Transmission Electron Microscopy Methods Research Articles

Revealing Epitaxial Deposition in Alkali Metal Batteries.

Alkali metal batteries have high energy densities required to power future devices; however, uneven metal deposition is a critical barrier to achieving long lifespans. We have developed an elegant noncryogenic transmission electron microscopy method which has facilitated the first observations of epitaxial deposition in alkali metal batteries. Using this method, we have confirmed epitaxial interactions between (002) sodium crystallite planes and (01-11) planes in zinc current collectors. Such epitaxial interactions decrease nucleation energy barriers and promote even metal growth. This study offers fresh inspiration for the development of electron microscopy techniques tailored to electron-sensitive battery materials and sets a new agenda for the development of battery technologies.

PREPARATION, CHARACTERIZATION, AND IN VITRO EVALUATION OF GEL CONTAINING NANOPHYTO-PHOSPHOLIPID COMPLEX OF KOPASANDA LEAF EXTRACT (CHROMOLAENA ODORATA (L.) R. M. KING AND H. ROB)

Objective: This study aims to prepare, characterize, and in vitro evaluation of the gel containing nanophyto-phospholipid complex of kopasanda leaf extract. Methods: Kopasanda dried leaf was extracted by extraction reflux method, followed by total phenolic content of extract measurement using Spectrophotometry UV-Vis method. The nanophyto-phospholipid complex was prepared using an antisolvent evaporation method with various ratios between extract and phospholipid of 1:1; 1:2; 1:3. The optimum ratio was evaluated by entrapment efficiency (%). The nanophyto-phospholipid complex formation was characterized by polydispersity index, particle size, Fourier Transform Infra-Red (FT-IR), and the Transmission Electron Microscope (TEM) method. The optimum nanophyto-phospholipid complex was formulated into gel preparation. The in vitro permeation study was performed to discover the influence of gel containing nanophyto-phospholipid complex compared with gel-containing extract without the nanophyto-phospholipid complex formation. Results: Thetotal phenolic content of kopasanda leaf extract was 117.214±3.054 mg/GAE. The optimum ratio of kopasanda leaf extract and phospholipid was 1: 2 with entrapment efficiency (%), particle size, and polydispersity index equal to 99.897±0.001%, 130.1 nm and 0.394. The morphology of the nanophyto-phospholipid complex was spherical and the complex formation was confirmed by the FTIR spectrum. The permeation test showed that the gel containing nanophyto-phospholipid complex had better diffusion than the gel without the nanophyto-phospholipid complex formation. Conclusion: The gel containing nanophyto-phospholipid complex formation exhibited the potential drug delivery system to increase the phenolic content permeation of kopasanda leaf extract.

Structure and Properties of the Electroexplosive Coating of the TiB2-Ag System after Electron Beam Treatment

A coating of the TiB2-Ag system was formed through the use of sequential operations of electroexplosive spraying and electron beam processing. The values of electrical conductivity (62.0 MS/m), Vickers microhardness (0.251-0.265 GPa at the point of measurement on a silver matrix and 25-32 GPa at the point of measurement at inclusions of boride phases), nanohardness (4.48 ± 0.76 GPa) were determined), Young’s modulus (116±29 GPa), wear parameter under dry friction-sliding conditions (1.2 mm3/N • m) and friction coefficient (0.5). Switching wear resistance during accelerated tests was 7000 on and off cycles with an electrical resistance of 10.01 - 11.76 LiOhm. The thickness of the coatings is 100 microns. The coatings are formed by a silver matrix with inclusions of titanium borides located in it with three types of sizes: nanocrystalline, submicrocrystalline and microcrystalline. Quantitatively, in the structural composition among titanium borides, titanium diboride and silver (56 wt. %) are formed predominantly (41 wt. %), while other titanium borides account for 3 wt. %. Structural transformations are described using complementary methods of X-ray phase analysis, scanning and transmission electron microscopy.

