Microscopy Techniques Research Articles

The DNA-PAINT palette: a comprehensive performance analysis of fluorescent dyes.

DNA points accumulation for imaging in nanoscale topography (DNA-PAINT) is a super-resolution fluorescence microscopy technique that achieves single-molecule 'blinking' by transient DNA hybridization. Despite blinking kinetics being largely independent of fluorescent dye choice, the dye employed substantially affects measurement quality. Thus far, there has been no systematic overview of dye performance for DNA-PAINT. Here we defined four key parameters characterizing performance: brightness, signal-to-background ratio, DNA-PAINT docking site damage and off-target signal. We then analyzed 18 fluorescent dyes in three spectral regions and examined them both in DNA origami nanostructures, establishing a reference standard, and in a cellular environment, targeting the nuclear pore complex protein Nup96. Finally, having identified several well-performing dyes for each excitation wavelength, we conducted simultaneous three-color DNA-PAINT combined with Exchange-PAINT to image six protein targets in neurons at ~16 nm resolution in less than 2 h. We thus provide guidelines for DNA-PAINT dye selection and evaluation and an overview of performances of commonly used dyes.

DNA-PAINT Probe Modifications Support High-Resolution Imaging with Shorter Binding Domains.

DNA-based Points Accumulation for Imaging in Nanoscale Topography (DNA-PAINT) is an effective super resolution microscopy technique, and its optimization is key to improve nanoscale detection. The state-of-the-art improvements that are at the base of this optimization have been first routinely validated on DNA nanostructure devices before being tested on biological samples. This allows researchers to finely tune DNA-PAINT imaging features in a more controllable in vitro environment. Dye-labeled oligonucleotide probes with short hybridization domains can expand DNA-PAINT's detection by targeting short nucleotide sequences and improving resolution, speed, and multiplexing. However, developing these probes is challenging as their brief bound state makes them difficult to capture under routine imaging conditions. To extend dwell binding times and promote duplex stability, we introduced structural and chemical modifications to our imager probes. The modifications included mini-hairpins and/or Bridged Nucleic Acids (BNA); both of which increase the thermomechanical stability of a DNA duplex. Using this approach we demonstrate DNA-PAINT imaging with approximately 5 nm resolution using a 4-nucleotide hybridization domain that is 43% shorter than previously reported probes. Imager probes with such short hybridization domains are key for improving detection on DNA nanostructure devices because they have the capability to target a larger number of binding domains per localization unit. This is essential for metrology applications such as Nucleic Acid Memory (NAM) where the information density is dependent on the binding site length. The selected imager probes reported here present imaging resolution equivalent to current state-of-the-art DNA-PAINT probes, creating a strategy to image shorter DNA domains for nanoscience and nanotechnology alike.

A Metallo‐ Silsesquioxane Synthesized from Cu (II) via a Cyanide Fe (III) Bridge: Synthesis and Application as an Electrochemical Sensor

AbstractA new metallohybrid silsesquioxane (S) was synthesized herein from copper and ferricyanide via a cyanide bridge to produce a new electroactive hybrid material (SCuH), which was then characterized by spectroscopic and microscopic techniques and cyclic voltammetry. The voltammetric behavior of SCuH employing a graphite paste electrode indicates a well‐defined redox couple with formal potential Eθ′=0.76±0.01 V. The electrode exhibited high sensitivity to nitrite and was successfully tested for nitrite detection. The linearity of the analytical curve was 2.0×10−4 mol L−1 − 1.0×10−3 mol L−1, with a limit of detection of 2.65×10−5 mol L−1, and sensitivity amperometric value of 57.63 mA/mol L−1. These findings suggest that this material displays exceptional potential for application in electrochemical sensors designed for nitrite detection.

Application of the EBSD Technique in the Study of Porosity and Permeability in Deformation Bands in Sandstone.

