Search Results (4,522)

This study investigates the preparation and performance of ultra-high-performance concrete (UHPC) incorporating manufactured sand as a full replacement for quartz sand. The mix design was optimized by integrating the compressible packing model (CPM) with an orthogonal experimental design. The influence of stone powder content in manufactured sand—0, 5, 10, and 15% by mass of fine aggregate—on fresh-state fluidity and 7d-mechanical properties was systematically evaluated. Hydration products and microstructural features were analyzed using X-ray diffraction (XRD), scanning electron microscope (SEM), and mercury intrusion porosimetry (MIP). Results show that the manufactured sand-based UHPC achieved a fresh-state fluidity of 185 mm and a 7-day compressive strength of 152.4 MPa. Both fluidity and compressive strength exhibited a unimodal trend with increasing stone powder content, reaching maxima at 10%. Microstructural analysis revealed intimate interfacial bonding between unhydrated particles and calcium silicate hydrate (C–S–H) gel; notably, the UHPC matrix with 10% stone powder displayed the densest microstructure. MIP results further demonstrated that an optimal stone powder content effectively reduced total porosity, with the lowest overall porosity and the highest volume fractions of harmless (≤20 nm) and less harmful (20–100 nm) pores observed at 10%. These microstructural refinements collectively underpin the superior mechanical performance of manufactured sand-based UHPC. Full article

Background/Objectives: Accurate determination of active pharmaceutical ingredient (API) particle size within dry powder inhaler (DPI) formulations is essential for ensuring effective pulmonary delivery but remains analytically challenging due to low API content and micronized particle size. Methods: In this study, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray microanalysis (EDX) was used to directly identify and calculate the API particle size within several different commercial DPI products fit for purpose under regulatory constraints. The method exploits unique elemental markers inherent to each API, enabling reliable discrimination from excipients without prior sample modification or API extraction. Results: Large-area SEM–EDX mapping was used to localize API particles, followed by high-magnification imaging and confirmatory spot microanalysis. Particle sizes were manually measured for at least 50 API particles per formulation using image analysis software, and particle size distribution parameters were calculated from equivalent spherical diameters. Conclusions: The methodology was successfully applied to Spiriva^®, Anoro^® Ellipta, and Relvar^® Ellipta inhalation powders, revealing micronized APIs with distinct morphological features and verifying systematic application across products. Cross-validation against laser diffraction measurements of pure APIs demonstrated statistical equivalence, confirming the robustness and analytical utility of the proposed method for particle size assessment in DPI formulations. Full article

The present study investigates the co-crystallization process of rivaroxaban (RIV), a poorly water-soluble potent oral anticoagulant, with niacinamide (NIA), a highly soluble and pharmaceutically acceptable co-crystal former, in two different molar ratios (1:1 and 1:2). The aim was to enhance the physicochemical and biopharmaceutical properties of rivaroxaban such as dissolution rate and aqueous solubility, by forming stable co-crystals through a solvent evaporation technique. The resulting co-crystals (RIV-NIA, 1:1 co-crystallization compound, F1 and RIV-NIA, 1:2 co-crystallization compound, F3) were characterized using scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD) and thermal analysis, which confirmed the formation of a new rivaroxaban–niacinamide co-crystalline phase. In vitro dissolution studies confirmed a significant enhancement in the dissolution rate of the two obtained co-crystals. These findings suggest that stoichiometric variation plays an important role in co-crystal performance and in improving solubility compared with the pure drug. Also, the obtained results suggest that niacinamide is an effective coformer for improving the dissolution and physicochemical properties of rivaroxaban. Full article

