Theoretical analysis of the thermally induced delamination of polymeric coatings in double-coated optical fibers

To maintain its mechanical strength, the glass fiber of optical fibers is coated by polymeric materials during the fabrication process, However, when the thermally induced shear stress at the interface of the glass fiber and primary coating is larger that its adhesive stress, the adhesive bond between the glass fiber and primary coating will be broken. When the polymeric coatings are delaminated from the glass fiber, the optical fiber will lose its mechanical strength. In this article, the thermally induced delamination of polymeric coatings in double-coated optical fibers is investigated. To minimize the coating's delamination, the thermally induced shear stress at the interface of the glass fiber and primary coating should be reduced. The method to minimize such a shear stress is to select suitable polymeric coatings as follows: The thickness and Poissòn's ratio of the primary coating should be increased, but the Young's modulus of the primary coating and the thickness, Young's modulus, and thermal expansion coefficient of the secondary coating should be decreased. Finally, the optimal design of commercialized double-coated optical fibers to minimize the thermally induced coating's delamination is also discussed.     

Determination of Quasiequilibrium Work of Adhesion of Elastic Coatings

Present methods for the determination of adhesion bonding of elastic polymeric materials entail certain experimental difficulties. In particular, the necessity of strict centering of the test specimen, and the difficulty associated with application of a homogeneously distributed stress over the whole cross-sectional area (homogeneous detachment or shear), or the excessive expenditure of work resulting from polymer deformation (peel).^1,2

We are suggesting a method to determine the quasi-equilibrium work of adhesion during the peeling process for elastic polymeric coatings, the value of which, as was demonstrated experimentally, does not depend on the coating thickness, deformation or rate of peeling.     

Effect of microstructure on the adhesion strength of TiBx coating on Ti6Al4V substrate

TiB_x coatings were deposited on Ti6Al4V and Si (100) wafer substrates by D.C. magnetron sputtering with various target-to-substrate distances (T.S. distances) from 50 mm to 200 mm. The influence of T.S. distance on the microstructure, hardness and adhesion strength of TiB_x coatings and Ti6Al4V substrate system was investigated. Results showed that the microstructure of TiB_x coatings transformed from dense to fibre columnar grain with the increase in T.S. distance, whilst the hardness decreased from 20.9 GPa to 9.4 GPa. The Rockwell-C indentation adhesion strength grade was also improved from HF6 to HF1. An adhesion evaluation factor G, which is related to the mechanical properties and the microstructure of TiB_x coating, is proposed based on the test results. The adhesion strength increased with G, which corresponded well with the results of indentation test. The high-speed rubbing test with a sliding speed of 300 m/s was performed to check the Al-adhesion resistance of the TiB_x coating against Al–hBN seal coating.     

Adhesion of diamond coatings on steel and copper with a titanium interlayer

Adherent diamond coatings on steel and copper were obtained by using a titanium interlayer. The adhesion of the coatings was evaluated by scratch tests and micro-indentation tests. The diamond coating on steel exhibited a much higher critical load than on copper, as revealed by the scratch tests. However, an observation on the back of the scratch-delaminated film and on the corresponding substrate surface showed that the detachment occurred between the diamond film and the titanium interlayer. Therefore, the difference in the critical scratch load is due mainly to a substrate effect, making it difficult to compare the adhesion of different coatings.On the other hand, Knoop indentation tests showed interesting results: a small indentation load causes round spallation in the film with no observable crack. An exponential sink-in deformation under the indentation is proposed, y=−a exp(−bx). The coating adhesion is considered to be equivalent to the deformation stress at the edge of the spallation zone. The adhesion of diamond coatings on steel and copper with a titanium interlayer is evaluated quantitatively using this model. Furthermore, a thermal quench method is proposed to estimate the coating adhesion. The results found are in agreement with the indentation model.     