Deformation bands are common constituents of porous clastic fluid reservoirs. Various techniques have been used to study deformation band structure and the associated changes in porosity and permeability. However, the use of electron backscatter diffraction technique is limited. Thus, more information is needed regarding the crystallographic relationships between detrital crystals, which can significantly impact reservoir rock quality. We employ microscopic and microstructural investigation techniques to analyze the influence of cataclastic deformation bands on pore space. Porosity measurements of the Cretaceous Ilhas Group sandstone in NE Brazil, obtained through computerized microtomography, indicate that the undeformed domains exhibit a total porosity of up to 13%. In contrast, this porosity is slightly over 1% in the deformation bands. Scanning electron microscopy analyses revealed the presence of grain fragmentation and dissolution microstructures, along with cement-filling pre-existing pores. The electron backscatter diffraction analyses indicated extensive grain fragmentation and minimal contribution from intracrystalline plasticity as a deformation mechanism. However, the c axes of quartz crystals roughly align parallel to the orientation of the deformation band. In summary, we have confirmed and quantified the internal changes in a deformation band cluster, with grain size reduction and associated compaction as the main mechanism supported by quartz cementation.

Triple effective water treatment agent: P(AA/AMPS) capped sulfur quantum dots boast remarkable antiscale, antibacterial, and real-time tracking capabilities

Recent research has explored nanomaterials as sustainable scale inhibitors for water treatment. This research specifically delved into the development of environmentally benign antimicrobial sulfur quantum dot scale inhibitors (P(AA/AMPS)-SQDs) by capping P(AA/AMPS) with varying molecular weights. The synthesized P(AA/AMPS)-SQDs underwent thorough characterization employing high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, and zeta potential analysis. The inhibitory efficacy of P(AA/AMPS)-SQDs on calcium carbonate (CaCO3) and calcium sulfate (CaSO4) scale formation was conducted under diverse conditions, including scale inhibitor concentration, reaction time, temperature, and pH using scanning electron microscopy and X-ray powder diffraction techniques. Remarkably, the water agent P(AA/AMPS)-SQDs showcased exceptional fluorescence, water solubility, and resilience to high temperatures. At specified concentrations, P(AA/AMPS)-SQDs demonstrated remarkable inhibition efficiencies, with over 98 % inhibition against the CaCO3 scale at 20 mg/L and over 97 % inhibition against the CaSO4 scale at 0.5 mg/L, significantly outperforming traditional scale inhibitors. Furthermore, P(AA/AMPS)-SQDs exhibited almost 100 % inhibition efficiency against Bacillus subtilis at a dosage of 150 mg/L. Furthermore, molecular dynamics simulation and quantum chemical calculations were employed to clarify the scale inhibition mechanisms of P(AA/AMPS)-SQDs. This multifunctional water treatment agent, integrating scale inhibition, antimicrobial properties, and online monitoring capabilities, lays a solid foundation for potential applications in engineering domains.

Enhanced Saccharification Yield of Alkali Pretreated Sugarcane Bagasse Utilizing Customized Cellulase Cocktail from Trichoderma harzianum and Trichoderma viride

The experiment was conducted during 2023 at Bioenergy Laboratory, Department of RBEE, College of Agricultural Engineering and Technology, CCSHAU, Hisar, Haryana, India. Compositional changes in sugarcane bagasse subjected to varying concentrations of sodium hydroxide (0.3% to 1.2%), revealing significant increases in glucan content (from 37.13% to 53.81%) alongside decreases in xylan, acid-insoluble lignin, acid-soluble lignin, ash, and other extractives. These changes were validated using microscopic technique SEM, confirming the efficacy of the pretreatment process. The utilization of a customized cellulase cocktail derived from Trichoderma harzianum and Trichoderma viride holds significant promise in enhancing the saccharification from alkali-pretreated sugarcane bagasse. This study investigates the synergistic effects of cellulase enzymes produced by these fungi on the hydrolysis of lignocellulosic biomass. The enzymatic hydrolysis process is optimized by varying enzyme dosages, reaction conditions, and incubation times to maximize the release of fermentable sugars. Results indicate a substantial improvement in saccharification efficiency with the customized cellulase cocktail, highlighting its potential for sustainable biofuel production. The pretreated sugarcane bagasse, when saccharified with Trichoderma harzianum and Trichoderma viride individually, released 254.43 mg g-1 and 325.53 mg g-1 of reducing sugars, respectively, after 40 h of incubation. In contrast, the combined enzymatic cocktail achieved a substantial increase in glucose yields (345.12 mg g-1) at 40 h, showcasing the synergistic effect of the combined enzymatic activity. This research contributes to advancing bioconversion technologies for utilizing lignocellulosic biomass resources efficiently and economically, thus addressing key challenges in sustainable energy production.

