Evolution Of Surface Morphology Research Articles

Revealing the surface structure and morphology evolution of Co nanoparticle supported on ZrO2 surfaces

The optimization of structure-dependent activity of supported metal catalysts has driven the dynamic determination of the morphology of Co nanoparticles on ZrO2 using atomic-level simulations. Density functional theory (DFT) calculations combined with ab initio molecular dynamics (AIMD) simulations were used to investigate the surface structure, nucleation mechanism and morphology evolution of Con clusters supported on different ZrO2 facets. As the size of the Con (n = 1–5) cluster increases, the competition between Co-Co bonding and the interaction of Con clusters with the ZrO2 surface further promotes the nucleation of larger clusters. Co atoms prefer to nucleate into large clusters on both c-ZrO2(111) and t-ZrO2(101) surfaces, but this behavior is unfavorable on the m-ZrO2(-111) surface. The analysis of electric properties suggests that the types of hybrid orbitals and the number of electron transfer accounts for the difference in energies of Con clusters on ZrO2 surfaces. Further, the AIMD simulations verified the stable structure of small Co5 cluster obtained by DFT, and predicted the morphology of large Co13 clusters on ZrO2 surfaces under realistic reaction conditions, consistent with the experimental SAM images. Our work provides an intuitive understanding of structure and morphology evolution of catalysts for the targeted design of catalysts to achieve the desired activity and explore more reaction possibilities.

Evolution of tooth surface morphology and tribological properties of helical gears during mixed lubrication sliding wear

In mixed lubrication, the interplay of lubricant flows, solid asperity contact, and material wear between tooth surfaces creates complex and unpredictable contact states on tooth surface. To comprehensively understand the interaction between the lubrication and wear characteristics of the rough tooth surfaces of helical gears, this study established a mixed lubrication sliding wear calculation model for helical gears based on the mixed elastohydrodynamic lubrication model and Archard’s model. Specifically, the study aimed to examine the effects of surface topography features on average film thickness, contact area ratio, and accumulated wear at the meshing point. The findings demonstrated that the texture and power spectral density distributions of a non-Gaussian reconstructed surface closely resembled those of the actual ground surface. Furthermore, for non-Gaussian rough surfaces, a larger wavelength ratio enhanced microwedge motion, which increased film thickness and reduced wear. Additionally, a negatively skewed surface demonstrated better lubrication performance compared to both positively skewed and Gaussian surfaces. This improved performance is evident in the smaller contact area ratio and lower accumulated wear value of the negatively skewed surface.

Infrared microlens formation on chalcogenide polymer surface via femtosecond laser pulse ablation

In this study, we introduced micro-optical surface formation via femtosecond (fs) laser pulse scanning to chalcogenide polymer (ChP), a promising material for cost-effective infrared applications. Employing this method, we successfully fabricated a large-area poly(sulfur-random-(1,3-diisopropenylbenzene)) (S-r-DIB) microlens array (MLA) component. Each micro-concave spherical surface was crafted with a single fs laser pulse, serving as a micro-concave lens surface. We achieved a quasi-periodic MLA sample with over 2 × 105 micro-lenslets within a 10 mm × 10 mm footprint. Additionally, precise locating of laser pulse irradiation enabled us to create a hexagonal MLA with a filling factor over 37 %. Morphological investigations and imaging tests confirmed the adequate surface quality of the fabricated components, with its uniformity revealed by the virtual foci grid in near infrared region. To elucidate the forming conditions and mechanisms, we studied the evolution of surface morphology under various laser irradiation conditions. Laser induced damage thresholds of S70-r-DIB30 were experimentally determined for both 800 nm and 400 nm wavelengths under single- and multi-pulse irradiation scenarios. We identified the optimal fabrication fluence window as 115–205 mJ/cm2 with 800 nm single-pulse irradiation. The bandgap of the S70-r-DIB30 was estimated as 2.06 eV, and energy band analysis confirmed distinctions in ablation morphology. Furthermore, we investigated sub-surface morphology evolution using orthogonal ultrafast pump–probe imaging, revealing diversity compared to traditional inorganic and polymeric optical materials due to differing absorption and etching mechanisms. The elastic wave velocity of 3.2 km/s in this ChP and etching velocity of 0.7 μm/pulse were experimentally determined. These findings deepen our understanding of ChP material interaction with fs lasers, offering insights for potential applications such as surface engineering, substrate cutting, and micro-structure formation.