Analysis of the mechanical properties of TiN/Ti multilayer coatings using indentation under a broad load range

In this study, physical vapor deposition was used to prepare TiN/Ti multilayer coatings as well as the corresponding monolithic coatings for comparison. Nanoindentation using a large load range (5–4800 mN) and finite element method (FEM) simulations were conducted to investigate the influence of various multilayer structures on the mechanical behavior of multilayer coatings. The nanoindentation results show that the TiN/Ti multilayer coating has the maximum hardness and Young's modulus while retaining good crack resistance and fracture toughness. The FEM results show that increasing the number of layers in the multilayer coatings reduced the hardness and Young's modulus as well as the maximum stress, while it increased the equivalent plastic strain. As the layer thickness ratio increased, both the hardness and Young's modulus gradually increased, and the stress in the coating reached its maximum at the highest thickness ratio. In addition, to consider the effect of the indentation depth on the coating, the influence of the number of layers and the layer thickness ratio on the multilayer coating is combined into the indentation response of the multilayer coating. Therefore, we establish an expression describing the relationship between the number of layers and the ratio of the layer thickness to the mechanical properties of TiN/Ti multilayer coatings.     

The influence of aluminium surface pretreatment on the corrosion stability and adhesion of powder polyester coating

One of the most important factors in corrosion prevention by protective coatings is the coating adhesion loss under environmental influence. Thus, adhesion strength is often used when characterizing protective properties of organic coatings on a metal substrate. In order to improve the adhesion of organic coating the metal substrate is often pretreated in some way. In this work, the adhesion of polyester coatings on differently pretreated aluminium surface (by anodizing, with and without sealing, by phosphating and by silane film deposition) was examined. The dry and wet adhesion of polyester coatings were measured by a direct pull-off standardized procedure, as well as indirectly by NMP test. It was shown that under dry test conditions all polyester coatings showed very good adhesion, but that aluminium surface pretreated by silane film showed superior adhesion. The overall increase of wet adhesion for polyester coating on aluminium pretreated by silane film was maintained throughout the whole investigated time period. The different trends in the change of adhesion of polyester coatings were observed for different aluminium pretreatments during exposure to the corrosive agent (3% NaCl solution). The highest adhesion reduction was obtained for polyester coating on aluminium pretreated with phosphate coating. The corrosion stability of polyester coated aluminium was investigated by electrochemical impedance spectroscopy in 3% NaCl solution. The results confirmed good protective properties of polyester coating on aluminium pretreated with silane film, i.e. greater values of pore resistance and smaller values of coating capacitance were obtained in respect to other protective systems, whereas charge-transfer resistance and double-layer capacitance were not measurable during 2 months of exposure to a corrosive agent.     

Evaluation techniques and improvements of adhesion strength for TiN coating in tool applications: a review

The adhesion between coating-substrate systems is an important factor in determining the performance and durability of coated engineering components. This paper reviews the microstructures and adhesion strength of titanium nitride (TiN) coating produced using two different processing methods: chemical vapor deposition and physical vapor deposition. Three methods to evaluate the adhesion strength of the coatings, namely the indentation test, laser spallation technique, and scratch test are presented and discussed in terms of their working principles, their advantages and disadvantages. The extrinsic and intrinsic factors influencing the adhesion strength of coating-substrate system, particularly for TiN coating, are also elaborated. The mechanisms and modes of coating failures in adhesion evaluation techniques are discussed with respect to the variation of coating-substrate system combination such as brittle, ductile, soft, and hard. Possible improvements on the adhesion strength of coating-substrate systems, focusing on the processing methods, compositions, and structures of coatings, are also reported.     

Evaluation of the bond strength of hard coatings by the contact fatigue test

The conventional contact fatigue test was applied to evaluate the bond strength between hard coatings and substrates. It was designated as an interfacial fatigue test for coated samples and was conducted with either cylindrical or spherical rolling. A shear stress range at the interface was derived based on the mechanics of elasticity and used as a measure of the interfacial fatigue strength between the coating and the substrate. It was found that the coating exfoliated after the coated specimen was subjected to a number of cycles under cyclic contact loading, but it would be intact when the cyclic load was decreased to a critical value. The shear stress range corresponding to this critical load was defined as the bond strength which would reflect the change in the physical and/or chemical state in the interfacial region. In the calculation of the shear stress range, the effects of the thickness and Young's modulus of the coatings were taken into account.     

