Experimental study on buckle evolution of thin inorganic layers on a polymer substrate

In this paper the behavior of a 250 nm and a 350 nm thick Indium tin oxide (ITO) layers deposited on a 200 μm thick high temperature aromatic polyester substrate (Arylite™) and spin coated with a 3 μm silica-acrylate hybrid coating (Hard Coat) is discussed. In-situ optical microscopy of the layered structures under uniaxial compressive strain was used to determine the buckle delamination rate at different applied strains. The effect of applied uniaxial compressive strain and layer thickness on the evolution of buckle width and height was investigated. The biaxial-residual stress, uniaxial compressive stress, poor adhesion at the interface and Poisson’s ratio are believed to be responsible for the formation of telephone-cord buckling.     

Effect of a hard coat layer on buckle delamination of thin ITO layers on a compliant elasto-plastic substrate: An experimental–numerical approach

Layer buckling and delamination is a common interfacial failure phenomenon in thin film multi-layer structures that are used in flexible display applications. Typically, the substrate is coated on both sides with a hybrid coating, called a hard coat (HC), which acts as a gas barrier and also increases the scratch resistance. In this paper 250 nm thick indium tin oxide (ITO) layers have been deposited on a 200 μm thick high temperature aromatic polyester substrate (Arylite^TM), with and without a 3 μm HC. In order to study the influence of this HC layer on delamination phenomena, two-point bending experiments are performed from which buckle width and height values are measured after straightening of the sample. An analytical model and a finite element (FE) model are developed to estimate the adhesion properties from the measured buckle geometries. In the numerical model, the initiation and propagation of the delamination process is described by cohesive zone elements, of which the parameters are extracted from response surface model (RSM) results. Furthermore, the numerical model is used to illustrate the significant change in buckle geometry upon load reversal, i.e. from loaded to straightened state, which is governed by the elasto-plastic behavior of the substrate material. It is concluded that the addition of a HC layer significantly decreases the adhesion of the ITO layer. The latter is determined as function of the actual mode angle.     

Effects of substrate compliance on circular buckle delamination of thin films

The present work analyzes circular delamination buckling in a film/substrate system based on the Von Karman nonlinear plate theory with the consideration of elastic deformation of the substrate. Due to the axisymmetry of circular buckling, the substrate deformation is modeled by coupled springs and the spring compliances are determined from the dimension analysis and finite element calculations. The numerical shooting method is used to solve the nonlinear post-buckling problem. The stress intensity factors, the energy release rate, and the phase angle are given here for a variety of the elastic mismatch between the film and the substrate. The results show that in some cases, the energy release rate can be several times larger than that derived from the widely used clamped edge condition.     

Elastic anisotropy effect on indentation-induced thin film interfacial delamination

Effect of elastic anisotropy on indentation-induced thin film interfacial delamination, especially, at the initiation and early growth stage, is examined. The indentation load is modeled as a constant pressure over an expanding semi-spherical cavity. The delamination process is approached by a cohesive zone model. The rest of the problem is formulated within the general anisotropic elasticity theory, and solved numerically by the boundary element method employing a special Green’s function for multilayers. The material system of a Cu(0 0 1) film on a Si(0 0 1) substrate is studied as an example. The interfacial damage initiation and crack development under indentation are captured in the simulation. By comparing the predictions with the materials being modeled as isotropic and as anisotropic (of the cubic symmetry as they are), it is shown that the elastic anisotropy of the copper film plays a significant role in determining the delamination pattern. In the isotropic model, the delamination crack fronts are circular reflecting the problem axisymmetry. In contrast, crack fronts are square with rounded corners in the anisotropic case. This significant difference necessitates a three-dimensional anisotropic stress analysis of the indentation-induced delamination of strongly anisotropic films.     

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.     

Influence of interfacial delamination on channel cracking of elastic thin films

Channeling cracks in brittle thin films have been observed to be a key reliability issue for advanced interconnects and other integrated structures. Most theoretical studies to date have assumed no delamination at the interface, while experiments have observed channel cracks both with and without interfacial delamination. This paper analyzes the effect of interfacial delamination on the fracture condition of brittle thin films on elastic substrates. It is found that, depending on the elastic mismatch and interface toughness, a channel crack may grow with no delamination, with a stable delamination, or with unstable delamination. For a film on a relatively compliant substrate, a critical interface toughness is predicted, which separates stable and unstable delamination. For a film on a relatively stiff substrate, however, a channel crack grows with no delamination when the interface toughness is greater than a critical value, while stable delamination along with the channel crack is possible only in a small range of interface toughness for a specific elastic mismatch. An effective energy release rate for the steady-state growth of a channel crack is defined to account for the influence of interfacial delamination on both the fracture driving force and the resistance, which can be significantly higher than the energy release rate assuming no delamination.     