The purpose of this study is the exploration of the catalytic performance of a ZSM-5 zeolite produced from iron-rich fly ash, without any additional iron loading, in removing paracetamol via a heterogenous Fenton reaction. The structural and textural characterization by powder X-ray diffraction and N₂ adsorption isotherms showed that a pure ZSM-5 phase was synthesized, but lower crystallinity and textural parameters were obtained when compared with commercial ZSM-5. The XPS analysis revealed significant amounts of iron and yttrium, which enhanced the electronic properties of the samples’ surface when compared with iron-impregnated commercial ZSM-5. The catalytic reaction was followed through UV-spectroscopy and kinetic models were applied to the data; the best fit was obtained for a pseudo-first-order model. All fly ash-based zeolites showed increased paracetamol removal when compared with commercial iron-loaded ZSM-5, which may be attributed to the more disordered structure, able to accommodate large paracetamol species (dimers). On the other hand, the effect of yttrium on the electronic properties of iron sites may increase the ^●OH radical formation, thus increasing the paracetamol removal rate, despite the progressive drop on paracetamol removal upon regeneration–reuse cycles due to Fe leaching. Full article

Water-based drill cuttings generated during onshore natural gas development are complex solid wastes that may pose environmental risks if improperly managed. This study evaluates the feasibility of reutilizing water-based drill cuttings as pavement base materials after stabilization using a novel composite stabilizer composed of cement, stabilizer liquid agent, and water-reducing powder (CLP stabilizer). Mix proportion optimization was conducted through compaction and 7-day unconfined compressive strength tests, followed by evaluation of road performance, including strength, compressive rebound modulus, water stability, and temperature shrinkage, with stabilized powder stabilized soil as a control. Microstructural characteristics were analyzed using X-ray diffraction and scanning electron microscopy, and environmental safety was assessed through heavy metal leaching tests and background soil investigation. The results show that the optimal mixture ratio of curing agent (5% cement + 2% liquid stabilizer + 8% superplasticizer powder) satisfies the strength requirement for pre-drilling road bases, exhibiting superior performance compared to the control group. When the stabilizer dosage reaches 9%, the 7-day unconfined compressive strength achieves a maximum of 3.38 MPa, representing a 51% increase over the control group. At a stabilizer dosage of 12%, the splitting tensile strength reaches a peak value of 0.901 MPa, showing a 60.3% improvement. These results indicate enhanced deformation resistance, water stability, and reduced temperature shrinkage rates. Microstructural analysis indicates that the formation of calcium silicate hydrate (C-S-H) gel and ettringite (AFt phase) leads to a denser structure and enhanced durability. Heavy metal concentrations comply with relevant standards, demonstrating controllable environmental risks and supporting sustainable pavement base application. Full article

As an extremely toxic heavy metal, lead is difficult to be degraded in the environment, and its curing and disposal is a key challenge in environmental pollution control. In this study, supersulfated cement (SSC) prepared from phosphogypsum, granulated blast furnace slag powder, and slaked lime as raw materials was used as curing cementitious material, and the curing effect and curing mechanism of SSC on lead ions were investigated by adopting testing methods such as compressive strength, electrical resistivity, X-ray diffraction (XRD), scanning electron microscopy (SEM), heavy metal ion leaching toxicity analysis, and ion concentration analysis of pore solutions. The results show that with an increase in Pb²⁺ concentration, the compressive strength of the SSC-cured paste gradually decreased, the electrical resistivity was obviously reduced, and the generation of hydration products was inhibited. The microanalysis results show that the microstructure of the cured paste became loose, and the concentration of lead ions in the SSC leach solution gradually increased, but it was much lower than the limit value stipulated in Chinese standards. Full article

In this work, Fe, Co, Ni, Cu, and Mo powders were used as starting materials to prepare high-entropy alloy (HEA) thin films by a coating and vacuum sintering process. Using the HEA thin film as the substrate, selenium was subsequently deposited by chemical vapor deposition (CVD) to obtain high-entropy alloy selenide thin films (HEASe). The phase structure, surface chemical states, morphology, and elemental distribution of the porous films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS). The electrocatalytic hydrogen evolution performance of the electrodes was evaluated using a three-electrode configuration in 0.5 M H₂SO₄, 1 M KOH, 1 M KOH + 0.5 M NaCl, and 1 M KOH + 0.5 M Na₂S solutions. The results indicate that the HEA selenide thin-film electrodes exhibit favorable electrocatalytic behavior in all four electrolytes. Among them, HEASe-450 shows the best overall performance. In 0.5 M H₂SO₄, it requires an overpotential of only 57.6 mV to reach a current density of 10 mA cm⁻², with a Tafel slope of 146.96 mV dec⁻¹. In 1 M KOH, the overpotential at 10 mA cm⁻² is 50.1 mV, and the corresponding Tafel slope is 142 mV dec⁻¹. In 1 M KOH + 0.5 M NaCl, the overpotential is 52.7 mV with a Tafel slope of 122.72 mV dec⁻¹. In 1 M KOH + 0.5 M Na₂S, an overpotential of 85 mV is required, and the Tafel slope increases to 236 mV dec⁻¹. Full article

