Search Results (97)

In recent years, an increasing number of national major projects have focused on the physicochemical properties of materials and the structural integrity of components in cryogenic environments. In situ neutron non-destructive testing offers a distinct advantage for scientific research conducted under cryogenic conditions. With the progressive advancement of neutron sources and neutron diffraction techniques, neutron probes have become indispensable for the in situ observation of lattice strain, phase transformation behavior, and residual stresses in materials at cryogenic temperatures. Based on the energy-resolved neutron imaging instrument (ERNI) at Beamline 13 of the China Spallation Neutron Source (CSNS), we have developed a cryogenic loading frame for in situ neutron diffraction tensile tests. This paper presents a detailed description of the mechanical structural design, cooling and control system, strength and thermal analyses, and experimental validation of the device. The apparatus enables in situ neutron diffraction experiments over a wide temperature range of 6–473 K, with an axial loading capacity of 50 kN. Furthermore, the device was employed to conduct in situ neutron diffraction measurements on austenitic 304 stainless steel at both room and cryogenic temperatures. The experimental results confirm that this equipment exhibits stable loading capability and precise temperature control, ensuring the reliability of the experimental data. Full article

Cavitation erosion is a phenomenon that causes the degradation of engineering components operating in fluids under oscillating pressure, and it occurs through the repeated implosion of cavitation bubbles adjacent to the solid surface. This complex phenomenon involves both the hydrodynamic factors of the liquid and the properties of the material being eroded. Cavitation erosion tests were performed using a vibratory apparatus with piezoceramic crystals, in accordance with the ASTM G32-2016 standard. As a reference material, a wrought aluminum-based alloy in the hot-rolled condition, EN AW-6082, was selected. For both alloys, mass losses were measured and erosion rates were calculated. The eroded surfaces were examined by X-ray diffraction (XRD), optical microscopy, scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The results indicate that the cavitation erosion resistance of the AZ 31B alloy in the hot-rolled condition is approximately 3.77 times lower than that of the reference material. This behavior is attributed to its lower hardness and heterogeneous microstructure, consisting of an α solid solution matrix with a hexagonal close-packed crystal structure and intermetallic particles of the Mg₁₇Al₁₂ type, which exhibit pronounced brittleness. Cavitation pits are observed mainly within the α-Mg solid solution grains and at the interfaces between the intermetallic phases and the α-Mg matrix. Full article

The aim of this paper is the analysis of the main elements of the patinas of an outdoor bronze monument by using portable energy-dispersive X-ray fluorescence (ED-XRF) equipment designed and assembled at the University of Salento. Thanks to the versatility of the ED-XRF portable apparatus, we carried out a scan based on a limited set of measurements that was representative of the studied surface of the monument before the restoration in a relatively short time and in a completely non-invasive way. We investigated the concentrations of copper, zinc, lead, chlorine, iron, tin and sulphur in the statue dedicated to the emperor Caesar Augustum, which was created in 1935 and later placed in Brindisi (Apulia, Southern Italy). Moreover, X-ray diffraction (XRD) and Raman spectroscopy were carried out for a sample of patina in order to identify its chemical composition. The information obtained can be helpful for restoration work on this statue and possible future monitoring. Full article

ZBLAN (ZrF₄-BaF₂-LaF₃-AlF₃-NaF) fluoride glass is a promising infrared optical fiber material because of its wide transmission window and low theoretical attenuation; however, unwanted crystallization during thermal processing can introduce scattering centers and degrade optical performance. Previous studies have mainly focused on temperature effects and microgravity-based crystallization suppression, while the role of mechanical vibration remains insufficiently understood. This study addresses this gap by investigating how controlled mechanical vibration influences crystallization onset, morphology, and structural evolution in ZBLAN glass during short-duration thermal treatment. ZBLAN samples were treated at selected temperatures with and without vibration using a custom heating–vibration apparatus and characterized by optical microscopy, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), atomic force microscopy (AFM), and X-ray diffraction (XRD). Temperature-only treatment produced a gradual transition from transparent amorphous glass to crystallized structures with increasing temperature. Vibration-assisted treatment altered crystallization behavior, producing distinct needle-like, bow-tie, and feather-like morphologies depending on temperature and vibration intensity. AFM confirmed a significant increase in surface roughness, while XRD verified structural evolution from amorphous to highly crystallized states. At higher vibration levels, irregular crystallization suggested that excessive sample movement may reduce thermal contact and change the effective heating condition. These findings demonstrate that mechanical vibration is a critical and controllable processing variable in ZBLAN fabrication and should be carefully managed to suppress unwanted crystallization in both terrestrial and space-based fiber manufacturing. Full article