Biosynthesis of microrubble-shaped nanoporous Co3O4/rGO NCs using leaves extract of Neolamarckia cadamba and its antibacterial/antioxidant performance

Nowadays, the whole globe is paying great attention for the sustainable development, eco-friendly and economical production of nanostructures materials. With this motivation, the present work portrayed one-step ‘in-situ’ bioinspired green fabrication of Co3O4–reduced graphene oxide nanocomposites (Co3O4–rGO NCs) for the first time utilizing an aqueous leaf extract of Neolamarckia cadamba. As-fabricated NCs were characterized by several analytical and electron microscopic techniques viz. X-ray diffraction (XRD), Fourier Transform-Infrared (FT-IR), Energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), BET (Brunauer-Emmett-Teller), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) to evaluate their phases, structure, shape, composition, chemical state, porosity, optical and morphological aspects. The XRD study revealed a cubic spinel symmetry of NCs, while crystallite size estimated around 25 nm. TEM spectroscopy exposed an average particle size 8–10 nm of Co3O4 grown on the surface of reduced graphene oxide (rGO NCs), whereas SEM analysis showed sharped microrubble-shaped morphology. The formation of NCs by doping metal oxide with rGO through in-situ method were confirmed by XRD, EDS, Raman, and XPS spectroscopy. The BET study estimated the specific surface area and pore size of NCs as 98 m2/g and 8.9 nm respectively. The Co3O4–rGO NCs demonstrated an effective bactericidal activity against S. aureus, E. coli, K. pneumoniae, and B. subtillis. Prominently it was found that, a significant antibacterial activity seen against E. coli and S. aureus at a concentration 0.1 mg/100 µL may be due to scaffold morphology, nanoscale-structures and nanoporosity of the NCs. Due to receiving significant antibacterial activity, material’s molecular docking was assessed. Furthermore, an antioxidant activity of leaf extract and NCs was evaluated by DPPH method. An outstanding biological study of bioinspired NCs revealed that material could be used as a potent antimicrobial agent.

Observation and characterization of titanium-like nano-filament in TiO2 memristor using superconducting electrode(s) and Andreev spectroscopy

A thin TiO2 semiconductor film embedded between two metal electrodes works as a memristor after being formed by soft breakdown. The forming creates a nano-filament that penetrates through the poorly conducting TiO2 film and connects the electrodes conductively. While previous works characterized the nano-filament properties (shape, composition, and resistivity) by electron microscopy techniques, we present a characterization by electrical measurements. In a typical memristor, both electrodes are made of normal metals. We study the metal/TiO2/metal memristors with a bottom electrode made of a superconducting NbN layer and a top electrode made of a normal (Pt) or superconducting (Nb) metal. The nano-filament connecting the electrodes touches the bottom electrode as a point contact, thus allowing us to perform point-contact Andreev reflection spectroscopy of the NbN superconductor. The spectra, measured below the critical temperature (15 K) of NbN, are analyzed theoretically. The analysis reveals the presence of one nano-filament and determines the nano-filament resistance, Sharvin resistance of the point contact, and Maxwell resistance of the electrodes. Moreover, it shows that the nano-filament is a conical-shaped Ti-like metal point contact with a tip diameter of ∼3–5 nm, Fermi velocity of 2×106m/s, and low-temperature resistivity of ∼10−8–10−7Ωm. Thus, the nano-filament in our device is not the Ti4O7 phase observed in previous works. Remarkably, the point contact spectrum of the superconducting NbN layer shows the Andreev peak typical for ballistic transport. This is because the point contact probes the NbN layer through a thin Al layer that mimics superconductivity of NbN via the proximity effect and eliminates the effects of tunneling and disorder.

