Cross-sectional Scanning Electron Microscopy Research Articles

Properties of Wedge Wire Bonded Connection Between a Composite Copper Core Aluminum Shell Wire and an 18650 Cylindrical Lithium-Ion Battery Cell.

Wedge wire bonding is a solid-state joining process that uses ultrasonic vibrations in combination with compression of the materials to establish an electrical connection. In the battery industry, this process is used to interconnect cylindrical battery cells due to its ease of implementation, high flexibility and ease of automation. Wire materials typically used in battery pack manufacturing are pure or alloyed aluminum and copper. While copper wires possess better electrical properties, the force used in the bonding process can lead to cell isolator damage and cell thermal runaway. This is an unacceptable result of the bonding process and has led to the development of new types of composite wires containing a copper core embedded in an aluminum shell. This material has the advantage of high copper electrical and thermal conductivity combined with less aggressive bonding parameters of the aluminum wire. The aim of this study was to establish a process window for the wedge wire bonding of 400 µm composite copper-aluminum Heraeus CucorAl Plus wire on the surface of a BAK 18650 battery cell. This study was conducted using a Hesse Bondjet BJ985 CNC wire bonder fitted with an RBK03 bond head designed for the bonding of copper wires. The methods used in this study included light and scanning electron microscopy of bond and battery cell cross-sections, shear testing on the XYZtec Sigma bond tester system, and energy dispersive spectroscopy. The results were compared with a previous study conducted using a wire of the same diameter and made out of high-purity aluminum.

Macroscopic Monograin Nano-Gyroid Thin Films in 4-inch Scale Through Shear-Rolling and Subsequent Solvent Annealing.

The gyroid structure from self-assembly is highly attractive for optical applications such as photonic crystals and metamaterials. However, due to the direction-dependent nature of these applications, achieving a monograin-level structure over a large area has remained challenging. In this study, the fabrication of unidirectionally oriented anisotropic nanocylinders of polystyrene-block-polydimethylsiloxane (PS-b-PDMS) is reported block copolymer thin films up to a 4-inch scale via a shear-rolling process, followed by solvent annealing to induce phase transition to nearly monograin gyroid structures. Grazing-incidence small-angle X-ray scattering (GISAXS) analysis and cross-sectional scanning electron microscope (SEM) images in the direction parallel to the shear-rolling direction reveal the preferential orientation with the (111) plane onto the YZ axis of the film, while only the (110) plane on the YZ axis of the film is observed in the perpendicular direction, with grain sizes approaching single-grain levels. For metamaterial applications, the PDMS domain is selectively removed, and gold is electroplated to produce monograin gold gyroid films.

Bisphenol A Polyoxyethylene Ether Sodium Sulfate as a New Leveler for Electrodeposition of Copper.

The electrochemical behavior of three types of bisphenol A polyoxyethylene ether sodium sulfate (BPA) is investigated through cyclic voltammetry striping tests. The results indicate that BPA-25 exhibited the most significant inhibition of Cu deposition. The nanotwinned Cu (nt-Cu) films are prepared by direct current electrodeposition in an acidic Cu sulfate bath containing a combination of conventional bath additives. Transmission electron microscopy (TEM) and cross-sectional scanning electron microscopy (SEM) results revealed that nt-Cu consisted of microcolumnar grains with high-density nanoscale coherent twin boundaries oriented parallel to the growth surface. The interaction between BPA-25 and the poly2-sulfur-2-propane sodium sulfonate (SPS) was further analyzed through galvanostatic measurements (GMs) and electron backscatter diffraction (EBSD). The results demonstrate that BPA-25 and SPS underwent competitive adsorption on the cathode surface, leading to the formation of nt-Cu. This growth mechanism provides a new perspective for the preparation of nt-Cu by using direct current electrodeposition.

