The critical need for effective uranium separation from complex aqueous solutions remains a central challenge in materials science today. Layered double hydroxides (LDHs) have emerged as promising uranium-absorbing materials. This study examines how different zinc-to-aluminum ratios (3,1, 2:1, and 1:1) affect both the structure and uranium(VI) absorption properties of Zn-Al LDHs. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), low-temperature N2 adsorption, and Zn K-edge extended X-ray adsorption fine structure (EXAFS) analyses revealed that while the crystal structure of the materials remained consistent, significant changes occurred in their porous and microstructures. EXAFS spectroscopy near the U L3-edge demonstrated that the dominant mechanism for U(VI) adsorption at pH 4.0 is inner-sphere complexation, involving negatively charged uranyl carbonate and hydroxyl complexes. Increasing the degree of Al substitution for Zn led to a logical enhancement in sorption capacity, reaching a maximum value of 47.2 mg/g at the optimal Zn/Al ratio of 2/1. Further increase in the substitution degree resulted in a shift towards a mesoporous structure, accompanied by a decrease in specific surface area and sorption capacity. Our findings demonstrate the potential of Zn-Al LDHs for U(VI) removal and provide a fundamental basis for future research aimed at developing more effective materials for the remediation of wastewater contaminated with hazardous radionuclides.
The article examines the synthesis and electrophysical properties of spinel ferrite ZnFe2O4, produced using the sol–gel method with a solid-state finishing process; as well as through classical ceramic technology with mechanochemical activation. The study includes a detailed analysis of the phase composition and crystalline structure using X-ray diffraction; infrared spectroscopy; mass spectrometry; and thermogravimetric and differential thermal analyses. These methods help identify thermal effects and the stages of synthesis. Impedance spectroscopy is used to investigate the electrophysical properties, revealing a significant influence of firing temperature on electrical ionic conductivity. The results show that the electrophysical properties differ based on the synthesis conditions and methods. This suggests potential applications for ZnFe2O4 as a cathode material in metal-ion batteries. The work highlights the importance of optimizing synthesis conditions to achieve high-performance characteristics in electrode materials.
The paper proposes an original one-stage method using spark plasma sintering technology (SPS) of manufacturing the ionizing radiation source (IRS) of closed type with a non-dispersible ceramic core based on pollucite obtained using aluminosilicate raw materials saturated (24.3 wt%) with cesium, and doped with 10-40 wt% CsCl. According to the XRD, EDX, AAS and DTA-TG data, optimal conditions for hydrothermal synthesis zeolite NaA were established, the consolidation kinetics and phase transformations into ceramic pollucite under SPS conditions were studied. The ceramics had a relative density of 99.8 % and mechanical strength up to 732 MPa, a low rate of cesium leaching 10-7 g/cm2 day and thermal resistance in air up to 1000 degrees C. It was confirmed by SEM and EDX that the destruction and deformation of pollucite ceramics in the composition with CsCl and steel at the boundary of their contact in the design of the IRS product was absent and diffusion of cesium outside the ceramics did not occur. The achieved cesium content in the ceramic core of the resulting the ionizing radiation source, which meets high quality and regulatory requirements, is 44.3 wt%. The results of the study may be promising for the manufacture of industrial products.
Composite sorbents based on Fe3O4 and Zn-Al-LDH with different weight ratios of magnetic and sorbing phases were obtained by the precipitation method. The optimal weight ratio of Zn/Fe was 16, which resulted in a 62
The dispersed Ca3La6(SiO4)6 biocomposite was obtained by treating a calcium silicate sol containing 0.1, 0.3, and 0.7 mol of La3+ under hydrothermal conditions. The composition, morphology, and structure of the biocomposite were studied by powder X-ray diffraction, SEM, and EDS methods. The reaction products (CaSiO3, CaLa4(SiO4)3O, Ca3La6(SiO4)6) depending on the La3+ concentration were determined. The structural characteristics of biocomposite powders with different La3+ contents were investigated by BET and DFT methods. The sorption characteristics of the materials towards 5-fluorouracil were studied depending on pH. The highest sorption capacity (0.768 mg/g at pH 3) was found for the Ca3La6(SiO4)6 sample containing 0.3 mol of La3+. Additionally, the biocompatible properties of biocomposite samples in contact with artificial blood plasma were evaluated by establishing the key changes in their composition, morphology, and structure upon the formation of the apatite bioactive phase on the accessible surface of the samples. These results hold promise for further development of new sorption materials, including biomaterials, for targeted drug delivery with a potential for practical application.
