Atomic Force Microscopy Measurements Research Articles

Atomic Force Microscopy Measurements of Cartilage in Intact and Regenerating Axolotl Limbs

Atomic Force Microscopy Measurements of Cartilage in Intact and Regenerating Axolotl Limbs

Inert Liquid Exfoliation and Langmuir-Type Thin Film Deposition of Semimetallic Metal Diborides.

Graphite is one of only a few layered materials that can be exfoliated into nanosheets with semimetallic properties, which limits the applications of nanosheet-based electrodes to material combinations compatible with the work function of graphene. It is therefore important to identify additional metallic or semimetallic two-dimensional (2D) nanomaterials that can be processed in solution for scalable fabrication of printed electronic devices. Metal diborides represent a family of layered non-van der Waals crystals with semimetallic properties for all nanosheet thicknesses. While previous reports show that the exfoliated nanomaterial is prone to oxidation, we demonstrate a readily accessible inert exfoliation process to produce quasi-2D nanoplatelets with intrinsic material properties. For this purpose, we demonstrate the exfoliation of three representative metal diborides (MgB2, CrB2, and ZrB2) under inert conditions. Nanomaterial is characterized using a combination of transmission electron microscopy, scanning electron microscopy, atomic force microscopy, IR, and UV-vis measurements, with only minimal oxidation indicated postprocessing. By depositing the pristine metal diboride nanoplatelets as thin films using a Langmuir-type deposition technique, the ohmic behavior of the networks is validated. Furthermore, the material decomposition is studied by using a combination of electrical and optical measurements after controlled exposure to ambient conditions. Finally, we report an efficient, low-cost approach for sample encapsulation to protect the nanomaterials from oxidation. This is used to demonstrate low-gauge factor strain sensors, confirming metal diboride nanosheets as a suitable alternative to graphene for electrode materials in printed electronics.

Characterization of identical lithium-ion battery electrodes before and after charge/discharge cycles via in-plane large-area polishing

As an effective method to fabricate a large-area cross-sectional sample for lithium-ion battery electrodes, we perform in-plane polishing of LiNi0.8Co0.15Al0.05O2(NCA) cathode samples and obtain a large cross-sectional area with a diameter of 1.5 mm. The polished cross-sections of NCA cathode particles are sufficiently flat to perform the atomic force microscopy (AFM) measurements on each cathode particle. Following AFM-based Kelvin probe force microscopy and scanning spreading resistance microscopy measurements, an identical in-plane polished NCA sample is assembled into a coin cell for the charge and discharge processes. After 90 charge/discharge cycles, the in-plane-polished sample is successfully disassembled from the coin cell without causing critical damage. In addition, a microcrack structure, which is a typical degradation feature of the cycles of NCA particles, is observed for the identical in-plane polished NCA sample. This indicates that the in-plane polishing method is effective for investigating identical NCA electrode samples before and after the charge/discharge process. Furthermore, the in-plane polishing method can be successfully applied to the large-area polishing of a Si-based anode which is a mixture of Si carbon complexes and graphite particles. This study presents a novel methodology for analyzing the degradation of lithium-ion battery electrode materials.

Machine learning approaches for improving atomic force microscopy instrumentation and data analytics

Atomic force microscopy (AFM) is a part of the scanning probe microscopy family. It provides a platform for high-resolution topographical imaging, surface analysis as well as nanomechanical property mapping for stiff and soft samples (live cells, proteins, and other biomolecules). AFM is also crucial for measuring single-molecule interaction forces and important parameters of binding dynamics for receptor-ligand interactions or protein-protein interactions on live cells. However, performing AFM measurements and the associated data analytics are tedious, laborious experimental procedures requiring specific skill sets and continuous user supervision. Significant progress has been made recently in artificial intelligence (AI) and deep learning (DL), extending into microscopy. In this review, we summarize how researchers have implemented machine learning approaches so far to improve the performance of atomic force microscopy (AFM), make AFM data analytics faster, and make data measurement procedures high-throughput. We also shed some light on the different application areas of AFM that have significantly benefited from applications of machine learning frameworks and discuss the scope and future possibilities of these crucial approaches.