Background: Tantalum in cytotoxicity tests showed no toxicity effect, as well as promoting bone regeneration through the differentiation, proliferation, mineralisation and adhesion of osteoblasts in in vitro and in vivo studies. This study aims to determine and compare the chemical composition, roughness and wettability of non-coated commercially pure titanium (CpTi) disc surfaces with CpTi discs that have been coated with tantalum oxynitride film (TaON) via a modified plasma sputtering coating technique. Methods: Two groups were tested that included the TaON-coated CpTi discs and non-coated CpTi discs. A modified reactive plasma sputtering apparatus was used for coating the CpTi discs with TaON at different time durations, i.e., 4, 6, and 8 h. The surface properties of the coated and non-coated discs were studied using X-ray diffraction (XRD) analysis, energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), and contact angle measurement. Results and Conclusions: The results showed that 8 h was the best coating duration. The XRD analysis showed the presence of a new peak in the case of the TaON-coated CpTi disc that was absent in the non-coated CpTi disc. Furthermore, the SEM analysis revealed that the TaON-coated CpTi disc showed a better distribution of surface roughness compared to the non-coated disc. The non-coated CpTi discs showed lower wettability compared to the TaON-coated CpTi discs. The result shows the importance of a TaON coat in changing the surface properties of CpTi which will be used in dental implants; this result will enhance the idea of surface treatment and its relationship with the enhancement and acceleration of bone formation around dental implants in future. The novelty of the newly modified reactive plasma sputtering technique used in this study as a coating technique for CpTi discs lies in the promising tantalum oxynitride, as Ta had no toxicity effect in cytotoxicity tests and promoted adhesion, proliferation, differentiation, the mineralisation of osteoblasts and bone regeneration in vitro and in vivo. The mean target of the work is to enhance the osseointegration of CPTi dental implants with different surface coatings including Ta oxide, nitride and oxynitride. The results of the first two coatings are already published, and the third coating technique is investigated in this study. Full article

Cavitation erosion is a critical problem for many engineering components, such as ship propellers, diesel engine exhaust valves, cylinder liners, pump impeller blades, hydraulic turbines, and bearings, which are exposed to high-velocity flowing fluids or to vibratory fluid motion. It represents a mechanical degradation of the surface caused by the continuous collapse of bubbles in the surrounding liquid, which seriously affects flow efficiency and component service life, increasing maintenance frequency and refurbishment costs. The intensity and evolution of the cavitation erosion phenomenon depend on the hydrodynamic conditions to which the component surface is exposed, the properties of the liquid, and the judicious selection of the most suitable material. This paper aims to modify the microstructure of a Ni-based superalloy by applying recrystallization annealing heat treatment in order to obtain surfaces resistant to cavitation erosion for components that handle fluids under local pressure fluctuations. Experimental tests are carried out using a vibratory apparatus with piezoceramic crystals operating at a frequency of 20 kHz and an amplitude of 50 µm. The cavitation erosion performance of the Ni-based superalloy INCONEL 625, heat treated by recrystallization annealing, are compared with that of austenitic stainless steel AISI 316L subjected to solution treatment. For both metallic alloys, based on mass loss measurements, the characteristic time-dependent curves of the mean cumulative erosion penetration depth, MDE(t), and the mean erosion rate, MDER(t), are determined. The comparison of these curves and of the parameters defined and recommended by the ASTM G32 standard demonstrates that, for the Inconel 625 superalloy, resistance to cavitation erosion increases by 77–81% compared to that of AISI 316L austenitic stainless steel. X-ray diffraction analyses (XRD) show that, in the microstructure of the Inconel 625 superalloy, in addition to austenite, MC-type carbides, M₂₃C₆ carbides, and intermetallic phases γ″ = Ni₃(Nb, Al, Ti) and δ = Ni₃(Nb, Mo) are also present. Full article

This study reports the fabrication of copper-based metal matrix composites reinforced with a combination of micro- and nano-sized titanium carbide (TiC) particles using the powder metallurgy route. The micro-TiC content was maintained at 5 wt.%, while the nano-TiC addition was systematically varied between 1 and 3 wt.% in increments of 1 wt.%. The consolidation of the blends was achieved by uniaxial compaction at 500 MPa, followed by sintering in a nitrogen atmosphere at 750–900 °C for 2 h. Tribological assessment under dry sliding conditions was performed using a pin-on-disk apparatus. Structural and microstructural examinations using X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive spectroscopy (EDS) confirmed a uniform incorporation of the reinforcements within the Cu matrix. The incorporation of nano-TiC up to 2 wt.% significantly enhanced density, hardness, and wear resistance, after which a marginal decline was observed. SEM analysis of worn surfaces revealed that adhesive wear, abrasion, and delamination were the primary wear mechanisms. To better understand the relationship between processing conditions and material responses, response surface methodology (RSM) was employed. The developed models for density, hardness, and wear loss showed good agreement with the experimental results, with confirmatory tests yielding errors of 1.59%, 2.06%, and 2%, respectively, thereby validating the approach’s reliability. Full article

