Film Cracking Research Articles

Full range fragmentation simulation of nanoflake filler-matrix composite coatings on a polymer substrate

This paper presents a comprehensive experimental and computational study to explore the damage evolution mechanisms of polymer matrix nanocomposite films consisting of rigid ceramic fillers coated on a polymer substrate. The weight ratio of montmorillonite (MMT) fillers in the polyvinyl alcohol (PVA) matrix ranges from 30 % to 70 %, and these are applied onto a polyethylene terephthalate (PET) substrate. Through experiments, apart from damage behaviors, the water vapor transmission rates are also measured to gain insight into moisture diffusion characteristics with varying weight ratios of fillers. The optimal weight ratio of nanocomposite films consisting of a PVA matrix with MMT fillers can vary depending on the purpose of damage resistance and moisture barrier characteristics. A peridynamic theory is employed to simulate various damage scenarios of bi-layer nanocomposite films. The solution strategy presented incorporates the use of the cut-boundary and finite element methods to reduce substrate thickness and make initial predictions of crack onset strains, respectively, under quasi-static loading conditions. Several damage scenarios are considered for thin and thick PVA films on the PET substrate, as well as weak to strong interfaces between the PET-PVA and PVA-MMT layers. Additionally, different distributions of MMT fillers are also considered by varying the distances between them and inserting inclusions. The peridynamic damage analyses encompass crack initiation, propagation, and final failure stages across a wide range of strains, including various damage modes such as matrix cracking, cracking at the filler-matrix, or matrix-substrate interfaces, leading to the cohesive film cracking and delamination.

Thermal stress concentration points and stress mutations in nano-multilayer film structures

In the multilayer film-substrate system, thermal stress concentration and stress mutations cause film buckling, delamination and cracking, leading to device failure. In this paper, we investigated a multilayer film system composed of a substrate and three film layers. The thermal stress distribution inside the structure was calculated by the finite element method, revealing significant thermal stress differences between the layers. This is mainly due to the mismatch of the coefficient of thermal expansion between materials. Different materials respond differently to changes in external temperature, leading to compression between layers. There are obvious thermal stress concentration points at the corners of the base layer and the transition layer, which is due to the sudden change of the shape at the geometric section of the structure, resulting in a sudden increase in local stress. To address this issue, we chamfered the substrate and added an intermediate layer between the substrate and the transition layer to assess whether these modifications could reduce or eliminate the thermal stress concentration points and extend the service life of the multilayer structure. The results indicate that chamfering and adding the intermediate layer effectively reduce stress discontinuities and mitigate thermal stress concentration points, thereby improving interlayer bonding strength.

Heterogeneous Integration of High Endurance Ferroelectric and Piezoelectric Epitaxial BaTiO3 Devices on Si

AbstractIntegrating epitaxial BaTiO3 (BTO) with Si is essential for leveraging its ferroelectric, piezoelectric, and nonlinear optical properties in microelectronics. Recently, heterogeneous integration approaches that involve growth of BTO on ideal substrates followed by transfer to a desired substrate show promise of achieving excellent device‐quality films. However, beyond simple demonstrations of the existence of ferroelectricity, robust devices with high endurance are not yet demonstrated on Si using the latter approach. Here, using a novel two‐step approach to synthesize epitaxial BTO using pulsed laser deposition on water‐soluble Sr3Al2O6 (on SrTiO3 substrates), successful integration of high‐quality BTO capacitors on Si is demonstrated, with remanent polarisation Pr = 7 µC cm−2, coercive field Ec = 150 kV cm−1, ferroelectric and electromechanical endurance of > 106 cycles. The study further addresses the challenge of cracking and disintegration of thicker films by first transferring a large area (5 mm x 5 mm) of the templated layer of BTO (≈30 nm thick) on the desired substrate, followed by the growth of high‐quality BTO on this substrate, as revealed by high‐resolution X‐ray diffraction (HRXRD) and high‐resolution scanning transmission electron microscopy (HRSTEM) measurements. These templated Si substrates offer a versatile platform for integrating any epitaxial complex oxides with diverse functionalities onto any inorganic substrate.