Hybrid spectral/finite element analysis of dynamic delamination of patterned thin films

A combined spectral and finite element analysis is performed to investigate the dynamic edge delamination of patterned thin films from a substrate. The analysis is motivated by an emerging experimental technique in which high-amplitude laser-induced stress waves initiate progressive interfacial debonding of thin film interfaces. The numerical method relies on the spectral representation of the elastodynamic solutions for the substrate and the finite element model for the thin film. A cohesive model is introduced along the interface of the bimaterial system to capture the decohesion process. The important role of the film inertia on the crack extension and the appearance of the mixed-mode failure are demonstrated by observing the traction stress evolution at various points along the bond line. Parametric studies on the effect of film thickness, interface fracture toughness, loading pulse shape and amplitude on the debonding process are performed. A semi-analytical investigation on the inertial effect is carried out to predict the final crack length as a function of the film thickness and pulse amplitude.     

A novel cylindrical punch method to characterize interfacial adhesion and residual stress of a thin polymer film

Adhesion of a pre-stressed silicone rubber film to a planar graphite surface was investigated by a new cylindrical punch method. A homemade apparatus was constructed to meet force and displacement resolutions of 0.1 μN and 10 nm. When the punch approached the intersurface force range across the punch-film gap, the film jumped into contact at “pull-in”. Upon unloading, once the tensile load reached a threshold, a spontaneous delamination occurred at “pull-off” with a non-zero contact circle. A theoretical model was constructed based a simple energy balance. The new method can be used to characterize an adhesion interface between a pre-stressed free-hanging film and a rigid substrate.     

Hydrogen effect on fracture toughness of thin film/substrate interfaces

The effect of hydrogen on the interface fracture toughness of two nano-film/substrate structures, Ni/Si and Cu/Si, were evaluated using four-point bend specimens with and without hydrogen charging. Hydrogen typically decreases the fracture toughness of materials. However, we found in this study that the interfacial toughness between the Ni film and the Si substrate increased due to the presence of hydrogen, while that of Cu/Si decreased. Nanoindentation experiments for the Ni and Cu films revealed that local plasticity in the Ni and Cu films is promoted by the charged hydrogen. The critical stress intensity at the Ni/Si interface crack considering the plasticity of Ni, namely the true fracture toughness, is scarcely influenced by the existence of hydrogen. The apparent increase in fracture toughness of the Ni/Si interface is due to the large stress relaxation near the crack tip caused by softening due to the presence of hydrogen. Although the promotion of plastic deformation of Cu relaxes the stress intensity at the Cu/Si interface crack, the apparent interfacial toughness still decreases because of the significant decrease in the true toughness due to the presence of hydrogen.     

无机薄膜电致发光器件中绝缘层材料的研究

薄膜电致发光（TFEL）技术将戍为平板显示技术的潮流和主体。简要介绍了平板显示技术的发展，同时对无机薄膜电致发光器件中绝缘层材料的选择进行了探讨。     

A spectral scheme for the simulation of dynamic mode 3 delamination of thin films

Motivated by recent developments in laser-induced spallation testing of thin film structures, we develop a spectral scheme for the simulation of dynamic failure of thin films. In this first study, we focus on the anti-plane shear (mode 3) loading case. The scheme relies on an exact spectral representation of the elastodynamic solutions in the substrate and in the film, and their combination through interface conditions that involve general cohesive failure and/or frictional contact models. A detailed modal analysis of the response of a single spectral mode is performed to assess the stability and precision of the resulting numerical scheme. A set of dynamic fracture problems involving non-propagating and propagating cracks are simulated to show the ability of the numerical scheme to capture the effect of wave reflection on the near-tip stress and displacement fields, and on the dynamic motion of a crack along the film/substrate interface.     

The surface effect on the strain energy release rate of buckling delamination in thin film-substrate systems

Gurtin-Murdoch continuum surface elasticity model is employed to study the buckling delamination of ultra thin film-substrate system. The effects of surface deformation and residual stress on the large deflection of ultra thin film are considered in analysis. A concept of effective bending rigidity (EBR) for ultra thin plate is proposed on the basis of Gurtin-Murdoch continuum theory and the principle of minimum potential energy. The governing equations with EBR are formally consistent with the classical plate theory, including both small deflection and large deflection. A surface effect factor is introduced to decide whether there is need to consider the surface effect or not. Combining the buckling theory and interface fracture mechanics, we obtain analytical solutions of the critical buckling load and the energy release rate of the interface crack in the film-substrate system. It is seen that the surface deformation and residual stress have significant effects on the buckling delamination of ultra thin film-substrate system.     

A shaft-loaded blister test for elastic response and delamination behavior of thin film-substrate system

The elastic response of a thin film of photoresist deposited on a silicon wafer is studied by using a shaft-loaded blister test method developed recently. Experiment data are compared with an analytical solution. Results demonstrated that under shaft loading, the thin film underwent a pure bending mode at small deformation and gradually transformed to a pure stretching mode at larger deformation. The effect of residual stress on elastic response is also studied. The delamination of thin film from substrate can be successfully measured under displacement control mode by the shaft-loaded blister test.     