Effects of carbon nanoparticle insertion on stress reduction in hydrogenated amorphous carbon films using plasma chemical vapor deposition

Stress reduction in hydrogenated amorphous carbon (a-C:H) films is of considerable interest for improving their performance as protective films. Herein, we reduced the compressive stress of the films by inserting carbon nanoparticles (CNPs) between two a-C:H layers to form an a-C:H/CNP/a-C:H sandwich structure using a system of plasma chemical vapor deposition (CVD). We measured the deposition features of the CNPs via transmission electron microscopy (TEM) and assessed the dependence of the stress on the thickness of the second a-C:H layer as a parameter of surface coverage, Cp. We represented the stress reduction as a function of Cp; mean size of large CNPs, and thickness of the first and second a-C:H layers. In addition, the surface and film morphologies were investigated using atomic force microscopy (AFM) and cross-sectional scanning electron microscopy (SEM). Compared with films without CNPs, those containing CNPs with 8.9 % Cp showed 36 % lower stress when the thickness of the second a-C:H layer was similar to that of the first (154 nm). The deposited CNPs exhibited two size groups, with mean sizes of the small and large CNPs of 5 and 16 nm, respectively. Stress reduction was strongly correlated with the distance between large CNPs. The insertion of CNPs between a-C:H films affects the surface morphology of the second layer, and the stress decreases when the growth stage of the film starts transitioning from three-dimensional (3D) to two-dimensional (2D).

Natural photosensitizer extraction from Delonix regia flowers for future photosensor for DSSCs applications

This study explores the utilization of Delonix regia (DR) (Gulmohar flower) as a natural photosensitizer in the fabrication of self-powered photosensors via dye-sensitized solar cells (DSSCs). Various photoanodes, including ZnO, ZnO/TiO2, and ZnO/TiO2/Nb2O5, were investigated for their performance enhancement in DR-based photosensors. The photoanodes were fabricated using different deposition methods sensitized with DR photosensitizer and characterized through X-ray diffraction analysis, Field emission scanning electron microscopy (FE-SEM), UV–visible, Fluorescence spectroscopy, and Fourier transform infrared spectroscopy (FTIR) analysis. The absorbance spectrum results indicate improved photosensitizer adsorption in visible light for the ZnO/TiO2/Nb2O5/DR photoanode compared to other configurations. The scanning electron microscopy (SEM) cross-section image of ZnO/TiO2/Nb2O5 confirmed the formation of a multilayer photoanode. Chronoamperometry experiments were conducted to evaluate the photo sensing behavior, focusing on sensitivity, photoresponsivity, specific detectivity, and quantum efficiency within the solar spectrum range. Among the devices, ZnO/TiO2/Nb2O5 exhibited the highest photoresponsivity (1.2 × 10 −3 A/W) and photodetectivity (26.78 × 104 Jones), demonstrating promising advancements in DR-sensitized photosensors. This research highlights the exceptional performance of DR-sensitized photoanodes, particularly ZnO/TiO2/Nb2O5, in advancing the capabilities of photo-sensing devices. The investigated configuration exhibited a rapid response speed of 723 ms and a remarkable sensitivity of 89.87% in detecting photo signals. These findings emphasize the potential of DR photosensitizers to enhance photo-sensing activities, with significant implications for diverse applications in photodetection. By leveraging the unique properties of DR, particularly its incorporation into ZnO/TiO2/Nb2O5, this study underscores the promising prospects for developing efficient self-powered photosensors. The insights gleaned from this work pave the way for further exploration and optimization in organic photosensors.

Synthesis of a novel bismuth molybdite/iron oxide thin film for oxytetracycline degradation in a photoelectrocatalytic system

In this study, heterostructures based on Bismuth molybdite/iron oxide (Bi2MoO6/Fe2O3) thin films were fabricated by a dip-coating technique using precursor solutions. The heterostructures were deposited on fluorine-doped tin oxide glass substrates. From a detailed characterization using X-ray diffraction and X-ray photoelectron spectroscopy, the formation of the orthorhombic phase for Bi2MoO6 and the co-existence of hematite and maghemite in Fe2O3 was demonstrated. Meanwhile, the field emission scanning electron microscopy cross-section images confirm the formation of well-defined Bi2MoO6 film under the Fe2O3 deposition. The optical band gap energies for the heterostructure obtained were estimated from the diffuse reflectance spectra and ranged from 2.3 to 3.5 eV. Photoluminescence analysis revealed an improved separation and faster transfer of photogenerated electrons and holes for the Bi2MoO6/Fe2O3 (Het) film. The best oxytetracycline (OTC) removal percentage through photoelectrocatalytic treatment was 96.85% using the Het. Besides, were carried out the variation of parameters which affect the OTC photoelectrocatalytic degradation as pH, potential applied, and scavenger assay. The 1O2 was the oxidant predominate, which attack the OTC ring to initiate and accelerate the degradation process. Based on the analysis of degradation intermediates and characteristics of Bi2MoO6/Fe2O3, possible degradation pathways and mechanisms of OTC were displayed. An enhancement of oxytetracycline degradation efficiency of Het fabricated compared to pristine oxides was achieved mainly due to avoid the charge recombination of photogenerated electron-hole pairs provided by Direct Z-scheme heterostructure. Finally, the Het fabricated represents a promising material for efficient and sustainable pharmaceutical removal applications.