Comparison of AlN/GaN heterojunctions grown by molecular beam epitaxy with Al and Ga assistance

Although conventional III-nitride molecular-beam-epitaxy growth theories indicate that high-quality AlN should be prepared in Al-assisted regimes, AlN/GaN heterojunctions grown in Ga-assisted regimes actually demonstrate superior performances. In this letter, we compared Al-assisted and Ga-assisted grown AlN/GaN heterojunctions and explored the underlying mechanisms. Aberration-corrected transmission electron microscope, energy dispersive spectrometer, and atomic force microscopy measurements indicate that the Al-assisted growth results in partly-relaxed AlN of high-density defects, deteriorating AlN/GaN interfaces, and surface morphology consisting of irregular and truncated atomic steps. The Ga-assisted growth produces high-quality pseudomorphic AlN with excellent AlN/GaN interfaces, surface morphology, and electrical properties. It is suggested that the better crystalline quality and higher performances of the Ga-assisted grown samples are attributed to a lower N subsurface diffusion barrier resulting from a higher energy of the fcc adsorption positions in the adlayer-enhanced-lateral-diffusion model and intense thermal motions of Ga adatoms. It helps to understand the kinetics of metal-adlayer-enhanced growth of AlN and AlN/GaN heterojunctions at atomic scale and optimize the growth processes. Meanwhile, it is demonstrated that amorphization and Al diffusion near the AlN surfaces occur due to Pt bombardment on highly tensile-strained AlN during focused-ion-beam fabrications. It implies that large strain in AlN/GaN heterojunctions might be an important issue to be considered for device reliability.

Imaging of micro-steps on as-grown surface of sapphire with X-ray phase contrast technique

Basal-faceted sapphire ribbons grown using the Stepanov–LaBelle technology have a low density of surface steps. We present our results on a study of steps on the surface of a ribbon, misoriented relative to the singular face (0001) by several arc minutes. The ribbon has been characterized by means of in-line phase contrast imaging technique at Pohang Light Source, South Korea. It was shown for the first time that a step height of about 1 μm can be determined directly from an image. The step height obtained using the phase contrast method was confirmed by atomic force microscopy measurements. We have found that the experimental contrast matches the theoretical simulations only if the calculated intensity profile has been convolved with a Gaussian function. The full width at half maximum of the Gaussian was independently got from previous measurements. We have obtained an analytical solution in the case of theoretical fully coherent phase contrast image. The inverse problem is easy to solve, since there is a direct proportionality between the contrast and the step height.

Surface Degradation of Mg2X-Based Composites at Room Temperature: Assessing Grain Boundary and Bulk Diffusion Using Atomic Force Microscopy and Scanning Electron Microscopy.

Practical application of thermoelectric generators necessitates materials that combine high heat-to-electricity conversion efficiency with long-term functional stability under operation conditions. While Mg2(Si,Sn)-based materials exhibit promising thermoelectric properties and module prototypes have been demonstrated, their stability remains a challenge, demanding thorough investigation. Utilizing atomic force microscopy (AFM) and scanning electron microscopy (SEM), we investigate the surface degradation of a composite material comprising Si-rich and Sn-rich Mg2(Si,Sn) solid solutions. The investigation reveals a pronounced dependence of stability on Sn content, with the Sn-rich phase Mg2Si0.13Sn0.87 displaying the formation of a nonprotective oxide layer. Subsequent AFM measurements provide evidence of dominating grain boundary diffusion of loosely bound Mg, compared to bulk diffusion, observed within a few days, ultimately resulting in a complete surface oxidation of the Sn-rich phase within several weeks. On the other hand, Mg2Si and Si-rich Mg2Si0.80±0.05Sn0.20±0.05 remain stable against Mg diffusion to the surface even after prolonged exposure. Comparison with previous investigations confirms that the degradation rate is found to be highly dependent on the Sn content, with markedly higher rates observed for x = 0.87 compared to x = 0.70 in Mg2Si1-xSnx. These findings contribute to a better understanding of the stability challenges associated with Mg2(Si,Sn)-based materials, essential for the development of robust thermoelectric materials for practical applications.

