Electron Microprobe Research Articles

A semiconducting supramolecular Co(II)-metallogel based resistive random access memory (RRAM) design with good endurance capabilities.

A highly efficient approach for synthesizing a supramolecular metallogel of Co(II) ions, denoted as CoA-TA, has been established under room temperature and atmospheric pressure conditions. This method employs the metal-coordinating organic ligand benzene-1,3,5-tricarboxylic acid as a low molecular weight gelator (LMWG) in DMF solvent. A comprehensive analysis of the mechanical properties of the resulting supramolecular Co(II)-metallogel was conducted through rheological investigation, considering angular frequency and thixotropic study. The hierarchical rocky network structure of the supramolecular Co(II)-metallogel was unveiled using field emission scanning electron microscopy (FESEM). Transmission electron microscopic (TEM) analysis showed rod-shaped structures via low-magnification high angle annular dark field (HAADF) bright field scanning transmission electron microscopic (STEM) imaging, while energy dispersive X-ray (EDX) elemental mapping confirmed its primary chemical constituents. The formation mechanism of the metallogel was examined via fourier transform infrared spectroscopy (FTIR) spectroscopy. The nature of the synthesized CoA-TA metallogel was affirmed through powder X-ray diffraction (PXRD) analysis. Furthermore, this study involved fabrication of Schottky diode structures in a metal-semiconductor-metal geometry based on cobalt(II) metallogel (CoA-TA), enabling observation of charge transport behavior. Remarkably, a resistive random access memory (RRAM) device utilizing cobalt(II) metallohydrogel (CoA-TA) demonstrated bipolar resistive switching at room temperature and under ambient conditions. The switching mechanism was investigated, revealing the formation and rupture of conductive filaments between metal electrodes that govern the resistive switching behavior. This RRAM device exhibited an impressive ON/OFF ratio (~ 414) and exceptional endurance over 5000 switching cycles. These structures offer great potential for diverse applications such as non-volatile memory design, neuromorphic computing, flexible electronics and optoelectronics. Their advantages lie in their fabrication process, reliable resistive switching behavior and overall performance stability.

Quantitative Characterization and Mapping Relationship between Microstructure, Composition, Orientation, and Mechanical Properties of Nickel-Based Superalloy Inconel 718

Abstract This study explores the relationship between the microstructure, composition, orientation, and mechanical properties of the nickel-based superalloy Inconel 718. Employing scanning electron microscopy (SEM), electron microprobe (EMP), nano-indentation, and other techniques, the study observes the structure, confirms the composition, determines orientation, and tests mechanical properties in specific micro-zones. Findings reveal a uniform grain distribution in Inconel 718, with a minor δ-phase presence at grain boundaries. There is a notable enrichment of Nb at the grain boundaries, whereas Fe and Cr levels are lower at these boundaries compared to the grain interiors. The indentation hardness and modulus at the grain boundaries are markedly higher than those within the grains. Moreover, grains with different orientations exhibit diverse microscale mechanical properties, such as hardness and elastic modulus. This research establishes a quantitative mapping relationship between the microstructure, composition, orientation, and mechanical properties of Inconel 718, providing a foundation for future multiscale (micro to macro) mechanical property investigations.

An Oxygen‐Self‐Produced Nanoplatform Based on MnO2 for Relieving Hypoxia

AbstractManganese dioxide (MnO2) nanoparticles are increasingly recognized for their potential in biomedical applications, particularly in the realm of hypoxic cancer therapy, due to their unique physicochemical characteristics. This investigation introduces a novel, template‐free synthesis strategy. The reducing groups inherent in bovine serum albumin (BSA) facilitate a redox reaction with potassium permanganate (KMnO4), while the abundance of functional groups in BSA is instrumental in the formation of MnO2. The transmission electron microscopy (TEM) analysis has characterized the synthesized MnO2 nanoparticles, termed BM NPs, as spherical particles with a mean diameter of 210 nm and zeta potential of −40.1 mV measured by dynamic light scattering (DLS). The Fourier transform infrared (FT‐IR) spectrum of BM NPs exhibits the characteristic peak of MnO2 at 1113 cm−1 and 620 cm−1. Furthermore, the elemental composition of BM NPs has been ascertained through energy‐dispersive X‐ray (EDX) elemental mapping analysis. Though concentration of BM NPs up to 200 μg/mL, the survival rate of 4T1 cells remained approximately 75 %. Given that BM NPs at a concentration of 100 μg/mL significantly alleviate cellular hypoxia, the high oxygen‐generating capacity of these nanoparticles is proved, suggesting their suitability as a drug delivery system, especially in the context of hypoxic tumor microenvironments.