Cross-sectional surface analysis of magnetic domains, microstructures, and magnetic properties of the low-temperature phase MnBi prepared by low-temperature vacuum sintering

In this work, the low-temperature phase MnBi prepared by a low-temperature vacuum sintering process at 325 °C was studied. We found a significant increase in the energy product from 2.63 MGOe in the 12-h sintered sample to 3.64 MGOe in the 48-h sintered sample. This improvement is attributed to the solid-liquid diffusion process. Cross-sectional scanning electron microscopy (SEM) reveals that MnBi forms at the external surface of Mn particles and along interior surfaces, notably within cracks. Transmission electron microscopy further demonstrates that the Mn ratio increases and Bi decreases with distance from the crack. The selected area diffraction showed variations in the Mn ratio with distance from cracks and identified both Bi and MnBi phases in the MnBi layer. Magnetic force microscopy (MFM) analysis exhibited large phase shifts indicating repulsive or attractive forces in single ferromagnetic domains. This provides valuable insight into magnetic domains in the MnBi regions near Mn cracks. The MnBi formation model, developed for the vicinity of single cracks with uniform MnBi content, partly explains the magnetic interactions and phase shifts observed near these cracks. These findings provide significant insights into the MnBi microstructural and magnetic properties, potentially useful in tailoring and engineering magnetic structures.

Magnification calibration of X-ray 3D microscopy using micro-line structures.

X-ray microscopy using computed tomography (CT) is an excellent three-dimensional imaging instrument. Three-dimensional X-ray microscopy (3DXRM) is a nondestructive imaging technique used to inspect internal and external structures in units of submicrometers or less. The 3DXRM, although attractive, is mostly used as an observation instrument and is limited as a measurement system in quantitative evaluation and quality control. Calibration is required for use in measurement systems such as coordinate measurement systems, and specific standard samples and evaluation procedures are needed. The certified values of the standard samples must ideally be traceable to the International System of Units (SI). In the 3DXRM measurement system, line structures (LSs) are fabricated as prototype standard samples to conduct magnification calibration. In this study, we evaluated the LS intervals using calibrated cross-sectional scanning electron microscopy (SEM). A comparison of the evaluation results between SEM and 3DXRM for the LS intervals provided the magnification calibration factor for 3DXRM and validated the LSs, whereby the interval methods and feasibility of constructing an SI traceability system were evaluated using the calibrated SEM. Consequently, a magnification calibration factor of 1.01 was obtained for 3DXRM based on the intervals of the LSs evaluated by SEM. A possible route for realizing SI-traceable magnification calibration of 3DXRM has been presented.

Optimization of photocurrent and surface wettability of new As10Bi30Se30Te30 thin films through annealing at different temperatures for optoelectronic applications

Group V-VI-based metal-doped double chalcogenides are essential in thermoelectric and suitable optoelectronic devices. The present investigation is based on optimising various optical, structural, and electrical behaviours of quaternary As10Bi30Se30Te30 films through thermal annealing at different temperature scales. The structural study by X-ray diffraction (XRD) exhibited the presence of various Bi2Se3, Bi2SeTe2, and Bi2Te3 phases in the annealed films. The crystallinity gradually enhanced after the annealing process. The microstructural modifications in the material have been confirmed through the Raman spectra. The elemental confirmation was verified from the energy dispersive X-ray (EDX) spectra, whereas the cross-sectional scanning electron microscopy (SEM) view showed the annealing-induced modifications in the films. The granular structure in the films is seen from the surface morphology study. The reduction of the energy gap from 1.36 ± 0.002 eV to 1.26 ± 0.001 eV upon annealing induced the increment in refractive index from 3.08 to 3.15. With annealing, the non-linear refractive index varied from 4.341x10−10 esu to 5.218 x10−10 esu. This indicates the narrowing of the bandgap and enhancement in the non-linear optical response of the material after the annealing process. The 3rd-order nonlinear susceptibility is also increased by annealing, thus making it suitable for nonlinear device applications. Annealing-induced surface change in the material enhances its surface wettability and makes it more hydrophilic. The linear enhancement in photocurrent with the voltage is ohmic and makes it suitable for various optoelectronic applications.