Zeolites have become promising adsorbents for wastewater treatment due to their enhanced adsorption capacity, stability of crystalline structure, high porosity and surface area. One of the primary goals of our study was to assess the effectiveness of employing NaY zeolite as a sorbent and potential solid matrix for immobilizing radionuclides. In this study NaY faujasite zeolite was obtained by hydrothermal synthesis and characterized by X Ray diffraction (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) methods. The prepared zeolite had NaY faujasite crystalline structure, characterized by developed surface area (370 m2/g) with micro-mesoporous structure, and spherical-like morphology with particles of 1-4 mu m in diameter. The isotherms adsorption modeling on Cs+, Sr2+, Co2+, Pb2+ and La3+ ions was performed. The isotherm well described by Langmuir equation with maximum adsorption capacity of q(Cs+) = 1,9 mmol/g, q(Sr2+) = 3,75 mmol/g, q(Co2+) = 1,82 mmol/g, q(Pb2+) = 2,54 mmol/g, q(La3+) = 3,83 mmol/g. Thermal behavior of metal-saturated adsorbents by differential thermal analysis (DTA) and thermal gravimetric (TG) techniques was studied. Each metal examined in this paper is responsible for the stable formation of radionuclides (137Cs, 90Sr, 60Co, La generally, the group of active lanthanides was modelled, Pb uranium fission residues) that are generated during the operation of nuclear power plants. To optimize sintering regimes, it has been proposed to achieve sorption saturation of stable ions such as Cs, Sr, Co, La, and Pb and transfer them into solid matrices. It was shown that the consolidation temperature for the obtained samples varies in the range of 935-1040 degrees C.
В статье представлены результаты изучения керамики культуры вальдивия и комплекса Сан-Педро с археологического памятника Реаль-Альто (Юго-Западный Эквадор). Исследованная в 2022 г. тестовая коллекция включает фрагменты сосудов двух морфолого-функциональных групп, относящихся к первым двум фазам культуры вальдивия (чаши и горшковидные сосуды), и керамики Сан-Педро (сосуды с горловиной и чаша). Сравнительный анализ проводился на основе выявленных технико-технологических признаков, соответствующих определенным стадиям производства посуды. Некоторые различия прослежены в составе пластичного сырья для формовочных масс и в технологии формовки изделий. Существенная разница выявлена в технологии обработки поверхности и орнаментации керамических сосудов. Это проявляется в использовании окрашенных или неокрашенных покрытий, применении качественного сплошного либо матового полосчатого лощения, нанесении разного по уровню сложности орнамента. Определены как отличительные особенности обжига посуды (вероятное применение разных теплотехнических устройств, различия в атмосферных режимах), так и черты сходства (приблизительно одинаковые температурные режимы). Выявлены различия технологического характера между двумя морфолого-функциональными группами керамики вальдивии: представленная чашами демонстрирует признаки использования более сложных и трудоемких приемов; группа горшковидных сосудов по технологическому уровню имеет определенное сходство с керамикой Сан-Педро. Полученные радиоуглеродные даты (4 640-4 450 л.н.) позволяют говорить об одновременности существования двух гончарных традиций. Различия технико-технологических характеристик керамики, вероятно, отражают культурную специфику носителей этих традиций.
This article unveils EMICA, a Python-based software tool revolutionizing electron microscopy image processing for amorphous alloys. EMICA addresses the unique challenges posed by these materials, which lack long-range order, by providing specialized capabilities for cluster analysis and spatial pattern recognition. This research explored software tool development and application through illustrative examples, answering the key question of how they enhance amorphous alloy analysis. By integrating advanced image processing techniques and algorithms, EMICA uncovers hidden patterns, offering quantitative insights into cluster distributions. The key message emphasizes the application's transformative impact on material science research, providing a specialized solution for electron microscopy image analysis in the amorphous alloy domain. Our key findings, presented through real-world examples and case studies, attest to the efficacy of the software in revealing nuanced details of amorphous alloy structures. From identifying subtle variations in atomic configurations to quantifying cluster distributions, EMICA represents a significant leap forward in the field of advanced electron microscopy image processing, contributing significantly to the advancement of this domain.
