Energy Dispersive X-ray Research Articles

Synthesis and Characterization of magnetic chitosan/oxidized schizophyllan nanocomposite film for Biomedical Application

This study aimed to synthesize antimicrobial nanocomposite films based on periodate oxidized schizophyllan (POSPG), chitosan (CS), and green synthesized magnetic silver/iron oxide nanoparticles (Ag/Fe3O4 NPs). The average size and polydispersity index (PDI) of the Ag/Fe3O4 NPs produced by starch were 85 nm and 0.17, respectively. The schizophyllan (SPG) was first produced from Schizophyllum commune. The solution casting method was employed to prepare nanocomposite films composed of POSPG, CS and different concentrations of Ag/Fe3O4 NPs (0.66, 1.33 and 2 μg/mL). According to the MTT results, 1.33 μg/ml was the maximum non-toxic concentration for loading into CS/POSPG, so this film, CS/POSPG@NP1.33, was selected for further study. The appearance of a peak at 8.3 ppm in nuclear magnetic resonance (NMR) spectrum of CS/POSPG film evidenced the imine bond formation. Energy dispersive X-ray (EDX) mapping illustrated the proper distribution of Ag/Fe3O4NPs into the matrix. The mechanical strength and water vapor permeability of the CS/POSPG@NP1.33 nanocomposite increased to 82.77±1.25 MPa and 0.640±0.02 mm.g/m2.h.kPa, respectively as compared to those reported for CS/POSPG film (63.49±0.7 Mpa and 0.576±0.015 mm.g/m2.h.kPa), while the swelling capacity decreased to 2.3±0.075. The normal human fibroblast cell survival reached 83.21±1.78% after exposure to the CS/POSPG@NP1.33, indicating its biocompatibility. The inhibitory effect of the nanocomposite against S. aureus, E. coli, MRSA, P. aeruginosa, and candida was 94.6±3.73%, 97.2±4.65%, 88.4±3.87%, 97.9±2.04%, and 84.6±1.95%, respectively. The eradication rate of the CS/POSPG@NP1.33 against the S. aureus biofilm was up to 47.55±1.72 %, which increased to 79.74±2.09% after exposure to a magnetic field.

Catalytic-assisted remediation and phytotoxicity evaluations of organic pollutants in the presence of metal-doped Bi2O3-based NPs catalyst.

The chemical co-precipitation method was used to synthesize a variety of pure Bi2O3 and substituted Bi2-2xCoxCdxO3 NPs (x=0.0-0.8) and doping influences were evaluated based on the optical, photocatalytic, morphological, and structural characteristics. Powder X-ray diffraction (PXRD), scanning electron microscope (SEM), Energy dispersive X-ray (EDX), Fourier-transform infrared spectroscopy (FTIR), and UV-visible techniques were used to explore the characteristics of the synthesized Bi2O3-based NPs. XRD measurements confirmed the monoclinic structure and a P21/c space group, whereas the particle size was between 22 and 41nm. The SEM analysis gives the morphology of the synthesized NPs that were diverse and agglomerated platelets, whereas the EDX measurements provide the presence of Co and Cd in Bi2-2xCoxCdxO3 NPs. Additionally, FTIR investigations confirmed the existence of functional groups in Bi2-2xCoxCdxO3 NPs. The ultraviolet-visible absorbance region displaying a considerable red shift allowed for tuning of the band gap from 2.64 to 2.37eV. By analyzing the degradation of Reactive Black 5 (RB-5) dye in the presence of sunlight, pure Bi2O3 NPs showed 65.04% whereas the substituted Bi2-2xCoxCdxO3 NPs demonstrated enhanced photodegradation (86.40%) in 105min. For the degradation of RB-5 dye, the effects of catalyst dosage, dye concentration, and pH variations were studied as well. The phytotoxicity experiment was also performed by comparing the germination of Triticum aestivum seeds in treated and untreated RB-5 dye. In the untreated dye solution, seed germination was 50% inhibited, and in the treated dye solution, germination was observed to be 80%. Additionally, recycling investigations were used to confirm the stability of these fabricated nanoparticles, and the results showed that nanomaterials exhibited significant stability and reusability. Co and Cd-doped Bi2O3 NPs are promising solar-active photocatalysts for dye removal from wastewater applications because of their improved photocatalytic activity and narrow bandgap.