Towards atom counting from first moment STEM images: Methodology and possibilities

Through a simulation-based study we develop a statistical model-based quantification method for atomic resolution first moment scanning transmission electron microscopy (STEM) images. This method uses the uniformly weighted least squares estimator to determine the unknown structure parameters of the images and to isolate contributions from individual atomic columns. In this way, a quantification of the projected potential per atomic column is achieved. Since the integrated projected potential of an atomic column scales linearly with the number of atoms it contains, it can serve as a basis for atom counting. The performance of atom counting from first moment STEM imaging is compared to that from traditional HAADF STEM in the presence of noise. Through this comparison, we demonstrate the advantage of first moment STEM images to attain more precise atom counts. Finally, we compare the integrated potential extracted from first-moment images of a wedge-shaped sample to those values from the bulk crystal. The excellent agreement found between these values proves the robustness of using bulk crystal simulations as a reference library. This enables atom counting for samples with different shapes by comparison with these library values.

Mechanisms of hardening of heavy-loaded rails made of hypereutectoid steel during long-term operation

Using transmission electron microscopy methods, the structural-phase states and defective substructure were studied at distances of 0; 2 and 10 mm from the surface along the central axis and rounding radius of rails head fillet. Differentially hardened long rails of the DT400IK category made of hypereutectoid steel have been studied after operation on the Trans-Baikal Railway (passed tonnage equal to 234.7 million tons gross). It has been established that steel strength characteristics are determined by certain physical mechanisms. A qualitative assessment of the contributions from crystal lattice friction, solidsolution strengthening, strengthening of the pearlite component, incoherent cementite particles, grain boundaries and subboundaries, dislocation substructure and internal stress fields was carried out, and their hierarchy was established. A quantitative assessment of the additive yield strength of steel in different directions was carried out depending on the distance from the rolling surface. It is shown that the main mechanisms of strengthening are strengthening by incoherent particles, long-range stress fields and substructural strengthening. The additive yield strength on the fillet surface is significantly greater than on the rolling surface of the head along the central axis.

Apigenin alleviates Sjögren’s syndrome-induced salivary gland epithelial cell ferroptosis via ERα signaling-mediated regulation of the ATF3/SLC7A1l axis

BackgroundIn Sjögren’s syndrome (SS)—an autoimmune disease characterized by dry mouth and eyes—salivary gland epithelial cells (SGECs) undergo ferroptosis, which disrupts their integrity and impairs saliva secretion. Apigenin, a phytoestrogen, is known to activate estrogen signalling and alleviate xerostomia in ovariectomized mice; however, its effect on SGEC survival and function in SS remains unclear. We hypothesized that apigenin alleviates SS symptoms and progression by inhibiting ferroptosis in SGECs and aimed to elucidate the underlying mechanism. MethodsApigenin (50 mg/kg) was orally gavaged to non-obese diabetic (NOD)/LtJ female mice (SS model); changes in SS functional indicators were analyzed using mRNA sequencing and bioinformatic analyses of submandibular glands. Interferon-gamma (IFN-γ)-stimulated SGECs were used to model SS in vitro; SGEC activity and aquaporin 5 (AQP5) expression were analyzed. Immunohistochemical staining, transmission electron microscopy, RT-qPCR, western blotting and other methods were used to verify the mechanisms. ResultsApigenin significantly increased salivary secretion and AQP5 expression while inhibiting ferroptosis and immune infiltration in NOD mouse submandibular glands. The oxidative stress gene ATF3 was upregulated and GPX4 was downregulated in NOD mice compared to that in control group (ICR mice); however, apigenin reversed this effect. IFN-γ treatment downregulated AQP5, SLC7A11, and GPX4 expression while promoting ATF3 expression and ferroptosis, which was mitigated by apigenin. ATF3 knockdown increased SLC7A11 and GPX4 expression, inhibiting SS and ferroptosis. Furthermore, apigenin inhibited ferroptosis in SGECs through ESR1 binding to ATF3. ConclusionApigenin alleviates SS by regulating SGEC ferroptosis via the ERα-regulated ATF3/SLC7A11 axis, highlighting its therapeutic potential in SS.

Wuzi-Yanzong-Wan Prevents the Defect of Cell-Cell Junctions between Sertoli-Germ Cells by Up-Regulating the Expression of TAp73.