First person – Angéline Geiser

ABSTRACT First Person is a series of interviews with the first authors of a selection of papers published in Journal of Cell Science, helping researchers promote themselves alongside their papers. Angéline Geiser is first author on ‘ A novel 3D imaging approach for quantification of GLUT4 levels across the intact myocardium’, published in JCS. Angéline is a PhD student in the lab of Prof. Gwyn W. Gould at Strathclyde Institute of Pharmacy and Biomedical Sciences, University of Strathclyde, Glasgow, UK, where her research focuses on the molecular study of metabolic disorders and cardiovascular diseases, with a newly spurred interest in super-resolution microscopy techniques.

Improved Cupressus sempervirens L. galls for methylene blue removal: adsorption kinetics optimisation using the DA-LS algorithm, characterisation, and machine learning modeling

ABSTRACT In this study, an investigation was conducted on the effectiveness of three bioadsorbents – galbuli of Cupressus sempervirens L. almond shells, and Luffa – for removing methylene blue (MB) from water. Various activation techniques and operational conditions were employed to enhance the adsorption capacity. The study focused on adsorption kinetics and equilibrium capacity. The results showed that microwave-dried galbuli of Cupressus sempervirens L. exhibited the highest adsorption capacity of 38.05 mg/g with an adsorption efficiency of 17.4%. To improve this capacity, the Dragonfly Algorithm-integrated least squares (DA-LS) was proposed to optimise the fitting of 32 adsorption isotherm models, which included a proposed modified Langmuir model. After optimisation, the sixth chemical treatment of Cupressus sempervirens L. reached a Langmuir isotherm qmax value of 84.44 mg/g, suggesting the high efficiency of the bioadsorbent compared to previous studies. Characterisation using microscopy and ATR-FTIR techniques revealed that chemical modifications led to rougher, microporous cellulose fibres and significant changes in the chemical structure, potentially enhancing the surface area and adsorption efficiency. To predict the adsorption capacity, the Support Vector Machine for Regression with DA (SVMR-DA) was utilised, achieving a root mean square error (RMSE) of 1.357 and an R2 of 0.9913. This high accuracy indicates a reliable model with a robust error distribution. These results suggest that Cupressus sempervirens L. can be an effective bioadsorbent for water treatment, with significant potential for industrial application.

Rational synthesis of highly efficient dual–Z–scheme InVO4/FeVO4/Ex–CQDs–g–C3N4 heterojunction for photo(electro)chemical water splitting and pollutant removal applications

BackgroundThe ever–growing concern for environmental pollution and the need for clean energy sources have driven research toward sustainable technologies. Semiconductor photocatalysis has emerged as a promising approach for both environmental remediation and clean energy generation due to its efficiency and environment–friendly nature. This work focuses on developing a novel photocatalyst capable of addressing two crucial environmental challenges: Cr(VI) removal and water splitting for clean hydrogen production. MethodsThis study presents the development of a dual–Z–scheme heterojunction photo(electro)catalyst based on a combination of metal vanadates (FeVO4 and InVO4) and ultrasound–exfoliated carbon–rich graphitic carbon nitride (Ex–C–g–CN), denoted as IVO/FVO/Ex–C–g–CN. The synthesized nanocomposite was thoroughly characterized using various spectroscopic and microscopic techniques (such as XRD, XPS, UV–DRS, FESEM, EDX, and PL) to understand its material properties and structure. These techniques are crucial for elucidating the relationship between the composition of the material and its photocatalytic performance. Significant findingsThe key innovation of this work lies in the design of the dual–Z–scheme heterojunction within the IVO/FVO/Ex–C–g–CN photo(electro)catalyst. This design fosters efficient separation of photogenerated charges, a critical factor for enhancing photocatalytic activity. The effectiveness of this approach is evident in the achieved removal efficiency of 97.17 % for 100 ppm Cr(VI) within just 60 min of visible light irradiation. This demonstrates the superior ability of the developed photocatalyst to address chromium contamination. Furthermore, the photocatalyst exhibits a remarkable photocurrent of 3.16 mA and a low onset potential of 112 mV for the photoelectrochemical oxygen evolution (OER) reaction. These findings highlight the potential of this material for solar–driven water splitting, a clean and sustainable method for hydrogen production. Additionally, the IVO/FVO/Ex–C–g–CN composite demonstrates excellent recyclability, maintaining high Cr(VI) removal efficiency over multiple cycles, indicating its reusability and cost-effectiveness. Overall, the exceptional photo(electro)catalytic performance of the IVO/FVO/Ex–C–g–CN dual–Z–scheme heterojunction positions it as a promising candidate for tackling environmental pollution and generating clean energy.