Insights into the expeditious photocatalytic performance of greenly fabricated CeVO4 nanoparticles using Polyalthia longifolia leaf extract

The application of nanomaterials to address environmental challenges has evolved substantially to eliminate pollutants from wastewater as part of environmental cleanup, a growing important research arena. Using green photocatalysts is a noteworthy and economical method that significantly advances environmentally sustainable remediation. This work disclosed the bio-inspired production of cerium vanadate nanoparticles (CeVO4 NPs) were prepared through a green chemistry protocol employing Polyalthia longifolia leaf extract. Key traits of CeVO4 nanoparticles were determined by applying a variety of characterization tools, including X-ray diffraction (XRD), Raman, Fourier transform infrared (FTIR), X-ray photoelectron spectroscopy (XPS), ultraviolet–visible diffuse reflectance spectroscopy (UVDRS), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX), and high-resolution transmission electron microscopy (HRTEM). CeVO4 nanoparticles displayed a pseudo-spherical topology with a particle size of 17.77 nm, and the band gap was determined as 2.76 eV. The photocatalytic ability of the as-produced CeVO4 NPs was scrutinized for the decomposition of Congo red (CR) dye. Under optimal conditions, the fabricated CeVO4 nanoparticles demonstrated excellent Congo red dye degradation performance. The effect of hydrogen peroxide (H2O2) dosage, nanoparticle dosage, dye concentration, contact time, scavenging test, and reusability of prepared photocatalyst had an excellent impact on dye decomposition ability. The findings revealed that in just 8 min, 97.79 % of the CR dye had been degraded completely. The pseudo-first-order (PFO) kinetics model aligns with the CR dye decomposition kinetics. In conclusion, this study describes the fabrication of a CeVO4 photocatalyst that exhibits impressive performance, particularly in natural sunlight, suggesting that it could be used in wastewater treatment.

Silicate-substituted bovine-derived hydroxyapatite as a bone substitute in regenerative dentistry.

Hydroxyapatite, renowned for its biocompatibility and osteoconductive properties, plays a fundamental role in bone regeneration owing to its resemblance to natural bone mineral, thus offering considerable potential for advancing tissue engineering strategies. In this article, the innovative integration of silicon ions into biogenic (bovine-derived) hydroxyapatite (SiBHA) via a tailored sol-gel process is reported. The resultant SiBHA scaffolds exhibited an interconnected microporous structure with a total porosity of 70% and pore dimensions ranging from 120 to 650 µm. Fourier-transform infrared spectroscopy and X-ray diffraction studies validated the effective incorporation of silicon ions into the BHA lattice, with energy-dispersive X-ray and inductively-coupled plasma mass spectrometry further confirming a Ca/P molar ratio for SiBHA between 1.63 and 1.74. Moreover, SiBHA scaffolds demonstrated commendable chemical and thermal stability. Of note, SiBHA scaffolds were found to display significantly enhanced mechanical properties, including compressive strength and Young's modulus, compared to the control BHA scaffolds. In vitro assessments highlighted the capacity of SiBHA scaffolds to foster cell viability, proliferation, and osteogenic differentiation of Saos-2 cells. Immunohistochemical analysis revealed a significant increase in osteonectin expression, a key bone matrix protein, after 14 days of incubation under osteogenic conditions. These findings highlight the biocompatibility and therapeutic potential of SiBHA scaffolds, suggesting their suitability as biomaterials for dental bone regeneration applications.

Boron contributes to enhance antimony tolerance in rice (Oryza sativa L.) by activating antioxidant system, modifying the cell wall component and promoting cell wall deposition of Sb.