The TAp73 gene is an anti-cancer gene that also affects the junction between Sertoli and germ cells. Inhibition of this gene causes infertility in male mice. Our previous research proved that Wuzi-Yanzong-Wan (WZYZW) can protect spermatogenesis and maturation by preventing TAp73 inhibition. This study aimed to investigate the effect of drug-containing serum of WZYZW on the defect of cell-cell junctions in the Sertoli-germ cells co-culture system in vitro. LC-HRMS was used to analyze the content of active ingredients in WZYZWmedicated serum. Then, primary extraction and co-culture of germ cells and Sertoli cells were carried out. Co-cultured cells were added with PFT-α to induce the TAp73 inhibition model, with WZYZW-medicated serum at 2.5%, 5%, and 10% treated in parallel. Sloughing of germ cells from Sertoli cells was calculated. Transmission electron microscopy (TEM), Immunofluorescence, qRT-PCR, and western blot methods were employed. The drug-containing serum of WZYZW contained schisandrin, hyperoside, geniposidic acid, ellagic acid, and quercetin. Using TEM assay, we observed restoration of the desmosomelike (Des), tight junctions (TJ), and basal ectoplasmic specialization (ES) structure following WZYZW treatment. WZYZW caused inhibition of peptidase and protease inhibitors (tissue inhibitor of metalloproteinase-1 (TIMP1), Serpina3n) by immunofluorescence analysis. Western blot and qRT-PCR analysis revealed that WZYZW was able to ameliorate the expressions of peptidase and protease inhibitors and cell adhesion factors, such as TAp73, TIMP1, Serpina3n, Desmocollin-3, N-cadherin, and Nectin-2. WZYZW-medicated serum could prevent the defect of cell-cell junctions between Sertoli-germ cells co-culture system in vitro by up-regulating the expression of TAp73.

THIN AND ULTRATHIN STRUCTURE OF ENVELOPES OF STEPHANOSTOMUM BACCATUM (TREMATODA: ACANTHOCOLPIDAE) METACERCARIAE IN YELLOWFIN SOLE, LIMANDA ASPERA.

The structure of the envelopes (capsule and cyst) surrounding metacercariae of Stephanostomum baccatum (Nicoll, 1907) in the second intermediate host, the yellowfin sole Limanda aspera (Pallas 1814), is examined with the methods of light and transmission electron microscopy. The cyst, presumably formed by secretions of the metacercarial tegument, consists of 2 layers: the outer, very thin layer of an electron-dense, finely granular substance and the inner layer composed of loose material of a moderate electron density that includes dense bodies varying in size, shape, and localization. The capsule, formed by the host's cells, is also organized into 2 distinct layers. The inner layer of the capsule is loose, consisting of evenly spaced debris of degenerated cells and lipid droplets with inclusions of intact macrophages between them. The outer layer of the capsule consists of parallel rows of cells arranged around the parasite, with fibroblasts and macrophages being dominant types and granulocytes and lymphocytes found in smaller numbers. Aggregations of collagen fibers are located in narrow spaces between the cells. The number of lipid droplets in the outer layer is significantly smaller than in the inner layer. The capsules formed around the examined trematodes have several structural features that distinguish them from those of S. baccatum and Stephanostomum sp. metacercariae recovered from other fishes of the family Pleuronectidae. The major morphological features of such capsules are the lack of epithelioid or giant multinucleated cells and the presence of numerous lipid droplets. Investigating the structural details of the envelopes surrounding metacercariae in trematodes, as well as other helminths, contributes to our scientific understanding of parasite biology, which can, in turn, have broader implications for understanding host-parasite interactions and evolutionary biology.

Deterministic Synthesis of a Two-Dimensional MAPbI3 Nanosheet and Twisted Structure with Moiré Superlattice.

The synthesis of extremely thin 2D halide perovskites and the exploration of their interlayer interactions have garnered significant attention in current research. A recent advancement we have made involves the development of a successful technique for generating ultrathin MAPbI3 nanosheets with controlled thickness and an exposed intrinsic surface. This innovative method relies on utilizing the Ruddlesden-Popper (RP) phase perovskite (BA2MAn-1PbnI3n+1) as a template. However, the precise reaction mechanism remains incompletely understood. In this work, we systematically examined the dynamic evolution of the phase conversion process, with a specific focus on the influence of inorganic slab (composed of [PbI6]4- octahedrons) numbers on regulating the thickness and quality of the resulting MAPbI3 nanosheets. Additionally, the atomic structure is directly visualized using the transmission electron microscopy (TEM) method, confirming its exceptional quality. To illustrate interfacial interactions in ultrathin structures, artificial moiré superlattices are constructed through a physical transfer approach, revealing multiple localized high-symmetry stacks within a distinctive square moiré pattern. These findings establish a novel framework for investigating the physics of interfacial interactions in ionic semiconducting crystals.