The use of ceramics as matrices for immobilization of radionuclides for the purpose of their safe long-term disposal or useful application is studied with an emphasis placed on phase stability, structural integrity, hydrolytic stability, etc. This work implements a combined approach based on the sol–gel citrate synthesis of nanosized La2Ti2O7 powder and its subsequent spark plasma sintering to produce dense ceramics. The phase composition and structure of the nanosized La2Ti2O7 powder and the ceramic samples obtained in the temperature range of 900–1300°C were studied by powder X-ray diffraction and SEM. It was shown that the conditions of synthesis of the powder ensure the formation of nanosized crystalline La2Ti2O7 grains, consolidation of which under spark plasma heating is accompanied by a change in the phase composition of La2Ti2O7 from a single-phase monoclinic structure to orthorhombic structure with a LaTiO3 impurity at temperatures above 1200°C. It was found that a change in the ceramic structure is accompanied by the formation of non-porous and defect-free monolithic samples. This type of change was shown to lead to an increase in the relative density (81.3–95.7
In this work, the products of the interaction of polyvinylsilsesquioxane (PVS) and polyvinyl-polydimethylsiloxane with tris(3-chlorosulfenyl-2,4-pentanedionate) aluminum were studied. The substances were isolated through the gelation stage, and after drying, insoluble crosslinked polymers are formed. Using data from thermogravimetry (TGA), diffractometry and positron annihilation spectroscopy (PAS), the structure and composition were investigated for the first time obtained polyaluminoorganylsiloxanes. The diffractometry data demonstrated that the obtained metallochelates are spatial mesomorphic polymers with a fractal structure. Based on the calculated data of the PAS, it is shown that the annihilation of positronium in the polymer matrix occurs on oxygen, while the size of the resulting fractal turns out to be less than the molecular volume of the elementary link. The results of the thermogravimetric study indicate a greater thermal stability of aluminum compounds compared to the chromium derivatives described earlier. According to scanning electron microscopy (SEM), it was found that the surface of the formed metallochelates corresponds to the characteristic monolithic morphology of xerogels.
The work is devoted to the study of the structural and sorption properties of metal exchangers obtained under conditions of extraction by hydrochloric acid (1:2) of the product of interaction of tris(3-chlorosulfenyl)-2,4-aluminum pentanedionate with vinyl trichlorosilane. The reaction was considered using two organic solvents – chloroform and toluene. A comparison of diffractometric parameters, elemental analysis, NMR spectra, thermogravimetric curves, as well as surfaces (SEM) and internal structure of isolated substances was presented. The capacity of the products with respect to Fe³⁺ is on the order of 7.1 mg·eq/g.
We have studied general trends in the formation of nanostructured sodium aluminosilicates with a Si/Al ratio from 1 to 5 in a multicomponent aqueous system. Data are presented on the elemental composition, morphology, and thermal behavior of the synthesized compounds and their Cs + sorption performance under static conditions. The results demonstrate that the sorption capacity of the sodium aluminosilicates (89.3–328.2 mg/g) exceeds that of some reported sorbents, which opens up the possibility of employing such aluminosilicates for Cs + removal from aqueous solutions.
A mesoporous adsorbent based on calcium silicate CaSiO3 for the removal and immobilization of cobalt Co-60 radionuclides in durable ceramic CaCoSi2O6 matrices was synthesized by hydrothermal conversion of boric acid production waste. The obtained material had a high Co2+ ions adsorption capacity of 220.8 mg/g. Cobalt adsorption was carried out mainly by ion exchange, which led to the formation of CaCoSi2O6 precursor ceramic matrices. The use of spark plasma sintering (SPS) technology at an optimal temperature of 1000 degrees C allowed the safe immobilization of Co2+ ions in CaCoSi2O6 ceramic matrices characterized by density (3.33 g/cm(3)), compressive strength (481 MPa) and microhardness (similar to 9.81 GPa). Sintered CaCoSi2O6 ceramic samples were characterized by high hydrolytic stability (cobalt leaching rate R-Co similar to 10(-7) g/(cm(2) x day)) and complied with the requirements for cured highly active waste GOST R 50926 96/ANSI/ANS 16.1.
A novel method for obtaining the MAX phase Ti2AlC from TiC, Al4C3, and Ti precursors has been demonstrated, involving activation of the mixture in a high-energy ball mill (HEBM) followed by Spark Plasma Sintering (SPS). The phase composition, mechanical characteristics, surface microstructure, and electrochemical behavior in neutral media (0.1 M Na2SO4) of heterogeneous composite ceramic materials TiC/Ti2AlC were studied as a function of sintering temperature (1200-1400 degrees C). SPS at 1200 degrees C yields materials with a relative density of 94.42 % and Ti2AlC mass content up to 57 %. These composite materials exhibit capacitive behavior according to cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) data, with a capacitance of 73 mF/g, suggesting their potential application as lead-free ceramic capacitors. Further increase in sintering temperature (1300-1400 degrees C) leads to increased electrical resistance and enhanced sample homogeneity.