Effects of tailored nitriding layers on comprehensive properties of duplex plasma-treated AlTiN coatings

Duplex-treated AlTiN coatings were deposited by advanced plasma assisted arc (APA-Arc) technology on pre-plasma nitrided AISI-H13 steel substrates using different N₂/H₂ flow ratios. The microstructures and properties of the AlTiN coatings were comprehensively characterized and analyzed. The results show that the N₂/H₂ flow ratios can tailor the thickness of compound layer during plasma nitriding process and the bright nitriding layer without compound layer is achieved. The properties of duplex-treated AlTiN coatings are well improved compared with monolayer AlTiN coating. The adhesion of the AlTiN coating is well enhanced by duplex treatment process, and adhesion grade increases from HF3-4 for monolayer AlTiN coating to HF1 for composite coatings. Moreover, the composite coatings with various thickness compound layers show different load-bearing capacities, and the interfacial adhesion force of the composite coating without compound layer reaches 61 N. The hardness of AlTiN coating is also enhanced by duplex treatment with the highest hardness of 2935 HV_0.05. Meanwhile, tribological properties of AlTiN coatings are also slightly improved by duplex treatments.     

Nanoindentation-induced delamination of submicron polymeric coatings

An elastic model is developed to estimate the interfacial strength between a submicron surface coating and a compliant substrate. The analysis uses a shear-lag model and assumes the plane-stress state in the surface coating. The critical indentation load for the indentation-induced delamination of the coating from the substrate increases with the third power of the indentation depth and is a linear function of the reciprocal of the coating thickness. The indentation-induced delamination of SR399 ultrathin surface coatings over acrylic substrate has been evaluated, using the nanonindentation technique for coating thicknesses of 47, 125, 220 and 3000 nm. For the submicron coatings, the dependence of the critical indentation load on the coating thickness supports the elastic model. The interfacial strength is found to be 46.9 MPa. In contrast, the polymeric coating of 3000 nm displays multiple “excursions” in the loading curve, and the critical indentation load is a linear function of the indentation depth.     

Layer-by-layer modification of thermoplastic coatings to improve adhesion

One of the causes leading to low bond strength between a coating and a substrate (adhesion strength) - if coatings are formed at elevated temperatures in air - is assumed to be a weak boundary layer generated in the region of adhesional contact: the boundary layer consisting mostly of low-molecular-weight products resulting from thermal oxidative degradation of the polymer. It has been verified experimentally that products of oxidation diffuse from the coating surface layer to the contact area. The oxidation process is supposed to be localized within that surface layer. A method has been devised to determine the thickness of the layer, and model experiments have been conducted to show that low-molecular-weight products of oxidation deteriorate the adhesion strength. Ways have been found to increase the adhesion strength of coatings by means of modification of the coating applied in a layer-by-layer manner. The idea is to introduce separately such modifiers as antioxidants, inorganic fillers possessing high adsorption capacities, and crosslinking agents into the coating surface layer. This method of coating modification allows one to eliminate the negative effects of the low-molecular-weight products generated in the surface layers during the formation.     

A compression test for adhesion evaluation of diamond coatings

A key requirement of an effective coating is its adequate adhesion to the substrate. Thus, reliable test methods to evaluate coating adhesion and to characterize the deposition parameters affecting it are necessary for the systematic development of such coatings. The conventional technique for measuring diamond coating adhesion, the scratch test, is unreliable because of wear of the stylus and influences of the substrate. Thus, a noncontact technique (compression test) of evaluating the adhesion of diamond coatings on brittle substrates was modelled and developed. This method utilizes the differences in Young's modulus between the coating and the substrate via application of an external load in order to generate interfacial stresses and debond the coating. An innovative three-dimensional numerical model, based on combining the variational and boundary integral approaches, was utilized to link the indirect (i.e. load) to the direct (i.e. debond shear stress or elastic energy of delamination) characteristics of adhesion. Factors affecting the adhesion strength of the diamond coatings are discussed in relation to the process parameters. This test offers an excellent alternative to conventional techniques for measuring the adhesion strength of diamond coatings on brittle substrates.     

