Search Results (434)

The mechanosynthesis by dry-milling and characterization of layered double hydroxides (LDH) containing Zn²⁺ in the layer and Cl⁻ as interlayer anion has been investigated. The solids were synthesized by mechanosynthesis, by means of a dry-milling method using a planetary mill. This kind of synthesis is totally ecological as the stoichiometric amounts of reactants have been used to obtain the original solids, so, there was no need for washing or calcination thus avoiding water or atmospheric contamination. To compare results and prove that Cl⁻ is the interlayer anion, a carbonate-LDH has been synthesized by the coprecipitation method. Original solids were calcined at 450 °C to obtain the oxides. Samples were fully characterized and used as catalysts in the paracetamol photodegradation to test the usefulness of these ecologically obtained solids as decontaminants. An assortment of techniques, such as XRD, FT-IR, TG-DTA, and N₂ adsorption–desorption isotherms, has been utilized to prove the goodness of the dry-mill method applied. The X-ray diffraction data and the FT-IR and thermal results confirmed that the samples synthesized were hydrotalcites with the Cl⁻ as the interlayer anion. The paracetamol photodegradation tests indicated that the dry milling procedure enhances the reaction. Full article

Photochromic molecules, capable of reversible isomerization under specific light irradiation, are pivotal for developing advanced photo-responsive materials. Azobenzene derivatives, in particular, are renowned for their significant conformational change, excellent reversibility, and high photostability. This study presents a novel cyclic diazo compound (CDTA) comprising two azobenzene units connected via flexible glycol chains. The photo-responsive behavior of CDTA doped into the liquid crystal 4-cyano-4′-octylbiphenyl (8CB) was systematically investigated. The composite exhibits a pronounced photo-induced phase transition from a liquid crystalline to an isotropic state under 365 nm UV irradiation, accompanied by a reversible change in light transmittance. The response kinetics were found to be highly dependent on temperature and dopant concentration. At 35 °C, the UV response time was accelerated to 6.8 s, attributed to the transition of the host 8CB from a smectic to a nematic phase. Furthermore, the composite demonstrated dual responsiveness: optical switching under UV light and electrical switching under an applied field in its nematic state. This work elucidates the interaction between molecular structure and photo-response in a liquid crystalline matrix, offering insights for designing next-generation smart windows and adaptive optical devices. Full article

A comparative study on the effects of mechanical treatment by high-energy ball milling on talc (2:1 layered silicate) and kaolinite (1:1 layer silicate) was performed. Industrial samples of talc and kaolin were characterized by XRF, thermal analysis (DTA and TG), and XRD methods. The XRD analysis evidenced the destruction of the crystalline structures of both talc and kaolinite and accessory minerals in the samples, showing an increase in the amorphous phases and a progressive change to a more disordered structure. It was found that high-energy ball milling resulted in a reduction of 48% of talc at 4 h of grinding, and the reduction increased up to ~80% at 32 h. The mechanical treatment produced a decrease in initial kaolinite content by 25% after 4 h of grinding and a reduction of ~70% after 32 h. It was deduced by this analysis that the structure of kaolinite is more difficult to destroy by high-energy ball milling than the structure of talc under the same experimental milling conditions. The structural alterations in talc and kaolinite were anisotropic, with crystal degradation along [00l], and there was a progressive loss of long-range order; moreover, the crystal dimensions following the c-axis direction became too small to produce coherent diffraction. A decrease in crystal size (coherent diffraction microdomain) was observed by the mechanical treatment, with an increase in microstrains produced by high-energy ball milling. Thus, the crystal size decreased from 280 to 200 Å in talc (direction perpendicular to 002) and from 250 to 210 Å in kaolinite (direction perpendicular to 001) after 16 h of grinding, with an important reduction in crystal size up to a value of 138 Å but only in the case of kaolinite at 80 h of grinding, with talc completely amorphous to X-rays at the same grinding time. Microstrains followed an inverse evolution compared to the crystal size, with an increase in the values obtained by progressive grinding in both talc and kaolinite. The values of microstrains were found to be of the same order for talc and kaolinite, although they were relatively higher for talc since it is associated with a greater degree of structural alteration than kaolinite. The XRD results showed an inverse correlation between both parameters, with their relative values being higher for talc compared with kaolinite. The present study is of basic interest for further investigations into the effects of high-energy ball milling using talc and kaolin as raw materials with reduced particle size, for instance, in the ceramic and paper industries. Full article