Boron (B) is essential for plant growth and helps mitigate metal toxicity in various crop plants. However, the potential role and underlying mechanisms of B in alleviating antimony (Sb) toxicity in rice remain unexplored. In this study, we investigated the effects of H₃BO₃ supplementation (30, 50, and 75μM) on morphological growth, physiological and biochemical traits, Sb content, and the subcellular distribution of Sb in rice plants under 100μM Sb stress during the seedling stage in a hydroponic system. The results revealed that Sb toxicity severely impaired rice growth, reducing shoot biomass by 38.3%, shoot and root length by 38.9% and 23.2%, and leaf relative water content by 15.5%. Supplementation with 30μMB mitigated these adverse effects by enhancing photosynthesis and chlorophyll synthesis, restoring root activity, and improving oxidative balance through increased antioxidant enzyme activities in rice tissues. Furthermore, B supplementation significantly reduced Sb concentration in roots by 56.28%, while promoting Sb distribution in the cell wall (CW) fraction. Scanning electron microscopy equipped with energy-dispersive X-ray (SEM-EDS) microanalysis confirmed that B enhanced Sb adsorption on root CWs. Fourier transform infrared spectroscopy (FTIR) analysis indicated increased carboxyl groups in the CWs following B application under Sb treatment. Moreover, B supplementation increased the levels of pectin and hemicellulose and elevated pectin methylesterase (PME) activity by 22.0%, 69.0%, and 29.0% in roots, respectively, thus promoting Sb chelation onto the CWs. Taken together, our results provide a scientific basis and theoretical guidance for applying B to alleviate Sb toxicity in crops.

Ethyl 2-butene phosphite as a film-forming additive for high voltage lithium-ion batteries

Increasing the charge cutoff voltage can significantly improve the capacity of lithium-ion batteries. However, the structural degradation of Ni-rich cathodes and high reactivity of electrolytes at the high-potential cathodes greatly affect the cycling stability. In this paper, a new type of cathode film-forming additive, ethyl 2-butene phosphite (EBP), is synthesized based on the molecular design of phosphite by increasing the functional group of carbon-carbon double bond and ring structure. Theoretical calculation shows that EBP has a higher HOMO level and can form a cathode electrolyte interphase (CEI) on the cathode electrode surface before the electrolyte in theory. The electrochemical performance of NCM622/Li half-cells is significantly enhanced by incorporating EBP into the electrolyte, achieving 72.52% capacity retention over 100 cycles at 0.5C. Scanning Electron Microscope (SEM), X-Ray Diffraction (XRD), X-ray Photoelectron Spectroscopy (XPS) and Energy Dispersive Spectroscopy (EDS) are used to characterize the morphology of the anode and cathode, revealing that EBP forms a dense and complete CEI film on the surface of the LiNi0.6Co0.2Mn0.2O2 electrode. This film effectively blocks direct contact between the electrolyte and the cathode active material, prevents the dissolution of transition metals, improves interfacial stability, and consequently enhances the high-voltage cycling performance of the battery.

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

Enhancing corrosion resistance of mild steel in acid pickling bath: An investigation of new quinazoline derivatives by synthesis, electrochemical analysis EFM, surface analysis, AFM, DFT and molecular dynamics simulation

The current study examines the ability of two novel heterocyclic Quinazoline derivatives, 2-(4-bromophenyl)-3-phenyl-2,3-dihydroquinazolin-4(1H)-one (DHQ-4-Br) and 2-(4-hydroxy-3-methoxyphenyl)-3-phenyl-2,3-dihydroquinazolin-4(1H)-one (DHQ-3-OMe-4-OH) to adsorb and protect mild steel against corrosion in a molar solution of hydrochloric acid (HCL). The two materials were identified using nuclear magnetic resonance (NMR) spectroscopy and the experimental investigation employed potentiodynamic polarization (PDP), electrochemical frequency modulation (EFM), and impedance spectroscopy (EIS). The findings demonstrated that DHQ-4-Br and DHQ-3-OMe-4-OH exhibit increasing inhibitory effectiveness as the concentration of the inhibitors increases. Polarization test results suggest that the two inhibitors exhibited mixed-type behavior. The inhibitory efficiency of DHQ-4-Br and DHQ-3-OMe-4-OH was 94.65 % and 83.94 % respectively. In addition, the Langmuir adsorption model was employed better to understand the adsorption process of the two compounds. The existence of a barrier layer surrounding the SM was demonstrated using scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDS), and atomic force microscopy (AFM). The results of the density functional theory (DFT) show that the inhibitors that can take electrons have the strongest interactions with the iron surface.