Supported phenylalanine on core-shell mesoporous microsphere as a catalyst for the synthesis of triazolo[1,2-a] indazole-triones and spiro triazolo[1,2-a] indazole-tetraones

In recent years, mesoporous silica materials have gained attention due to their unique properties, such as high surface area, pore volume, size, and chemical stability. These characteristics make them effective in various fields, particularly efficient supports in heterogeneous catalytic reactions. The present study developed a novel type of core-shell mesoporous microsphere material by anchoring phenylalanine on a core-shell SiO2@NiO@MS support. The catalyst support (SiO2@NiO@MS) was synthesized through homogeneous precipitation and sol-gel methods, with NiO encapsulated within the porous silica. The catalyst was characterized using various techniques, including Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), Elemental mapping analysis, N2 adsorption-desorption, Transmission electron microscopy (TEM), Vibrating sample magnetometer (VSM), and Thermogravimetric analysis (TGA). It was then employed for the synthesis of triazolo[1,2-a]indazole-trione and spiro triazolo[1,2-a]indazole-tetraones compounds from 4-phenyl urazole, dimedone, and aromatic aldehydes or isatin derivatives. This synthetic approach offers multiple advantages, including high yields, faster reaction times, low catalyst requirements, and environmentally sustainable conditions.

Silver doping effect on the electrochromic performance of the WO3 thin films produced by thermal evaporation in vacuum

Ag doped WO3 thin films are successfully fabricated by thermal evaporation method in vacuum as precursor, and then annealed at 450 °C in nitrogen gases atmosphere. Cyclic voltammetry, repeating chronoamperometry, chronocolumetry and optical transmittance are recorded in 1 M LiClO4/propylene carbonate electrolyte. The color of the WO3 thin films changes from transparent to the blue under the applied potential of -1.8 and +1.9 V. XRD studies show that all the films have a polycrystalline structure of WO3. The molecular formation is also confirmed by Raman and X-Ray photoelectron spectroscopy (XPS). The EDS elemental mappings clearly confirm the homogeneous distribution of Ag, W and O elements into the WO3 network. From the optical studies, indirect band gap energy of the WO3 decreases as Ag doping level increases. The best coloration and bleaching times (2.33 and 1.25 s) are obtained for the Ag(2%):WO3 thin films, compared to the pure WO3 (3.79 and 1.96 s). The produced WO3 films exhibit high reversibility (39.6/69.1%), high coloration efficiency values (26.3/141.2 cm2/C), and good cycling stability. From the EIS measurements, the charge-transfer resistance is Ag(2%):WO3 < the pure WO3 < Ag(5%):WO3 < Ag(8%):WO3, which means that Ag(2%):WO3 has the biggest electrochemically active surface area. Electronic energy levels of the pure WO3 and the Ag:WO3 thin films are also given. From the Mott-Schottky studies, it is determined that the donor concentration of the materials is of the order of 1014-1015 cm−3. In the literature, there are very limited studies related to electrochromic thin films by thermal evaporation in vacuum. In this sense, the reported results in this study are promising for the electrochromic applications.

One Pot Green Synthesis of Zr doped NiO Nanoparticles using Annona squamosa Seed Extract: Characterization and Biological Properties

Pure and Zr-doped NiO nanoparticles were successfully synthesized through green synthesis using extract of Annona squamosa seeds. The synthesized nanoparticles were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, UV-vis spectroscopy, field emission scanning electron microscopy (FESEM), EDAX (energy dispersive X-ray analysis) and elemental mapping analysis. The addition of zirconium dopant has been integrated into the single-phase NiO lattice structure as indicated by characterization findings. Furthermore, the antibacterial, antifungal and antioxidant properties of Zr-doped and undoped NiO NPs were thoroughly examined. As a result of the strong Zr-doped NiO NPs synergistic effect, the results showed that the Zr-doped NiO NPs have improved the biomedical properties when compared to the undoped NiO NPs. The optimized size and shape of the nanoparticles contributed significantly to their improved effectiveness against the microorganisms and oxidative stress.