The study investigates the catalytic activity of vanadium-containing catalysts in the selective oxidation of 4-methylpyridine (4-MP) in the gas phase. V-Cr, V-Ti, and V-Ti-Cr catalysts were synthesised and studied. The phase composition and structural features of the catalysts were determined by X-ray diffraction (XRD) and Raman spectroscopy, and their thermal stability was investigated using thermogravimetric analysis (TGA/DTA). Textural characteristics were evaluated by low-temperature nitrogen adsorption–desorption (BET, BJH), surface morphology was studied using scanning electron microscopy (SEM), and the distribution of elements was investigated using energy-dispersive X-ray spectroscopy (EDX). The chemical composition of the catalysts was determined using inductively coupled plasma atomic emission spectrometry (ICP-OES) and catalytic activity was evaluated in the selective gas-phase oxidation reaction of 4-methylpyridine in the temperature range 280–380 °C. It was found that an increase in temperature is accompanied by an increase in the conversion of 4-methylpyridine, but at the same time, deep oxidation reactions intensify. The best result is achieved on the V-Ti-Cr catalyst, for which the conversion of 4-MP reaches 86.88% and the selectivity is 73.06% at 320 °C. However, V-Ti provides moderate stable performance, while V-Cr demonstrates relatively low efficiency. Thus, it can be concluded that the nature of the temperature dependence of 4-methylpyridine conversion reflects the different nature of the active centres and their stability. Full article

Maize is a globally significant cereal crop, while Albic soils in Northeast China are characterized by low available phosphorus (P), poor humus (HS) quality, and constrained maize yield. The synergistic effects of P fertilization on maize yield and HS quality in these soils remain poorly understood. This three-year field experiment was conducted to determine the optimal P application rate for concurrently enhancing crop productivity and HS quality. Four P application rates were established: 0 kg P₂O₅ ha⁻¹ (no P application, P0), 40 kg P₂O₅ ha⁻¹ (low P application, LP), 80 kg P₂O₅ ha⁻¹ (moderate P application, MP), and 120 kg P₂O₅ ha⁻¹ (high P application, HP). Soil nutrients status, HS fractions, dissolved organic matter (DOM) fluorescence characteristics, and structural properties of humic acid (HA) were systematically analyzed following standard analytical procedures. Principal component analysis (PCA) and Pearson correlation analysis were integrated to facilitate comprehensive data interpretation. Results indicated that the MP treatment achieved the highest maize yield (12,257.1 kg ha⁻¹) and soil organic matter (SOM, 14.8 g kg⁻¹) content, with no further yield improvement observed under HP. The MP treatment significantly increased DOM carbon content (C_DOM, 0.350 mg L⁻¹) and its humification index (HIX, 6.80), promoting the transformation of labile DOM into stable HS. HA under MP treatment exhibited enhanced structural stability, as evidenced by a lower H/C ratio (1.72), a higher O/C ratio (0.880), and a reduced E₄/E₆ ratio, reflecting increased aromatic condensation and a greater abundance of oxygen-containing functional groups. Fourier transform infrared (FTIR) spectroscopy and differential thermal analysis (DTA) confirmed that MP improved the structural complexity and thermal stability of HA. In contrast, P0 and LP restricted nutrient availability and HS formation, whereas HP induced soil acidification (pH 5.68) and disrupted HS equilibrium. Principal component analysis (PCA) and correlation analysis revealed significant positive associations between the MP treatment and SOM, C_DOM, and maize yield. This implied that moderate P input promoted stable soil organic carbon accumulation and nutrient availability, synergistically enhancing maize productivity—consistent with the study’s core goal of optimizing P management for concurrent yield and HS quality improvement in Albic soils. Accordingly, this study concluded that moderate P application (80 kg P₂O₅ ha⁻¹) was optimal for Albic soils, synergistically enhancing both maize productivity and HS quality. These findings provided theoretical support for precise P management in sustainable agricultural systems within the Albic soil regions of Northeast China. Full article