Ultrasonic Cavitation Erosion Behavior of GX40CrNiSi25-20 Cast Stainless Steel through Yb-YAG Surface Remelting.

Laser beam remelting is a relatively simple and highly effective technique for the physical modification of surfaces to improve resistance to cavitation erosion. In this study, we investigated the effect of laser remelting on the surface of cast stainless steel with 0.40% C, 25% Cr, 20% Ni, and 1.5% Si on cavitation erosion behavior in tap water. The investigation was conducted using a piezoceramic crystal vibrator apparatus. Base laser beam parameters were carefully selected to result in a defect-free surface (no porosity, material burn, cracks) with hardness capable of generating better resistance to cavitation erosion. The experimental results were compared with those of the reference material. Surface morphology and microstructure evolution after cavitation tests were analyzed using an optical metallographic microscope (OM), scanning electron microscope (SEM), and hardness tests to explore the mechanism of improving surface degradation resistance. The conducted research demonstrated that surfaces modified by laser remelting exhibit a 4.8-5.1 times greater increase in cavitation erosion resistance due to the homogenization of chemical composition and refinement of the microstructure, while maintaining the properties of the base material.

Modelling and experimental study of surface morphology evolution during layer growth on nanograting structures

Coating nano/micro-structured elements with a single or multi-layered film can greatly enhance their functionality. The experimental enhancement, however, is significantly limited by the smoothing and distortion of the structural profile after coating. This requires a comprehensive understanding of the layer growth behavior on nanoscale non-isotropic surface with a proper model to analyze and predict the structure evolution. Here, a simplified linear growth model with single free parameter was successfully used for analysis of the smoothening of grating grooves. The model enables a quantitative description of the evolution of surface morphology from substrate to the top surface with sub-nanometer accuracy. Based on this, the smoothing behavior of single-Si layer and W/Si multilayer growth on nanoscale gratings (period ∼ 40 nm) and flat substrates were studied experimentally, for applications in X-ray optics. The smoothing effect of the W/Si multilayer coating is more pronounced than that of the single Si layer for both substrate types. The corrugated nanogratings suppressed the smoothing effect as compared to the flat isotropic surface. These works provide new guidance to predict and control the growth of layers on nanostructures.

Harnessing ion beam erosion engineering for controlled self-assembly and tunable magnetic anisotropy in epitaxial films

The engineering of the surface morphology and the structure of the thin film is one of the essential technological assets for regulating the physical properties and functionalities of thin film-based devices. This study presents an easy and handy approach to tailor the surface structure of epitaxial thin films utilizing low-energy ion beam. Here, we investigate the evolution of the surface structure and magnetic anisotropy (MA) in epitaxial Fe/MgO (001) model systems subjected to multiple cycles of ion beam erosion (IBE) after thin film growth. The growth of Fe film occurs in the form of three–dimensional islands and exhibits intrinsic biaxial MA. Following a few cycles of IBE, an induced uniaxial magnetic anisotropy leads to a split in the hysteresis loop, and the film displays almost uniaxial magnetic switching behavior. More distinctly, we present a clear and conclusive evidence of (2 × 2) reconstruction of the Fe surface due to the atomic rearrangement by IBE. Furthermore, 57Fe isotope sensitive nuclear resonance scattering measurement provides insight into the depth-resolved magnetic information due to the modified surface topography. We also demonstrate that thermal annealing can reversibly tune the surface reconstruction and induced UMA. The feasibility of the IBE technique by adequately selecting IBE parameters for surface structure modification has been highlighted apart from conventional tailoring of the morphology for the tuning of UMA and introduces a new dimension to our understanding of self-assembled surface morphology evolution by IBE.