Revolutionizing acridine synthesis: novel core-shell magnetic nanoparticles and Co-Zn zeolitic imidazolate framework with 1-aza-18-crown-6-ether-Ni catalysts

Nanoparticles have emerged as a critical catalyst substrate due to their exceptional features, such as catalytic efficiency, high stability, and easy recovery. In our research, we have developed an innovative and environmentally friendly magnetic mesoporous nanocatalyst. Using the co-precipitation method, we produced magnetic nanoparticles (Fe3O4) and coated them with Zeolitic imidazolate frameworks (ZIFs) to enhance their surface area and chemical stability. The resulting substrate was functionalized with 1-aza-18-crown-6-ether and nickel metal. Our prepared catalyst has been rigorously evaluated using advanced techniques, including X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Brunauer-Emmet-Teller (BET), vibrating sample magnetometry (VSM), scanning electron microscopy and energy dispersive X-ray (SEM-EDS), inductively coupled plasma (ICP), elemental mapping analysis (EMA), thermogravimetric analysis (TGA), and transmission electron microscopy (TEM). By synthesizing acridine derivatives, we have demonstrated the exceptional efficiency of our catalyst in organic compound synthesis. Through optimization, we have established the ideal parameters for catalytic processes, including catalyst amount, temperature, time, and ultrasonic use. Our catalyst has been proven to exhibit remarkable physical and chemical properties, such as porosity, temperature resistance, and recyclability. Notably, our heterogeneous nanocatalyst has shown outstanding performance and can be recycled six times without any loss in efficiency, affirming its potential in acridine.

Macrophage-T cell hybrid membrane-camouflaged biomimetic nanoparticles ameliorate autoimmune myocarditis via suppressing macrophage pyroptosis by target gene silencing

Abstract Background Current management of myocarditis mainly relies on conventional approaches and immunosuppressive therapies. However, these strategies often yield limited efficacy. Our previous research revealed the pivotal role of macrophage pyroptosis in myocarditis pathogenesis. Therefore, targeted intervention to inhibit macrophage pyroptosis may provide new insights into myocarditis treatment. Purpose We previously identified interferon regulatory factor 1 (IRF1) as the key modulator of macrophage pyroptosis in myocarditis. In this study, we synthesized a nano-delivery platform consisting of a macrophage-T cell hybrid membrane-coated zeolitic imidazolate framework-8 (ZIF-8) encapsulating IRF1-small interfering RNA (siRNA@ZIF@HM). We aimed to evaluate its targeting capability and therapeutic efficacy for macrophage pyroptosis in myocarditis. Methods The fabrication of siRNA@ZIF@HM was validated using transmission electron microscopy (TEM) and dynamic light scattering (DLS). Cellular uptake, cytotoxicity, endolysosome escape, IRF1 silencing, and anti-pyroptotic effect were assessed using mouse bone marrow-derived macrophages and the mouse macrophage cell line J774A.1 and RAW264.7. An experimental autoimmune myocarditis (EAM) mouse model was induced in Balb/c mice for in vivo investigations. Pharmacokinetics and targeting capability were determined with ex vivo fluorescence imaging and immunofluorescence staining. Subsequently, mice were randomly allocated into control, EAM + siRNA, EAM + siRNA@ZIF, and EAM + siRNA@ZIF@HM groups to assess the therapeutic efficacy. Additionally, the biodistribution and biosafety of siRNA@ZIF@HM were also evaluated. Results TEM, DLS, and element mapping confirmed the successful fabrication of siRNA@ZIF@HM, with a diameter of approximately 130 nm. The nanoparticle exhibited pH responsiveness and membrane markers of macrophage and T lymphocytes (Figure 1). It demonstrated high targeting specificity for pro-inflammatory macrophages and myocarditis. Immunofluorescence microscopy revealed successful endolysosome escape of IRF1-siRNA in macrophages. Consequently, the nanoparticle significantly silenced IRF1 protein expression and suppressed macrophage pyroptosis both in vivo and in vitro, resulting in the amelioration of autoimmune myocarditis (Figure 2). Furthermore, the nanoparticle showed good biocompatibility with no significant changes observed in other organs. Conclusions The pH-responsive, macrophage-T cell hybrid membrane-coated biomimetic nanoparticle demonstrates promising capability for targeted siRNA delivery to myocardial inflammation sites, particularly pro-inflammatory macrophages. Additionally, targeting IRF1-mediated macrophage pyroptosis represents a potential therapeutic strategy for myocarditis treatment.Figure 1Figure 2

