Energy Dispersive X-ray Spectroscopy Research Articles

Synthesis, Characterization, and Electrocatalytic Properties of PrMn0.5M0.5O3 (M = Cr, Fe, Co, Ni) Perovskites

In this paper, the synthesis, characterization, and investigation of electrocatalytic properties of perovskites of general formula PrMn0.5M0.5O3 (M = Cr, Fe, Co, Ni) are presented. The synthesis was conducted by the solution combustion method using glycine as a fuel. The perovskite with the formula PrMn0.5Fe0.5O3 was also synthesized by the sol–gel combustion method with citric acid as fuel. The obtained perovskites were investigated by X-ray powder diffraction (XRPD), scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX), infrared spectroscopy, and cyclic voltammetry. The XRPD patterns showed that the compounds are pure and isostructural within the series. The unit cell parameters of the compounds were determined within the Pnma space group, and several crystallochemical parameters were calculated and discussed. The recorded SEM images of the perovskites revealed a porous morphology, while the EDX analysis confirmed the 2:1:1 atomic percentage ratio of Pr:Mn:M. Within this investigation, the electrocatalytic properties of the obtained perovskites towards oxidation of OH− ions and H2O2 oxidation in phosphate buffer were studied by cyclic voltammetry, using a paraffin-impregnated graphite electrode (PIGE) modified with microcrystals of the investigated perovskites. PrMn0.5Fe0.5O3 showed high electrocatalytic activity for OH− oxidation, while both PrMn0.5Fe0.5O3 and PrMn0.5Co0.5O3 exhibited significant efficiency for H2O2 oxidation, with a distinct oxidation peak with a peak potential of 0.6 V.

Methodology for evaluation of lithium-ion black-mass battery recycling

Abstract In response to the growing demand for critical raw materials, the European Commission is actively pursuing strategies to recycle these materials from various sources, including disused batteries. One of the significant challenges in this endeavor is the heterogeneous nature of the materials arriving at recycling plants, necessitating effective process evaluation. In this study, crushed scooter batteries were utilized, and a range of analytical techniques were employed to initially characterize the composition of the raw material and subsequently evaluate previous physical separation processes efficiently, effectively, and economically. The analytical methods utilized included scanning electron microscopy with energy-dispersive X-rays spectroscopy (SEM–EDS), X-ray fluorescence spectroscopy (XRF), X-ray diffraction (XRD), atomic absorption spectroscopy (AAS), loss of ignition (LOI), and differential scan calorimetry (DSC). In addition, two separation techniques were conducted: froth flotation and sink-and-float tests. The cathode's oxide type was identified through XRD analysis, and statistical methods were applied to all XRF analyses. Furthermore, the other analytical methods facilitated the determination of flux compositions, enabling the assessment of process performance. Regarding the robustness of the presented method, as is well known, performing a complete characterization of a material, including XRD, AAS, XRF, DSC, and SEM, could comprise a relatively high time if it is to identify the efficiency of a process (we estimate in several days, and even weeks). However, by reducing the analytical methods to LOI, XRF, and stream sampling, it is possible to conduct process efficiency evaluation in a few hours. This methodology would give the opportunity to achieve effective verifications in a short time and reduce possible efficiency problems in a treatment plant of this type of material.

Deterioration of White Tempera Mock-Ups Paints in a SO2-Rich Atmosphere

Historical tempera paints exposed to pollutant gases suffer chemical and mineralogical deterioration which manifests through physical changes. Knowledge about these changes is fundamental to develop strategies for preventive conservation of wall paintings. In this research, binary tempera mock-ups composed of calcite, gypsum or lead white mixed with a proteinaceous binder (i.e., egg yolk or rabbit glue) were exposed to an aging test by using SO2-rich atmosphere exposure to learn about the degradation mechanisms and forms related to the pigment–binder interaction. Reference (unaltered) and aged mock-ups were studied from a physical point of view, characterizing the morphological changes by using stereomicroscopy and profilometry, color variations by using spectrophotometry, gloss changes, and reflectance changes by using a hyperspectral camera. Also, mineralogical and chemical changes were studied by means of X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy with energy-dispersive X-ray spectroscopy. Egg-yolk-based paints showed higher chromatic changes than their counterparts made of rabbit glue binder. Also, sulfate and sulfite salts precipitated on the surface of the aged paints regardless of their binder, influencing the painting reflectance which subsequently increased. Egg-yolk-based mock-ups exhibited roughness increases while the rabbit-glue-based paints showed roughness reduction, with the exception of lead-white-based paints. Therefore, the important influence of the type of binder and the interaction between the binder and the pigment on the durability of tempera paints in atmospheres rich in SO2 was confirmed.