Fast microwave carbonization of aluminum-coated plastic wastes and perspectives: The examples of CDs and snack bags

Aluminum-coated plastics, such as CDs and snack bags, are widely used and consumed around the world. Since millions of CDs and trillions of snack bags end up in landfills and oceans as plastic waste every year, we suggest here an easy, fast, and cost-effective method for transforming this significant volume of garbage into added-value carbon using microwave technology. The proposed method differs from existing time- and energy-consuming pyrolytic processes employed in the traditional carbonization of this sort of waste. Conceptually, direct irradiation of the aluminum-coated plastic items in a domestic microwave oven heats up the metallic coating, thus triggering carbonization of the plastic substrate. The resulting carbon, which is characterized by means of X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) techniques, has structural similarities to carbons produced from CDs and snack bags using pyrolytic methods. In other words, the microwave technique produces similar effect, but it is faster and more energy efficient. We finally demonstrate some practical uses of the derived materials in gunpowder production, carbothermal production of metals and grey paint formulations.

Identification and Characterization of Elusive α Precipitates in Cu–Al–Ni Shape Memory Alloys with Combined Electron Microscopy Techniques

Identification and Characterization of Elusive α Precipitates in Cu–Al–Ni Shape Memory Alloys with Combined Electron Microscopy Techniques

Experimental study on hybrid fiber reinforced high performance concrete properties: Investigatingcomprehensive energy consumption capacity

The brittleness of concrete in tension increases with higher compressive strength, necessitating the study of cementitious composites that combine high strength and ductility. This study investigated the fresh and mechanical properties of high-strength concrete (HPC) incorporating fibers: steel, basalt, and polyethylene (PE). Hybrid fiber reinforced high performance concrete (HyFHPC) was created by tailoring mix proportions, with eight series of specimens cast, each carrying different fiber combinations alongside plain HPC as a reference. Compressive, tensile, and flexural tests were conducted, and results were analyzed. The electron microscopy techniques were employed to observe the microstructural morphology and perform elemental analysis of the composites. Findings revealed a dense HPC matrix with 1.5 % total fiber content, exhibiting uniform dispersion and ideal bonding. Digital image correlation (DIC) technique was utilized to analyze strain distribution and crack development of specimens in tension and bending, proving effective in tracking the strain and crack evolution. Statistical analysis of five influencing elements—cubic compressive strength, axial compressive strength, tensile energy dissipation, tensile fracture energy, and energy release rate—revealed Series F9 (S0.5P1) as optimal for comprehensive energy consumption performance. HyFHPC demonstrated enhanced strength, ductility, and toughness compared to HPC with mono fiber or none. The hybridization achieved positive synergy and improved reinforcing efficiency while conserving resources.

Probing photoinduced electron transfer events in phenylferrocene-corrole dyad.