Cr-based composite coatings with superior wear resistance are in growing demand for high-performance applications in the automotive, aerospace, and general manufacturing sectors. In this study, an Al10Cu alloy produced via powder metallurgy was coated with a chromium/nanodiamond (Cr/ND) composite layer using an electrodeposition process to enhance its tribological performance. The coatings were characterized using scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray diffraction. The resulting Cr/ND layer exhibited a uniform thickness of 73.5–76.2 μm and markedly improved surface hardness (809.4 HV), representing a 15-fold increase over the uncoated alloy (53.6 HV). Pin-on-disk tribological testing under dry sliding conditions showed complete elimination of detectable mass loss (0.00 mg vs. 0.55 mg for uncoated) within the measurement system resolution, indicating excellent resistance to both abrasive and adhesive wear. XRD analysis revealed the formation of a hexagonal close-packed Cr₂H phase with incorporated nanodiamond particles. To capture and predict the temporal evolution of the friction coefficient, a customized dual-layer long short-term memory neural network—optimized with a look-back window of 3 timesteps and ReLU-activated dense layers—was implemented. The model achieved superior predictive performance on the coated system, with validation and test R² values of 0.9973 and 0.9965, respectively, demonstrating enhanced modeling accuracy for surface-engineered materials. These findings demonstrate a significant advancement in wear protection for aluminum alloys and introduce a robust data-driven approach for real-time friction prediction in engineered surfaces. Full article

In order to realize the large-scale resource utilization of solid waste in building materials, geopolymer mortar was prepared by alkali excitation technology with municipal solid waste incineration fly ash (MSWIFA), waste glass powder (WGP) and metakaolin (MK) as raw materials. After 28 days of curing, compressive strength and heavy metal leaching concentration of MSWIFA-WGP-MK geopolymer mortar were measured. The microstructure and phase composition of geopolymer samples were examined using scanning electron microscopy, energy-dispersive spectroscopy and X-ray diffraction analysis. The results demonstrated that the compressive strength of mortar increased as the MSWIFA content decreased and the alkali activator (AA) content increased. The mortar containing 30% MSWIFA and 35% AA achieved the highest 28-day compressive strength of 70.9 MPa. The high compressive strength was strongly associated with the compact microstructure, as revealed through scanning electron microscopy. The heavy metals in MSWIFA were solidified well in geopolymer matrix, and the leaching concentrations of heavy metals were below the regulatory thresholds. Based on the test results of mortars, concrete pavement bricks were produced. The performance of the optimized concrete paving brick satisfied requirements of the specification. The results indicated that the MSWIFA and WGP can be utilized in building materials. Full article

FeCrMnNi-based alloys, derived from the well-known Cantor high-entropy alloy, have attracted increasing attention due to their excellent strength–ductility balance. Additively manufactured FeCrMnNi variants are characterized by superior hardness compared to their conventionally processed counterparts. In the present study an optimized composition of the FeCrMnNi medium-entropy alloy was additively manufactured via laser-based powder bed fusion and subsequently subjected to systematic heat treatments. CALPHAD simulations were applied to select the specific composition and post-processing heat treatment conditions, where the latter aimed at promoting the evolution of a dual-phase microstructure. Experimental characterization included X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and electron backscatter diffraction, as well as Vickers hardness and tensile testing. A microstructure could be established dominated by a face-centered cubic (FCC) phase with minor fractions of a secondary phase in the non-treated condition. The evolution of an additional body-centered cubic (BCC) phase upon heat treatment at and above 700 °C was observed. The emerging BCC phase as well as increasing fractions of the secondary phase were accompanied by significantly increased hardness and strength, surpassing the literature values of similar compositions. However, a heat treatment at 1000 °C resulted in recrystallization and an increase in grain size, while the decreasing fraction of the secondary phase eventually led to a reduction in strength. These findings underscore the combined potential of composition optimization and targeted post-processing to enhance the mechanical performance of additively manufactured FeCrMnNi alloys. Full article