Assessment of bond strength and bioactivity on a prototype resin-based luting agent containing a novel bioactive monomer.

A prototype luting agent based on a resin composite containing a novel bioactive monomer (a calcium salt of 4-methacryloyloxyethyl trimellitate; CMET) was developed, and its shear bond strength to tooth materials (dentin and enamel) and bioactivity was compared with those of commercially available resin-based luting systems. Extracted bovine incisors were embedded in a mold with a potting material. The labial bonding surface of the embedded tooth was wet-ground using #400 silicon carbide abrasive paper until sufficient superficial enamel or dentin was exposed. The bonding and luting agents assessed included our experimental bonding agent and luting agent, Prime&Bond Universal, Calibra Ceram, Multilink Primer A + B, Multilink Automix, Panavia V5 Tooth Primer, Panavia V5, RelyX Universal Resin Cement, SA Luting Multi, and SpeedCem Plus. The experimental luting agent was a novel material containing CMET. Shear-bond-strength testing was performed at 0 and 5000 thermocycles. To evaluate the in vitro bioactivity, specimens were immersed in 22mL of simulated body fluid (SBF) at 37°C for 5days. Scanning electron microscopy combined with energy-dispersive X-ray spectroscopy was used to examine the chemical composition of the specimen surfaces after immersion in the SBF. In conclusion, the shear bond strength to dentin and enamel, and durability of the novel bonding and luting agents were similar to those of commercially available resin-based luting systems. Furthermore, the novel luting agent had bioactive potential.

Analysis of the adhesion structure between the cycloolefin polymer and the copper seed layer formed using medium-vacuum sputtering

We have developed a novel approach for the fabrication of 6G communication antenna substrates by directly sputtering a copper seed layer onto a resin with low dielectric properties and low adhesiveness, without relying on a metal adhesion layer such as titanium. This study presents a detailed analysis of the effects of two surface modification methods—vacuum ultraviolet (VUV) irradiation and oxygen plasma treatment—performed before sputtering the copper seed layer on the interfacial structure between a cycloolefin polymer (COP) film and copper plating layer. Using scanning transmission electron microscopy, energy-dispersive x-ray spectroscopy, and selected area electron diffraction, we confirmed that both surface modification methods promote the formation of polycrystalline Cu2O at the interface between the COP film and the copper plating layer. VUV irradiation enhances the smoothness of the COP surface, resulting in the uniform distribution of hydrophilic functional groups. These functional groups stably interact with the sputtered copper, leading to the oxidation of copper during annealing and the formation of a consistent Cu2O layer. In contrast, oxygen plasma treatment selectively etches regions of the COP surface with high oxygen affinity, creating fine structures and concentrating the hydrophilic functional groups in the recessed areas. After sputtering, copper interacts with these localized functional groups, and during annealing, limited diffusion causes the copper to oxidize and aggregates into a Cu2O particle structure. Thus, this study demonstrates that the structures of polycrystalline Cu2O formed at the interface vary depending on the surface modification methods and elucidates the mechanisms behind these differences through analysis of surface morphology and the distribution of functional groups induced by each method.