Study on the electrical performance degradation mechanism of β -Ga2O3 p-n diode under heavy ion radiation

The impact of heavy ion irradiation on the β-Ga2O3 p-n diode and its physical mechanism have been studied in this Letter. After the irradiation fluence of 1 × 108 cm−2, it is observed that the electrical performance of the device is significantly degraded. The forward current density (JF) is reduced by 49.4%, the reverse current density (JR) is increased by more than two orders of magnitude, and the breakdown voltage (VBR) is decreased by 30%. Based on the results of the deep-level transient spectroscopy measurement, it is concluded that acceptor-like traps generated with an energy level of EC-0.75 eV in the β-Ga2O3 drift layer dominate the JF degradation of the device, which are most likely related to Ga vacancies. These acceptor-like traps result in the reduction of change carrier concentration, which in turn leads to a decrease in JF. In addition, according to the conductive atomic force microscope measurements and theoretical calculation, it is clearly observed that the latent tracks induced by heavy ion irradiation can act as leakage paths, leading to a significant degradation of JR and VBR.

Enhanced Electrochemical Detection of Nonelectroactive Compounds Based on Surface Supramolecular Interactions on Chevron-like Graphene Nanoribbons Modified through Click Chemistry.

In this study, we have developed a nanostructured electrochemical sensor based on modified graphene nanoribbons tailored for the analysis of nonelectroactive compounds via a surface competitive assay. Stigmasterol, a nonelectroactive phytosterol, was selected as a representative case. Chevron-like graphene nanoribbons, chemically synthesized, were immobilized onto glassy carbon electrodes and covalently functionalized to allow the on-surface formation of a supramolecular complex. To this end, the nanoribbons were first modified through a diazotization process by electrochemical reduction of a 4-azidoaniline diazonium salt, leaving the electrode surface with azide groups exposed to solution. Next, the incorporation of a ferrocene group, as a redox probe, was carried out by a click chemistry reaction between ethynylferrocene and these azide groups. Finally, the recognition event leads to the formation of a supramolecular complex between ferrocene and a macrocyclic receptor on the electrode surface. To this end, the receptors cucurbit[7]uril, cucurbit[8]uril, and β-cyclodextrin were evaluated, with the better results obtained with β-cyclodextrin. Atomic force microscopy and scanning electron microscopy measurements were performed for the morphological characterization of the resulting electrochemical platform surface. The ability of β-cyclodextrin to form an inclusion complex with ferrocene or with stigmasterol allows to perform a competitive assay, which translates into the decrease and recovery of the ferrocene electrochemical signal. For stigmasterol determination, a linear concentration range between 200 and 750 μM and a detection limit of 60 μM were obtained, with relative errors and relative standard deviations less than 7.1 and 9.8%, respectively.

Novel hybrid interference and atomic force microscopy

Abstract A novel hybrid microscope which combines an interference microscopic (IM) and an atomic force microscopic (AFM) measurement mode is introduced. It is realised by adding an AFM probe to an IM, where the AFM probe can be mechanically switched in or out of the beam path of the IM. When the AFM cantilever is out of the beam path, the system works in the IM measurement mode for noncontact and fast optical measurements. When the AFM cantilever is in the beam path, it works in the AFM measurement mode, where the AFM tip interacts with sample surfaces for measurements. The deformation of the AFM cantilever induced by the tip-sample interaction force is detected from interference fringes, which are formed by the interference of the light beam reflected from the backside of the AFM cantilever and a reference beam in the IM. This novel design has a high-level synergy of AFM and IM technologies and provides several promising application potentials. For instance, it can bring high-resolution AFM measurements whenever and wherever needed in IM measurements, thus, to complement the lateral resolution limits of IM; The AFM measurement mode can provide measurement results with higher topography fidelity, thus, to offer in-situ reference areal surface metrology for IM measurements. In the paper, design concept, realisation of a prototype instrument, and experimental results illustrating the performance of the prototype instrument are detailed. 