The fabrication of NiTiZr alloys by solid-state routes remains challenging due to limited atomic diffusion and the high reactivity of Ti and Zr. Mechanical alloying offers a potential pathway for synthesising such systems; however, complete alloy formation is not always achieved under practical milling conditions. Researchers have infrequently explored the mechanical alloying of NiTiZr, and this study systematically investigates the effect of milling time on microstructural evolution rather than claiming complete alloy synthesis. A high-energy planetary ball mill was used to mechanically process elemental powders of Ni, Ti, and Zr for 5–28 h. The examination revealed that longer milling times resulted in progressive crystallite refinement and increased lattice strain, while particle morphology evolved from irregular to more globular shapes due to repeated fracture and cold welding. After 28 h of milling, limited reacted regions containing Ni, Ti, and Zr were observed (~4.6% area fraction), while most of the powder remained heterogeneous and polyphasic, with no evidence of complete Ni₅₀Ti₃₀Zr₂₀ alloy formation. X-ray diffraction showed significant peak broadening without systematic 2θ peak shifts, indicating severe plastic deformation and crystallite refinement rather than definitive solid-solution formation of the allot. Differential scanning calorimetry revealed exothermic thermal events between 300 °C and 470 °C, which are attributed to defect recovery and thermally activated structural rearrangements rather than confirmed martensitic or crystallisation transformations. These results demonstrate that high-energy ball milling alone is effective for particle size reduction and defect generation but insufficient for producing a fully homogeneous Ni₅₀Ti₃₀Zr₂₀ alloy within 28 h. Additional activation energy, such as post-milling heat treatment or extended processing, is required to promote complete alloying in this system. Full article

The modification of road bitumen using micro-sized carbonaceous materials offers a promising route to enhance pavement performance; however, the influence of microdispersed coke derived from coal and petroleum sources has not been sufficiently clarified. In this study, coal and petroleum coke from Pavlodar Petrochemical Plant LLC (Pavlodar, Kazakhstan) were mechanochemically activated and used as the modifiers for BND 100/130 bitumen, produced by Asphaltbeton 1 LLC (Almaty, Kazakhstan). X-ray diffraction and scanning electron microscopy were used to determine the structure and morphology of the resulting coke powders. Standard tests and the Superpave Multiple Stress Creep and Recovery (MSCR) methodology were used to determine the physico-mechanical and rheological properties of the modified binders. Microdispersed granular coke powders produced after mechanochemical activation had a minimum average particle diameter of 8.28 µm (petroleum coke) and 16.64 µm (coal coke), and were mainly an amorphous carbon phase with traces of graphite. Addition of 1 wt.% microdispersed coke resulted in better performance of binder and an enhancement in grades of BND 100/130 to BND 70/100, in line with ST RK 1373-2013. MSCR testing showed that Jnr_3.2 is between 2.0–3.0 kPa⁻¹, which is in the S category of AASHTO M 332-20. This study showed how micro-sized coal and petroleum coke can be effectively used as a high-carbon modifier in bitumen, which reflects the possibility of their practical use in asphalt pavements that are subjected to normal traffic conditions. Full article