Photofixation Pd Functionalization of ZnO Thin Films for Efficient Photocatalytic Removal of Doxycycline Antibiotic in Aqueous Phase

In this work, we demonstrate the co-catalytic modification of ZnO films via the photodeposition of palladium (Pd) to enhance the photocatalytic degradation of doxycycline (DC). Pristine ZnO films were synthesized using a sol–gel method and deposited onto glass substrates via dip-coating. The films were subsequently modified with Pd through chemical photodeposition under UV light, which facilitated the photoreduction of an aqueous 5 × 10−3 M Pd2+ precursor. The influence of varying UV photodeposition doses (2.5, 5, and 10 J/cm2) on the morphology and chemical composition of the Pd-modified films was investigated to control Pd surface coverage and chemical state. Characterization techniques included scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and X-ray photoelectron spectroscopy (XPS). At low UV doses (2.5 J/cm2), approximately 1.6 at.% of Pd was photodeposited, primarily as PdO, while higher UV doses (5–10 J/cm2) increased the metallic Pd0 content. The photocatalytic degradation of DC was evaluated in both distilled and tap water, where Pd/ZnO films demonstrated significantly higher removal efficiency (40–380% higher) than pristine ZnO films, with those containing higher Pd0 levels exhibiting the greatest activity. Across all samples, removal efficiency in tap water was approximately double that in distilled water.

Source identification and characterization of water-insoluble single particulate matter in rainfall sequences

ABSTRACT Analysis of atmospheric pollutants in rainwater provides valuable information on the environmental impacts of both natural and anthropogenic pollution sources. Air pollution studies often show that particulate matter (PM) collection on filters is used for subsequent analysis. However, this approach can result in significant particle accumulation on filters and complicate their characterization by semi-quantitative analytical techniques. In this study, insoluble PM in sequentially collected rainwater samples was analyzed for particle size, morphology, and chemical composition. Scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectrometry (EDS) and a particle size analyzer were used for these analyses. By combining SEM–EDS data with particle size distribution analyses, chemical composition findings, and upper atmosphere back-orbit modeling, specific sources of insoluble particles in rainwater were identified. In addition, rainwater samples were analyzed for pH, electrical conductivity, and major anions and cations. The pH values varied from 6.19 to 7.04, while the electrical conductivity values varied from 5.35 to 83.53 μS/cm. Among the major ions, relatively high concentrations of Ca2+, SO42−, and NO3− were detected, while F−, Mg2+, Na+, and Cl− were observed in lower concentrations. The contributions of sea salt were evidenced by the presence of Cl− and Na+ ions.

A Cobalt-based Nanostructured Electrode Prepared by a Fast Chemical Method

The demand for nanomaterials is rapidly increasing in most applications, such as energy storage devices. Many nanomaterial synthesis methods are energy-consuming methods requiring high temperatures, prolonged reaction time, complicated steps, or expensive equipment. Herein, nanostructures of cobalt hydroxide chloride, Co2(OH)3Cl, have been directly deposited on carbon cloth microfibers by a fast and simple step of chemical bath deposition. Co2(OH)3Cl nanoparticles appear in only 10 minutes of the deposition time, then the nanoflakes are grown in 60 minutes, as imaged by scanning electron microscope. The crystal structure of Co2(OH)3Cl is characterized using X-ray diffraction, while the results of energy-dispersive X-ray spectroscopy confirm the elemental analysis. The electrochemical energy storage mechanism of Co2(OH)3Cl electrode in potassium hydroxide electrolyte depends on the semi-reversible redox reactions as investigated by the cyclic voltammetry and by the galvanostatic charge-discharge measurements. As a result, the prepared electrode in 60 min exhibits a maximum specific capacitance of 313 F/g versus 293 F/g for the prepared electrode in 10 min, both at 1 A/g. The good electrochemical performance is attributed to several features, including the nanoflakes morphology that enables electrolyte ions to penetrate the electrode freely, the well-crystallized structure, and the solid electronic path between the current collector and the active material indicated by the Nyquist plot of electrochemical impedance spectroscopy. Our cost-effective synthesis of cobalt hydroxide chloride nanostructures on woven substrates offers flexible binder-free electrodes in alkaline electrolytes. This research opens up the potential for these materials to be used as a power source in smart textiles and wearable electronics, thereby contributing to the advancement of these fields.