Specific Nickel recovery using screen-printed carbon electrode electrografted with ionic liquid

This study presents an innovative electrochemical method for selectively extracting nickel ions from aquatic solutions, employing electrodes enhanced with electrografted ionic liquids. Specifically, a styrenyl-imidazolium ionic liquid (SI-IL) was synthesized, featuring a double bond for immobilization and an imidazole group targeting nickel ions. The electrografting process ensured uniform SI-IL distribution on the electrode's surface, as confirmed by scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS). SI-IL-treated electrodes exhibited notable selectivity towards nickel ions, efficiently recovering them as nanoparticles while reducing the required reduction potential. In pH conditions similar to industrial wastewater, SI-IL modified electrodes demonstrated substantial enhancement in nickel recovery rates compared to unmodified electrodes.

Biosynthesis and Application of Biological Thin Films for Heavy Metal Ion Biosorption from Aqueous Solution

This study investigates the biosynthesis and application of Mycelium Bio-Films (MBFs) derived from pure Common oyster mushroom (COM) for heavy metal ion biosorption from aqueous solutions. The research focuses on the growth mechanism of MBFs and their potential for Cu (II) ions removal. MBFs were synthesized through a hyphae cultivation process and characterized using Scanning Electron Microscopy (SEM), Fourier-Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), and Energy-Dispersive X-ray Spectroscopy (EDS) mapping. Batch biosorption experiments were conducted to determine optimal operational parameters and adsorption mechanisms. Key findings reveal optimal biosorption conditions at pH 5, with a 40-minute contact time, and 100mg/L initial Cu (II) concentration using 0.2g of biosorbent in 10mL aqueous solution at room temperature with 150rpm agitation. Under these conditions, a maximum adsorption efficiency of 82.8% was achieved. The adsorption process best fits Pseudo-second-order kinetics and Langmuir isotherm, indicating chemisorption, complexation, and ion exchange as primary mechanisms. Functional groups involved in biosorption include carboxyl, hydroxyl, and amide groups. Importantly, MBFs demonstrate high reusability potential through diluted acid elution. This research contributes to environmental remediation by presenting a novel, sustainable biosorbent for heavy metal removal. The MBFs show promise for industrial wastewater treatment applications, offering an eco-friendly alternative to conventional adsorbents and contributing to filling the lack of biobank collections. Future studies could explore the efficacy of MBFs with other heavy metals and investigate potential scale-up for large-scale implementation.

Phyto-mediated fabrication of silver nanoparticles from Scrophularia striata extract (AgNPs-SSE): a potential inducer of apoptosis in breast cancer cells.

Breast carcinoma stands out as the most widespread invasive cancer and the top contributor to cancer-related mortality in women. Nanoparticles have emerged as promising tools in cancer detection, diagnosis, and prevention. In this study, the antitumor and apoptotic capability of silver nanoparticles synthesized through Scrophularia striata extract (AgNPs-SSE) was investigated toward breast cancer cells. The produced AgNPs-SSE were identified using scanning electron micrograph (SEM), energy-dispersive X-ray (EDAX) spectroscopy, Fourier-transform infrared (FTIR) spectroscopy, and X-ray diffraction (XRD). The cell-killing effects of AgNPs-SSE on MDA-MB231 mammary carcinoma cells were evaluated in vitro using the MTT assay over 24h. Apoptosis induction was conducted by cell cycle analysis, annexin V-FITC/PI staining, reactive oxygen species (ROS) generation, and Hoechst staining. Additionally, the gene expression of βcatenin, GSK3β, and CyclinD1 was analyzed using quantitative real-time PCR (qRT-PCR). Microscopic analysis confirmed the successful fabrication of globular AgNPs-SSE, with a mean particle dimension of 19 ± 10nm. The MTT assay revealed that IC50 value of AgNPs-SSE was 48.5µg/mL for mammary carcinoma cells and 114µg/mL for normal cells. Annexin V-FITC/PI staining specified that 85.88% of cancer cells treated with AgNPs-SSE underwent either early or late apoptosis. Treatment with AgNPs-SSE also caused a considerable rise in the subG1 cell cycle population and ROS production. Furthermore, the upregulation of βcatenin and downregulation of CyclinD1 gene expression confirmed the apoptotic mechanism. In conclusion, the findings suggest that phyto-synthesized AgNPs-SSE can restrain the expansion of breast carcinoma cells and provoke apoptosis through oxidative stress. These results highlight the potential of AgNPs-SSE as an antitumor agent against breast cancer.