Failure behavior analysis of oxide film formed on super-heater tubes of boiler during deep peak process

High-temperature components in the supercritical power plant experienced alternating thermal stresses under deep peak regulation, accelerating the cracking and spalling of the oxide film formed on the steam-side of super-heaters and re-heaters. This study employed the corrosion testing and finite element simulations to investigate the failure behavior of oxide films on super-heaters made by heat-resistant steelsT91 and austenitic HR3C during deep peak conditions. The experimental results indicate that the oxide film on T91was a double layer film containing Fe3O4 and Fe-Cr oxides, which was much thicker than that on HR3C. The spalling of the outer oxide film on T91 was more severe than that of HR3C. The analysis of thermal stress-strain under various loads and oxide film thicknesses revealed the significant shear stress between Fe3O4 and Fe-Cr within the oxide film on T91 steel. The significant shear stress caused the bigger strain within the oxide film on T91 steel, causing the spalling of the oxide film. Compared to the strain within the oxide film on T91 steel, the stress-strain within Cr2O3 oxide film on HR3C steel was notably lower than that on T91 steel. The failure behaviors of the oxide film on T91 and HR3C were quantitatively explained through experimental result and stress-strain simulation with the oxide film. The failure models of the oxide film on investigated steels were put forward.

In-situ reaction-generation self-healing superior antioxidation layer induced by Al-Y sol-gel film on the AISI304 steel

In this study, an Al-Y sol-gel film is prepared on the AISI304 steel and its effect on the high temperature oxidation resistance is evaluated by the cycle oxidation at 900 ℃ in the air. The resulting intact oxide layer, composed of (Al, Cr)2O3 and MnCr2O4 phases, effectively slowing down the oxidation rates at 900 ℃. The general cracks in the sol-gel film during the oxidation process are found to be self-healed by a growing spinel MnCr2O4 phase from the substrate, attributed to its low Gibbs free energy and the sufficient Cr source from the adjacent substrate. Furthermore, the oxide layer originates from the interaction between sol-gel film and the substrate which enhances the binding between the oxide layer and the substrate. Thus, it could be confirmed that a self-healing superior antioxidation layer is generated on the surface of AISI304 steel through an in-situ reaction induced by the Al-Y sol-gel film during high-temperature oxidation procedure.

Electrohydrodynamic Printing Grid-Structured Catalytic Layers with Excellent Bending Resistance for Flexible Al-air Batteries.

The catalytic film of a flexible Al-air battery is generally a brittle film formed by brushing a slurry onto the surface of carbon cloth. Fatigue bending can easily lead to cracking of the catalytic film and shedding of the active material. This study innovatively proposes a novel grid-structured catalytic layer prepared by electrohydrodynamic printing. Experiments have verified that, compared with traditional catalytic films, the grid-structured catalytic layer exhibits excellent bending resistance. After 10 000 fatigue bending cycles, its relative resistance is ≈1/9 that of the traditional catalytic film. The printed grid-structured catalytic layer is applied to a flexible Al-air battery, which maintains a power density retention rate as high as 92% after the same number of bending cycles. Compared to traditional catalytic films, the electrodynamically printed grid-structured catalytic layer proposed in this study demonstrates both excellent electrochemical performance and bending resistance. This advancement holds significant importance for the development and application of flexible metal-air batteries.

Effects of hard anodizing on mechanical and electrochemical characteristics of aluminum alloys under tribocorrosion condition

In this research, the effects of hard anodizing on the mechanical and electrochemical characteristics of aluminum alloys under tribocorrosion conditions was investigated. Compared with dry conditions, friction coefficient of aluminum alloys under tribocorrosion conditions increased, whereas that of hard anodized specimens decreased. This was attributed to corrosive ions in the solution corroding the transfer film of the counter-body and tribofilm of the hard anodized specimen. In potentiodynamic polarization experiments under tribocorrosion conditions, the aluminum alloys exhibited high current density with applied load. However, at potentials above –0.05 V, current density decreased and was reversed. This is believed to be due to the corrosive ions preferentially reacting with the generated wear debris, thereby reducing the oxidation reaction with wear track. However, the current density of the hard anodized specimens increased with load and potential. In addition, the increasing rate in the wear width and depth was significant under tribocorrosion conditions (Width: 42.65 %, Depth: 32.63 %). This is due to the cavitation and fluid impact generated during friction/wear accelerating the cracking and damage of the hard anodizing film with the brittleness and porousity. However, the tribocorrosion resistance of the hard anodized aluminum alloy was improved by more than 97 %.