Sustainable Geopolymer Tuff Composites Utilizing Iron Powder Waste: Rheological and Mechanical Performance Evaluation

Geopolymers are a sustainable alternative to Portland cement, with the potential to significantly reduce the carbon footprint of conventional cement production. This study investigates the valorization of industrial waste iron powder (IP) as a fine filler in geopolymers synthesized from volcanic tuff (VTF). Composites were prepared with IP substitutions of 5%, 10%, and 20% by weight, using sodium hydroxide and sodium silicate as alkaline activators. Microstructural and phase analyses were conducted using scanning electron microscope coupled with energy dispersive X-ray spectroscopy (SEM-EDS), X-ray fluorescence (XRF), X-ray diffraction (XRD), and differential scanning calorimetry (DSC), while rheological properties, compressive strength, and flexural strength were assessed. The impact of curing temperatures (25 °C and 80 °C) on mechanical performance was evaluated. Results revealed that air content increased to 3.5% with 20% IP substitution, accompanied by a slight rise in flow time (0.8–2 s). Compressive and flexural strengths at 25 °C decreased by up to 22.48% and 28.39%, respectively. Elevated curing at 80 °C further reduced compressive and flexural strengths by an average of 45.30% and 64.68%, highlighting the adverse effects of higher temperatures. Although these formulations are not suitable for load-bearing applications, the findings suggest potential for non-structural uses, such as pavement base layers, aligning with sustainable construction principles by repurposing industrial waste and reducing reliance on energy-intensive cement production.

Advancing Source Apportionment of Atmospheric Particles: Integrating Morphology, Size, and Chemistry Using Electron Microscopy Technology and Machine Learning.

To further reduce atmospheric particulate matter concentrations, there is a need for a more precise identification of their sources. The SEM-EDS technology (scanning electron microscopy and energy-dispersive X-ray spectroscopy) can provide high-resolution imaging and detailed compositional analysis for particles with relatively stable physical and chemical properties. This study introduces an advanced source apportionment pipeline (RX model) that uniquely combines computer-controlled scanning electron microscopy with computer vision and machine learning to trace particle sources by integrating single-particle morphology, size, and chemical information. In the evaluation using a virtual data set with known source contributions, the RX model demonstrated high accuracy, with average errors of 0.60% for particle number and 1.97% for mass contribution. Compared to the chemical mass balance model, the RX model's accuracy and stability improved by 75.6 and 73.4%, respectively, and proved effective in tracing Fe-containing particles in the atmosphere of a steel city in China. This study indicates that particle morphology can serve as an effective feature for determining its source. The findings highlight the potential of electron microscopy technology coupled with computer vision and machine learning techniques to enhance our understanding of atmospheric pollution sources, offering valuable insights for PM health risk assessment and evidence-based policy-making.

Effect of Pre-Procedural Antiseptic Mouthwash On The Dentin Bond Strength of Dental Adhesives.

To evaluate the effect of pre-procedural antiseptic mouthwashes on dentin bond strength of different adhesive systems. Flat occlusal dentin surfaces from 120 extracted human molars were randomly divided into four groups according to mouthwashes (0.12% chlorhexidine = CHX, 1% hydrogen peroxide = HP, 0.2% povidone-iodine = PI, and no mouthwash/control) and three subgroups of adhesives used (Clearfil SE Bond; CSE, Single Bond Universal = SBU in etch-and-rinse (ER) or self-etch (SE) modes) (n = 8). Composite resin was built up, and all bonded teeth were stored in 37°C distilled water for 24 h. Stick-shaped specimens were prepared and subjected to microtensile bond strength (µTBS) test. Failure mode analysis was determined using a light microscope. A resin-dentin interface was observed using scanning electron microscopy (SEM, n = 2). Elemental analysis in the PI group was further examined by SEM with energy-dispersive X-ray spectroscopy. The µTBS data were statistically analyzed by two-way analysis of variance (ANOVA) and Duncan's multiple comparison (P < 0.05). Rinsing with PI followed by SBU-SE demonstrated significantly higher µTBS than the control group (P < 0.05). Rinsing with HP showed significantly lower bond strength for CSE (P < 0.05). However, the effect of adhesive systems was not observed for all mouthwashes used (P > 0.05). SEM/EDX revealed the iodine deposition in the underlying dentin, where the highest amount of iodine was found for SBU-SE. CHX and PI can be recommended as pre-procedural antiseptic mouthwashes since they show no negative impact on µTBS for all tested adhesives. The dentin bond strength of CSE is hampered in the HP mouthwash group, and this should be a concern for the use of self-etching adhesive afterward.

