Stress In Thin Films Research Articles

Nanoscale stress and microstructure gradients across a buckled Mo-Cu bilayer: Cu self-annealing triggered by interface delamination

Residual stresses in thin film structures significantly impact their mechanical properties and affect interface delamination. Highly compressively stressed thin films buckling is the predominant interfacial failure mode due to strain energy release. In the present study the effect of cross-sectional stress and microstructural gradients of thin films on the buckling behavior are explored in a model material system consisting of a thin Cu film sputtered onto glass and a highly compressively stressed 500 nm thick Mo overlayer causing buckling delamination at the Cu-glass interface. Employing synchrotron cross-sectional X-ray nano-diffraction, multiaxial X-ray elastic strain and microstructure distributions were explored across the cross-section of the adhering and buckled bilayer, respectively. In the adhering state, a gradual thickness evolution of columnar microstructure and residual stress was found for Mo, while in Cu, no microstructure changes and only minimal stress variations were detected along the film thickness. After delamination, diffraction peak broadening and changes in unstrained lattice parameters in the Cu sublayer indicated structural defect annihilation and grain coarsening. These microstructural changes were further validated via cross-sectional transmission electron microscopy. The evaluated residual stress distributions across the two sublayers of the pristine and buckled bilayer were used to quantify the released strain energy per unit area due to buckling, amounting to 0.61 J/m². Further cross-validation of experimental stress results with finite element simulations strengthened the experimental findings, providing a comprehensive understanding of the stress distribution across the buckled bilayer.

Determining the bilinear flow stress of thin films by comparing load/depth and sink-in/pile-up behavior between nanoindentation and FEM

Abstract It is known from the literature that the load-depth curve obtained by nanoindentation cannot uniquely determine the plastic flow stress behaviour of the material. In this study, the sink-in/pile-up of nanoindentation is another important information for predicting the elastic-plastic behaviour of thin film. Therefore, by comparing load/depth behaviour and sink-in/pile-up from nanoindentation with finite element analysis, the bilinear flow stress of the coating can be determined. Commercial TiN coatings are currently used as an example for this study. The bilinear flow stress of TiN can be determined by this method: the elastic modulus of 343.007 GPa, the yield stress of 10.458 GPa and the tangent modulus of 214.080 GPa. In addition, the stress of loading and unloading during the nanoindentation of the thin film was also investigated.

Effects of die top system and trenches on large thin die mechanical robustness

Abstract Power MOSFET dies in the automotive industry are becoming larger (> 5 x 5 mm) and thinner (< 50 µm) to meet high-performance and lifetime requirements. Ensuring the mechanical robustness of these large ultrathin chips is crucial for reliable electronic devices and high-throughput packaging processes. The high aspect ratio and advanced chip designs incorporating trench technology present significant challenges in semiconductor assembly, packaging, and testing. This paper introduces an experimental front-end strategy aimed at strengthening the front side of large ultrathin dies using various die-top systems. Industry-equivalent 50 µm thick dummy power MOSFET dies were fabricated to evaluate the efficacy of different chip designs and materials, such as polyimide, in mitigating fracture risks. Fabrication-induced stresses and warpage in the device layers were measured using a thin-film stress measurement tool. Additionally, the frontside strength of the ultrathin dies was assessed using the three-point bending method, with the resulting data analyzed via two-parameter Weibull distribution plots. Results demonstrated that the deposition of 5 µm polyimide (PI) on the nitride die topside significantly increased die strength from 339 MPa to 760 MPa, with 5 µm PI proving more effective for die strengthening than 10 µm. The interaction between the metal-trench layer and the die was found to be critical to the robustness of ultrathin dies, influenced by the pattern and layout of the trenches. Die-top metallization designs, such as meandering patterns, showed promising improvements in die strength compared to standard designs. A proposed chip layout aims to maximize polyimide coverage for clip-bonded products on the die topside, leveraging its strengthening effect. The study also demonstrated that dummy reference chips can facilitate rapid and straightforward evaluation of extensive design experiments to identify robust chip designs.