Optimization of laser patterning process for eco-friendly tin-halide perovskite solar module – with a nanosecond green laser

The tin-based perovskite solar cells are promising future eco-friendly photovoltaic technology with increasing efficiency, which relies on fluorine-doped tin oxide (FTO) or indium tin oxide (ITO) as a transparent conducting oxide (TCO) for front contact. In the monolithic module fabrication process interconnections are executed by a series of three scribes with two different lasers 1064 nm and 532 nm. This study aims to simplify the interconnection process in tin-based perovskite solar modules by using a single visible laser source to perform all three scribes. The study uses an inverted device structure of Glass/TCO/ Poly(3,4-ethylenedioxythiophene): Polystyrene sulfonate (PEDOT: PSS)/Formamidinium-tin-iodide (FASnI3)/C60/Bathocuproine (BCP)/Ag and a 532 nm nanosecond pulsed laser source to pattern the ITO and FTO (P1 scribe), the PEDOT: PSS/FASnI3/C60/BCP stack (P2 scribe), and the PEDOT: PSS/FASnI3/C60/BCP/Ag (P3 scribe). The quality of the P1 scribe is assessed by examining the edges, completeness of film removal, cracking, film delamination, and elemental mapping using a stylus profiler, optical microscope, and energy dispersive x-ray spectroscopy. The P1 scribe is completely removed with line widths of 70 µm and 110 µm of ITO and FTO, respectively, without damage to the glass substrate. The profiles are steep, and the electrical isolation is greater than 40 MΩ. The same 532 nm laser is used for P2 and P3 scribes. The ablation of PEDOT: PSS during P2 and P3 scribe is studied by Raman spectroscopy. The results show that the use of a single 532 nm laser source can simplify the patterning process of monolithic tin-based perovskite solar modules, and potentially reduce production costs.

Study on the restoration of glass slides dating back to the 1940s

The Museum of Sun Yat-sen University houses a collection of antique glass slides dating back to the 1940s. These historical artifacts not only serve as a record of the past but also bring history to life. During extended storage, the emulsion layer on glass slides may harden and become brittle, leading to cracking and buckling. This study suggests a method to enhance the physical property of the emulsion layer by using a combination of nonionic surfactant isomeric alcohol ethoxylates eight (TO-8) and waterborne epoxy resin (WER). We investigated the microscopic action mechanism of the two on the emulsion layer of glass slides using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), water contact angles, and other techniques. Our study revealed that TO-8 can significantly eliminate the spherulitic crystal structure of the emulsion layer, as well as improve its softness and hydrophilicity. The addition of the WER ensures that the cracking and warping of the emulsion layer film is fully corrected, resulting in a flat surface. Additionally, the size of the emulsion layer film remains stable even after wetting. The WER has minimal impact on the image information of glass slides. The emulsion layer of the glass slides, restored using the softening protection solutions developed in this study, showed almost full recovery of image information. This research holds significant theoretical and practical value for repairing cracked and warped emulsion layers on glass slides.

Enhancing flexible electronics: Unveiling the role of strain rate in the performance of molybdenum-coated PET films

This work analyzes the mechanical and electrical properties of molybdenum (Mo) thin films at 100 and 200 nm thicknesses under different strain and strain rate circumstances. The study examines Mo film deposition by RF magnetron sputtering on PET substrates and their mechanical stress behavior. The investigation reveals distinct patterns of crack initiation and propagation, where primary cracks predominantly appear perpendicular to the direction of applied strain, and secondary cracks develop due to stress redistribution, displaying a complex interplay between film thickness, strain rate, and crack morphology. A key finding of this study is the observation of more advanced and irregular crack patterns in thicker films (200 nm) subjected to higher strain rates (1000 mm/min), suggesting a heightened sensitivity to mechanical stress and a more chaotic fracture process compared to thinner films or those under lower strain rates. Additionally, instances of film edge delamination, particularly under high strain conditions, highlight the challenges in maintaining film-substrate adhesion and integrity under extreme mechanical deformation. The research provides critical insights into the mechanical robustness and electrical performance of Mo thin films, emphasizing the influence of microstructural properties, deposition parameters, and external stressors on their applicability in high-tech industries. The findings underscore the importance of optimizing deposition techniques and understanding material behavior under stress to enhance the durability and reliability of Mo thin films in practical applications, ranging from semiconductor devices to photovoltaic systems.

Significant improvement in hot corrosion resistance of Inconel 690 by laser shock peening

The effects of laser shock peening (LSP) with different peening times on the hot corrosion behavior (molten salt of 75 wt% Na2SO4 + 25 wt% NaCl) of Inconel 690 at three different temperatures (700 °C, 800 °C, 900 °C) were investigated. The corrosion conditions of the three specimens were also compared in the extreme case, i.e. after 900 °C, 300 h of hot corrosion. The results showed that LSP effectively prevented the surface oxides from shedding. As times of LSP increased, the strengthening effect improved and the rate of weight loss gradually slowed down. The dense oxide film generated by the high Cr content of the material itself, LSP-induced high-density dislocation structure, mechanical twinning and grain refinement is one of the key factors in improving the hot corrosion resistance of Inconel 690. The CRS layer and microhardness layer are another key factor in preventing the cracking of the oxide film to enhance the hot corrosion resistance. Under extreme conditions, the hot corrosion resistance of LSPed specimens is still better than that of unLSPed specimen.