Aluminum–Silica Core–Shell Nanoparticles via Nonthermal Plasma Synthesis

Aluminum nanoparticles (Al NPs) are interesting for energetic and plasmonic applications due to their enhanced size-dependent properties. Passivating the surface of these particles is necessary to avoid forming a native oxide layer, which can degrade energetic and optical characteristics. This work utilized a radiofrequency (RF)-driven capacitively coupled argon/hydrogen plasma to form surface-modified Al NPs from aluminum trichloride (AlCl3) vapor and 5% silane in argon (dilute SiH4). Varying the power and dilute SiH4 flow rate in the afterglow of the plasma led to the formation of varying nanoparticle morphologies: Al–SiO2 core–shell, Si–Al2O3 core–shell, and Al–Si Janus particles. Scanning transmission electron microscopy with a high-angle annular dark-field detector (STEM-HAADF) and energy-dispersive X-ray spectroscopy (EDS) were employed for characterization. The surfaces of the nanoparticles and sample composition were characterized and found to be sensitive to changes in RF power input and dilute SiH4 flow rate. This work demonstrates a tunable range of Al–SiO2 core–shell nanoparticles where the Al-to-Si ratio could be varied by changing the plasma parameters. Thermal analysis measurements performed on plasma-synthesized Al, crystalline Si, and Al–SiO2 samples are compared to those from a commercially available 80 nm Al nanopowder. Core–shell particles exhibit an increase in oxidation temperature from 535 °C for Al to 585 °C for Al–SiO2. This all-gas-phase synthesis approach offers a simple preparation method to produce high-purity heterostructured Al NPs.

Effects of Graphene Nanoplatelets and Nanosized Al4C3 Formation on the Wear Properties of Hot Extruded Al-Based Nanocomposites

This study investigates the influence of graphene nanoplatelets (GNPs) and the formation of nanosized Al4C3 on the tribological performance of hot extruded aluminum-based nanocomposites. Al/GNP nanocomposites with varying GNP contents (0, 0.1, 0.5, and 1.1 wt.%) were fabricated through powder metallurgy, including ball milling, compaction, and hot extrusion at 500 °C, which was designed to facilitate the formation of nanosized carbides during the extrusion process. The effect of GNPs and nanosized carbides on the tribological properties of the composites was evaluated using dry friction pin-on-disk tests to assess wear resistance and the coefficient of friction (COF). Microstructural analyses using scanning electron microscopy and energy-dispersive X-ray spectroscopy confirmed the uniform distribution of GNPs and the formation of nanosized Al4C3 in the samples. Incorporating 0.1 wt.% GNPs resulted in the lowest wear mass loss (1.40 mg) while maintaining a stable COF (0.52), attributed to enhanced lubrication and load transfer. Although a higher GNP content (1.1 wt.%) resulted in increased wear due to agglomeration, the nanocomposite still demonstrated superior wear resistance compared to the unreinforced aluminum matrix. These findings underscore the potential of combining nanotechnology with precise processing techniques to enhance the wear and friction properties of aluminum-based composites.

Study on the processing of thermoplastic polyvinyl alcohol with ammonium salts by melt spinning and its potential as a precursor fiber

Polyvinyl alcohol (PVOH) has all the essential requirements to be used as an alternative precursor for carbon fiber (CF) production. Within this work, three different commercially available, thermoplastically processable PVOH grades together with three different ammonium salts as stabilizing agents were investigated using the melt spinning process with regard to their processing into CF precursor filaments. Precursor filaments could be spun at up to, 500 m min−1. The distribution of the salts over the filament cross-section was evaluated using energy-dispersive X-ray spectroscopy analysis, whereas the quantitative determination was carried out using Kjeldahl nitrogen analysis. The thermal properties were characterized using thermogravimetric analysis. An increase in the ammonium iodine (NH4I) concentration to 10.0 wt.% leads to 22.4 wt.% mass residue at 1000°C. The precursor filaments were carbonized in a laboratory tube furnace up to 1000°C and initial tests were carried out on the resulting CFs.