Optimising Sodium Borohydride Reduction of Platinum onto Nafion-117 in the Electroless Plating of Ionic Polymer–Metal Composites

The effects of process parameters on the electroless plating of ionic polymer–metal composites (IPMCs) were studied in this work. Specifically, the NaBH4 reduction of platinum onto Nafion-117 was characterised. The effects of the concurrent variation of NaBH4 concentration, stir time and temperature on surface resistance were studied through a full factorial design. The three-factor three-level factorial design resulted in 27 runs. Surface resistance was measured using a four-point probe. A regression model with an R2 value of 97.45% was obtained. Surface resistance was found to decrease with increasing stir time (20 to 60 min) and temperature (20 to 60 °C). These responses were attributed to increased platinisation rates, resulting in more uniform electrode deposition, confirmed by scanning electron microscopy (SEM) and energy-dispersive X-ray (EDAX) analysis. Surface resistance decreased, going from 1% to 5% NaBH4 concentration, but increased from 5% to 10% concentration. This behaviour was attributed to surface morphology: increased grain size inducing porous electrodes, in line with findings in the literature. The maximum tip displacement, measured through a computer vision system, as well as the maximum blocking force, measured through an analytical balance setup, were obtained for all 27 samples. The varying results were discussed with regards to surface and cross-sectional SEMs, alongside EDAX analysis.

The impact of pulsed Nd:YAG laser on the surface of n-Si and photo-electrical performance of silicon solar cells

Texturizing the surface of a silicon solar cell enhances performance by reducing reflection losses. Pyramidal texturization via wet chemical etching is standard in manufacturing, while plasma etching is often used for vertical hole texturization. Laser texturization offers a chemical-free, user-friendly alternative to plasma etching. Infrared (IR) transmission studies indicate that laser-textured samples transmit more IR light through n-Si than normally textured samples, suggesting that vertical grooves from laser texturization allow deeper light penetration. Analyses using cross-sectional Field Emission Scanning Electron Microscopy (FESEM), Energy Dispersion x-ray (EDX), and Energy Dispersive Spectroscopy (EDS) demonstrate the effects of laser texturization on the front surface of textured n-Si wafers. However, silicon solar cells with laser-textured surfaces demonstrated lower conversion efficiencies (1.20% to 4.30%) compared to conventionally textured cells (14.30%). The short-circuit current density (JSC) was also lower in laser-textured cells, below 17 mA cm−2, compared to 34.44 mA cm−2 in normally textured cells. At the same time, higher laser power (114 W) during texturization also led to the lowest JSC and open-circuit voltage (VOC), indicating that laser texturization may introduce defects and dislocations that degrade Si properties.

Time-dependent 532 nm laser irradiation for tuning in optical, structural, and surface wettability changes of Te/In2Se3 thin films for optoelectronic applications

Laser irradiation for tuning the optoelectronic parameters of semiconducting thin films is widely applicable and has many benefits. The aim of the study is 532 nm laser irradiation of Te/In2Se3 film at different laser exposure time scales. The bilayer structure and its conversion to a single layer with laser annealing were confirmed from cross-sectional scanning electron microscopy. At the same time, the element's appearance was found in the EDX analysis. FESEM probed the corresponding surface structure change. XRD and Raman's spectroscopy analyzed the increase in crystallinity with laser irradiation by mixing Te into the In2Se3 layer and related microstructural changes. The shift in Raman peak with lasing time signifies the effect of time of exposure. There is a systematic decrement in the transmittance of the films. Also, the absorption edge shift resulted in the decrement in bandgap with laser irradiation. The static refractive index and optical density increased as well. The skin depth was decreased with a minimal change in the optical electronegativity. The nonlinear refractive index increased from 1.638 × 10–9 esu to 1.773 × 10–9 esu by 60 min laser irradiation. Similarly, there was an increment in 3rd-order nonlinear susceptibility from 1.58 × 10–10 esu to 1.73 × 10–10 esu. The surface wettability test confirmed the hydrophilic nature of the samples with decreasing hydrophilicity by laser irradiation. The tuning in different properties of the Te/In2Se3 film by laser irradiation is suitable for various optoelectronic applications.