Iris‐Inspired Microparticles with a Two‐Factor Authentication Security Feature for Wet‐Phase Enhanced Anti‐Counterfeiting Strategies

AbstractThis article presents an iris‐mimicking polymeric microparticle with randomly generated silica film cracks to be utilized as a wet‐phase micro security taggant. The microparticles are designed to replicate the capillary patterns in the human iris, providing high data capacity and stability, making them ideal for authentication. Furthermore, the microparticles integrate a QR code within the pupillary zone of the iris, enabling pupillary authentication to enhance two‐factor identification and elevate overall security levels an unprecedented feature absent in conventional iris recognition systems. The resulting artificial iris‐mimicking microparticles have high coding efficiency and unique characteristics and can be authenticated in the wet phase, making them suitable for use as micro security taggants.

Fracture mechanism of metallic film with nano to sub-micron thickness on polycrystalline substrate

Understanding the fracture behaviors of ultrathin metallic films on polycrystalline substrates is essential to preventing failures of extensive coated components. This study investigates the fracture mechanisms of niobium films with nano to sub-micron thickness deposited on stainless steels, serving as a model system. Cracks of the 100-nm films are demonstrated to be primarily induced by out-of-plane dislocation slips in the substrate. However, as the film thickness increases to 500 nm, our findings reveal that the deposited films no longer solely succumb to substrate plasticity. Instead, they influence substrate deformation by forming an interface-affected zone with intense heterogeneous interactions. In this zone, both the accumulation of geometrically necessary dislocations and a transition from dislocation to twinning accommodated plasticity occur. The extensive deformation twinning creates ultrahigh steps, ultimately resulting in film cracking. These in-depth microscopic insights pave the way for advancements in ultrathin coatings and offer valuable knowledge for future research.

Synergistic effect of temperature, concentration and solution flow on corrosion and passive film of austenitic SS 304L and 316L in concentrated sulfuric acid

The synergistic effect of temperature, sulfuric acid concentration and solution flow on the corrosion behavior and passive film properties of austenitic SS 304L and 316L have been investigated in concentrated sulfuric acid. Design of experiment was used and electrochemical techniques were employed. It was found that investigated parameters synergistically affect the corrosion behavior and passive film properties. Surface films formed at high concentrations are less defective and increasing temperature and solution flow introduced more defects; however, the passive film repairs itself. Increasing the temperature and solution flow resulted in higher passive film coverage and cracking of the passive film, respectively.

Effect of fluid scour on stress distribution of film-substrate system

Under strong fluid scour in special service environment, the film-substrate system is prone to weaken its mechanical properties due to the additional shear stress by fluid, resulting in film debonding. The present study establishes a mechanical model incorporating the fluid shear stress for a film-substrate system with partial debonding. The debonding length, scour strength and thermal mismatch are considered in the model, respectively. Fluid induces compressive stress on inflow side and tensile stress on outflow side. Potential debonding behavior of film by the additional shear stress is qualitatively analyzed. Results show that the compressive stress by fluid releases part of the tensile stress of thermal mismatch, may mitigate surface cracking of film. The surface scour effect is amplified by the partial debonding, and is further enhanced with the increase of debonding length. The unevenness of stress distribution at the interface is intensified by the debonding and fluid scouring. The fluid scour poses a potential threat to the film-substrate system.

Peridynamic fracture analysis of film–substrate systems

When subjected to mechanical, thermal, or other loads, film–substrate systems may undergo complex cracking behaviors, which encompass film and substrate cracking, interfacial debonding, and their combinations, exhibiting rich fracture patterns, such as three-dimensional helical cracks. Identifying the mechanisms underlying these fracture phenomena may lead to more advanced strategies for technologically significant applications. In this paper, we develop an interfacial cohesive peridynamic method for fracture analysis of multiple-phase materials. Particularly, we focus on the modeling of coupled film cracking and interfacial debonding in film–substrate systems. By introducing cohesive interfacial bonds to describe the mechanical properties of the interfaces and adopting a displacement-based cohesive failure criterion, the model is able to predict the critical condition and path of interfacial crack propagation. The robustness of the interfacial cohesive peridynamic method is validated through a series of representative examples. We also demonstrate its efficacy in simulating three-dimensional cracks and identify the essential role of the interfacial energy release rate in controlling the cracking mode transition from a restricted pattern to a helical pattern. The numerical predictions of cracking paths and stress distributions agree well with the previous experimental results. This study provides a valuable tool for analyzing different cracking patterns in film–substrate systems and composite materials.