A microwave–hydrothermal (M-H) method was developed for synthesizing barium silicate from solutions of barium salts and sodium silicate. Advanced techniques (DTA, XRD, IR spectroscopy, SEM and TEM) were used to study the optical, granulometric, electrical and other functional characteristics of barium silicate. BaSiO₃ synthesized at 100 °C is an amorphous nano-sized powder (10–20 nm); however, the product synthesized at 240 °C has a crystalline structure (20–27 nm), whereas the crystalline phase of BaSiO₃ is typically obtained using known methods at temperatures above 400 °C (12–40 nm). During M-H synthesis, it was found that the structure formation mechanism and particle size of BaSiO₃ changed due to the peculiar features of microwave heating. The synthesized barium metasilicate exhibits a high diffuse reflectance coefficient of 92%. It is a wide-band-gap semiconductor with a band gap width of Eg = 4.1 eV. Both amorphous and crystalline phases of BaSiO₃ exhibit high photocatalytic activity in the UV range. This study shows that the developed M-H method enables the production of nano-sized powder and enhances the functional properties of barium silicate. Compared with conventional methods, the M-H method is more efficient due to reduced synthesis time and lower energy costs. Full article

Antimony nanomaterials are becoming increasingly important in advanced functional applications, including catalysis, sensing, optoelectronics, and energy systems, motivating the development of reliable synthetic routes capable of producing high-purity Sb at the nanoscale. This study establishes a direct Zn-mediated reduction pathway for converting SbCl₃ into elemental Sb using acetone, ethanol, and methanol as reaction media. SbCl₃ was first dissolved in each solvent, followed by controlled addition of Zn powder under mild heating (60 °C), magnetic stirring, and ultrasonic agitation. Acetone proved the most effective medium, achieving ~94% of the theoretical Sb yield, while suppressing the formation of the SbOCl intermediate observed in alcoholic solvents. Structural and compositional analyses using XRD and SEM/EDS confirmed the formation of a pure phase, nanocrystalline Sb with mean crystallite sizes of ~25 nm in acetone, ~27 nm in ethanol, and ~21 nm in methanol. TGA/DTA measurements from room temperature up to 800 °C revealed oxidative conversion to off-white antimony oxide under O₂ atmosphere and the formation of molten Sb droplets under N₂ atmosphere, consistent with the expected thermal transitions of high-purity Sb. Overall, the findings demonstrate that Zn-driven reduction of SbCl₃ in high-purity organic media provides an efficient and scalable approach for producing Sb nano-powders with solvent-dependent yields and nanoscale structural characteristics. Full article

This study investigates the sustainable reuse of industrial enamel frit production waste generated during enamel application processes and evaluates its potential from a process-oriented glass-forming and -shaping perspective. Enamel frit waste collected from an industrial production line in Türkiye was subjected to comprehensive characterization, including XRD, XRF, TG/DTA, dilatometry, and CIE Lab* color analysis, with the primary aim of assessing forming compatibility rather than final product performance. Following calcination and controlled fritting, the waste material was processed through mold-based glass-forming experiments using firing schedules derived from thermal analysis. The results reveal pronounced chemical and thermal heterogeneity among enamel frit production wastes, leading to variable melting behavior across samples. Nevertheless, selected waste compositions exhibited sufficient viscous flow for shaping at reduced firing temperatures of approximately 850 °C. This study demonstrates that selected enamel frit production wastes—obtained from industrial enameling processes in slurry, powder, or granular form—can be reshaped into glass forms under controlled low-temperature conditions. The novelty of this study lies in investigating industrial enamel production frit waste as a reusable material within a circular economy framework, specifically focusing on its application in mold-based glass forming for artistic and educational contexts, thereby fostering collaboration between industrial waste management and glass art practice. Full article