Development of Kopasanda Leaves Extract (Chromolaena odorata (L.)) Phytosome Using Solvent Evaporation Method.

Kopasanda (Chromolaena odorata (L.) R.M.King &H.Rob) or siam weed exhibited various pharmacological activities such as anticancer, antidiabetic, and wound healing activities. The phenolic content of kopasanda leaf extract was high in the range of 56.15 mg GAE/g-242.3 mg GAE/g. But, it reported that phenolic compounds exhibited poor bioavailability because of their physicochemical properties. The phytosomes system improves the effectiveness of phytoconstituents. Aims of the research as prepare and evaluate the phytosome from kopasanda leaf extract. Kopasanda dried leaves were extracted by the sonication method. The solvent evaporation method was used in the phytosome preparation with various concentrations between extract and phospholipid ( 2:1; 1:1; 1:2; and 1:3). Furthermore, phytosome formation was analyzed for its entrapment efficiency, Polydispersity Index (PDI), particle size, spectroscopy infra-red (IR), and Transmission Electron Microscope (TEM) method. The total phenolic content (TPC) of crude was 110.969 ± 0.752 mgGAE/g. The optimum phytosome was gained with a concentration between extract and phospholipid (1:3). It resulted in the entrapment efficiency of 99.930 ± 0.001%, particle size, and polydispersity index equal to 206.5 ± 8.613nm and 0.528 ± 0.038. The morphology of the phytosome was spherical and the phytosome formation was verified by the IR spectrum by comparing the phytosome and the physical mixture of extract and phospholipid. The results obtained showed that phytosome containing kopasanda leaf extract was formed using the solvent evaporation method.

Structural Study on the Novel Plasmonic Optical Materials with Copper Selenide Nanoparticles

Background: Semiconductor-doped materials have been treated actively throughout the last decades and continue to be of great interest because of the challenges of the features due to various nanosize effects. Among other semiconductors, copper chalcogenides demonstrate the interesting plasmonic properties in line with quantum confinement effects provided by the size factor. Objective: This study aims to study the structural and optical features of the sol-gel-derived silica glasses with copper selenide nanoparticles, demonstrating the appearance of the plasmonic light absorption in the near IR range. Method: The samples under study were fabricated through an original sol-gel technique, which realized the simultaneous synthesis of copper selenide and sintering of mesoporous silica. The copper selenide glasses were characterized with X-Ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and optical absorption spectroscopy. Results: Formation of nanocrystalline Cu2-xSe particles of the size range from 10 nm through 100-150 nm is established with XRD and TEM techniques. The principal optical properties are presented by the featured absorption in the visible and near-IR ranges. Eg was evaluated for the direct transitions in the range of 2.10-2.36 eV. The plasmonic resonance in the nanoparticles due to increased carrier concentration originated by intrinsic deficiency of Cu2-xSe nanoparticles with variable stoichiometry. Its energy can be controlled by the Cu/Se ratio in the synthesis procedure. Conclusion: The silica sol-gel glasses with copper selenide nanoparticles were fabricated and characterized by XRD and TEM methods, and their optical absorbance spectra were investigated. The principal optical properties are presented by the featured absorption in the visible and near-IR ranges: the steplike proper absorption of the semiconductor particles characterized by Eg and the intense near-IR band is associated with the localized plasmonic resonance in the nanoparticles due to increased carrier concentration.