Influence of elevated temperature exposure on the residual compressive strength and radiation shielding efficiency of ordinary concrete incorporating granodiorite and ceramic powders

This research investigates the potential of utilizing types of construction waste as partial cement replacements within concrete formulations. Notably, granodiorite and ceramic powders were introduced at varying substitution ratios. The impact of these waste materials on the compressive strength and radiation shielding effectiveness of traditional concrete was evaluated under both ambient and elevated temperature conditions. Additionally, several microstructural tests like X-ray diffraction (XRD), Thermogravimetric analysis (TGA), and Energy dispersive X-ray (EDX) were conducted to assess the influence of using the optimal replacement ratios of the investigated waste powders on the studied properties of concrete. Results revealed a substantial improvement in the investigated properties of the concrete. Remarkably, a 7% substitution with waste granodiorite powder (WGDP) yielded the optimal mix for compressive strength, exhibiting increases of 24.7%, 26.1%, 22%, and 28% at room temperature, 400 °C, 600 °C, and 800 °C, respectively. Likewise, a 7% replacement with waste ceramic powder (WCP) exhibited quantifiable improvements in compressive strength, with approximately 23.1%, 23.5%, 25.6%, and 32.6% at room temperature, 400 °C, 600 °C, and 800 °C, respectively. For microstructure analysis, XRD analysis confirmed enhanced pozzolanic activity with reduced portlandite and increased calcium silicate hydrate (CSH) formation for the optimal WGDP and WCP mixes compared to the control mix. TGA analysis revealed higher CSH decomposition in modified mixes, indicating greater pozzolanic reaction. Furthermore, density and EDX analyses showed denser microstructures in waste powders-incorporated mixes due to finer particle packing and secondary hydration effect. The radiation shielding investigation show that the optimum WCP mix (C7) enhances the attenuation capability of concrete. The optimum WGP mix (GD7) also contributes positively to attenuation, though to a lesser extent than C7. Ordinary concrete (CO) exhibits the lowest LAC, indicating its baseline performance in linear attenuation. Thus, the studied CM-concrete samples provide the best protection against fast neutrons which pave the way for the utilization of industrial waste, especially ceramic and granodiorite waste, in enhancing the properties of concrete towards radiation shielding against gamma rays and neutrons.

Enhanced photocatalytic degradation of Rhodamine B using polyaniline-coated XTiO3(X = Co, Ni) nanocomposites

In this study, novel polyaniline-coated perovskite nanocomposites (PANI@CoTiO3 and PANI@NiTiO3) were synthesized using an in situ oxidative polymerization method and evaluated for the photocatalytic degradation of Rhodamine B (RhB) a persistent organic pollutant. The nanocomposites displayed significantly enhanced photocatalytic efficiency compared to pure perovskites. The 1%wt PANI@NiTiO3 achieved an impressive 94% degradation of RhB under visible light after 180 min, while 1wt.% PANI@CoTiO3 reached 87% degradation under UV light in the same duration. X-ray diffraction (XRD) confirmed that the crystalline structures of CoTiO3 and NiTiO3 remained intact post-polymerization. At the same time, Fourier transform infrared spectroscopy (FTIR) verified the successful deposition of PANI through characteristic functional group vibrations. Diffuse reflectance spectroscopy (DRS) revealed reduced band gaps of 2.63 eV for 1wt.% PANI@NiTiO3 and 2.46 eV for 1wt.% PANI@CoTiO3, enhancing light absorption across UV and visible ranges. Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS) analysis demonstrated the uniform distribution of PANI, ensuring consistent surface activity and efficient charge transfer. The photocatalytic test confirmed a pseudo-first-order degradation mechanism. The study elucidates the degradation mechanism through intermediate identification via HPLC-MS analysis, highlighting N-de-ethylation, aromatic ring cleavage and eventual mineralization into CO2 and H2O as critical pathways. Furthermore, the 1wt.%PANI@NiTiO3 nanocomposite demonstrated excellent stability and recyclability, maintaining its degradation efficiency over four consecutive cycles with minimal change. These findings highlight the potential of PANI@XTiO3 nanocomposites for sustainable and efficient wastewater treatment, addressing diverse environmental challenges by tailoring photocatalysts to specific light sources.