Mechanical spectroscopy of thin layers of PPV polymer on Si substrates

The vibrating reed technique with electro“static” excitation and optical detection has been applied to investigate thin layers of poly-phenylene-vinylene, deposited by spin coating onto microfabricated Si cantilevers, during temperature cycling programs between 90 and 540 K at a rate of 1 K/min. From the vibration frequencies the Young’s modulus of the film can be estimated to be about 10 MPa at room temperature in the precursor phase (if prepared from a solution in toluene), which increases by conversion to the conjugate bonded polymer to about 50 MPa. The temperature dependence of internal friction reveals the processes of γ relaxations (crankshaft motion of side branches in the precursor) and β-relaxation (movements of a few monomer blocks in the polymer chain), as well as peaks indicating the structural transformations during conversion, and possibly a glass transition in the amorphous precursor phase. After conversion only the β-relaxation persists.     

Effects of substrate temperature on the surface of polymer thin films prepared by R.F. sputtering with a polyimide target

In this study, we characterized polymer thin films deposited by a conventional radio frequency sputtering apparatus introduced into argon and nitrogen gases with a polyimide target onto copper substrates.Heating effects due to heating the copper substrate at 250 °C in the sputtering on tribological and adhesion properties of thin films were investigated with measuring friction coefficient, wear durability and pull strength. Surface roughness of the nitrogen sputtered thin film decreased by the heating. Friction coefficient of argon and nitrogen sputtered thin films prepared at 250 °C was almost the same level as that prepared at room temperature, respectively. Wear durability of these thin films and adhesion strength between these thin films and copper substrate decreased by the heating.     

The effect of a non-circular drawing sequence on delamination characteristics of pearlitic steel wire

In this study, a non-circular drawing (NCD) sequence was applied to investigate the effect of deformation behavior, microstructure and texture evolution on delamination characteristics of pearlitic steel wire under torsional deformation mode. The multi-pass NCD sequence was numerically and experimentally applied up to the 12th pass in comparison with conventional wire drawing (WD). For investigation of the deformation characteristics of the drawn wires, three-dimensional finite element and flownet analyses were carried out. These simulation results indicated that the NCD could impose relatively homogeneous plastic deformation on the wire compared to the WD. From the scanning electron microscopy and X-ray diffraction results, globular cementite and cylindrical texture component, which might increase likeliness of delamination fracture, were rarely observed in the NCD drawn wire. In the torsion test, the delamination fracture was observed in the WD drawn wire for the 10th pass while it did not occur for the 12th pass NCD. In addition, the ultimate tensile strength (UTS) of 2300 MPa grade wire was manufactured by the NCD and the UTS value was 257 MPa higher than the one of the WD. Therefore, it was demonstrated that the multi-pass NCD could impose relatively homogeneous plastic deformation on the wire, resulting in high-torsional ductility with better strength compared to the WD.     

Fiducial marks as measures of thin film crack arrest toughness

Carbon fiducial marks are formed during thin film local delamination processes induced either by indentation, forming circular blisters, or by residual stress relief through telephone cord blister formations. Hydrocarbons are sucked into the crack tip during the delamination processes, outlining the crack tip opening angle, which can be used to back calculate thin film adhesion using elastic or plastic analyses presented in the paper.     

The fracture of brittle thin films on compliant substrates in flexible displays

One mechanical issue in flexible organic light emitting displays (OLED) is the fracture of extremely thin brittle conducting transparent oxide films deposited on thin flexible substrates. Understanding the behaviour of these films under flexed condition is essential for designer of flexible OLED. Controlled buckling experiments on the film and substrate have been designed to study the fracture of the films under both tension and compression. Fracture of the film is superficially similar in both tension and compression. However, under tension a channelling crack is formed, while under compression, the film delaminates, buckles and cracks in a tunnelling motion. The fracture toughness of the film and the delamination toughness have been estimated from these experiments. Design to maximise the flexibility of the device is discussed.     

Stress and structural studies of ZnO thin films on polymer substrate under different RF powered conditions

The ZnO films are deposited on flexible substrate Teflon by radio frequency (RF) magnetron sputtering. The structure and residual stress of the films are revealed by XRD analysis. We find that the increase of RF power results in the change in the nature of stress and the difference of the grain size in the ZnO films on Teflon substrate. This indicates the possibility of the stress relaxation by increasing the RF power. Considering the (002) orientation and the mechanical stress, we suggest that the ZnO film deposited at RF power of 200 W for 1 h is optimal.     

Fractal properties of AlGeNi layers on GaAs surfaces

The thermal interactions of thin AlGe and AlNiGe layers with a bulk GaAs monocrystal were investigated. The heat treatment of these systems was carried out in the working chamber of a scanning electron microscope. The SEM pictures were analysed using a fractal mathematical technique. It was found that the surface of the samples has fractal character. No temperature dependence of the fractal dimension was observed. The samples were also studied using the structural entropy versus filling factor maps of the samples in order to find their localization properties. The SEM pictures of AlGe perform mostly as a Gaussian functions, whereas the AlNiGe samples show usually a behaviour with exponential decay.