Double layer packaging based on active black chickpea protein isolate electrospun nanofibers and intelligent salep film containing black chickpea peel anthocyanins for seafood products

In this study, a double-layer active and intelligent packaging system was developed based on two main natural macromolecules i.e. protein and carbohydrate with green perspective. Firstly, the salep-based films containing different concentrations (0–8 % w/w) of the inclusion complex of β-cyclodextrin/black chickpea anthocyanins (βCD/BCPA) were produced. The salep film containing 8 % of βCD/BCPA complex was specified as the optimized film sample based on its performance as a color indicator. The electrospinning of black chickpea protein isolate nanofibers (BCPI NFs) containing citral nanoliposomes (NLPs) was done on the optimized salep film. The cross-sectional field emission scanning electron microscopy approved the creation of double-layer structure of the developed film. The study of chemical and crystalline structure, as well as the thermal properties of the film exhibited the physical attachment of BCPI electrospun NFs on salep film. The effectiveness of the developed system was studied in detection of spoilage and increasing the shelf life of seafood products, including shrimp and fish fillet. The performance of the intelligent layer in detection of freshness/spoilage was acceptable for both seafood products. In addition, the active layer of the film controlled the changes of pH, total volatile basic nitrogen, oxidation, and microbial load in samples during storage time.

Thermal cycling characterization of an integrated low-inductance GaN eHEMT power module

To exploit the potential of wide-bandgap semiconductors in high-frequency applications, innovative packaging designs are developed to minimize the parasitic inductance of power modules. This study presents an integrated power module with a hybrid PCB/DBC structure, which uses top-side cooling prepackaged GaN enhancement-mode high-electron-mobility transistors. The module achieves a remarkably low parasitic inductance of 2.65 nH. However, there is relatively scarce research on the reliability of this heterostructure, particularly its sensitivity to thermomechanical stress due to the coefficients of thermal expansion mismatch among material interfaces. In this work, the thermal cycling characteristics of the integrated power module are comprehensively investigated. Electrical and thermal parameters were periodically and separately measured offline on a simplified package to monitor the health conditions and decouple possible synergy and competition effects among the failure modes from all packaging components. A thorough failure analysis was conducted using nondestructive visual inspections and scanning acoustic microscopy, complemented by destructive cross-sectional examination and scanning electron microscopy. The findings identified the delamination of the DBC upper copper layer, which exhibited a conchoidal fracture interface, as the primary factor that contributed to the failure of the power module with increased thermal resistance. Furthermore, the study dissected its initiation and propagation mechanisms. This investigation provides valuable insights for the development of more reliable low-inductance power module designs.

(Invited) Spatially–Resolved Luminescence Properties of Etched Quantum Well Microstructures

Fabrication processes for photonic devices, especially micro- or nano-photonic devices, call for some kind of control of the materials’ optical properties at the stage of the final device. Our study focusses on measuring the optical quality of quantum well (QW) containing materials after device processing, using steps such as etching which allows fabrication of optical waveguides for example. We first designed and realized specific material structures based on an InP substrate, with a series of InAsxP1-x quantum wells such as illustrated on the figure. The samples were grown by gas-phase molecular beam epitaxy. The samples were characterized by spatially-resolved photoluminescence (PL) at low temperature (10 K). The top right part shows a typical spectrum measured from the sample we have grown: sharp lines associated with each QW can be clearly identified thanks to a careful grading of the As/P composition in each QW, while keeping its thickness to a constant value (typically 7 to 8 nm). Then we etched the samples (in the form of rectangular ridges as shown) using different etching processes, based either on wet etching or reactive ion etching (RIE), and recorded the PL spectra with high spatial resolution across the obtained structures. In parallel, the samples after etching were also characterized by cross-sectional scanning electron microscopy. Data processing from the series of PL spectra was then performed in order the characterize the effects of etching on the QW materials.We show PL intensity profiles across a series of etched stripes of different widths resulting from a RIE process. These intensity profiles were obtained from the lines associated with the different QWs in the structure. One can observe, first of all, that the PL intensity gradually increases from the edges to the center of the stripes, over a range of up to 10 µm. One can also observe that for “wide” stripes, i.e. 30 or 50 µm, the PL intensity for each line saturates at the same level in the central part. However, for the narrower stripes (10 or 20 µm), the PL signal does not reach the same level. This is the signature of some PL-limitation phenomenon, which extends its effects far from the etched sidewalls. A “standard” phenomenon resulting solely from non-radiative recombination at the etched sidewalls is excluded. Non-radiative recombination can only affect regions which are less than one charge carrier diffusion length from the sidewalls. Diffusion length in our materials is less than 1 µm. Therefore, some kind of “long range” interaction seems to affect our samples. We propose that this long range interaction is due to some stray static electric field resulting from the presence of residual ions left by the etching process at the sidewalls. The electric field affects the PL intensity through dissociation of excitons. Moreover, we observed that different conditions for the etching process (wet etching versus RIE, crystallographic orientation of the stripes) impact the magnitude of this PL intensity quenching.[1] Pearton S 1997 Materials Science and Engineering: B 44 1–7[2] Landesman J P, Isik-Goktas N, LaPierre R R, Levallois C, Ghanad-Tavakoli S, Pargon E, Petit-Etienne C and Jiménez J 2021 Journal of Physics D: Applied Physics 54 445106[3] Fiore A, Rossetti M, Alloing B, Paranthoen C, Chen J X, Geelhaar L and Riechert H 2004 Physical Review B 70 205311[4] Bludau W and Wagner E 1976 Physical Review B 13 5410–5414 Figure 1