Towards Solid-State Batteries Using a Calcium Hydridoborate Electrolyte.

Solid-state batteries created from abundant elements, such as calcium, may pave the way for cheaper and safer electrical energy storage. Here we report a new type of solid calcium hydridoborate electrolyte, Ca(BH4)2·2NH2CH3, with a high ionic conductivity of σ(Ca2+) ~ 10-5 S cm-1 at T = 70 °C, which is assigned to a relatively open and flexible structure with apolar moieties and weak dihydrogen bonds that facilitate migration of Ca2+ ions in the solid state. The compound display a low electronic conductivity, providing an ionic transport number close to unity (tion = 0.9916). Calcium plating is observed for a Ca|Ca(BH4)2·2NH2CH3|Pt electrochemical cell and the electrodes are investigated using scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDS) that reveal a rugged Ca anode surface owing to the stripping process and the presence of Ca-containing domains on the Pt working electrode from the plating process. Improved electrochemical reversiblity was achieved in a three-electrode cell configuration using a CaxSn counter and reference electrode and a Sn working electrode, CaxSn|Ca(BH4)2·2NH2CH3|Sn, providing reversible Ca plating and stripping.

Sustainability metrics targeted optimization and electric discharge process modelling by neural networks

Aluminium and its alloys, especially Al6061, have gathered significant interest among researchers due to its less density, great durability, and high strength. Due to their lightweight properties, the precise machining of these alloys can become expensive through conventional machining operations for intricate products. Therefore, non-traditional machining such as electric discharge machining (EDM) can potentially be opted for the cutting of Al6061. EDM is often criticized due to its low machining rates, therefore, in the current work, cryogenic treatment (CT) has been performed on the brass electrode to evaluate the improvement in the machining rates. In addition, kerosene oil (KO) has been engaged in traditional EDM which is replaced with the deionized water (DI) based dielectric as a sustainable alternative. The machining variables such as spark voltage (SV), pulse-on-time (PON), peak current (IP), and Al2O3 powder concentration (CP) have been chosen to determine the material removal rate (MRR), surface roughness (SR), and specific energy consumption (SEC) while comparing non-treated (NT), and cryogenically treated (CT) brass electrodes during EDM. The results were analyzed through optical micrographs, scanning electron microscopy (SEM) analysis, energy dispersive x-ray (EDX) examination, and 3D surface plots. An artificial neural network (ANN) has been constructed for the better prediction of output responses. Moreover, multi-response optimization through the non-dominated sorting genetic algorithm (NSGA-II) has also been performed. The magnitudes of MRRCT, SRCT, and SECCT obtained by multi-response optimization are 64.82%, 27.45%, and 46.60% are better than the values obtained by un-optimized settings of CT brass electrodes. However, the optimal magnitudes of processing parameters are IP = 24.85 A, SV = 2.18 V, PON = 119.11 µs, and CP = 1.05 g/100 ml.

A Semi-Automated Machine-Learning Tool for Assessing Building Phases: Discriminant Analysis of Mortars from the 2022 Excavation at the Sarno Bath Complex in Pompeii

