为加载过程中使膜发生初始剥落的外载 ,用涂层压入仪可精确测定。 pc 值对基体硬度和表面粗糙度的变化敏感。故用涂层压入仪可以实现用压入法考察膜 /基结合强度     

A study towards improving mechanical properties of sol-gel coatings for polycarbonate

Scratch-resistant coatings based on 3-glycidoxypropyltrimethoxysilane and tetraethylorthosilicate with a cross-linking agent and different amounts of colloidal silica are prepared on polycarbonate substrates by sol-gel technique. The failure mode of this type of coating on soft plastic substrate under pencil scratch test is studied. It is found that the pencil scratch failure contains a gouge failure under the static pressure and a film cracking failure under the sliding of the pencil tip. The gouge failure is due to the early plastic deformation in the substrate, while the film cracking is due to the tensile stress in the film induced by the sliding and friction of the pencil tip. Factors influencing the static gouge failure and sliding cracking failure are investigated. It is found that the cross-linking agent and colloidal silica filler increase the intrinsic cross-linking, hardness, elastic modulus and fracture toughness of the coating material, therefore, reduce the film cracking tendency; whereas the increased layer thickness and multi-layer coating improve the pencil scratch resistance significantly via delayed plastic deformation in the substrate. Based on these analyses, we conclude that the main factors towards improved pencil scratch resistance are: layer thickness, elastic modulus, fracture toughness and intrinsic hardness of the coating material. Pencil hardness is increased from grade 2B to 5H by adjusting these parameters.     

Modeling of multiple cracking and decohesion of a thin film on a polymer substrate

Thin brittle films on polymer substrates are finding increasing use as gas barriers for example in the medical and food packaging industries and also for the next generation of ultra-light displays based on flexible polymer substrates. In order to determine the durability of the barrier under thermal and mechanical loads, test procedures and corresponding data reduction methods are needed to feed the analysis models. One of the tests frequently employed for this kind of multi-layer material systems is the fragmentation test, whose designation comes from the progressively denser pattern of parallel cracks developing when the specimen is loaded under uniaxial tension. From the crack-density versus strain data obtained, a critical strain for crack growth and an assessment of the adhesion of the coating to substrate can be obtained. However, no accepted data reduction methods exist to extract material properties from the test or inversely, successfully predict the crack density as a function of a set of material properties without fitting parameters. In an earlier paper, the authors presented a finite element based analysis methodology to determine the fracture toughness of both the coating and the interface from the fragmentation data. In the simulations, the plastic constitutive behavior of the substrate and the debonding of the coating from the substrate were explicitly included, the latter by use of a cohesive zone model. In this paper an extension of this methodology is presented that enables crack-density evolution with strain to be predicted. The results presented comprise comparisons with experiments to validate the methodology and the influence of (i) coating toughness, (ii) interface toughness and (iii) coating thickness on crack density versus strain.     

镶嵌结构界面金刚石涂层研究进展

对平面结构和镶嵌结构界面金刚石涂层的界面结构特点、受弯曲应力应变时的失效方式进行了分析,指出镶嵌结构界面金刚石涂层是提高膜/基体结合力的有效方法;综述了镶嵌结构界面金刚石涂层的国内外研究现状,并指出了今后镶嵌结构界面金刚石涂层的发展方向。     

冷喷涂304不锈钢涂层的弯曲力学行为研究

采用冷喷涂(CGDS)技术在IF钢基体上制备304不锈钢涂层.用SHIMADZU液压伺服疲劳试验机对304不锈钢涂层样品进行三点弯曲实验,用扫描电子显微镜来研究冷喷涂304不锈钢涂层的断裂行为.结果表明:冷喷涂304不锈钢涂层的断裂行为为脆性断裂;裂纹萌生于涂层表面,随着载荷和力矩的增加,裂纹向涂层内部扩展,裂纹在涂层...     

Mechanical and electrical behaviors of polymer particles. Experimental study of the contact area between two particles. Experimental validation of a numerical model

The present paper is devoted to the analysis of mechanical and electrical behaviors observed on particulate polymer granular materials. The constituting particles obtained these physical properties by coating the polymer spherical substrate with a conducting polymer: polypyrrole (PPy) which confers electrical conducting properties to the particle, while preserving its mechanical properties. Particle contacts dominate the behavior of the granular media and, consequently, size, morphology, roughness and plasticity of the particles play a crucial role in this behavior. Scanning electron microscope (SEM) and atomic force microscope (AFM) were used to study the surface state and the contact area between neighbors. An experimental set up, based on the measurement of the displacement of contacting particles subjected to a normal force and of the variation of the electrical resistance of the packing, allowed the study of both the mechanical and electrical behaviors of the particle system. The experimental results took into account the plastic deformation under varying loading and unloading conditions; they were consistent with theories of contact mechanics, thus validating the existing models.     