Compressive stress reduction in sputter-deposited yttrium aluminum nitride (Y0.2Al0.8N) thin films for BAW resonators with high electromechanical coupling

In the past decade, rare earth elements have found increasing interest in enhancing the piezoelectric coefficient of aluminum nitride (AlN) thin films. Until now, scandium has been the most successful rare earth element to enhance the piezoelectric coefficient (d33) up to 600 %. In this research paper, we present a 250 % increase in d33 to 12.5 pC/N for sputter-deposited yttrium alloyed aluminum nitride (Y0.2Al0.8N) thin films compared to pure AlN. However, this increase in d33 comes with a substantial increase in compressive layer stress well above 1 GPa. Therefore, a chamber pressure sweep technique is introduced, resulting in a 40 % reduction in the stress level without significantly affecting the crystallographic film parameters to facilitate device integration. Even more, high compressive stress in thin films is a critical concern in piezoelectric MEMS devices such as bulk acoustic wave (BAW) resonators, as it can adversely affect the piezoelectric material properties and hence, the electromechanical performance. For this purpose, we demonstrate that the pressure sweep technique improves the electromechanical coupling factor of Y0.2Al0.8N to 7.02 %, being substantially above the reference value of 6.02 % set by pure AlN. In summary, the findings from this study may stimulate further effort to integrate YxAl1-xN thin films in BAW filter devices for future telecommunication applications.

A Practical Approach for Determination of Thermal Stress and Temperature-Dependent Material Properties in Multilayered Thin Films.

Multilayered thin films are essential to most microelectro-mechanical systems (MEMSs). The reliability and predictability of the behavior of such systems, especially when intended for usage at high temperatures or in harsh environments, demand the consideration of thermo-mechanical properties of the individual films of the multilayer arrangement during the design stage. This paper introduces a newly derived analytical model for the convenient indirect determination of the temperature-dependent Young's modulus and the thermally induced stress of individual layers within a multilayered thin film system, i.e., a multilayer-adapted Stoney equation. It is based on sample curvature measurement and requires data from only a single experiment. Experimental and numerical investigations of the new models are carried out using a five-layered sample of a RuAl metallization system developed for wireless high-temperature acoustic sensing. The results highlight the usability of the new model in practical MEMS analysis, enabling insights into complex layer stacks by overcoming current experimental limitations.

Temperature-Dependent Residual Stresses and Thermal Expansion Coefficient of VO2 Thin Films

This study aims to investigate the thermomechanical properties of vanadium dioxide (VO2) thin films. A VO2 thin film was simultaneously deposited on B270 and H-K9L glass substrates by electron-beam evaporation with ion-assisted deposition. Based on optical interferometric methods, the thermal–mechanical behavior of and thermal stresses in VO2 films can be determined. An improved Twyman–Green interferometer was used to measure the temperature-dependent residual stress variations of VO2 thin films at different temperatures. This study found that the substrate has a great impact on thermal stress, which is mainly caused by the mismatch in the coefficient of thermal expansion (CTE) of the film and the substrate. By using the dual-substrate method, thermal stresses in VO2 thin films from room temperature to 120 °C can be evaluated. The thermal expansion coefficient is 3.21 × 10−5 °C−1, and the biaxial modulus is 517 GPa.

Optical, Electrical, Structural, and Thermo-Mechanical Properties of Undoped and Tungsten-Doped Vanadium Dioxide Thin Films.

The undoped and tungsten (W)-doped vanadium dioxide (VO2) thin films were prepared by electron beam evaporation associated with ion-beam-assisted deposition (IAD). The influence of different W-doped contents (3-5%) on the electrical, optical, structural, and thermo-mechanical properties of VO2 thin films was investigated experimentally. Spectral transmittance results showed that with the increase in W-doped contents, the transmittance in the visible light range (400-750 nm) decreases from 60.2% to 53.9%, and the transmittance in the infrared wavelength range (2.5 μm to 5.5 μm) drops from 55.8% to 15.4%. As the W-doped content increases, the residual stress in the VO2 thin film decreases from -0.276 GPa to -0.238 GPa, but the surface roughness increases. For temperature-dependent spectroscopic measurements, heating the VO2 thin films from 30 °C to 100 °C showed the most significant change in transmittance for the 5% W-doped VO2 thin film. When the heating temperature exceeds 55 °C, the optical transmittance drops significantly, and the visible light transmittance drops by about 11%. Finally, X-ray diffraction (XRD) and scanning electron microscope (SEM) were used to evaluate the microstructure characteristics of VO2 thin films.