Impact of temperature and salinity on fines detachment: AFM measurements and XDLVO theory

Fine particle detachment and subsequent migration can lead to severe pore plugging and consequent permeability decline. Therefore, it is crucial to quantify the critical condition when fine particle detachment occurs. The frequently observed deviations or even contradictions between experimental results and theoretical predictions of fines detachment arise from an insufficient understanding of adhesion force that can be highly influenced by salinity and temperature. To clarify the intrinsic influence of salinity and temperature on fines detachment, adhesion forces between carboxyl microspheres and hydrophilic silica substrates in an aqueous medium were measured at various salinities and temperatures using atomic force microscopy (AFM). The AFM-measured adhesion force decreases with increasing salinity or temperature. Trends of mean measured adhesion forces with temperature and salinity were compared with the DLVO and XDLVO theories. DLVO theory captured the trend with temperature via the impact of temperature on electric double layer interactions, whereas XDLVO theory captured the observed trend with salinity via the impact of salinity on the repulsive hydration force. Our results highlight the significance of hydration force in accurately predicting the fate of fines in porous media.

Grafting of nonpolar polyisoprene as midblock and polar polylactide as outer block onto cellulose to produce bio-based thermoplastic elastomers

Sustainable cellulose-graft-diblock copolymers (cellulose-graft-polyisoprene-block-polylactide, MCC-g-PI-b-PLLA, MCC was chemically modified microcrystalline cellulose) were designed and delicately synthesized for the first time by a mild and facile procedure via combining ring-opening polymerization and reversible addition-fragmentation chain transfer polymerization techniques, which conquered the difficulties in synthesis due to the distinct chemical properties among the MCC backbone, PI and PLLA blocks. Two separate glass transition temperatures were detected for MCC-g-PI-b-PLLA copolymers by differential scanning calorimetry, indicative of microphase separation, consistent with small-angle X-ray scattering and atomic force microscopy measurements. The α-form crystals of PLLA outer blocks were revealed by wide-angle X-ray diffraction measurement. The monotonic and step-cyclic tensile tests revealed that the mechanical property could be tuned by changing the molecular mass of PI midblock. The two ends of the soft PI midblock were anchored by rigid cellulose backbone and hard PLLA outer block, respectively, which served as physical crosslinking points. The rigid cellulose backbones brought the PI rubbery domains and PLLA hard domains together to form a whole hierarchical microstructure, endowing the copolymers with distinguished mechanical property. This work provided a feasible approach to producing environmental-friendly cellulose-based copolymers with fully biomass-derived feedstocks, having a promotional impact on the development of sustainable polymer-based materials.

Molecular-level studies of extracellular matrix proteins conducted using atomic force microscopy.