The role of thickness on the structural and luminescence properties of Y2O3:Ho3+, Yb3+ upconversion films

The structural, surface, and upconversion (UC) luminescence properties of Y2O3:Ho3+,Yb3+ films grown by pulsed laser deposition, for different numbers of laser pulses, were studied. The crystallinity, surface, and UC luminescence properties of the thin films were found to be highly dependent on the number of laser pulses. The X-ray powder diffraction analysis revealed that Y2O3:Ho3+,Yb3+ films were formed in a cubic structure phase with an Ia 3¯\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\overline{3 }$$\\end{document} space group. The thicknesses of the films were estimated by using cross-sectional scanning electron microscopy, depth profiles using X-ray photoelectron spectroscopy (XPS), and the Swanepoel method. The high-resolution XPS was used to determine the chemical composition and oxidation states of the prepared films. The UC emissions were observed at 538, 550, 666, and 756 nm, assigned to the 5F4 → 5I8, 5S2 → 5I8, 5F5 → 5I8, and 5S2 → 5I7 transitions of the Ho3+ ions. The power dependence measurements confirmed the involvement of a two-photon process in the UC process. The color purity estimated from the Commission International de I’Eclairage coordinates confirmed strong green UC emission. The results suggested that the Y2O3:Ho3+,Yb3+ UC transparent films are good candidates for various applications, including solar cell applications.

Nanomechanical and microstructural properties of experimental bilayered zirconia ceramics after hydrothermal aging

Two experimental ceramic systems, 3Y-TZP/5Y-PSZ (3Y/5Y) and 4Y-PSZ/5Y-PSZ (4Y/5Y), underwent analysis before (3Y/5Yi or 4Y/5Yi) and after hydrothermal aging (3Y/5Ya or 4Y/5Ya) to simulate low-temperature degradation (LTD). The samples were sintered and characterized using scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy, alongside nanoindentation tests to measure elastic modulus (Em) and hardness (H). Assessments were conducted on the external surfaces and at individual layers on cross-sectioned samples at predetermined regions of interest (ROIs). Degraded superficial regions were observed in the cross-sectional SEM images of the 3Y and 4Y zirconia layers after aging. XRD indicated a tetragonal→monoclinic phase transformation in the aged groups for both 3Y (66 % m-ZrO2) and 4Y (29 % m-ZrO2). Raman spectroscopy revealed monoclinic phase amounts of 86 % for 3Y and 62 % for 4Y in the degradation regions observed in the SEM micrographs. Monoclinic phase peaks were virtually no longer detected in either material beyond a depth of 15 μm. Hydrothermal aging significantly diminished the H and Em values for the 3Y and 4Y zirconia surfaces. For the analysis of different zirconia surfaces within the same subgroup, all pairwise comparisons showed statistically significant differences, except for the values of H of 3Y/5Yi and Em for 4Y/5Yi. Regarding the nanoindentation results of cross-sectioned samples, the aging protocol did not affect the H and Em values of the equivalent ROIs (layers), regardless of the bilayered system. However, significant differences in H values were observed among the ROIs (layers) within the same bilayered system. Despite surface changes, nanomechanical properties remained preserved below the surface and at the interfaces of bilayered materials after aging. Nanoscale H values varied among some layers and interfaces, whereas the Em values exhibited differences across certain surfaces.