Effect of YF3 Coating Process on Film Stress

YF3 rare-earth fluoride coating material has received wide attention as an alternative to ThF4 low refractive index material, but the film layer can be seriously affected due to the different coating processes. Therefore, to investigate the rules between the coating processes of YF3 rare-earth fluoride coating materials, YF3 thin films were coated with different deposition rates and substrate temperatures. The stresses of YF3 thin films under different processes were obtained by a thin film stress meter, and the microscopic morphology of the thin films was characterized by atomic force microscopy. The results show that: YF3 monolayer film is tensile stress; in the deposition rate between 0.5nm/s~1.5nm/s, with the increase of the coating deposition rate YF3 monolayer film stress tends to decrease, the roughness of the film is also gradually increased, and the overall thickness of the film surface decreases; in the substrate temperature is greater than 50 ℃, the film stress is significantly reduced.

A New Method for Evaluating the Influence of Coatings on the Strength and Fatigue Behavior of Flexible Glass

Flexible glass is an interesting substrate for a variety of displays, especially bendable or foldable ones, as it shows excellent surface properties and appealing haptics. With the necessary skill, flexible glass can be coated with thin films of different functionality, such as electrical or optical thin films, using plasma processes. In displays, thin film coatings such as transparent conductive electrodes and/or antireflective layer stacks are of major importance. Despite its attractive surface properties, however, flexible glass is still brittle, and its strength must be examined and monitored during any functionalization process, especially with regard to the fatigue behaviour. Currently, specific setups for cyclic fatigue testing of coated flexible glass are not available. Therefore, a new test method is presented herein for easy-to-handle rapid strength and fatigue testing using an endurance testing machine. This method overcomes two issues with the commonly used two-point bending test: the correct insertion of specimens is much easier, and both strength and fatigue testing using the same setup are now possible. Finite element method (FEM) simulation outcomes and first experimental simple fracture tests show that results comparable to those with a two-point bending test setup can be achieved with less effort. This makes it possible to analyze the fracture behaviour of flexible glass under cyclic loading and to evaluate the influence of thin film stress and other coating properties on its performance.Graphical

Electromagnetic response analysis of high temperature superconducting coated conductor tape with local debonding: Case of transporting current in an external magnetic field

In this article, the electromagnetic mechanical behavior of a long superconducting coating tape within a local internal cracking was analyzed when it transport current in a perpendicular magnetic field. Based on the superconducting critical state model, the distribution of current and magnetic field within the structure were calculated. Then, the control equation for the correlation between the flux pinning force inside the superconducting thin film and the shear force at the substrate interface was given using the plane strain method of linear elasticity theory. Combined with the Chebyshev polynomial solution, the distribution patterns of normal stress inside the superconducting thin film and shear stress at the substrate interface were finally obtained. The results indicate that, unlike the phenomenon observed under a single field excitation, the stress distribution in the structure exhibits an asymmetric distribution when both transport current and external magnetic field are applied. The normal stress inside the superconducting thin film is significantly larger on the right side of the structure than that on the left side, and the same distribution law is found in the shear stress at the substrate interface. The stress concentration occurs at the separation point between the film and the substrate. When the Young's modulus of the substrate material is high, the normal stress inside the superconducting film is low, while the shear stress at the interface is high, and vice versa. All these results provide theoretical guidance for the application of superconducting tapes.

Stretchable Substrates with 3D Wave Patterned Surface for Enhanced Mechanical Stability of Indium Tin Oxide Electrodes

AbstractFlexible electronic devices have promising applications in many future technologies such as wearables, implantables, robotics, and displays. Among the distinct types of mechanical flexibility, stretchability stands as a significant challenge. A particularly demanding objective is the realization of a high‐performance transparent electrode that endures stretching and can be mass produced, all while avoiding additional restrictions on device density. In this work, it is demonstrated that a 3D wave patterned surface provides a threefold improved strain performance of deposited indium tin oxide electrodes, in a statistical comparison of 3D wave patterned and planar surfaces, where indium tin oxide electrodes are stretched to electrical failure. Moreover, this platform alleviates residual thin film stress, allowing for easier handling of the substrates. This study demonstrates the feasibility of attaining stretchability for upcoming electronic devices using a scalable platform that incorporates high‐performance transparent electrode materials using only conventional materials and fabrication steps.