Damage resistance of SiC and Si3N4 coatings with control of microstructure and thickness

We investigated the contact damage and indentation stress–strain behavior of silicon carbide (SiC) coatings and binary coatings consisting of SiC and silicon nitride (Si₃N₄), synthesized on graphite substrates with porosities of 10 and 13% by a solid–vapor reaction, in order to determine the coatings’ damage resistance. The coating thickness was affected by the porosity of the substrate. The coatings on the substrate with 13% porosity showed a graded interface structure below the top dense layer. The SiC coatings were thicker than the SiC/Si₃N₄ composite coatings. The SiC coatings made the substrates hard, and SiC-coated substrates exhibited higher stress–strain curves than the substrates alone, but the SiC/Si₃N₄ composite coatings appeared unaffected. The coating thickness played an important role in limiting the effect of damage. The hardness values of the SiC coatings were higher than those of the substrates and the SiC/Si₃N₄ coatings. These corresponded well with the indentation stress–strain curves. The values of each coating showed saturated points depending on the applied load. This indicated that the substrate itself influenced the damage resistance of the coatings because of the layered structure of a harder coating with a softer substrate. The coatings enhanced contact damage and transmitted the damage to the substrates at a high load of P = 2000 N. Both coatings showed an extensive subsurface damage, independent of the porosity of the substrate. In cyclic indentation tests, the contact diameters linearly increased with the number of cycles and depended on the porosity of the substrate, showing smaller contact diameters by coating the substrate.     

紫铜基体上组合电刷镀厚镍层的工艺

研究了快速镍、低应力镍刷镀时间对紫铜表面镍镀层的厚度、显微硬度及结合强度的影响。单层快速镍及单层低应力镍较适宜的刷镀时间为15～20min。采用15min快速镍与15min低应力镍交替组合刷镀镍,所得镍镀层的厚度、显微硬度及耐淬火次数分别达50μm、400HV及46次,镀层组织清晰而均匀,镀层与镀层之间、镀层与基体之间结合良好,符合理想厚镍镀层的性能要求。     

Cracking analysis of HVOF coatings under Vickers indentation

The fracture strength of five HVOF coatings, which are made of hard metals, Tribaloy alloy, and superalloys, respectively, coated on 1018 low carbon steel substrate, is studied under Vickers indentation, associated with FEA stress computation. The cross sections of the coating specimens are examined on a Hitachi Model S-570 scanning electron microscope (SEM), which investigates the quality and measures the geometry of the coatings. The mechanical properties of the coatings and the substrate are determined in the cross sections using the nano-indentation technique. The cracking behavior of the coatings under different indentation loads is investigated using a Vickers hardness tester. Three-dimensional finite element analysis (FEA) simulation of the Vickers indentation test is conducted to determine the stress fields in the coating/substrate systems in order to understand the fracture mechanisms of the coatings under the indentation loads using the ABAQUS software package. The FEA stress results are in good agreement with the experimental observation of Vickers indentation.     

Adhesion of calcium phosphate coatings on polyethylene (PE), polystyrene (PS), poly(tetrafluoroethylene) (PTFE), poly(dimethylsiloxane) (PDMS) and poly-L-lactic acid (PLLA)