Extracellular matrix (ECM) proteins provide anchorage and structural strength to cells and tissues in the body and, thus, are fundamental molecular components for processes of cell proliferation, growth, and function. Atomic force microscopy (AFM) has increasingly become a valuable approach for studying biological molecules such as ECM proteins at the level of individual molecules. Operational modes of AFM can be used to acquire the measurements of the physical, electronic, and mechanical properties of samples, as well as for viewing the intricate details of the surface chemistry of samples. Investigations of the morphology and properties of biomolecules at the nanoscale can be useful for understanding the interactions between ECM proteins and biological molecules such as cells, DNA, and other proteins. Methods for preparing protein samples for AFM studies require only basic steps, such as the immersion of a substrate in a dilute solution or protein, or the deposition of liquid droplets of protein suspensions on a flat, clean surface. Protocols of nanolithography have been used to define the arrangement of proteins for AFM studies. Using AFM, mechanical and force measurements with tips that are coated with ECM proteins can be captured in ambient or aqueous environments. In this review, representative examples of AFM studies are described for molecular-level investigations of the structure, surface assembly, protein-cell interactions, and mechanical properties of ECM proteins (collagen, elastin, fibronectin, and laminin). Methods used for sample preparation as well as characterization with modes of AFM will be discussed.

Cracking the Pericellular Matrix Code: Exploring how MMP-2, -3, and -7 influence matrix breakdown and biomechanical properties

IntroductionThe intricate process of articular cartilage remodeling, pivotal for both physiological functions and osteoarthritis (OA) progression, is orchestrated through a balance of matrix synthesis and breakdown, which is mediated by matrix metalloproteinase enzymes (MMPs). At the heart of this remodeling lies the pericellular matrix (PCM), a specialized microenvironment encapsulating each chondrocyte and composed mainly of collagen type VI and perlecan. The aim of this study was to assess the impact of MMP-2, -3, and -7 on the structural integrity and biomechanical attributes of the PCM. MethodsHuman articular cartilage explants (N=10 patients) were incubated with activated MMP-2, -3, or -7, individually or in combination. Structural alterations in the PCM were evaluated by immunolabeling. The biomechanical properties of the PCM were measured using atomic force microscopy (AFM). ResultsCollagen type VI structural integrity and fluorescence intensity uniformly decreased across all enzyme groups, while perlecan was selectively affected by MMP-3 and -7. AFM measurements demonstrated decreased PCM stiffness after incubation with individual MMPs, leading to an overall ~31 % reduction in elastic modulus for each enzyme. Combinations of enzymes induced comparable significant biomechanical alterations (~35 %), except for MMP-2+MMP-7. DiscussionThis study highlights the significant influence of MMP-induced alterations in PCM composition on biomechanical properties, mirroring characteristics observed in early OA. Each MMP showed specificity in breaking down PCM, and an intriguing interplay, especially between MMP-2 and -7, indicated reduced efficacy in lowering PCM stiffness. Overall, MMP-2, -3, and -7 directly induce functional and structural PCM modifications.

Quantitative evaluation of the difference in residual collectors in sulfide and non-sulfide flotation processes

In this study, three separate flotation systems were studied to define the residual collectors found in different recycled water for sulfide (xanthate-chalcopyrite), non-sulfide with anionic (NaOL-dolomite) and cationic (DTAB-quartz) collector processes. The adsorption/desorption of collectors and the adsorption morphology were studied by the zeta potential and atomic force microscopy (AFM) measurements, the adsorption energy and configurations were simulated by the density functional theory-based first principal calculations. It was found that butyl xanthate (BX) was adsorbed on chalcopyrite surface with pronounced protrusions by chemisorption, and the residual BX in slurry was 5.79 %. While sodium oleate (NaOL) formed scattered protrusions on dolomite surface by weak adsorption, the residual NaOL in slurry was 30.74 % that reacted with the Ca2+ or Mg2+ cations. The dodecyl trimethyl ammonium bromide (DTAB) adsorbed on quartz surface through hydrophobic aggregations and the residual DTAB in slurry was 16.57 %. This work might provide a guidance for understanding reagent consumption and flotation performance in typical mineral flotation systems.