The surface morphologies and internal pores evolution of a CuSn10 alloy fabricated by laser powder bed fusion

The fabrication of high quality copper alloys using laser powder bed fusion (LPBF) technology remains challenging due to their low laser absorption and high thermal conductivity. LPBF often involves intrinsic defects, such as rough surface and internal pores, which largely deteriorate the performance of as-built copper alloy components. Here we studied the effect of scanning speed on the evolution of surface morphologies and internal pores of LPBF-fabricated CuSn10 alloy. The melt flow behaviors were studied by both experiments and in situ observations where combined a high-speed camera with an infrared thermal imager. With increasing the scanning speed, the morphology of melt track evolves from a continuous track to a discontinuous one, whereas the internal defects change from a great number of spherical pores to many irregular pores. A higher scanning speed decreases the peak temperature of the melt pool and causes less overlaps between neighboring melt tracks, thus deteriorating wetting behaviors. It is expected that the obtained results are beneficial for guiding the additive manufacturing of copper alloy parts with high metallurgical quality and thus promoting their industrial applications.

Development of Ce/Cu co-doped dendritic mesoporous silica nanoparticles (DMSNs) as novel abrasive systems toward high-performance chemical mechanical polishing

Development of novel abrasive systems with functional activities and physicochemical properties are of great significance in the reactive oxygen species (ROS)-enhanced chemical mechanical polishing. In this work, Ce single-doped and Ce/Cu co-doped dendritic mesoporous silica nanoparticles (DMSNs), namely Ce−DMSNs and Ce/Cu−DMSNs, were produced via a simple impregnation and thermolysis procedure. The Ce and/or Cu species involved in DMSNs frameworks were characterized through X-ray diffractometry, infrared spectroscopy, scanning electron microscopy, energy dispersive spectrometry, transmission electron microscopy, X-ray photoelectron spectroscopy, and nitrogen adsorption/desorption techniques. We report the evolution of surface morphology and roughness, defects, peak-to-valley data, image surface area difference, and material removal efficiency during ROS-enhanced polishing experiments toward silica materials. All the pure, Ce single-doped, and Ce/Cu co-doped DMSNs abrasive systems offered nearly defect-free surfaces with close-to-atom scale roughness. It might be attributed to the “springlike effect” and “soft polishing/abrasion”, possibly originating from the low-modulus DMSNs carriers. Among these abrasives, the Ce/Cu co-doped DMSNs systems achieved an evident improvement in removal efficiency, especially under ultraviolet irradiation-assisted polishing conditions. The coexisted Ce(Ⅲ)/Ce(Ⅳ) and Cu(Ⅰ)/Cu(Ⅱ) couples might be responsible for the effective production of ROS in photocatalysis and Fenton-like processes, thereby contributing to the Si–OH and Ce(Ⅲ)−O–Si bonding formations. The role of the developed Ce/Cu co-doped DMSNs abrasive systems in ROS-enhanced polishing processes was discussed.

Investigation of interfacial properties of Ag–Cu/Si3N4 composite ceramic substrates by interface reaction of Si3N4 and CuO

The surface metallization of Si3N4 ceramics with the Ag–Cu conductive paste containing CuO was systematically investigated. The interfacial reactions between CuO and Si3N4 promoted the surface metallization of the ceramic substrate in an argon atmosphere. The effects of Ag and Cu relative contents on the evolution of the thick film surface morphology were studied. The electrical properties and tensile strength of composite ceramic substrates were enhanced through the generation of Ag–Cu eutectic solution within the thick film layer. The effect of brazing time on the properties of Ag–Cu/Si3N4 composite ceramic substrates was investigated. Mechanical testing and scanning electron microscopy (SEM) were used to analyze the interface tensile strength of the Ag–Cu/Si3N4 composite substrates and the morphology of the Ag–Cu film, and the bonding mechanism of the composite ceramic substrate was studied. When the sample was brazed at 800 °C for 20 min, the maximum tensile strength of 23.6 MPa between the Ag–Cu film and ceramic substrate was obtained, the lowest resistivity of 6.22 μΩ•cm was obtained. The bonding interface between thick film layer and the ceramic substrate formed the Ag–Cu mechanical structure was benefit for improving the comprehensive performance of the Cu/Si3N4 composite ceramic substrate.