This study explores the influence of precursor nature on the structural and mechanical characteristics of hydroxyapatite–yttria partially stabilized zirconia (HAp–YSZ) nanocomposites designed for biomedical applications. Precursor powders for obtaining these ceramic composites were synthesized via wet coprecipitation, using different calcium phosphate precursors: dibasic and monobasic ammonium phosphates for hydroxyapatite, and zirconyl chloride with yttrium acetate for YSZ. The dried precipitated powders were thermally treated at 600 °C and 800 °C and characterized by X-ray diffraction (XRD), thermal analysis (DTA–TG), transmission electron microscopy (TEM), and BET surface area measurements. The nanocomposites containing 70–90 wt.% HAp and 10–30 wt.% YSZ were sintered between 1000 °C and 1400 °C. Microstructural and physical properties were evaluated using scanning electron microscopy (SEM), open porosity, and compressive strength testing. Results revealed that precursor type and calcination temperature strongly affected crystallinity, particle size, and phase composition, influencing both porosity and mechanical strength of the final materials. An optimal sintering temperature of approximately 1200 °C was identified, balancing densification and phase stability. The findings demonstrate that controlling precursor chemistry and heat treatment enables fine-tuning of nanocomposite structure and performance, supporting their potential as bioactive, mechanically enhanced ceramics for orthopedic implant applications. Full article

The possibility of transforming debris from a ceramic clinker into high quality foam granulate is discussed. The foaming process, which was carried out at temperatures 150–200 °C higher than the production process, was studied by HSM and DTA-TG coupled with MS. Phase and structural transformations were investigated by XRD and SEM, respectively. The results highlight that the foaming mechanism is related to the release of oxygen due to a reduction in Fe³⁺ to Fe²⁺ after the melting of hematite and the dissolution of pseudobrookite present in clinker waste. Granules obtained after 30 min of holding at 1280 °C are impermeable to water and, depending on the cooling applied, have a density between 0.4 and 0.7 g/cm³, porosity between 70 and 85 vol %, and compressive strength between 0.7 and 1.1 MPa. These results meet the requirements for high-quality fire-resistance lightweight aggregates. Full article

In this article, the thermal and mechanical properties of mortars reinforced with polypropylene (PP) fibres have been studied. Particularly, the effect of polypropylene fibres’ addition on the thermal behaviour of fine-grained building mortars at high temperatures was studied using simultaneous thermal analysis. Two types of polypropylene fibres, differing in shape and size, were used as fillers. The thermal behaviour of cement mortar samples with and without fibres was described. Special attention was given to the thermal behaviour of fibre-reinforced cement mortars subjected to the high temperatures of 100 °C, 200 °C, 300 °C, 400 °C, 500 °C, and 600 °C. Comparative studies using simultaneous thermal analysis (STA) were also performed for non-heated samples (20 °C). The TG, DTG, and DTA curves were analysed to investigate the effects related to the dehydration and the decomposition of hydration and carbonation products. Compared to mortar samples without fibres, the results showed that the presence of polypropylene fibres contributes to an increase in the thermal stability of the samples. It has been proven that the impact of the type and amount of PP fibres in the tested range (1.8 kg/m³ vs. 3.6 kg/m³) on the thermal stability of specimens of tested cement composites was found not to be significantly visible. Next, extensive research was performed on the impact of fire environmental exposure on the variability in the strength parameters of the mortars. Tensile strength tests were conducted based on the standards specified by the Polish Committee for Standardization. The research material consisted of high-strength, fine-grained building mortars, modified by an original method with polypropylene fibres at concentration of 1.8 kg/m³, 3.0 kg/m³, and 3.6 kg/m³. For reference, ordinary mortars without fibres were used, as well. Tensile strength was evaluated for mortar samples, which were exposed to temperatures of 100 °C, 200 °C, 300 °C, 400 °C, 500 °C, and 600 °C, respectively. Special attention was paid to the thermal behaviour of cement mortars reinforced with polypropylene (PP) fibres, subjected to high temperatures. Based on the obtained test results, a detailed statistical analysis was developed, along with comprehensive temperature–parameter relationships, which could enable an approximate post-failure assessment of the mortar’s condition. The main outcomes of this paper include optimal fibre dosage, which is 3.6 kg/m³, identified optimal fibre type, namely F fibre, as well as plateau in tensile strength for temperatures between 200 °C and 400 °C for fibre-reinforced samples. Full article