Physical and enhanced photocatalytic MO dye degradation behaviour of Zn doped β-Ga2O3 microrods

This work explored the effects of Zn doping on the structural, micrographic, optical and photocatalytic behaviour of gallium oxide (β-Ga2O3) microrods. The X-ray diffractogram (XRD) and Raman spectral analyses confirmed the monoclinic structure of β-Ga2O3, with a shift to lower angles in the XRD pattern indicating Zn incorporation into the Ga2O3 lattice. The Scanning electron microscopy (SEM) images revealed a rod-like shape, with the diameter decreasing from 604 nm to 573 nm with Zn doping. Further analysis using TEM, HR-TEM, SAED, EDX, and elemental mapping confirmed the shape, crystallinity, crystal structure, and elemental distribution. The interplanar spacings were measured as 0.4 and 0.2 nm, corresponding to the (002) and (−311) planes of β-Ga2O3. UV–Vis diffuse reflectance spectroscopy (UV–Vis DRS) showed a slight shift in the absorption edge, while photoluminescence (PL) analysis demonstrated strong UV and weak visible light emission. Photocatalytic results revealed a high efficiency of dye degradation,(i.e) 98 % (20 ppm) and 89 % (30 ppm) against methyl orange (MO) dye aqueous solution over 150 min, with a rate constant of 0.02/min and 0.01/min, respectively for 1.5 wt% Zn doping. This suggests that the Zn-doped material holds promise as a photocatalyst for wastewater treatment applications.

Elemental mapping in single-particle reconstructions by reconstructed electron energy-loss analysis.

For macromolecular structures determined by cryogenic electron microscopy, no technique currently exists for mapping elements to defined locations, leading to errors in the assignment of metals and other ions, cofactors, substrates, inhibitors and lipids that play essential roles in activity and regulation. Elemental mapping in the electron microscope is well established for dose-tolerant samples but is challenging for biological samples, especially in a cryo-preserved state. Here we combine electron energy-loss spectroscopy with single-particle image processing to allow elemental mapping in cryo-preserved macromolecular complexes. Proof-of-principle data show that our method, reconstructed electron energy-loss (REEL) analysis, allows a three-dimensional reconstruction of electron energy-loss spectroscopy data, such that a high total electron dose is accumulated across many copies of a complex. Working with two test samples, we demonstrate that we can reliably localize abundant elements. We discuss the current limitations of the method and potential future developments.

Thallium enrichment mechanism and geological significance of the Xiangquan thallium deposit in Anhui Province, China

The discovery of the independent thallium (Tl) deposit in Xiangquan, Anhui Province, provides an example for the study of the enrichment and mineralization of the highly dispersed rare metal element Tl. In this paper, a range of methods are used to characterize the enrichment, depletion, migration and occurrence state of Tl in different types of rocks and ores: lithogeochemistry; electron microprobe and principal component analysis; and exploring the significance of geochemical anomalies on the geological indication of Tl deposit formation. The results show that Tl is mainly distributed in silicified rocks of the Ordovician Lunshan Formation, and its average content is 307.08 μ g g –1 . The contents of As, Sb, S, Fe 2 O 3 and Tl in wall rocks, altered rocks and ores are significantly correlated, indicating a close relationship with Tl accumulation. The geochemical characteristics confirm that pyrite in the study area originates from submarine hot-water deposition. The main carrier of Tl is pyrite of hydrothermal sedimentary origin, in which Tl occurs as isomorphs in fine grains of pyrite. Tl mineralization may be accompanied by silicification, and the metallogenic environment is in a relative oxidation state. The mineralization process results in the geochemical differentiation of elements. Under the influence of tectonic and low-temperature hydrothermal activities, ore-forming elements migrate to structurally favourable conditions for mineralization to occur. This study provides a basis for further understanding the mechanisms of co-enrichment and separation of Tl and guidance for Tl mineral exploration.