Numerical simulation of free-surface evolution in laser polishing of 100 Cr6 bearing steel

Abstract This research focuses on the laser surface polishing process of 100 Cr6, employing a moving Gaussian heat source. It establishes a two-dimensional transient model for laser polishing, taking into account the integrated effects of fluid flow and temperature fields, as well as the combined influence of capillary and thermocapillary forces. The model was used to perform numerical simulations to study the evolution of surface morphology during the laser polishing process. The investigation specifically examines how laser power and scanning speed influence the quality of the polishing outcome. The results demonstrate that an optimal surface roughness of approximately 0.571 μm is attained at a laser power setting of 200 W and a scanning speed of 300 mm/s.

Formation of partially embedded Au nanostructures: Ion beam irradiation on thin film.

The Au partially embedded nanostructure (PEN) is synthesized by ion irradiation on an Au thin film deposited on a glass substrate using a 50 keV Ar ion. Scanning electron microscopy results show ion beam-induced restructuring from irregularly shaped nanostructures (NSs) to spherical Au NSs, and further ion irradiation leads to the formation of well-separated spherical nanoparticles. Higuchi's algorithm of surface analysis is utilized to find the evolution of surface morphology with ion irradiation in terms of the Hurst exponent and fractal dimension. The Au PEN is evidenced by Rutherford backscattering spectrometry and optical studies. Also, the depth of the mechanism behind synthesized PEN is explained on the basis of theoretical simulations, namely, a unified thermal spike and a Monte Carlo simulation consisting of dynamic compositional changes (TRIDYN). Another set of plasmonic NSs was formed on the surface by thermal annealing of the Au film on the substrate. Glucose sensing has been studied on the two types of plasmonic layers: nanoparticles on the surface and PEN. The results reveal the sensing responses of both types of plasmonic layers. However, PEN retains its plasmonic behavior as the NSs are still present after washing with water, which demonstrates the potential for reusability. RESEARCH HIGHLIGHTS: Synthesis of PENs by ion irradiation Utilization of Higuchi's algorithm to explore the surface morphology. Unified thermal spike and TRIDYN simulations being used to explain the results. Glucose is only used as a test case for reusability of substrate.

Droplet asymmetry bouncing on structured surfaces: A simulation based on SPH method

The impact of a liquid droplet onto a macro-structured super-hydrophobic surface, results in an asymmetric spreading-retraction process and a significant decrease in contact time. The process involves large deformation of droplets and evolution of surface morphology, so it is difficult to efficiently simulate using traditional grid-based methods. In this study, a numerical model is established using the mesh-free smoothed particle hydrodynamics (SPH) method to simulate the interaction of liquid droplets with solid surfaces exhibiting complex macro-textures. Leveraging the Lagrange nature of SPH, liquid droplets can be model using free surface boundary condition. The weakly compressible SPH formulation is employed to discretize the governing equations of liquid. Surface tension is captured by introducing an additional negative pressure term, inducing attractive forces among fluid particles. Kernel functions are carefully chosen to mitigate stress instability resulting from droplet spreading and retraction. The model is then applied to simulate the dynamic processes of droplets impact on flat and non-flat super-hydrophobic surfaces. The bouncing dynamics of droplets are investigated under varying conditions, including Weber number, size, and morphology of macro-scale surface structures. Our simulation results for contact time, maximum diameter, and droplet morphology align closely with experimental observations. The contact time of the droplet exhibits a dependency on its size and surface geometry, with a transition towards planar geometry diminishing asymmetric spreading effects. The findings highlight the significance of Weber number and cylinder diameter in determining contact time, providing insights for the design of optimized surface structures for specific droplet impact parameters. In addition, the use of a free-surface condition for modeling proved computationally efficient for 3D simulations. The model effectively reproduces nonlinear behaviors such as droplet spreading, splashing, and bouncing, highlighting the significant advantage of SPH in simulating such problems.