Background/Objectives: This study aimed to perform a comparative analysis of the original Viagra^® product and sildenafil-containing tablets obtained from illegal sources (the darknet). Specifically, the analyzed material consisted of samples seized by Polish law enforcement authorities from unverified vendors operating within the Central European darknet market. The study utilized thermal methods, specifically Thermogravimetry (TG), Derivative Thermogravimetry (DTG), and calculated Differential Thermal Analysis (c-DTA), as well as colorimetric analysis based on the International Commission on Illumination (CIE) L*a*b* system. Methods: Thermal analyses enabled the assessment of the thermal stability of the tested samples, identification of characteristic stages of thermal decomposition, and determination of differences in thermal behavior between the pure substance, the original preparation, and darknet samples. In turn, color measurements in the CIE L*a*b* space allowed for an objective comparison of tablet appearance and determination of the degree of color similarity to the original product. Results: The obtained results showed that only a few samples (V1, V3, V4, V6, V8) exhibited features similar to the original Viagra^®, both in terms of thermal profile and color. Most of the tested tablets were characterized by significant variability in physicochemical properties, indicating a lack of quality control and inconsistency in formulation. Samples V2 and V7 deviated particularly strongly—both thermally and visually—suggesting that they might not contain the original active substance or contained it in a different chemical form. Conclusions: The use of combined thermal and colorimetric methods proved to be an effective tool in the identification of counterfeit pharmaceutical products, enabling simultaneous evaluation of their composition and authenticity. The results confirm the validity of employing integrated physicochemical analyses for the detection of falsified medicines present on the illegal market. Full article

Cerium (Ce³⁺)-doped gadolinium orthoborate (GdBO₃) phosphor powders were synthesized via an aqueous sol–gel route, with systematic variation in solution pH (2, 5, and 8) and annealing temperature (600–1200 °C, in 100 °C increments) to investigate their influence on structural, optical, and scintillation properties. The materials were comprehensively characterized using thermogravimetric and differential thermal analysis (TG–DTA) to assess thermal behavior, X-ray diffraction (XRD) for crystal structure determination, Fourier-transform infrared spectroscopy (FTIR) for vibrational analysis, and both photoluminescence (PL) and radioluminescence (RL) spectroscopies to evaluate optical and scintillation performance. All samples crystallized in the hexagonal GdBO₃ vaterite phase (space group P6₃/mcm). The PL and RL emission spectra were consistent with the Ce³⁺ 5d–4f transitions, and scintillation yields under X-ray excitation were quantified relative to a standard Gadox phosphor. A decrease in photoluminescence quantum yield (PLQY) was observed at annealing temperatures above 800 °C, which is attributed to the incorporation of Ce³⁺ into the host lattice. Scintillation decay profiles were recorded, enabling extraction of timing kinetics parameters. Overall, the results reveal clear correlations between synthesis conditions, structural evolution, and luminescence behavior, providing a rational basis for the optimization of Ce³⁺-doped GdBO₃ phosphors for scintillation applications. Full article