An alternative chlorine-assisted optimization of CdS/Sb2Se3 solar cells: Towards understanding of chlorine incorporation mechanism

The current strategies in the development of Sb2Se3 thin film solar cells involve fabrication and optimization of superstrate and substrate device architectures, with the preferable choice for TiO2 and CdS heterojunction layers. For CdS-based superstrate cells, several studies reported the necessity to apply CdCl2 or other metal halide-based post-deposition treatment (PDT), highlighting improvement of CdS/Sb2Se3 device efficiency. However, the need, effect, and mechanism of such PDT are very often not described. Additionally, the fact that many groups have not succeeded in demonstrating its benefits suggests that this strategy is not straightforward, requiring a deeper understanding towards a more unified concept. The present study proposes an alternative approach to the challenging CdCl2 PDT of CdS in CdS/Sb2Se3 device, involving controllable Cl incorporation in CdS films by systematically varying the concentration of NH4Cl in the CBD precursor solution from 1 to 8 mM. Structural and electrical characterizations are correlated with advanced measurements of Scanning Kelvin Probe, surface photovoltage, and atomic force microscopy to understand the impact of Cl incorporation on the properties of CdS films and CdS/Sb2Se3 devices. The validity of Cl incorporation in the CdS lattice and interdiffusion processes at the CdS-Sb2Se3 interface is confirmed by secondary ion mass spectrometry analysis. It is demonstrated that incorporation of 1 mM of NH4Cl, as a Cl source in CBD CdS, can boost the PCE of CdS/Sb2Se3 by ∼20 %. With this approach, we offer new perspectives on the optimization methodology for Cl-based CdS/Sb2Se3 device processing and complementary understanding of the physiochemistry behind these processes.

Advanced evaluation of novel quinoline derivatives for corrosion inhibition of mild steel in acidic environments: A comprehensive electrochemical, computational, and surface study

Corrosion poses a significant threat to the integrity and longevity of iron and its alloys, which are crucial materials for modern industry and infrastructure. This study investigates the effectiveness of two recently synthesized inhibitors based on quinoline structures: MPQ (2-methyl-5-(propoxymethyl) quinolin-8-ol) and AAQ ((((2-aminoethyl)amino)methyl)-2-methylquinolin-8-ol) in protecting steel against environmental degradation, particularly in acidic and chloride-rich conditions such as hydrochloric acid. The inhibitors exhibited significant corrosion inhibition efficiencies of 92.37 % for MPQ and 84.13 % for AAQ, as demonstrated through electrochemical analysis. Surface characterization techniques, including SEM-EDX(Scanning Electron Microscopy with Energy Dispersive X-ray analysis), AFM (Atomic Force Microscopy), and contact angle measurements, revealed the formation of a protective barrier film that reduces the corrosion rate. Additionally, theoretical calculations using the Gaussian package provided insights into the adsorption behaviors and protective mechanisms of the inhibitors on mild steel surfaces. The findings contribute to the ongoing search for viable corrosion inhibitors, offering prospects for application in industries and critical infrastructures to enhance corrosion protection and durability.

Sensing performance of Schiff base-calix[4]arene including amide units for detection of pharmaceutically active compounds on QCM sensor system

This study aimed to investigate the sensing performance of a Quartz Crystal Microbalance (QCM) sensor coated with a calix[4]arene derivative (calixarene phenol amide, CPhA), containing both Schiff base and amide groups against various pharmaceutically active compounds (PhACs) such as ibuprofen, diphenhydramine, naproxen, and ascorbic acid in aqueous media. CPhA was successfully coated on the QCM crystal surface, and its surface properties were studied using Atomic Force Microscopy (AFM) and contact angle measurements. Sensing studies showed that the CPhA-coated QCM sensor detected more PhACs than the compound 4 (unfunctionalized derivative)-coated sensor. The highest frequency variation and binding ratio values were achieved with the QCM sensor with a relatively low coating amount. The CPhA-coated QCM sensor achieved higher adsorption capacity and was significantly more sensitive to all PhACs than the compound 4-coated one. The fabricated sensor showed remarkable reproducibility for all PhACs except naproxen (NAP). The fabricated sensor exhibited a remarkable sensing performance for detecting PhACs, which is promising for developing novel calix[4]arene-coated QCM sensors for PhACs.