Morphology evolution and non-uniformity removal mechanism analysis of diamond nanocone arrays by reactive ion etching

Microstructures of diamond can be fabricated by reactive ion etching and during this process the evolution of surface morphology can affect the electric field near the microstructure. These changes in the electric field will alter the trajectory of ions, thereby affecting the number of ion bombardments on the surface regions of the microstructure. Consequently, this will affect the removal rate of the material on the microstructure surface and consequently affects the evolution of microstructure morphology. In order to understand the morphology evolution process of diamond during etching. H2 and Ar were used as the reactive gases to etch the nanocrystalline diamond (NCD) films with masks. The electric field near the microstructure and the trajectories of reactive ions was stimulated. The number of H+ and Ar+ bombardments at various regions on the diamond microstructure surface has been recorded and analyzed. By observing the cross-sectional morphology of the microstructure at different periods, the etching process of nanocones was analyzed. The study found that the microstructure of the diamond surface would gradually be etched into convex shaped and waist drum shaped and cone. By stimulating the electric field near the microstructure, it was found that the electric field distorted near the microstructure, causing the electric field lines initially perpendicular to the diamond surface to be diverted. As a result, the trajectory of the particles originally arrived perpendicularly to the diamond surface was distorted and hence they bombarded against the sidewall of the diamond microstructures. The angle between the ion trajectory and the electric field line also increased gradually.

Modeling the coverage of MoS2 and WS2 thin films using in-situ spectroscopic ellipsometry

In-situ spectroscopic ellipsometry (SE) was used to analyze monolayer and few-layer samples of molybdenum disulfide (MoS2) and tungsten disulfide (WS2) grown by metalorganic chemical vapor deposition (MOCVD) on sapphire substrates. MoS2 and WS2 film growth times ranged from 5 – 40 min to achieve a range of film coalescence and surface coverage from less than a monolayer to considerable bilayer and additional layers. Post-growth measurements using atomic force microscopy, photoluminescence and Raman spectroscopy were used to assess the evolution of surface morphology and film properties with growth time to determine the areal coverage of monolayer, bilayer, multilayer and void regions. The room temperature SE spectra were modeled using an effective medium approximation to obtain the monolayer and bilayer dielectric functions of MoS2 and WS2. Using these distinct dielectric functions, changes in ellipsometry parameters associated with partial to full coverage of monolayers and bilayers were simulated. Such simulations will enable improved control of the layer-by-layer deposition of MoS2 and WS2 by monitoring in-situ spectroscopic ellipsometry.

Surface roughness evolution and heterogeneous plastic deformation of austenitic stainless steel during micro deep drawing: Modeling and experiment

The present work involves the numerical simulation and experimental study on the surface roughness evolution and heterogeneous plastic deformation (strain localization and concomitant surface morphology evolution) in grain scale of micro deep drawn parts of austenitic stainless steel (ASS) 304 foils. A three-dimensional modeling framework was used to simulate the micro deep drawing (MDD) process. The simulation involved the development of a Voronoi-based polycrystalline geometry model (VPGM), a multi-stress-strain response model, and a crystal plasticity finite element methods (CPFEM) model. The results indicate that CPFEM model exhibits higher accuracy in the localized stress and strain, thickness distribution fluctuation and surface roughness evolution of the fabricated parts compared to multi-stress-strain response model. Therefore, the plastic deformation heterogeneity in MDD is in-depth discussed based on CPFEM model. The results show that the coarse-grained foils correspond to the intense strain localization, which is the main cause of surface roughening. Considering the average grain size is close to the thickness of ASS foils, mounding features on the rough surface may readily develop further into potentially fractured sites during deformation. On the other hand, crystal orientation influence plastic deformation by affecting the slip behavior of materials. The effect of crystal orientations including {011} 〈211〉 (Brass), {011} 〈100〉 (Goss), and {112} 〈110〉 components on deformation is discussed. The results indicate a strong correlation between the magnitude of the Schmid's factor and the ease of deformation. Additionally, variations in Schmid's factor across different directions result in differences in deformation accumulation, which affects the thickness distribution along the radial direction and the distribution of earrings and wrinkles along the circumferential direction of the fabricated micro parts.