This study presents the results of the analyses of 15 structural mortars from the building at civ. 21, level +0 of the Sarno Bath complex in Pompeii. These samples were collected during recent stratigraphic excavations (year 2022) for detailed in-laboratory compositional characterization, aiming to trace the construction phases of the originating walls. The 2022 samples were firstly analyzed via quantitative phase analysis–X-ray powder diffraction. The resulting quantitative mineralogical profiles were then processed alongside those analyzed in previous studies from level +0 structures of the Sarno Baths using multivariate statistical methods, including principal component analysis (PCA) and discriminant analysis, applied to quantitative phase analysis (QPA)–X-ray powder diffraction data (XRPD), to identify and map the construction phases. This approach enabled the correlation of the 2022 samples with previously established construction phases. Polarized-light optical microscopy and scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDS) were then primarily used for validation purposes. These methods highlighted the compositional differences between samples and revealed significant features related to the use of specific raw materials. These results confirm the reliability of the semi-automated sample processing proposed in this research, adopting discriminant analysis as a machine-learning-based tool for defining construction phases in Pompeian contexts.

Evaluation by Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy of the Effects of Root Canal Instrumentation on the Radicular Dentine.

One area of technological advancement has been the shift from stainless steel hand tools to nickel-titanium (Ni-Ti) rotary tools. This paper aims to perform an invitro comparative study to evaluate the efficacy of five endodontic manual and rotary instruments such as Kerr files, Orodeka Plex V, ProTaper Flydent NiTi super files, and ProTaper Flydent NiTi super files in combination with an ultrasonic endodontic E3D Diamantata EMS scaler used for root canal shaping. The following aspects were highlighted: effective removal of smear layer (SL) from the dentinal tubules in the coronal 1/3, middle 1/3, and apical 1/3 of the root canal, appearance of cracks in the dentinal walls by SEM analysis, and highlighting of dentin mineral content and remnant debris by EDX analysis. In the study, 48 monoradicular, uninjured teeth were taken and divided into four groups, each with 12 teeth to be canal modeled, then longitudinally sectioned; the active surface was metallized for SEM-EDX analysis. From the SEM micrograph analysis, the morphology of the crystallites, the distribution of SL components, and the highlighting of instrumentation path traces/amplitudes were observed. By analyzing the SEM photomicrographs at 750 and 800× magnification, it was possible to highlight the cracks in the root dentinal walls. Thus, in comparison with Lots I and II which did not present cracks, in Lot III multiple cracks of the root dentinal walls were identified, especially in the coronal 1/3, and in Lot IV cracks were present with preponderance in the coronal and apical 1/3 of the root canals. The EDX images with atom mapping show very well the rather homogeneous elemental distribution for Ca, N, and P, respectively inhomogeneous for Na, Ca, Si, C, N, O, and P elements, as a result of the presence of remnant products from the processing of the root dentinal walls. Root canal instrumentation performed with both manual Kerr needle instrumentation by a convection technique and the rotary, Orodeka system, by crown-down technique, resulted in minimal SL formation in all three root canal areas, unlike the ProTaper FlyDent system. Most cracks were recorded in the case of the ProTaper Flydent rotary instruments and the one in which it was paired with a diamond ultrasonic scaler. The occurrence of dentinal cracks causes a decrease in dentinal microhardness, favoring the occurrence of root fractures.

Elastomeric Biocomposites of Natural Rubber Containing Biosynthesized Zinc Oxide

Zinc oxide (ZnO) particles were successfully synthesized through the green method using aloe vera extract and zinc nitrate (1:1). The structure, morphology and properties of the biosynthesized ZnO (bioZnO) particles were analyzed by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), time of flight secondary ion mass spectrometry (TOF-SIMS) and thermogravimetry (TG). The morphology and the size of ZnO particles were elucidated by scanning electron microscopy (SEM) with energy-dispersive X-ray spectroscopy (EDS). Then, the ability of bioZnO to activate sulfur curing of natural rubber (NR) was tested and compared to commercial ZnO traditionally used as vulcanization activator. The bioZnO showed similar activity in the vulcanization process to commercial ZnO. NR composites containing bioZnO were pro-ecological in nature and exhibited better mechanical characteristics and durability against thermo-oxidative aging than NR with commonly used micrometric ZnO. Moreover, NR vulcanizates containing bioZnO showed good mechanical properties in dynamic conditions and satisfactory thermal stability. The present research is new and in addition to the analysis of biosynthesized ZnO particles, the effect of the activator in the vulcanization process of the NR elastomer and its influence on the properties of the final products were additionally discussed.