In this work the method of obtaining composite ceramics based on perovskite and pyrochlore of compositions YxZrxSr1-3xTiO3 (x = 0.1, x = 0.2, x = 0.3) and Y2(ZrxTi)2O7 (x = 1) using the technology of reactive spark plasma sintering has been investigated. A comprehensive study of phase transformations, structure formation and physical and mechanical characteristics of ceramics depending on the ratio of Sr2+/Y3+/Zr4+ has been carried out by XRD, SEM, EDS and “diffraction movie” methods at the synchrotron radiation source. High hydrolytic stability of ceramics is proved and the mechanism of low leaching rate of Sr2+ < 10–7 g cm−2 day, Y3+ and Zr4+ < 10–5 g cm−2 day is described, which corresponds to GOST R 50926-96 and ANSI/ANS 16.1. The results of the work are promising for conditioning of radioactive waste and production of radioisotope products.
The interaction of polyvinylsilsesquioxane (PVS) and polyvinyl,-polydimethylsiloxane with tris (3-chlorosulfenyl-2,4-pentanedionate) chromium was investigated. During the reaction, gels were obtained, after drying of which dark purple substances were isolated. The composition and structure of these substances were studied for the first time using thermogravimetry, diffractometry and positron annihilation spectroscopy (PAS). The densities of metallochelate polymers were found pycnometrically, and according to diffractometry data, it was revealed that the connection products are spatial reticular mesomorphic polymers with a fractal structure. Using the PAS data, it was concluded that there is a direct correlation between the volume of the positronium trap and the coherent scattering region (CSR) determined using X-ray diffraction. Based on the regular decrease in the interplane distance when introducing a chromium atom into the silsesquioxane chain, it was found that the synthesized polymetallorganosiloxanes have a different structure in comparison with typical representatives of this class of compounds. For a product with polyvinylsiloxane, enlarged SEM images were obtained and the morphology of the initially formed gel and dried solid powder was described.
In this study, we explored the atomic structure and orderliness of amorphous alloys through advanced electron microscopy and analytical techniques. Amorphous alloys, characterized by disordered atomic structures, exhibit promising applications in technology. The research addresses a crucial knowledge gap by investigating cluster distribution, particle arrangement, and orderliness within the amorphous matrix. High-resolution electron microscopy (HREM) images are analyzed using diverse algorithms and software tools. The study establishes a correlation between angles approaching 180 degrees and increased orderliness within clusters, highlighting the reliability of angle distribution analysis. Robust indicators, including Div (SP(B/V)) and Div (Mu(B/V)) metrics, assess and compare amorphous alloy samples. Kullback-Leibler (K-L) divergence indicates the significance of cluster ordering, validated by the S-K test. Radial Distribution Function (RDF) analysis uncovers local short-range order, deepening understanding despite limited orderliness discernment. These findings not only enhance our understanding of metallic glasses or amorphous alloys but also offer opportunities for tailored design and improved applications across various technological domains.
Abstract—Layered double zinc and aluminum hydroxide modified with hexacyanoferrate(II) ions was synthesized for the first time by reverse deposition. The obtained samples were studied by X-ray phase analysis, scanning electron microscopy, and low-temperature nitrogen adsorption, and their sorption characteristics with respect to uranium U(VI) were studied. The sorption capacity for the modified material under static conditions, determined by the Langmuir equation, was q_max^ l = 156.70 ± 12.38 mg/g (at phase ratio V/m = 1000 mL/g, in a monocomponent solution of uranyl nitrate UO2(NO3)2 at a temperature T = 25°C and sorption time t = 24 h). Layered double zinc and aluminum hydroxide modified with hexacyanoferrate(II) ions is a promising sorbent for purification of liquid media from uranium U(VI) due to its high capacity and specific surface area, the possibility of effective use in a wide range of pH [4, 10], and low cost.
The water pollution with Cs+ and Sr2+ radionuclides in the nuclear fuel cycle is a pressing environmental problem. The selective adsorption of radionuclides onto inorganic sorbents of zeolite structure, exhibiting the ion-sieve effect, is a promising procedure for the treatment of the liquid radioactive waste formed. Titanosilicate of the CST structural type, corresponding to the formula Na1.64H0.36Ti2O3SiO4(H2O)1.84, was prepared by hydrothermal synthesis performed at 190°С and a pressure of 1.3 MPa for 24 h. This sorbent allows efficient removal of the Cs+ and Sr2+ cations from liquid media. The sorption exchange capacity qeq is 1.58 mg-equiv/g for Cs+ and 2.56 mg-equiv/g for Sr2+. Preliminary oxidation of Ti3+ to Ti4+ with H2O2 increases the sorption capacity for Cs+ and Sr2+. The phase composition, elemental composition, specific surface area, and pore size of the materials synthesized were determined. The titanosilicates obtained can be used as sorbents for liquid radioactive waste treatment.