Corrosion mapping of intermetallic in a dissimilar weldment using in-situ alternating current scanning electrochemical microscopy

In the present work, in-situ corrosion activity mapping across explosively welded 304 L SS-Zr-4 dissimilar joint interfaces was performed using intermittent contact alternating current-scanning electrochemical microscopy (IC-AC-SECM). Two weld joint samples, one with a regular interface and another with an irregular interface, were examined for their local surface activities at an open circuit potential in tap water without using a redox mediator. The SEM micrographs showed the formation of intermetallics at localized regions of the irregular interface weld sample but not in the regular interface sample. The 304 L SS regions of the welds were relatively anodic, with current and impedance magnitude values of 270 ± 20 nA and 380 ± 20 kΩ respectively, when compared to the Zr-4 regions with the corresponding values of 160 ± 20 nA and 630 ± 20 kΩ, due to galvanic coupling effect. The IC-AC-SECM technique enabled the in-situ determination of corrosion activity of localized intermetallic region within the weldment. The current and impedance magnitude values of the intermetallic region were ∼ 240 nA and ∼ 450 kΩ, respectively, showing only a slightly lesser anodic activity as compared to the 304 L SS base metal. The results obtained from the IC-AC-SECM mapping showed a good correlation with the EDS elemental mapping of the dissimilar weldment with intermetallic. The findings indicate the effectiveness of the IC-AC-SECM technique for the in-situ localized corrosion mapping of dissimilar weld joints, showcasing its potential for various applications in assessing weld integrity.

Engineering the Atomic Interface of Refractory‐Metal‐Reinforced Copper Matrix Using Direct Ink 3D Printing

Herein, 3D printing involving metallic materials with substantially distinct melting temperatures and their immiscibility presents a formidable challenge. Nevertheless, it may be possible to overcome this challenge using the direct ink writing (DIW) method within such immiscible systems. In this article, a successful fabrication of Cu‐based composites utilizing the additive manufacturing process that is DIW technique, followed by a post‐sintering process, is presented. The secondary addition to the Cu–matrix includes tantalum (Ta), tungsten (W), and niobium (Nb). The rheological properties of the composite inks are also analyzed for the DIW technique. The underlying reasons behind the increased mechanical, wear, and thermal properties are assessed through experimental and molecular dynamics simulations. Microstructural analysis is conducted using optical and scanning electron microscopes. Mechanical, electrical, thermal, and wear properties are evaluated at ambient temperature, and comparisons are established with DIW‐processed pure Cu. Elemental mapping through energy‐dispersive spectroscopy and high‐resolution transmission electron microscopy confirm the distribution of W, Ta, and Nb particles within the composite. The 3D printing of immiscible alloy components opens new avenues for exploring novel material properties, mixtures, and composite materials, thus fostering the development of innovative materials.

Effect of water quenching into strength, hardness and microstructure of the welded AA 6061 plates

Purpose The purpose of this study is to find the effect of heat treatment on the mechanical proeprties of aluminum. Aluminum exhibits a good response to heat treatment, especially quenching, according to the mechanical property improvement. The presence and orientation of secondary phases (Al-Fe-Mn-Si) are greatly affected by the quenching process. Design/methodology/approach The present work deals with the effect of water quenching on the mechanical properties of welded AA 6061 plates which were joined by using metal inert gas (MIG) welding, tungsten inert gas welding and friction stir welding (FSW). Three tests like tensile, bending and hardness were considered. The microstructural variation was analyzed by optical microscopy and elemental mapping through field emission scanning electron microscope. Findings A significant enhancement in the tensile strength and hardness was achieved on postquenched specimens. This improvement in mechanical properties is caused by the distribution of fine alloying elements throughout the metal solution rather than precipitation at the grain boundaries. In comparison to the “untreated specimens,” an improvement of 76.7%, 25.32% and 56.81% in the tensile strength of quenched TIGW, MIGW and FSW specimens, respectively, was observed. Originality/value The quenching process has increased the strength of the MIG welded joint over the base metal. The MIG welded joint has a larger flexural modulus than the other two welded plates, according to the results of the bending test. Furthermore, a uniform distribution of hardness was observed in postquenched welded specimens. It was found that welded zone was harder than heat-affected zone. Out of all the specimens, the base metal zone has the lowest hardness.