Linear vs. Non-linear Behaviour in Ion Irradiation Nanostructuring of Nickel and Silicon Surfaces

Spontaneous nanometre-scale quasi-periodic ripple-like structures are formed at the surface of polycrystalline Ni films and Si(111) single crystal wafers by irradiation with a broad Ar+ ion beam at room temperature and studied with Atomic Force Microscopy as a function of fluence. The development of these structures can be reproduced by numerical solution of a continuum equation describing the evolution of surface morphology under ion irradiation, using realistic coefficients derived from material properties. In particular, we demonstrate that differences observed in pattern formation on the two surfaces under the conditions studied, such as wavelength stability and exponential growth of interface width for the Ni surfaces compared with wavelength coarsening and interface width saturation on Si(111), can be understood in terms of a cross-over between linear and non-linear behaviours.

The Study on Corrosion Resistance of Ti-6Al-4V ELI Alloy with Varying Surface Roughness in Hydrofluoric Acid Solution

The corrosion resistance of titanium alloy poses a crucial challenge, significantly affecting its prospect for service and application. The present study aimed to investigate the corrosion resistance of Ti-6Al-4V ELI alloys with varying surface roughness in hydrofluoric acid solution, in order to assess the influence of roughness on their corrosion resistance performance. The weight loss percentage, surface morphology evolution, and roughness variation of Ti-6Al-4V ELI alloys before and after exposure to hydrofluoric acid corrosion were characterized. While the weight loss and weight loss percentage of the Ti-6Al-4V ELI alloy increased with prolonged corrosion, the overall weight loss rate decreased. The accumulation of TiF3 phases and depletion of the Ti-6Al-4V ELI matrix mutually led to the alterations of the surface roughness. Due to the inability to prevent fluoride ions from contacting with the Ti-6Al-4V ELI alloy, continuous corrosion occurred in hydrofluoric acid. Based on these experimental results and analysis, the corrosion mechanism of the Ti-6Al-4V ELI alloy corroded by hydrofluoric acid solution was elucidated. Furthermore, an analysis was conducted to explore the influence of corrosion time on mechanical properties by analyzing the decay in compressive properties of the Ti-6Al-4V ELI titanium alloy after hydrofluoric acid corrosion treatment. The bearing capacity of the Ti-6Al-4V ELI alloy deteriorated over the corrosion time.

Investigating the Dynamic Mechanical Properties and Strengthening Mechanisms of Ti-6Al-4V Alloy by Using the Ultrasonic Surface Rolling Process.