Suppression of crack formation in wafer-scale amorphous SiNx films by residual hydrogen-ligands manipulation

Plasma-Enhanced Chemical Vapor Deposition (PECVD) of amorphous silicon nitride (SiNx) thin films is a critical procedure in microelectronics serving as a surface passivation layer and dielectric barrier. However, intrinsic film stress continuously builds up along with PECVD growth, leading to film cracking. How to achieve crack-free PECVD amorphous SiNx film within a large thickness range remains a critical unresolved challenge in semiconductor industry. In this study, we revealed that high residual NH ligands from the NH3 precursor could induce excessive tensile strain at the SiNx/Si wafer interface and consequently aggravate SiNx film crack formation. With a heating pretreatment on the wafer, residual H ligands were effectively reduced to achieve homogenous chemical composition in SiNx film. As a result, the crack number declined ∼42% and the remaining crack length was substantially shorter in contrast to the original SiNx film. This work demonstrates the crucial role of residual ligands on internal strain regulation and points out a pathway to achieve crack-free PECVD SiNx films in industrial manufacturing.

Low energy impact damage characteristics of epoxy coating on the surface of sandwich composites

AbstractWhen composite honeycomb sandwich structures are subjected to low energy impacts, the upper panel or the honeycomb core often suffers large damages, which are invisible, but affects the structural safety. To achieve non‐destructive detection of these damages, an epoxy resin film (ERF) was designed as a functional coating to display the internal failure features on structure surface. The effect of low energy impacts on the damage modes of the ERF was first investigated, and then the correspondence between the ERF damage characteristics and the structural internal failure was established. Simulation and experimental results showed that with the increase of impact energy, cracks on the ERF expanded from the radial radiation with a small extension range to the circumferential pattern with an increased damage area. Meanwhile, localized delamination appeared inside the upper panel, while the degree of flexure and crushing damage to the core continued to increase. Based on the analysis of the crack extension pattern of the ERF and the damage state of the upper panel and honeycomb core, a specific link between the ERF crack characteristics and the internal damages to the sandwich structure was obtained, which might offer a novel non‐destructive testing method for composite impact damages.Highlights Low energy impact damage in honeycomb sandwich structures was a concern. Impact damage response of epoxy resin film on sandwich composites was studied. Crack extension of the film showed a particular change from radial to annular. Specific link between film crack and sandwich structure damage was established. The results would be helpful for damage detection in sandwich composites.

Effect of tensile cracks on the corrosion protection properties of anodic oxide films on 5083 Al alloy

Sulphuric Acid Anodic Oxide (AAO) film is a common method for corrosion protection of 5083 Al alloys, and cracks may occur in the AAO film due to stress damage. In this study, cracks in the AAO film on 5083 Al alloy were pre-prepared by mechanical tension, and the cracks on the corrosion protection property of AAO film were in-situ investigated by scanning electrochemical microscopy (SECM). The morphology and composition of the AAO film were measured by SEM, XRD and XPS. The results show that the corrosion protection performance of AAO film for 5083 Al alloy decreases with the increase of cracks, which is due to the fact that cracks can act as diffusion channels for corrosive media, resulting in serious corrosion reaction. SECM shows the local current at the cracks of the AAO film first increases and then decreases due to the cracks being gradually repaired by the deposited corrosion products (Al(OH)3, Al(OH)2Cl, and AlOOH). A repair mechanism of cracks in AAO film on 5083 Al alloys is revealed during the corrosion process.

Enthalpy-Driven Self-Healing in Thin Metallic Films on Flexible Substrates.

Self-healing microelectronics are needed for costly applications with limited or without access. They are needed in fields such as space exploration to increase lifetime and decrease both costs and the environmental impact. While advanced self-healing mechanisms for polymers are numerous, practical ways for self-healing in metal films have yet to be found. A concept for an autonomous intrinsic self-healing metallic film system is developed, allowing the healing of cracks in metallic films on flexible substrates. The concept relies on stabilizing metastable thin films with high mixing enthalpy via segregation barriers. This allows the films to possess autonomous intrinsic self-healing capabilities triggered by cracking at temperatures not detrimental to flexible microelectronics. The effect will be shown on metastable Mo1-xAgx thin films, stabilized via a Mo segregation barrier. Without a segregation barrier, the system is known to exhibit spontaneous Ag particle formation on the surface. This property is controlled and directed to heal cracks and partially restore the electro-mechanical properties of the multilayer system. This mechanism opens up the field of self-healing thin metallic films that could profoundly impact the design of future microelectronics.