To avoid dependence on conventional raw materials, global emphasis has been placed on obtaining alternative plant celluloses and the chemical synthesis of cellulose. The use of synthetically derived cellulose as a precursor for cellulose nitrates (NCs) is currently absent in global practice, which underscores the undoubted relevance of this research. Cellulose nitrate (NC) was synthesized in a 138% actual yield by nitration of synthetic cellulose (SC)—a new type of cellulose—prepared by electropolymerization from an aqueous glucose solution in the presence of catalytic tungsten–vanadium heteropolyacid of the 1–12 series with the chemical formula H₆[PW₁₀V₂O₄₀]: a nitrogen content of 11.83%, a viscosity of 198 mPa·s, a high solubility of 91% in an alcohol–ether solvent, and an ash content of 0.05%. SEM provided a general concept of the morphological structure of SC and SC-derived NC. The initial SC consisted of flat, curly fibers with a smooth surface approximately 10–20 μm wide, with no aggregation observed. The fibers of SC-derived NC had a cylindrical shape with a diameter of up to 25 μm and a rough surface. FT-IR spectroscopy revealed that SC and SC-derived NC have the main functional groups characteristic of classical cellulose (3346, 2901, 1644, 1429, 1162, and 1112 cm⁻¹) and nitrate esters of cellulose (1650, 1278, 832, 747, and 689 cm⁻¹), respectively. For the first time, a full-profile analysis discovered that SC is made up of the monoclinic phase of cellulose Iβ with an antiparallel chain arrangement. SC with a crystallinity index (CrI) of 81–86% was shown to undergo amorphization upon nitration, with the CrI declining to 17% and the crystallite sizes decreasing from 44 × 62 × 59 × 94 Å to 29 × 62 × 26 × 38 Å. Coupled TGA/DTA revealed that SC exhibits a high-temperature endothermic peak of decomposition of 374 °C, with a weight loss of 84%. The thermostable SC-derived NC exhibits a high onset temperature of intense decomposition of 200 °C and an exothermic peak of 208 °C, with a weight loss of 88%, and is characterized by a high specific heat of decomposition of 7.74 kJ/g. This study provides new insights into the functionalization of SC with a high degree of polymerization, expanding the classical concepts of cellulose nitration. Full article

This study demonstrates the complete transformation of almond shell waste into a high-performance carbon material for carbon paste electrode (CPE) fabrication. The biocarbon was synthesized via carbonization at 800 °C and subsequently activated with CO₂, resulting in a semicrystalline structure rich in carbonyl groups—consistent with its lignocellulosic origin (34.25% cellulose, 13.48% hemicellulose, 48.03% lignin). Carbonization increased the total pore volume of carbonized almond (CAR_ALD) by nearly 13-fold and the specific surface area by over two orders of magnitude compared to raw almond (RAW_ALD), while CO₂ activation further enhanced activated almond’s (ACT_ALD) surface area (~19%) and pore volume (~35%). To improve electrochemical performance, Bi₂O₃ doped with Sm was applied as a surface modifier. Comprehensive characterization (N₂ physisorption X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopic Analysis (FTIR), X-Ray Photoelectron Spectroscopic Analysis (XPS), Thermogravimetric and Differential Thermal Analysis (TG-DTA), Cyclic voltammetry (CV), Electrochemical impedance spectroscopy (EIS)) confirmed the material’s structural integrity, graphitic features, and successful modifier incorporation. Electrochemical testing revealed the highest current response (48 µA) for the CPE fabricated from CAR_ALD/Bi₂O₃-Sm, indicating superior electrocatalytic activity and reduced charge transfer resistance. Notably, this is the first report of a fully functional CPE working electrode fabricated entirely from waste material. Full article