The demand for titanium alloy has been increasing in various industries, including aerospace, marine, and biomedical fields, as they fulfilled the need for lightweight, high-strength, and corrosion-resistant material for modern manufacturing. However, titanium alloy has relatively low hardness, poor wear performance, and fatigue properties, which limits its popularization and application. These disadvantages could be efficiently overcome by surface strengthening technology, such as the ultrasonic surface rolling process (USRP). In this study, the true thermo-mechanical deformation behavior of Ti-6Al-4V was obtained by dynamic mechanical experiment using a Hopkinson pressure bar. Moreover, USRP was applied on the Ti-6Al-4V workpiece with different parameters of static forces to investigate the evolution in surface morphology, surface roughness, microstructure, hardness, residual stress, and fatigue performance. The strain rate and temperature during the USRP of Ti-6Al-4V under the corresponding conditions were about 3000 s-1 and 200 °C, respectively, which were derived from the numerical simulation. The correlation between the true thermo-mechanical behavior of Ti-6Al-4V alloy and the USRP parameters of the Ti-6Al-4V workpiece was established, which could provide a theoretical contribution to the optimization of the USRP parameters. After USRP, the cross-sectional hardness distribution of the workpiece was shown to initially rise, followed by a subsequent decrease, ultimately to matrix hardness. The cross-sectional residual compressive stress distribution of the workpiece showed a tendency to initially reduce, then increase, and finally decrease to zero. The fatigue performance of the workpiece was greatly enhanced after USRP due to the effect of grain refinement, work hardening, and beneficial residual compressive stress, thereby inhibiting the propagation of the fatigue crack. However, it could be noted that the excessive static force parameter of USRP could induce the decline in surface finish and compressive residual stress of the workpiece, which eliminated the beneficial effect of the USRP treatment. This indicated that the choice of the optimal USRP parameters was highly crucial. This work would be conducive to achieving high-efficiency and low-damage USRP machining, which could be used to effectively guide the development of high-end equipment manufacturing.

Influence of deposition pressure on the microstructure and mechanical properties of sputter-deposited MoNbTaW refractory multi-principal element alloy thin films

A systematic investigation into the effects of deposition pressure on the microstructure and mechanical properties of MoNbTaW refractory multi-principal element alloy (RMPEA) films deposited on Silicon (100) substrates using direct current magnetron sputtering (DCMS) is presented. The deposition pressure was varied from 3 Pa to 0.3 Pa at a homologous temperature (T/Tm) ≤ 0.1. The crystal structure, surface morphology, cross-sectional microstructure and mechanical properties were studied using X-ray diffraction, scanning and transmission electron microscopy and nanoindentation. X-ray diffraction findings indicate a single-phase BCC structure throughout the pressure range. An evolution in surface morphology was observed, coupled with a transition from a void-rich to a densified microstructure as the deposition pressure decreased, in line with the structure zone model. Additionally, variations in crystallographic orientations were detected, with changes in I(110)/(211) suggesting an interplay between film growth dynamics and crystallographic orientation shifts with the deposition pressure. The mechanical properties have shown significant improvement, with hardness and modulus values increasing from 7GPa to 12 GPa and 135 GPa to 243 GPa, with a decrease in deposition pressure. The study provides insights into the deposition mechanism, highlighting that microstructural changes and variations in crystallographic orientations are influenced by deposition pressure-induced alterations in adatom energy and surface mobility, thus affecting the films' mechanical properties.

Millisecond X-ray reflectometry and neural network analysis: unveiling fast processes in spin coating.

X-ray reflectometry (XRR) is a powerful tool for probing the structural characteristics of nanoscale films and layered structures, which is an important field of nanotechnology and is often used in semiconductor and optics manufacturing. This study introduces a novel approach for conducting quantitative high-resolution millisecond monochromatic XRR measurements. This is an order of magnitude faster than in previously published work. Quick XRR (qXRR) enables real time and in situ monitoring of nanoscale processes such as thin film formation during spin coating. A record qXRR acquisition time of 1.4 ms is demonstrated for a static gold thin film on a silicon sample. As a second example of this novel approach, dynamic in situ measurements are performed during PMMA spin coating onto silicon wafers and fast fitting of XRR curves using machine learning is demonstrated. This investigation primarily focuses on the evolution of film structure and surface morphology, resolving for the first time with qXRR the initial film thinning via mass transport and also shedding light on later thinning via solvent evaporation. This innovative millisecond qXRR technique is of significance for in situ studies of thin film deposition. It addresses the challenge of following intrinsically fast processes, such as thin film growth of high deposition rate or spin coating. Beyond thin film growth processes, millisecond XRR has implications for resolving fast structural changes such as photostriction or diffusion processes.