Capsaicin mitigates ventilator-induced lung injury by suppressing ferroptosis and maintaining mitochondrial redox homeostasis through SIRT3-dependent mechanisms

BackgroundVentilator-induced lung injury (VILI) is one of the severe complications in the clinic concerning mechanical ventilation (MV). Capsaicin (CAP) has anti-inflammatory and inhibitory effects on oxidative stress, which is a significant element causing cellular ferroptosis. Nevertheless, the specific role and potential mechanistic pathways through which CAP modulates ferroptosis in VILI remain elusive.MethodsVILI was established in vivo, and the pulmonary epithelial cell injury model induced by circulation stretching (CS) was established in vitro. Both mice and cells were pretreated with CAP. Transmission electron microscopy, ELISA, Western blot, immunofluorescence, RT-PCR, fluorescent probes, and other experimental methods were used to clarify the relationship between iron death and VILI in alveolar epithelial cells, and whether capsaicin alleviates VILI by inhibiting iron death and its specific mechanism.ResultsFerroptosis was involved in VILI by utilizing in vivo models. CAP inhibited ferroptosis and alleviated VILI's lung damage and inflammation, and this protective effect of CAP was dependent on maintaining mitochondrial redox system through SITR3 signaling. In the CS-caused lung epithelial cell injury models, CAP reduced pathological CS-caused ferroptosis and cell injury. Knockdown SIRT3 reversed the role of CAP on the maintaining mitochondria dysfunction under pathological CS and eliminated its subsequent advantageous impacts for ferroptosis against overstretching cells.ConclusionThe outcomes showed that CAP alleviated ferroptosis in VILI via improving the activity of SITR3 to suppressing mitochondrial oxidative damage and maintaining mitochondrial redox homeostasis, illustrating its possibility as a novel therapeutic goal for VILI.Graphical

Physics of hardening of the rolling surface of rail head from hypereutectoid steel after operation

In Russia, with its extensive railway system, for more than 5 years, special-purpose rails of increased wear resistance and contact endu­rance of the DH400RK category were produced from steel with a carbon content >0.8 %. On the head rolling surface of differentially hardened long rails made of hypereutectoid steel after long-term operation, transmission electron microscopy methods revealed the morphological components of the structure: lamellar pearlite, fragmented pearlite, destroyed lamellar pearlite, globular pearlite, completely destroyed pearlite, subgrain structure. The contribution of hardening due to: lattice friction, solid solution hardening, pearlite hardening, incoherent cementite particles, grain boundaries and subboundaries, dislocation substructure and internal stress fields were quantified. A hierarchy of these mechanisms was made and it was noted that for the fillet surface of the rail head, the main hardening mechanism is hardening by incoherent particles, as well as mechanisms caused by internal long-range (local) stresses, internal shear stresses (“forests” of dislocations) and substructural hardening. For the rolling surface along the central axis of the rail head, the main role in hardening belongs to long-range stress fields (especially its elastic component), hardening by incoherent particles and substructural hardening. Taking into account the volume fractions of the morphological components and their yield strength, the additive yield strength on the head rolling surface in the center and on the fillet was determined: 7950 and 2218 MPa, respectively. The paper presents a physical interpretation of the difference in values of the additive yield strength on the rolling surface of the rail head in the center and on the fillet.

Morphology-dependent support effect of PdCu/alpha-Fe2O3 catalysts on Suzuki-Miyaura cross-coupling reaction

The palladium-catalyzed Suzuki-Miyaura cross-coupling (SMC) reaction has received worldwide attention as a powerful and convenient synthetic tool for the formation of biaryl compounds. However, these reactions are highly dependent on the activity and stable of catalysts. Herein, the support morphology-dependent catalytic performance of SMC reactions was investigated. The truncated hexagonal bipyramid (α-Fe2O3-O) and rod-shaped morphologies of alpha-Fe2O3 (α-Fe2O3-R) were used as support to prepare PdCu nanoparticles (NPs) catalysts by NaBH4 reduction method. For PdCu/α-Fe2O3-R catalysts, the smaller size of PdCu NPs and more low coordination Pd sites leading to its superior catalytic performance for SMC reactions. Furthermore, it can be easily recycled through centrifugation and reused several times without obvious loss on its catalytic performance. Identical location transmission electron microscopy method was used to investigate the structural evolution of PdCu/α-Fe2O3-R catalysts. The results found that its structure almost unchanged during the catalytic reaction.