Herein, we investigated PhFC (10-phenylferrocenyl-5,15-diphenyl corrole), a corrole-based donor-acceptor (D-A) dyad, to understand the energy/electron transfer reaction dynamics. Phenylferrocene acts as the donor moiety when attached to the meso position of the corrole ring in the PhFC D-A system. The photophysical properties of the PhFC dyad and its parent molecule, TPC (5,10,15-triphenyl corrole), were studied by UV-vis spectroscopy, steady state fluorescence spectroscopy, TCSPC and optical microscopy techniques. A slight red shift and broadening of both the Q-band and Soret bands are observed in the absorption spectra of the PhFC dyad in comparison to TPC, representing the weak electronic interaction between the phenylferrocene moiety and corrole ring. The fluorescence emission spectrum of the PhFC dyad is significantly quenched (>80%) in comparison to TPC, attributed to the photoinduced electron transfer (PET) from phenylferrocene to the corrole ring. We observed that the electron transfer rate in the PhFC system is solvent dependent. Our theoretical investigation supported the experimental findings on the electron transfer mechanism. The HOMO and LUMO arrangements of these PhFC dyads demonstrate the electron density distribution and the ability of the donor moieties to transfer electrons to the corrole moiety. Fluorescence lifetime imaging microscopy (FLIM) was used to image the homogeneous lifetime distribution of the PhFC dyad and TPC.

Impact of Ultrafiltration on the Physicochemical Properties of Bovine Lactoferrin: Insights into Molecular Mass, Surface Morphology, and Elemental Composition

The large-scale isolation of bovine lactoferrin (bLF) typically involves using large amounts of concentrated eluents, which might introduce impurities to the final product. Sometimes, protein pre-concentration is required for the greater accuracy of experimental results. In this research, the supplied bLF sample was subjected to additional ultrafiltration (UF) to eliminate possible small impurities, such as salts and peptides of bLF. Beforehand, the basic characterization of native bLF, including surface-charge properties and the structural sensitivity to the various pH conditions, was performed. The study aimed to evaluate the difference in molecular mass, primary structure, surface morphology, and elemental composition of the protein before and after UF. The research was provided by application of spectroscopic, spectrometric, electrophoretic, and microscopic techniques. The evident changes in the surface morphology of bLF were observed after UF, while the molecular masses of both proteins were comparable. According to MALDI-TOF/MS results, UF had a positive impact on the bLF sample representation, improving the identification parameters, such as sequence coverage and intensity coverage.

Design and decoration of copper nanoparticles into lignosulfonate-starch bionanocomposite: Characterization and evaluation of its therapeutic properties on burn wound

In this report, eco-friendly synthesis for the production of copper nanoparticles by employing the sodium lignosulfonate (NaLS) mixed starch composite (NaLS-Starch/Cu NPs). NaLS-Starch mixed hydrogel has notable reducing and stabilizing potential for preparation of Cu nanoparticles. Characterization of NaLS-Starch/Cu NPs bionanocomposite was subjected to analysis of spectroscopic and microscopic techniques, including FE-SEM, TEM, EDS-elemental mapping, particle size distribution, XRD and ICP. TEM images displayed the spherical structured NaLS-Starch/Cu NPs, averaging 5–10 nm size. NaLS-Starch/Cu NPs were applied to cure the induced burn wounds in 60 Wistar rats. A group was considered as control group. The animals were treated with basal, tetracycline 3 % and NaLS-Starch/Cu NPs 3 % for 30 days and the treatment efficacy was determined according to the burn wound area reduction and molecular and histological characteristics. Taken together, these results support therapeutic use of NaLS-Starch/Cu NPs as potent ointment that may be proposed for burn wound healing. NaLS-Starch/Cu NPs ointment increased the levels of platelet-derived growth factors (PDGF) and fibroblast growth factor (bFGF). The mean wound surface, in all groups treated by NaLS-Starch/Cu NPs was larger than control group.

Imaging Single Prussian Blue Nanoparticles with Extraordinary Low-Spin Iron Capacity.