Calcium phosphate (CaP) coatings can be applied to improve the biological performance of polymeric medical implants. For clinical applications, a strong adhesion of the coating to the polymeric substrate is important. Therefore, the adhesion of rf magnetron-sputter-deposited CaP coatings on five polymers was studied: polyethylene (PE), polystyrene (PS), poly(tetrafluoroethylene) (PTFE), poly-L-lactic acid (PLLA) and poly(dimethylsiloxane) (PDMS). To influence the adhesion, the interface was varied in six different ways, e. g. by a plasma or ion-beam pretreatment, or by using a Ti interlayer. The adhesion was determined by using scratch, tensile and 180^° bend tests. Especially the polymers PE and PS needed a bombardment by energetic particles prior to or during coating deposition, to enable the formation of chemical bonds between the coating and the polymer, which gave adhesion. On PLLA and PDMS, being oxygen containing polymers, it was easier to establish a strong interface. An overtreatment of the polymeric substrates gave worse adhesion, probably due to the formation of weak low molecular weight (LMW) layers on the polymer. On PTFE, the use of a Ti interlayer was necessary to prevent the PTFE from UV degradation during coating deposition, as this caused cohesive failure within the PTFE. The results showed that each polymer requires a different approach for obtaining optimal adhesion. The observed adhesion could often be explained in the terms of processes occurred during the pretreatment of the polymers or the deposition of the coating.     

Adhesion improvement of RF-sputtered alumina coatings as determined by the scratch test

One of the most important problems to overcome in the production of coatings, a major technology in surface modification, is the maximization of coating to substrate adhesion. In spite of its limitations, the scratch technique is most used in adhesion characterization studies. In this study, the adhesion of alumina coatings deposited by RF magnetron sputtering on AISI M2 high speed steel (HSS) was evaluated by the scratch test. An attempt to improve the adhesion of the alumina coatings was investigated by the deposition of an intermediate layer of Ti or TiN. The influence of the substrate surface roughness, the intermediate layer thickness, and the sputter etch cleaning on the coating adhesion was studied.     

铝合金车轮涂膜压痕影响因素研究

为探究铝合金车轮表面涂膜压痕产生因素,根据铝合金车轮涂膜表面压痕状态,表征了涂膜硬度、涂层固化度、涂层组分等性能,研究了涂装工艺及包装工艺对铝合金车轮涂膜表面压痕的影响。结果表明：仓储运输过程中车轮表面温度为影响压痕的主要因素,温度超过 45 ℃将大幅度提升压痕产生概率;涂料相变点硬度变化是压痕产生的根本原因,通过控制车轮包装温度、储存温度、运输温度可以杜绝压痕产生;延长包装后日光下存放时间会增加压痕产生概率。     

Effect of five kinds of pores shape on thermal stress properties of thermal barrier coatings by finite element method

Thermal ablation is a very important technique to characterize the thermal properties of coating systems. On account of the concentration of thermal stress, thermal barrier coatings (TBCs) often break off from the substrate partly or completely during the thermal erosion. In this paper, the thermal erosion simulation of finite element geometric models based on the possible pore shapes were implemented, especially, the influence of pore shapes on the distribution of coating temperature, X component of stress, Y component of stress, XY-shear stress and von-Mises stress were focused on. The effects of the different porosity of square pore coatings on thermal insulation properties and thermal stresses were discussed in term of the simulation results. The simulation results indicate that different shape pores not only affect the thermal stress distribution above the contact area between the bond coating and top coating surface, but also affect the plastic deformation behavior of TBCs. The micromechanism was discussed in details in this study. The computed results verified that, the computational method can successfully predict thermal shear, crack initiation and normal failure mode of the studied TBCs. All the results are in good agreement with the corresponding experimental findings. The failure mechanism factors in this paper are of great importance to explain the failure micro-mechanism of TBCs.     

Comparison of the adhesion of diamond films deposited on different materials

Indentation tests combined with acoustic emission spectra were used to compare the adhesion of diamond films deposited on various substrates, including Ti, Cr, Si and Ti coated Cu. We show that indentation in the diamond coatings may cause the following failure modes: (a) the substrate cracking; (b) the film cracking and localised detachment; and (c) the film delamination and the delamination propagation. Acoustic emission during indentation loading provided essential information in predicting what mode of failure occurs. Combined with the acoustic emission spectra, the indentation tests are reliable in comparing the adhesion of diamond films deposited on the same or similar substrate materials. However, the comparison of the film adhesion on very different substrates, like Cu and Ti, is not so straightforward. Acoustic emission spectra also revealed that indentation caused substrate cracking prior to the failure of the film/substrate interface for diamond coatings on Si. In this case, the indentation tests are not valid to compare the coating adhesion.