The strength of uncoated and coated ultra-thin flexible glass under cyclic load

<abstract> <p>Ultra-thin flexible glass with thicknesses of 100 µm or below is a substrate in the fields of optics, electronics, and semiconductors. Its brittleness is challenging in production processes like physical vapor deposition processes, especially in roll-to-roll production. In many cases, multiple geometric deformations take place and each step, like coating or cutting, influences the glass strength. By now, the relation between the strength of ultra-thin glass under quasi-static conditions and its strength under cyclic load has not been studied. Moreover, the effect of coatings has not been investigated. Both aspects are crucial to design reliable production processes. Therefore, the strength of ultra-thin glass under cyclic load was studied for uncoated and coated substrates. Two coating types were investigated: a single indium tin oxide film and a seven-layer antireflective layer stack. The coatings significantly influence the strength of the underlying glass in both test modes. The barrier properties, thin film stress, and the morphology/crystalline structure are identified as the major characteristics influencing the strength.</p> </abstract>

Process-induced residual stress in a single carbon fiber semicrystalline polypropylene thin film

During the processing of semicrystalline thermoplastic composites, various models for the prediction of residual stress have been proposed but experimental validation is limited. In this study, a modeling framework is developed to predict the evolution of residual stress in a single carbon fiber embedded in a semicrystalline polypropylene thin film subjected to non-isothermal cooling. Validation is based on in-situ measurement of axial fiber strain after processing using micro-Raman Spectroscopy. A material model for polypropylene (50% equilibrium crystallinity) is presented that incorporates the effects of non-isothermal cooling on crystallinity-dependent resin shrinkage and crystallinity-dependent resin modulus from the amorphous polymer melt to room temperature. The evolution of residual stress is calculated using a finite element (FE) model with a user-developed subroutine incorporating the resin material models. Single-fiber polypropylene films are fabricated using a range of fiber pretension levels to prevent fiber waviness during cooling and to induce a wide range of axial strain levels in the fiber for model validation. The fiber axial strain was measured over the length of the fiber, from the free edge into the bulk, capturing the ineffective length region where strain builds up and plateaus. A good correlation has been obtained between the model results and the in-situ measurements of axial compression strain in the fiber. A key finding was the importance of including temperature-dependent resin modulus and that the contribution of crystallinity shrinkage to residual strain in the carbon fiber is relatively low. The model developed in this study is also compared to residual stress models in the literature which shows the importance of including the effects of crystallization and cooling rate on temperature and crystallinity-dependent modulus and resin shrinkage for accurate predictions.

Quantitative study of the thickness-dependent stress in indium tin oxide thin films

A quantitative analysis of stress in indium tin oxide (ITO) films with varying thicknesses was conducted using high-precision stylus profilometry. The experimental results revealed a transition of the stress type from tensile to compressive as the ITO film thickness increased. Further investigation of the surface morphology of the ITO films indicated that the tensile stress originated from the impingement and coalescence of newly deposited equiaxed grains, while the observed compressive stress was attributed to the incorporation of excess material in the boundaries of columnar grains. The ability to monitor stress evolution in sputtered ITO films on glass substrates provides valuable insights for process control in ITO device manufacturing.

Effect of Ion Flux Variation in DC Magnetron Sputtering on the Deposition of Cubic Boron Nitride Film

Cubic boron nitride (cBN) thin films were deposited using DC magnetron sputtering, and the effect of the ion flux on the deposition behavior and residual stress of the cBN thin films was investigated. To increase the ion flux, the magnetic force ratio of the central/peripheral permanent magnets inserted in the magnetron sputtering source was reduced. Due to the complementary relationship between ion flux and energy for cBN deposition, the critical bias voltage required for cBN nucleation decreased as the ion flux increased. The cBN content of the films was relatively higher under the deposition condition of the increased ion flux. This was interpreted to indicate the thinning of the intervening hexagonal boron nitride (hBN) layer formed prior to cBN nucleation. Comparing the compressive residual stress of the cBN films, the residual stress was relieved as the bias voltage decreased regardless of the ion flux. The increase in ion flux made it possible to deposit the cBN films at a low bias voltage, thereby depositing cBN films with lower residual stress. The results showed that reducing ion energy by increasing ion flux for cBN deposition is a promising method for depositing low-stress cBN thin film having thin intervening hBN layer.