Corrosion behaviour of nitroxy-QPQ additively manufactured 17-4 PH steel on marine and nuclear reactor components

The study investigates the corrosion behavior of untreated and nitroxy QPQ treated 17-4 PH stainless steel under NaCl environments. Potentiodynamic polarization tests reveal that the nitroxy layer forms an oxide coating, leading to a passivation phase with gradually increasing current density. Oxidation at different temperatures shows variation in corrosion potential, with the lowest current density observed at 450 °C, indicating enhanced corrosion resistance. SEM images of untreated steel show severe crevice and pitting corrosion, whereas nitroxy QPQ treated surfaces exhibit reduced corrosion, with minimal disturbance at 450 °C. Elemental analysis confirms the formation of oxides and nitrides, with increased oxygen content in oxide layers and decreased nitrogen content due to the formation of chromium nitrides. The oxide layer, enriched with oxygen, nitrogen, and chromium, acts as a passive film, protecting against corrosion even in NaCl environments. Elemental mapping further illustrates the correlation between oxidation temperature and corrosion resistance, with higher temperatures resulting in reduced corrosion rates. The combined nitriding and oxidation process enhances corrosion resistance by forming a dense and adherent oxide layer, serving as a barrier against corrosive agents.

Splicing Dysregulation of Non-Canonical GC-5′ Splice Sites of Breast Cancer Susceptibility Genes ATM and PALB2

Background/Objectives: The non-canonical GC-5′ splice sites (5′ss) are the most common exception (~1%) to the classical GT/AG splicing rule. They constitute weak 5′ss and can be regulated by splicing factors, so they are especially sensitive to genetic variations inducing the misrecognition of their respective exons. We aimed to investigate the GC-5′ss of the breast/ovarian cancer susceptibility genes, ATM (exon 50), BRIP1 (exon 1), and PALB2 (exon 12), and their dysregulation induced by DNA variants. Methods: Splicing assays of the minigenes, mgATM_49-52, mgBRIP1_1-2, and mgPALB2_5-12, were conducted to study the regulation of the indicated GC-5′ss. Results: A functional map of the splicing regulatory elements (SRE) formed by overlapping exonic microdeletions revealed three essential intervals, ATM c.7335_7344del, PALB2 c.3229_3258del, and c.3293_3322del, which are likely targets for spliceogenic SRE-variants. We then selected 14 ATM and 9 PALB2 variants (Hexplorer score &lt; −40) located at these intervals that were assayed in MCF-7 cells. Nine ATM and three PALB2 variants affected splicing, impairing the recognition of exons 50 and 12, respectively. Therefore, these variants likely disrupt the active SREs involved in the inclusion of both exons in the mature mRNA. DeepCLIP predictions suggested the participation of several splicing factors in exon recognition, including SRSF1, SRSF2, and SRSF7, involved in the recognition of other GC sites. The ATM spliceogenic variants c.7336G&gt;T (p.(Glu2446Ter)) and c.7340T&gt;A (p.(Leu2447Ter)) produced significant amounts of full-length transcripts (55–59%), which include premature termination stop codons, so they would inactivate ATM through both splicing disruption and protein truncation mechanisms. Conclusions: ATM exon 50 and PALB2 exon 12 require specific sequences for efficient recognition by the splicing machinery. The mapping of SRE-rich intervals in minigenes is a valuable approach for the identification of spliceogenic variants that outperforms any prediction software. Indeed, 12 spliceogenic SRE-variants were identified in the critical intervals.

High‐Performance Na‐Storage and Sodiation Behavior Identification in Cellulose‐Derived Hard Carbon by High‐Resolution Element Mapping Microscopy

Nowadays, hard carbon is one of the most promising anode materials for sodium‐ion batteries. However, the Na‐storage performance of hard carbon varies for different precursors and synthetic processes due to disparities in the dopant content, dimensions, and categories of defects, graphitic domains, which lead to controversial explanations for the energy storage mechanism. Herein, self‐freestanding membrane of cellulose‐derived carbon fibers is presented, delivering a reversible Na‐storage capacity of 330 mAh g−1 at 50 mA g−1 due to abundant ordered graphitic zones with enlarged interlayer spacings around 0.39 ± 0.03 nm. Benefiting from a robust solid electrolyte interphase layer rich in NaF nanocrystals, the membrane also holds a superior rate capability of 100 mAh g−1 at 2 A g−1 and long‐term cycling stability with capacity retention of 82.6% at 1.5 A g−1 for 4000 cycles. A clear sodiation behavior of Na+ intercalation into enlarged carbon graphitic layers at the slope step above 0.10 V and Na cluster evolution in the micropores at the plateau step around 0.01–0.10 V is disclosed by high‐resolution element mapping microscopy, different from the accepted mechanism of Na+ intercalation into graphitic layers at the plateau step.