Utilization of a Selective Paper-Based Flexible Electrochemical Sensor for Epinephrine Determination in Artificial Sweat Using Nickel Oxide and Sulfur-Doped Graphene Conductive Ink

Abstract Epinephrine (adrenaline, EP) is a crucial hormone that regulates the body's response to emergencies. During periods of stress or danger, it is responsible for rapidly mobilizing the body by elevating heart rate, blood pressure, and respiratory rate. Consequently, the accurate and rapid measurement of EP is of significant importance. In this study, sulfur-doped graphene (S-Gr) synthesized using Yucel’s method, and nickel oxide (NiO) were utilized as conductive materials to develop conductive inks. Furthermore, a paper-based flexible electrochemical sensor was constructed for EP determination. The optimum conductive ink for sensor fabrication was identified through optimization process. The sensor was characterized using various techniques, including cyclic voltammetry, electrochemical impedance spectroscopy, field-emission scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray diffraction analysis, and Fourier transform infrared spectroscopy. The sensor demonstrated a detection limit of 33.16 nM, and its cost-effective and user-friendly design renders it an advantageous option for practical applications. The results obtained from the analytical studies indicated that the sensor exhibits high selectivity towards EP and can successfully detect EP in artificial sweat samples. In conclusion, the proposed sensor serves as a model for future flexible and wearable devices.

Microanalysis of minerals in Rhizophora mangle L. leaves from Marambaia mangroves reveal low presence of potentially toxic elements

The mangroves of Marambaia, area bathed by the Bay of Sepetiba, is located in an area protected by the Brazilian Army and has a remarkable level of environmental protection among ecosystems around the bay. Leaf content of minerals and potentially toxic elements in a typical species of mangrove of Rhizophora mangle L. were analyzed from samples collected in Marambaia. Microanalyses of minerals were done by Energy Dispersive X-Ray Spectroscopy coupled to Scanning Electron Microscope (EDX-SEM) that showed the elemental composition and its relative quantity in R. mangle leaves. The major mineral deteced were Na, Ca and Cl, and low concentration of Zn.

Microwave-Assisted In-Situ Synthesis of Polyethersulfone–ZnO Nanocomposite Membranes for Dye Removal: Enhanced Antifouling, Self-Cleaning, and Antibacterial Properties

Microwave-assisted synthesis presents a promising method for enhancing the formation of nanocomposites due to its rapid heating and uniform energy distribution. In this study, we successfully fabricated polyethersulfone–zinc-oxide (PES-ZnO) nanocomposite membranes by exposing PES/ZnCl2/DMF dope solutions to microwave radiation. Before synthesizing the membranes, zinc-oxide nanoparticles (ZnO-NPs) were optimized in an organic phase using microwave radiation to ensure effective nanoparticle formation. The synthesis of ZnO-NPs in DMF solvent was validated through UV–Vis spectroscopy, X-ray diffraction (XRD), and Dynamic Light Scattering (DLS). We examined the surface morphology and roughness of the PES-ZnO membranes through Atomic Force Microscopy (AFM) and Scanning Electron Microscopy (SEM). Moreover, we assessed the membranes’ hydrophilicity, permeability, and physicochemical properties through contact-angle measurements, pure water flux tests, water uptake assessments, and porosity tests. Energy-dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD) verified the successful integration of ZnO nanoparticles (ZnO-NPs) into the membrane matrix. The results indicate that including ZnO-NPs significantly improves the membrane’s permeability and hydrophilicity. The nanocomposite membranes exhibited high dye rejection efficiency, with ZnO-NPs facilitating photocatalytic self-cleaning properties. Antibacterial tests also demonstrated a substantial inhibition of common bacteria, suggesting enhanced resistance to biofouling. This research highlights the potential of microwave-assisted PES-ZnO nanocomposite membranes as effective and sustainable solutions for wastewater treatment, offering scalable applications along with added benefits of antifouling, self-cleaning, and antibacterial properties.