In-Situ Liquid-Electrochemical X-Ray and Electron Microscopy for Multi-Modal Energy Materials Characterization

In-situ liquid cell electron and x-ray microscopy have enabled dynamic studies of electrochemical reactions in energy materials and revealed relationships between the performance, structure, and chemical composition of these material systems. Such fundamental relationships are critical to improving the performance of batteries, catalysts, and other energy materials. Growing research interest in energy materials systems has accelerated the development of in-situ liquid-electrochemical microscopy techniques into mature and robust characterization workflows using novel and versatile scientific hardware.Multiple characterization techniques or in-situ processing steps are often required to fully understand the mechanisms governing the behavior of energy materials for all relevant length scales and environmental conditions. A multi-modal workflow combining in-situ liquid-electrochemical transmission electron, X-ray synchrotron and scanning electron microscopy methods is presented. The breadth of research applications is discussed, including the study of chemical dynamics and structural changes to micron-scale LixFePO4 battery particles during lithium-ion insertion/extraction, electrocatalytic behavior of β-Co(OH)2 platelet particles, and electrochemical oxidation of copper nanoparticles under reductive electrolytic conditions. New insights into these materials systems provided by these experiments will directly inform the development of predictive models for material performance and guide improvement of material design and synthesis.New scientific hardware and method development has been critical to in-situ nano-scale liquid cell microscopy and spectroscopy of electrochemical systems. Therefore, best-practice hardware and method design and development for these in-situ liquid-electrochemical microscopy experiments are also discussed. The connections between potentiostat, holder, and on-chip leads must be carefully considered with respect to different ground potentials, and the incorporation of real bulk-scale reference electrodes in this hardware has yielded quantitatively higher fidelity data with less degradation from further electrochemical cycling. Heating the sample or illuminating with light during in-situ electrochemical data collection has begun to further expand the range of environmental conditions that can be incorporated into experiments.

Optimized EBSD-TEM method for the investigation of Al/Al2O3 interfacial orientation mismatch

The combined electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM) method has been commonly applied to investigate material interfaces, from the perspectives of orientation and atomic structure. However, the loose combination is inadequate to capture some slight deviation from the ideal mismatch of interface, which limits an in-depth understanding of the interface. In this study, the combined EBSD-TEM method was systematically optimized and applied to investigate Al-Al2O3 heterogeneous nucleation interface. In this optimized EBSD-TEM method, the cylindrical equidistant projection was employed to illustrate the orientation mismatch relationship instead of the widely used pole figure. Lattice planes and directions from two phases are systematically presented in one figure, which provides a thorough perspective to identify all the potential matching features within the interface, meanwhile ensures a precise guidance for TEM sampling and observation. Such guidance is crucial for interface investigations, thereby this optimized EBSD-TEM method has great potential to be widely applied. Complex interface configurations of Al-Al2O3 interfaces were revealed, including the tilting of Al phase low-indexed planes relative to the interface and the deviations of matched lattice direction pairs between two phases. The complex interface configurations urge further development in the theory of nucleation interface mismatch.

An Integrated Solution to FIB-Induced Hydride Artifacts in Pure Zirconium.

The preparation method of transmission electron microscopy (TEM) samples for pure zirconium was successfully executed using a focused ion beam (FIB) system. These samples unveiled artifact hydrides induced during the FIB sample preparation process, which resulted from stress damage, ion implantation, and ion irradiation. An innovative solution was proposed to effectively reduce the effect of artifact hydrides for FIB-prepared samples of hydrogen-sensitive materials, such as zirconium alloys. This development lays the groundwork for further research on the micro/nanostructures of zirconium alloys after ion irradiation, thereby facilitating the study of corrosion mechanisms and the prediction of service life for nuclear fuel cladding materials. Furthermore, the solution proposed in this study is also applicable to TEM sample preparation using FIB for other hydrogen-sensitive materials such as titanium, magnesium, and palladium.

STUDY OF THE COMBINED EFFECT OF POST-SYNTHETIC ALKALINE TREATMENT AND NICKEL MODIFICATION OF MFI ZEOLITE ON THE DYNAMICS OF ITS DEACTIVATION IN THE PROCESS OF REFINING STRAIGHT-RUN GASOLINE