This research aims to investigate the modifications of the structural, dielectric, and sensing properties of CaFeO_3−δ ceramics produced by solid-state reaction induced by varying sintering temperatures in the range of 1000–1200 °C. A single crystallographic orthorhombic (Pcmn) structure was revealed by X-ray diffraction with Rietveld analysis, both for the powders and sintered ceramics, irrespective of the sintering temperature. The increase in the sintering temperature induces better densification and a larger grain size. Dielectric measurements reveal a pronounced enhancement of the relative permittivity, reaching 2 × 10⁵ at 1 kHz and 330 °C for the sample sintered at 1200 °C/4 h. This composition also displays the highest electrical conductivity, 0.4 S/m at 1 MHz. Cole–Cole analysis indicates a clear deviation from ideal Debye behavior, while the relaxational features of the dielectric permittivity suggest a strong correlation between the dielectric response and Fe-related conduction mechanisms. Gas sensing tests show that the ferrite ceramics exhibit consistent ethanol response trends. The ceramic sintered at 1200 °C/4 h achieved the highest sensitivity, of 56.28%, which can be attributed to its higher density, larger ceramic grains, and reduced low-frequency conductivity. The CaFeO_3−δ ceramic sintered at 1200 °C/4 h shows a combination of high permittivity, enhanced conductivity, and strong ethanol sensitivity, making it a promising material for dielectric components, capacitive devices, and gas sensing applications. Full article

A Cu-containing FeCrMnNiAl multi-principal element alloy was processed by laser-based and electron beam-based powder bed fusion (PBF-LB/M and PBF-EB/M) to investigate processing–microstructure–property relationships. In focus were alloy variants with a relatively high Cu content. Two PBF-LB/M scan strategies, employing a Gaussian beam with and without a re-scan with a laser featuring a flat-top profile, were compared to PBF-EB/M processing, followed by heat-treatments between 300 °C and 1000 °C. The phase constitution, elemental partitioning and grain boundary characteristics were analyzed by X-ray diffraction, electron backscatter diffraction and energy-dispersive X-ray spectroscopy. Mechanical behavior was assessed by hardness and tensile testing. Both manufacturing routes promoted the evolution of stable multi-phase microstructures composed of face-centered-cubic (FCC)- and body-centered-cubic (BCC)-type phases across all heat-treatment conditions. PBF-LB/M processing resulted in finer, dendritic microstructures and suppressed formation of a Cu-rich FCC phase due to higher cooling rates, whereas PBF-EB/M promoted the evolution of Cu-rich FCC segregates and equiaxed grain morphologies. Heat-treatment above 700 °C led to recrystallization, accompanied by an increase of the FCC phase fraction, grain coarsening, and recovery. At lower heat-treatment temperatures, the changes in microstructure are different. Here, it is assumed that small, non-clustered Cu-rich precipitates formed at the grain and sub-grain boundaries, although this assumption is only based on the assessment of the mechanical properties. The size of these precipitates is below the resolution limit of the techniques applied for analysis in the present work. Additional structures seen within the Cu-rich areas of PBF-EB/M-manufactured samples treated at lower temperatures also seem to have an influence on the hardness and yield strength. All of the conditions investigated exhibited pronounced brittleness, limiting reliable tensile property evaluation and indicating the need for further optimization of processing strategies and microstructural control for high-Cu-fraction-containing multi-principal element alloys. Full article

Laser processing has been widely investigated as an effective approach for improving surface properties and consolidating advanced materials, particularly complex alloys such as titanium aluminides (TiAl). In this study, laser surface remelting was applied to binary (Ti-45Al) and ternary (Ti-45Al-2Co and Ti-45Al-2Ni) alloys produced by powder metallurgy via blended elemental (BE) and pre-alloyed (PA) powder routes. Laser powers of 50 and 100 W were employed, resulting in a high-energy-density surface remelting regime applied to both green compacts and sintered samples with relatively high initial porosity, under an argon-controlled atmosphere. Microstructural and phase analyses were performed using scanning electron microscopy (SEM) and X-ray diffraction (XRD), while mechanical behavior was assessed by instrumented microindentation. Laser processing promoted the formation of a dense and homogeneous surface layer, approximately 150 μm thick, accompanied by significant microstructural refinement and enhanced hardness and elastic modulus. While rapid solidification led to crack formation in laser-treated sintered samples, the green compacts exhibited defect-free modified layers. Overall, the results demonstrate that laser surface remelting is an effective strategy for enhancing the surface integrity and mechanical performance of TiAl alloys processed by powder metallurgy. Full article