MXene-rGO nanocomposite based electrochemical immunosensor for detection of endosulfan - An organochlorine pesticide.

Endosulfan (Ed), a widely used organochlorine pesticide, is classified as a persistent organic pollutant (POP). Its long half-life, resistance to degradation, and bioaccumulation in the food chain contaminates soil, water, and air. Such widespread environmental damage triggers monitoring its levels for ensuring compliance with safety regulations and protecting public health. In the current work, Ed was chemically altered and coupled with a carrier protein to elicit an immunological response. The purified in-house generated antibodies against Ed (Ed-Ab) were characterized by sodium dodecyl-sulfate polyacrylamide gel electrophoresis (SDS-PAGE). MXene, a class of 2D inorganic compounds, is known to depict significant optoelectrical potential. Herein, we have synthesized a novel nanocomposite of MXene and reduced graphene oxide (rGO). For designing the MXene-rGO biosensor, Ed-Ab were combined with the nanocomposite post characterization by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDAX), X-ray photoelectron spectroscopy (XPS) and Fourier Transform infrared spectroscopy (FTIR). Using the differential pulse voltammetry (DPV), electrochemical parameters such as pH, temperature, scan rate and response time of the electrode were evaluated. The fabricated electro-immunosensor was employed for the detection of endosulfan wherein the limit of detection (LOD) for Ed was determined to be 0.497ppt with a linear range of 0.1ppt-1ppm. The composed electrode's working efficacy and sensitivity against similar cross-reactive pesticides was also determined. The MXene-rGO based nanocomposite depicted potential for determination of Ed traces in environmental samples.

Microstructural study with enhanced dielectric and magnetic properties of M−type Nd doped Ba1-xNdxFe12O19 (x = 0–0.20) hexaferrites synthesized via sol–gel auto-combustion route

In the present study, we have examined the influence of Nd doping on the structural, morphological, magnetic, and dielectric properties of barium hexaferrite (Ba1-xNdxFe12O19; 0 ≤ x ≤ 0.20) samples synthesized via the sol–gel auto-combustion route. The XRD patterns confirm the formation of the hexagonal phase, in addition to minor traces of Fe2O3 impurity in the samples. Doping with Nd3+ ions produced strain in the crystal, and the samples retain their hexagonal phase with space group P63/mmc, as ensured by the Rietveld refinement method. FTIR spectroscopy were performed for microstructural analysis, which shows the corresponding stretching and bending bands of iron and oxygen in the samples. The Raman spectra confirmed the Raman fundamental modes at various wavenumbers, which also confirm the hexagonal structure of the samples. The electronic states of all metal ions state were confirmed through x-ray photoelectron (XPS) spectroscopy analysis, which show that iron is present in two oxidation states (Fe2+ and Fe3+) in all the prepared samples. XPS spectra also revealed that the Nd-doped sample is more defective as compared to pure sample. Scanning electron microscopy (SEM) micrographs shows that the non-uniform particle size in the nanometer range. Elemental composition is confirmed using energy dispersive x-ray spectroscopy (EDS) measurement. Additionally, magnetic measurements using a vibrating sample magnetometer (VSM) revealed that the hysteresis loops for 5 % Nd-doped sample shows the maximum value 44.3 emu/g of magnetization, and its values decrease for further increase in Nd doping concentration. The dielectric measurements were performed at room temperature in the frequency range of 1 Hz to 10 MHz, when Nd3+ is doped at the Ba site, it enhances the dielectric constant, dielectric loss, tangent loss, and ac conductivity of the synthesized samples.

The boron content analysis by energy dispersive X-ray spectroscopy and the study of boron refractivity in borosilicate optical fibers

The boron content analysis by energy dispersive X-ray spectroscopy and the study of boron refractivity in borosilicate optical fibers