In attempts to obtain high-capacity Prussian blue nanomaterials, current efforts are predominantly focused on the particle-ensemble-level understanding of their structure-activity relationships. Complementarily, it would be insightful to screen out extraordinary individuals from the nanoparticle population. Using a simple and efficient technique of bright-field microscopy, this work enables, for the first time, quantitative characterization of the overall two-redox-center electrochemistry of single Prussian blue nanoparticles many at a time. Quantitative optical voltammograms with little interference from solvent breakdown and non-Faradaic electrode charging/discharging are extracted for each single nanoparticle, revealing clear heterogeneity among them. On this basis, the microscopic method allows a detailed comparative analysis between the two redox-active sites. It is found that while the synthesized nanoparticles show a similar specific capacity of the high-spin (HS-Fe) sites with STD/mean = 30%, most individual nanoparticles exhibit monodispersedly small capacities of the low-spin iron (LS-Fe) sites, only about of the HS-Fe capacity. Most importantly, it is discovered that there is always a small fraction (∼8%) of the single nanoparticles showing an impressively tripled LS-Fe capacity. Facilitated by optical imaging, the discovery of this easily overlooked extraordinary subpopulation confers alternative opportunities for targeted efforts for material chemists to improve synthesis and material design based on these unusual individuals, which in turn implies the general significance of nanoparticle screening.

Fast Reduction of 4-Nitrophenol and Photoelectrochemical Hydrogen Production by Self-Reduced Bi/Ti3C2Tx/Bi2S3 Nanocomposite: A Combined Experimental and Theoretical Study.

The distinctive properties of 2D MXenes have garnered significant interest across various fields, including wastewater treatment and photo/electro-catalysis. The integration of inexpensive semiconductor nanostructures with 2D MXenes offers a promising strategy for applications such as wastewater treatment and photoelectrochemical hydrogen production. In this study, we employed an in situ hydrothermal method to immobilize 1D Bi2S3 nanorods and self-reduced metallic bismuth nanoparticles (Bi NPs) onto Ti3C2Tx MXene nanosheets, resulting in the formation of a Bi/Bi2S3/Ti3C2Tx (0D/1D/2D) composite catalyst, which demonstrates an outstanding efficacy in both the reduction of 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) and photoelectrochemical hydrogen production. Remarkably, a 4-NP reduction efficiency of 100% was achieved only in 4 min with a reduction rate of 1.14 min-1, which is outstanding, and it is ∼3.8 times faster than pristine Bi2S3 nanorods (0.3 min-1). Furthermore, the photoelectrochemical assessment reveals that the Bi/Bi2S3/Ti3C2Tx catalyst displays remarkable hydrogen evolution reaction (HER) efficiency in an alkaline electrolyte. It exhibits a significantly lower overpotential and Tafel slope of 73 mV and 84 mV/dec, respectively, compared to pristine Bi2S3 nanorods, which are found to be 129 mV and 145 mV/dec under light illumination. The superior reduction performance of 4-NP and charge transfer mechanism is further investigated through density functional theory (DFT) calculations, alongside validation using various microscopic and spectroscopic techniques. Interestingly, the DFT analysis revealed modifications in the partial density of states of Bi2S3 within the band gap region due to the successful anchoring of Ti3C2Tx nanosheets and metallic Bi NPs, facilitating efficient charge transport and separation across the local junctions. Ultraviolet photoelectron spectroscopy provided insights into band alignment and interfacial charge transfer across the Bi/Bi2S3/Ti3C2Tx junction on a microscopic scale. This work is significant for the development of MXene-based hybrid catalysts, and it provides a deeper understanding of the reduction mechanism of organic pollutants and superior charge transport in the hybrid system for photoelectrochemical hydrogen production.

Correlated 4D-STEM and EDS for the classification of fine Beta-precipitates in aluminum alloy AA 6063-T6

Tuning the properties of aluminum alloys AA 6063-T6 involves artificial aging to induce precipitate formation, particularly β’’ and β’ phases. Previous characterization challenges due to their similar appearance are addressed here by correlating 4D scanning transmission electron microscopy (4DSTEM) and energy-dispersive spectroscopy (EDS) mapping. This approach allows us to analyze the structure and composition of precipitates individually, overcoming limitations of conventional imaging and structural analysis techniques when the precipitates appear simultaneously, as is often the case. We present detailed characterizations of needle-shaped Beta precipitates, revealing distinct diffraction patterns (DPs) and compositional differences. The method's applicability extends beyond aluminum alloys, offering a promising strategy for complex composite material characterization with multimodal scanning transmission electron microscopy (STEM) techniques.