To determine the combined effect of post-synthetic treatments on the catalytic properties of MFI type zeolite (other names ZSM-5 or pentasil) during the upgrading of straight-run gasoline fraction of oil, MFI zeolite was synthesized and on its basis a sample was obtained, treated with an alkaline solution, as well as a nickel-containing sample after alkaline treatment of the zeolite. Modification of zeolite powder treated with an alkaline solution with nanosized nickel powder was carried out by dry mechanical mixing of the original powders in a vibrating mill. The activity and dynamics of deactivation of the obtained zeolite catalysts during the upgrading of straight-run gasoline fraction of oil were studied. Along with determining the characteristics of the target reaction products - high-octane gasoline, an analysis of the resulting gaseous hydrocarbons was carried out and the amount of carbon compaction products was determined. It has been shown that post-synthetic treatments of zeolite have a positive effect on the qualitative composition and yield of catalysates and reduce the rate of deactivation of zeolite catalysts. Post-synthetic alkaline treatment of MFI zeolite significantly reduces its aromatizing and cracking activity, resulting in an increased yield of high-octane gasoline with improved environmental characteristics. The introduction of nickel nanopowder into alkali-treated zeolite further enhances this tendency. Carrying out post-synthetic treatments of zeolite increases the time of stable operation of the resulting zeolite systems in the process of upgrading straight-run gasoline and reduces the amount of carbon compaction products formed. The state, location and dimensions of the zeolite carrier, nickel particles and carbon compaction products were determined using the transmission electron microscopy method. It has been shown that oxidative regeneration of a carbonized catalyst makes it possible to almost completely remove the resulting carbon deposits from the surface of both the active component and the zeolite support. For citation: Velichkina L.M., Gerasimov E.Yu., Vosmerikov A.V. Study of the combined effect of post-synthetic alkaline treatment and nickel modification of MFI zeolite on the dynamics of its deactivation in the process of refining straight-run gasoline. ChemChemTech [Izv. Vyssh. Uchebn. Zaved. Khim. Khim. Tekhnol.]. 2024. V. 67. N 8. P. 103-112. DOI: 10.6060/ivkkt.20246708.10t.

Application of Weak-Beam Dark-Field STEM for Dislocation Loop Analysis†.

Nanoscale dislocation loops formed by irradiation can significantly contribute to both irradiation hardening and embrittlement of materials when subjected to extreme nuclear reactor environments. This study explores the application of weak-beam dark-field (WBDF) scanning transmission electron microscopy (STEM) methods for quantitative irradiation-induced defect analysis in crystalline materials, with a specific focus on dislocation loop imaging and analysis. A high-purity Fe-5 wt% Cr model alloy was irradiated with 8 MeV Fe2+ ions at 450°C to a fluence of 8.8 × 1019 m-2, inducing dislocation loops for analysis. While transmission electron microscopy (TEM) has traditionally been the primary tool for dislocation imaging, recent advancements in STEM technology have reignited interest in using STEM for defect imaging. This study introduces and compares three WBDF STEM methods, demonstrating their effectiveness in suppressing background contrasts, isolating defect information for dislocation loop type classification, providing finer dislocation line images for small loop analysis, and presenting inside-outside contrast for identifying loop nature. Experimental findings indicate that WBDF STEM methods surpass traditional TEM approaches, yielding clearer and more detailed images of dislocation loops. The study concludes by discussing the potential applications of WBDF STEM techniques in defect analysis, emphasizing their adaptability across various material systems beyond nuclear materials.

Laser synthesis of oxide nanoparticles with controlled gas condensation

In this work, the oxide nanopowders of Al2O3, ZrO2, Y2O3, Gd2O3, CeO2, and SiO2 were synthesized by CW CO2 laser vaporization technique with controlled gas condensation in an inert atmosphere. Methods for controlling the size of the resulting nanoparticles by adjusting the gas composition and pressure during the vaporization process have been demonstrated. The potential for producing ultrasmall oxide nanoparticles with dimensions less than 5 nm has been shown. The size distribution of nanoparticles taken from different parts of the evaporation-condensation tract was studied using scanning (SEM) and transmission (TEM) electron microscopy methods. The effect of synthesis conditions (pressure and composition of the inert gas) on characteristics of the nanoparticles is discussed. Using a wide class of simple oxides as the example, it is shown that the powders synthesized by the laser method consist of three types of particles: target spherical particles with a diameter of 3–20 nm (more than 98%), larger spherical particles with a diameter of 50–200 nm, and shapeless large particles with sizes more than 200 nm. The possibility of separating large particles from the main particles using the original labyrinth system for gas pumping is shown. The obtained particles with controlled sizes can be effectively used in various applications, in particular, for the preparation of catalysts and adsorbents.