Green Synthesis of Some 2‐Amino‐4 h‐Benzo[H]Chromene Derivatives in the Presence of Bimetallic Nanocomposite Based on Magnetic Mesoporous Silica Nanoparticles at Ambient Conditions

AbstractIn this research, some of 2‐amino‐4H‐benzo[h]chromene derivatives were synthesized by multicomponent reaction of 1‐naphthol, benzaldehyde derivatives and malononitrile. The reaction was performed under green conditions using water as the solvent in the presence of heterogeneous nano catalyst containing Co(II) and Cu(II) stabilized on magnetic mesoporous silica nanoparticles/tannic acid (M–MSN/TA/Co(II),Cu(II)) at room temperature. The prepared catalyst showed excellent efficiency and its magnetic properties allow easy separation. The structure and morphology of prepared catalyst was identified using Fourier transform infrared (FT‐IR), X‐ray diffraction (XRD), field emission scanning electron microscopy (FE‐SEM), energy dispersive X‐ray spectroscopy (EDX), elemental mapping, thermogravimetric analysis (TGA) and vibrating‐sample magnetometry (VSM) analysis. All of products were obtained in high to excellent yields (78–94 %) after short reaction times (20–45 min) in optimal conditions and their structures were confirmed using FT‐IR and Proton nuclear magnetic resonance (1H NMR) spectroscopic techniques. This study shows that the M–MSN/TA/Cu(II), Co(II) presents a good catalytic activity, reusability and stability compared to other catalysts.

Structural Changes in Copper Slags During Slow Cooling

The objects of the study were converter slags from the Balkhash copper plant in their initial state and after heat treatment. Using mineralogical and X-ray phase analysis, scanning electron microscopy (SEM), and electron probe microanalysis (EPMA), it was found that the initial converter slag and its thermally treated samples have identical matrices with almost complete coincidence in mineral and phase compositions. The distinguishing feature is the quantitative ratio of mineral components in the slag mass. Almost all of the iron is oxidized and present in the form of fayalite, magnetite, and magnetite, with other elements (silicon, copper, zinc, and aluminum) incorporated into its lattice. The structure of all slag samples indicates an association of sulfur exclusively with copper. Copper in the slags was identified in both metallic and sulfide forms. Slow cooling of the converter slag after its remelting contributes to the reduction in the sulfide–metal suspension in the volume of the melt and its coarsening. During slow cooling, structural changes occur not only in the main oxide part of the slag but also in the polymetallic globules.

Occurrences of the Rare, REE Minerals Daqingshanite, Törnebohmite, Biraite, Sahamalite, and Ferriperbøeite from the Sheep Creek Area, Montana, USA

Over 30 small, discontinuous, tabular carbonatite bodies are located in the Sheep Creek area, Ravalli County, southwest Montana. The age and origin of these REE-Nb-rich deposits are currently being investigated. The purpose of this paper is to document the occurrence of several rare minerals, including daqingshanite, törnebohmite, biraite, sahamalite, and ferriperbøeite, in two of the carbonatite bodies. These minerals are found in association with monazite, hydroxylbastnäsite, ferriallanite, calcite, dolomite, baryte, quartz, actinolite, apatite, celsian, and Sr-rich aragonite. Automated SEM-EDS was used to target the areas of interest in polished specimens for more detailed spot SEM-EDS and electron probe microanalysis. Raman spectra were also acquired for each of the rare minerals. The complex mineralogy of the Sheep Creek carbonatites is most likely due to several overlapping thermal events, including primary magmatic, overprinting hydrothermal, and supergene weathering stages. The rare minerals described in this study are believed to be hydrothermal and/or carbothermal in origin, although no estimates of temperature are available at this time.