Computational tool for analyzing stress in thin films

A computational model has been developed to analyze calculations of residual stress in thin films determined from in-situ wafer curvature measurements. The model is based on several physical mechanisms that have been proposed to control the stress, including the effect of growth kinetics, grain growth and energetic particle bombardment. From a set of data, the program determines a set of kinetic parameters that can be used to understand the processes controlling stress. These parameters can be used to estimate the stress that will develop under different processing conditions in order to obtain a desired stress state. Several examples are described that illustrate the program's capabilities, including the effects of growth rate, growth temperature and particle energy (via chamber pressure in sputter deposition). Interested researchers may obtain the program and associated documentation to use the program to analyze their own data.

Enhanced mechanical strength of vortex fluidic mediated biomass-based biodegradable films composed from agar, alginate and kombucha cellulose hydrolysates

Biodegradable, biomass derived kombucha cellulose films with increased mechanical strength from 9.98 MPa to 18.18 MPa were prepared by vortex fluidic device (VFD) processing. VFD processing not only reduced the particle size of kombucha cellulose from approximate 2 μm to 1 μm, but also reshaped its structure from irregular to round. The increased mechanical strength of these polysaccharide-derived films is the result of intensive micromixing and high shear stress of a liquid thin film in a VFD. This arises from the incorporation at the micro-structural level of uniform, unidirectional strings of kombucha cellulose hydrolysates, which resulted from the topological fluid flow in the VFD. The biodegradability of the VFD generated polymer films was not compromised relative to traditionally generated films. Both films were biodegraded within 5 days.

Tensile stress regulated microstructures and ferroelectric properties of Hf0.5Zr0.5O2 films

The discovery of ferroelectricity in HfO2 based materials reactivated the research on ferroelectric memory. However, the complete mechanism underlying its ferroelectricity remains to be fully elucidated. In this study, we conducted a systematic study on the microstructures and ferroelectric properties of Hf0.5Zr0.5O2 (HZO) thin films with various annealing rates in the rapid thermal annealing. It was observed that the HZO thin films with higher annealing rates demonstrate smaller grain size, reduced surface roughness and a higher portion of orthorhombic phase. Moreover, these films exhibited enhanced polarization values and better fatigue cycles compared to those treated with lower annealing rates. The grazing incidence x-ray diffraction measurements revealed the existence of tension stress in the HZO thin films, which was weakened with decreasing annealing rate. Our findings revealed that this internal stress, along with the stress originating from the top/bottom electrode, plays a crucial role in modulating the microstructure and ferroelectric properties of the HZO thin films. By carefully controlling the annealing rate, we could effectively regulate the tension stress within HZO thin films, thus achieving precise control over their ferroelectric properties. This work established a valuable pathway for tailoring the performance of HZO thin films for various applications.

Effect of static elastic stress on the corrosion behavior of 7A04 aluminum alloy exposed to real marine atmospheric environment

Aluminum alloy structural materials are widely subjected to the interactive effect of atmospheric corrosion under thin liquid film and elastic stress during the actual service. This study utilized the real marine atmospheric environment as the corrosion environment of thin liquid film for 7A04 aluminum alloy, and the specially designed outdoor device was used to apply varying levels of static elastic tensile stress at the same time, and then the corrosion damage behavior of 7A04 alloy under the interactive effect was studied. The research indicates that the 7A04 alloy suffers from pitting and exfoliation corrosion under the test conditions. The applied elastic tensile stress can accelerate the corrosion damage process of 7A04 alloy, and the degree of acceleration increases with increasing stress levels and exposure time. Moreover, the applied stress can also significantly accelerate the deterioration of the mechanical properties of 7A04 alloy, which has a more prominent effect on the elongation after fracture. Additionally, the corrosion mechanism of 7A04 alloy under the interactive effect was also discussed in this paper.

Parameters influencing the fracture of Mo films and their wider significance

Fragmentation testing has been used for decades to assess thin film fracture and delamination. Hooke’s law is generally used to determine a film fracture stress from the crack onset strain observed in micrographs or measured as an electrical resistance increase. While this method is in theory suitable in the elastic regime, it neglects important film characteristics, such as residual stress, microstructure, or film architecture. Thus, there is a need to improve fracture analysis using fragmentation to avoid significant errors in measuring fracture stress or apparent fracture toughness of thin films. In-situ X-ray diffraction fragmentation experiments can measure the film fracture stress even for individual layers being part of a multilayer. Which characteristics influence the apparent fracture behavior will be demonstrated on Mo thin films on polyimide.Graphical abstract