A numerical study of contact damage and stress phenomena in curved porcelain/glass-filled polymer bilayers

Finite Element Analysis is used to examine contact damage induced by Hertzian indentation of a porcelain coating on a glass-filled polymeric substrate. Different forms of cracking in the porcelain coating are studied –“Hertzian” cone cracks close to the indenter, more distant “outer” cone cracks, and “radial” cracking at the coating/substrate interface. The effects of porcelain coating thickness and radius of curvature on the critical stresses for initiation of these cracks are examined. The predicted critical load curves suggest that for systems with compliant substrates (relative to the coating) with a given radius of curvature, there is an optimum porcelain coating thickness that maximises the critical load for cone cracking. Conversely, for a given coating thickness, the effects of curvature vary significantly – for thinner coatings, where outer cone cracks are dominant, highly convex surfaces are more resistant to cracking, whereas for thicker coatings, which are more prone to Hertzian cone cracking, concave surfaces produce a higher predicted critical load. Curvature is observed to have little effect on the critical load for the formation of radial cracks, which remains the dominant mode of failure in cases of thin coatings on compliant substrates.     

Mechanical and thermal properties of physical vapour deposited alumina films Part II Elastic, plastic, fracture, and adhesive behaviour

Two mechanical characterization techniques were used to deduce the elastic, plastic, fracture, and adhesive properties of non-reactive physical vapour deposited alumina films of varying thickness on Al₂O₃-TiC substrates deposited at two different substrate biases. Depth-sensing indentation at both nano- and macroscopic load scales was used to determine the elastic and plastic properties of the films. Gravity-loaded Vickers indentation was performed to examine the fracture properties of the film and of the interface. Novel fracture mechanics models were developed to describe indentation-induced film fracture by channel cracks and indentation-induced interface delamination. The former model was used to determine the film toughness and the latter model was used to deduce the interfacial fracture resistance of the films and correctly predicted the effect of changing film thickness. Both models described the measured crack lengths with indentation load well and were used to identify the transition from radial and lateral cracking to channel and interfacial cracking.     

Crack initiation at free edge of interface between thin films in advanced LSI

Since electronic devices are made of multi-layered sub-micron films, delamination along the interface is one of the major failure mechanisms. This paper aims to develop a method for evaluating the mechanical criterion of interface cracking between thin films on a substrate. The focus is put on crack initiation from the free edge of the interface where the stress concentrates due to the mismatch of elastic deformation. In the evaluation, it is important to exclude plastic deformation and fracture of the thin metal film, because they bring about ambiguity on the measured magnitude of interface strength. In this study, an experimental method is proposed on the basis of fracture mechanics concepts, and the validity is examined by tests on Cu (conductor metal)/TaN (barrier metal) interface in a large-scale integrated circuit. The critical stress intensity at delamination crack initiation is successfully analyzed by the boundary element method.     

玻璃纤维/环氧树脂复合材料与镀层界面的Ni颗粒强化工艺

针对玻璃纤维/环氧树脂复合材料与镀层结合界面强度低的问题,基于复合材料/镀层间的机械互锁原理及传统塑料基体化学镀工艺,提出通过增强颗粒的桥接作用,增加含有增强颗粒的过渡层来强化镀层界面的复合材料金属化方法。对金属化后的玻璃纤维/环氧树脂复合材料试件采用拉伸试验法测量镀层的结合强度,并通过截面和断面的显微观测,分析了增强颗粒对于镀层界面的强化机制;同时获得了玻璃纤维/环氧树脂复合材料表面粗糙度和增强颗粒质量分数对含有过渡层的镀层结合强度的影响规律。结果表明:采用上述金属化方法可以显著提高镀层的界面强度,与传统的金属化工艺制备试件相比,玻璃纤维/环氧树脂复合材料在不同表面粗糙度下,镀层结合强度平均提高161%;同时,镀层的结合强度随着增强颗粒质量分数的增加,呈现先增大后减小的趋势,当增强颗粒的质量分数为50%时,镀层的结合强度达到最大。      

Coatings with intrinsic stress profile: Refined creep analysis of (Ti,Al)N and cracking due to cyclic laser heating

A refined non-linear creep analysis of ceramic coatings has been performed by means of an improved substrate curvature technique in vacuum facilitating increased sensitivity by noise reduction. In this way the intrinsic stress profile may be derived from the time-dependent substrate curvature. Creep and stress parameters of 0.5 μm (Ti,Al)N-coatings have been found. At 500 °C the stress varies between − 1 GPa at the surface and + 0.2 GPa at the interface with the silicon substrate. From the onset of crack formation as observed in cyclic laser shock experiments a coating tensile strength of about 0.7 GPa is deduced. The number of cycles to cracking and delamination/spalling vs. maximum coating temperature as derived from creep simulation agrees quantitatively rather well with the experimental data. A rough estimate of the interface fracture toughness on WC/Co substrates yields 11 N/m as a lower bound.     

An interface crack in a coating-substrate composite with mixed-mode Dugdale corrections

Considering both plane stress and plane strain conditions, the plastic zone size and the crack tip opening displacement of an interface crack between a coating and a semi-infinite substrate under a normal load on the crack surfaces are investigated by the mixed-mode Dugdale model. In the model, stresses applied in the plastic zones satisfy the Von Mises yield criterion. The plastic zone size can be calculated by satisfying the condition that the complex stress intensity factors vanish. After the plastic zone size is solved, the crack tip opening displacement can be obtained by dislocation theories. In numerical examples, a uniform load is considered, and the effects of the normalized elastic modulus (the ratio of the elastic modulus of the coating to the elastic modulus of the substrate) and the normalized crack depth (the ratio of the coating thickness to the interface crack length) on the normalized plastic zone size and the normalized crack tip opening displacement are examined. Numerical examples show in the case of thin coatings, the value of the normalized plastic zone size decreases with increasing the normalized elastic modulus.