Influence of power ramps on the physical properties of AZO thin films deposited at room temperature by RF magnetron sputtering technique

Abstract Aluminum-doped zinc oxide (AZO) thin films were deposited on glass substrates at room temperature by RF sputtering technique. Power ramps between 125 and 105 W were applied with a step of 4 W by intervals of 15, 7.5 and 1.8 min, for 180 min at 1.60 Pa. In this study, we investigated the structural, morphological, electrical, and optical properties of AZO films. X-ray Diffraction analysis showed that the films have a wurtzite-type hexagonal crystalline structure with a preferential crystallographic orientation (002) normal to the c axis. The average transmittance is greater than 76% for the wavelength range in the visible spectrum. The bandgap values were found between 3.32 and 4.01 eV, and refractive index was 1.79–2.60. Atomic force microscope measurements show homogeneous films with a roughness between 17–22 nm. A minimum resistivity value of 2.0 × 10−3 Ω cm was obtained for the film by using a power ramp of 4 W/1.8 min.

(Invited) A Study of the SEI Layer Cross-Talk in Si/C Composite Li-Ion Anodes

Composite electrodes, especially silicon/carbon (Si/C) anodes, present significant opportunities for advancing the energy density of lithium-ion batteries (LIBs). However, challenges emerge, particularly in performance metrics when a high weight percentage of Si beyond 8-10 wt.% is employed 1. A nuanced understanding of the solid electrolyte interphase (SEI) in Si/C composites is imperative to overcome these limitations and enhance energy density. Conventional techniques such as ex-situ X-ray photoelectron spectroscopy and cryogenic electron microscopy face inherent drawbacks, including exposure to ultrahigh vacuum and the need for solvent washing, potentially altering the SEI layer 2. In contrast, nano-FTIR, utilizing Fourier transform infrared near-field spectroscopy, overcomes these challenges, enabling non-destructive probing of the SEI layer's chemistry and structure at room temperature within an inert atmosphere 3–5.In this study, we engineer custom-patterned electrodes featuring amorphous Si on atomically flat highly ordered pyrolytic graphite (HOPG) to emulate model composite electrodes. Leveraging nano-FTIR spectroscopy, near-field nanoscale white-light imaging, and atomic force microscopy measurements, our investigation reveals that the SEI on HOPG is enriched in organic lithium ethylene decarbonate (LiEDC), while the SEI on lithiated silicon unveils the presence of inorganic Li2CO3. Notably, we unveil a unique "mixed" SEI layer zone at the Si/HOPG interface, comprising a mixture of dominant SEI species from the surfaces of both the lithiated Si and the HOPG. The coexistence of these species suggests the formation of an SEI layer with presumably unique physicochemical properties, forming along Si-C interfaces in Si/C composite electrodes. These findings provide a comprehensive approach to studying model composite electrodes and offer valuable insights into optimizing the surface passivation of Si/C composite electrodes for high-performance LIBs. Acknowledgments This research was supported by the US Department of Energy (DOE)’s Vehicle Technologies Office under the Silicon Consortium Project directed by Brian Cunningham and managed by Anthony Burrell. References V. G. Khomenko and V. Z. Barsukov, Electrochim Acta, 52, 2829–2840 (2007).J. Wu, M. Ihsan-Ul-Haq, Y. Chen, and J. K. Kim, Nano Energy, 89, 106489 (2021).X. He, J. M. Larson, H. A. Bechtel, and R. Kostecki, Nat Commun, 13, 1398 (2022).I. Yoon, J. M. Larson, and R. Kostecki, ACS Nano, 17, 6943–6954 (2023).A. Dopilka, Y. Gu, J. M. Larson, V. Zorba, and R. Kostecki, ACS Appl Mater Interfaces, 15, 6755–6767 (2023).