Polymer-Supported Graphene Sheet as a Vertically Conductive Anode of Lithium-Ion Battery.

The increasing demand for electric vehicles necessitates the development of cost-effective, mass-producible, long-lasting, and highly conductive batteries. Making this kind of battery is exceedingly tricky. This study introduces an innovative fabrication technique utilizing a laser-induced graphene (LIG) approach on commercial Kapton film to create hexagonal pores. These pores form vertical conduction paths for electron and ion transportation during lithiation and delithiation, significantly enhancing conductivity. The nongraphitized portion of the Kapton film makes it a binder-less, free-standing electrode, providing mechanical stability. Various analytical techniques, including scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Raman spectroscopy, and atomic force microscopy (AFM) are utilized to confirm the transformation of a 3D porous graphene sheet from a commercial Kapton film. Cross-sectional SEM images verify the vertical connections. The specific capacity of 581 mAh g-1 is maintained until the end, with 99% coulombic efficiency at 0.1C. This simple manufacturing method paves the pathway for future LIG-based, cost-effective, lightweight, mass-producible, long-lasting, vertically conductive electrodes for lithium-ion batteries.

Multiscale phonon thermal transport in nano-porous silicon

We performed a comprehensive multi-scale phonon-mediated thermal transport study of nano-porous silicon (np-Si) films with average porosities in the range of φ = 30%–70%. This depth-resolved thermal characterization involves a combination of optical methods, including femtosecond laser-based time-domain thermo-reflectance (TDTR) with MHz modulation rates, opto-thermal micro-Raman spectroscopy, and continuum laser wave-based frequency domain thermo-reflectance (FDTR) with kHz modulation rates probing depths of studied samples over 0.5–1.2, 2–3.2, and 23–34 μm, respectively. We revealed a systematic decrease in thermal conductivity (k) with the rise of φ, i.e., with the lowering of the Si crystalline phase volumetric fraction. These data were used to validate our semi-classical phonon Monte Carlo and finite element mesh simulations of heat conduction, taking into account disordered geometry configurations with various φ and pore size, as well as laser-induced temperature distributions, respectively. At high φ, the decrease in k is additionally influenced by the disordering of the crystal structure, as evidenced by the near-surface sensitive TDTR and Rutherford backscattering spectroscopy measurements. Importantly, the k values measured by FDTR over larger depths inside np-Si were found to be anisotropic and lower than those detected by the near-surface sensitive TDTR and Raman thermal probes. This finding is supported by the cross-sectional scanning electron microscopy image indicating enhanced φ distribution over these micrometer-scale probed depths. Our study opens an avenue for nano-to-micrometer scale thermal depth profiling of porous semiconducting media with inhomogeneous porosity distributions applicable for efficient thermoelectric and thermal management.

Thickness Variation of Conductive Polymer Coatings on Si Anodes for the Improved Cycling Stability in Full Pouch Cells.

Si-dominant anodes for Li-ion batteries provide very high gravimetric and volumetric capacity but suffer from low cycling stability due to an unstable solid electrolyte interphase (SEI). In this work, we improved the cycling performance of Si/NCM pouch cells by coating the Si anodes with the conductive polymer poly(3,4-ethylenedioxythiophene) (PEDOT) prior to cell assembly via an electropolymerization process. The thicknesses of the PEDOT coatings could be adjusted by a facile process parameter variation. Glow-discharge optical emission spectroscopy was used to determine the coating thicknesses on the electrodes prior to the cell assembly. During electrochemical testing, improvements were observed closely linked to the PEDOT coating thickness. Specifically, thinner PEDOT coatings exhibited a higher capacity retention and lower internal resistance in the corresponding pouch cells. For the thinnest coatings, the cell lifetime was 18% higher compared to that of uncoated Si anodes. Postmortem analyses via X-ray photoelectron spectroscopy and cross-sectional scanning electron microscopy revealed a better-maintained microstructure and a chemically different SEI for the PEDOT-coated anodes.