To investigate the mechanical behavior and energy evolution characteristics of various rock materials under impact loading, dynamic impact tests were conducted on five representative rock types using a split Hopkinson pressure bar (SHPB) apparatus, combined with X-ray diffraction (XRD) and scanning electron microscopy (SEM) techniques. The dynamic mechanical response, energy characteristics, mineral composition, and associated microstructural features of these typical rocks were systematically analyzed. The results show that basalt exhibits the highest peak strength, followed by blue sandstone and granite; all three display typical brittle failure characteristics, whereas red sandstone and green sandstone demonstrate greater ductility and plastic deformation capacity. By introducing the energy-time density index, the energy-time density of the rocks ranks from strongest to weakest as follows: green sandstone, red sandstone, granite, blue sandstone, and basalt. An innovative dynamic strength–energy-time density mapping model was established to elucidate the clustering and distinguishing characteristics of these rock materials. Assay results and mesoscopic images confirm the relationship between mineral composition and the fine structure of rock fragmentation mechanisms, highlighting that the critical transition from intergranular to transgranular fracture is the key mechanism governing impact pulverization. Furthermore, fractal analysis reveals that higher fractal dimensions are associated with more complex microcrack structures and may correlate with the corresponding energy dissipation intensity. These findings provide profound insight into the failure mechanisms of rocks under dynamic loading, offering significant theoretical value and engineering application prospects, particularly in fields such as mining excavation and rock mass stability assessment. Full article

Background: Lycopene is a powerful antioxidant, classified as a carotenoid. Numerous studies confirm its beneficial effects in both the prevention and treatment of various diseases. However, its therapeutic application is significantly limited due to its poor water solubility and low bioavailability from natural sources. Developing a formulation with improved therapeutic characteristics could enhance the effectiveness of lycopene, making it more suitable for medical and nutritional use. The objective of this work was to apply hot-melt extrusion to produce extrudates containing an acetone-based lycopene extract combined with selected polymers, aiming to enhance its dissolution properties. Methods: Lycopene-rich extracts were prepared using ultrasound-assisted extraction with acetone. The obtained extract was processed via hot-melt extrusion together with PVP VA64 and Soluplus. The resulting extrudates were characterized using attenuated total reflectance Fourier-transform infrared spectroscopy (ATR-FTIR) and X-ray diffraction (XRD). Dissolution behavior was assessed using a paddle apparatus, and collected samples were quantified by HPLC. Antioxidant capacity was determined via DPPH radical-scavenging analysis. Results: The polymers PVP VA64 and Soluplus improve lycopene’s dissolution in acidic environments while showing its antioxidant potential. Conclusions: The formulation combining lycopene obtained through hot-melt extrusion with PVP VA64 and Soluplus polymers will enable its wider and more effective application. Full article

We revisit the Extended Uncertainty Principle (EUP) from an operational viewpoint, replacing wavefunction-based widths with apparatus-defined position constraints such as a finite slit of width $\mathrm{\Delta }x$ or a geodesic ball of radius R. Using Hermitian momentum operators consistent with the EUP algebra, we prove a sharp lower bound on the product of momentum spread and preparation size in one dimension and show that it reduces smoothly to the standard quantum limit as the deformation vanishes. We then extend the construction to dimensions two and three on spaces of constant curvature and obtain the corresponding bound for spherical confinement, clarifying its geometric meaning via an isometry to $S^2$ and $S^3$. The framework links curvature-scale effects to operational momentum floors and suggests concrete tests in diffraction, cold-atom, and optomechanical settings. Full article

Background/Objectives: Hot-melt extrusion (HME) has become a key technology in pharmaceutical formulation, particularly for enhancing the solubility of poorly soluble Active Pharmaceutical Ingredients (APIs). While horizontal HME is widely adopted, vertical HME remains underexplored despite its potential benefits in footprint reduction, feeding efficiency, temperature control, and integration into continuous manufacturing. This study investigates vertical HME as an innovative approach in order to optimize drug polymer interactions and generate stable amorphous dispersions with controlled release behavior. Methods: Extrusion trials were conducted using a vertical hot-melt extruder developed by Rondol Industrie (Nancy, France). Acetylsalicylic acid (ASA) supplied by Seqens (Écully, France) was used as a model API and processed with Soluplus^® and Kollidon^® 12 PF (BASF, Ludwigshafen, Germany). Various process parameters (temperature, screw speed, screw profile) were explored. The extrudates were characterized by powder X-ray diffraction (PXRD) and small-angle X-ray scattering (SAXS) to evaluate crystallinity and microstructure. In vitro dissolution tests were performed under sink conditions using USP Apparatus II to assess drug release profiles. Results: Vertical HME enabled the formation of homogeneous amorphous solid dispersions. PXRD confirmed the absence of residual crystallinity, and SAXS revealed nanostructural changes in the polymer matrix influenced by drug loading and thermal input. In vitro dissolution demonstrated enhanced drug release rates compared to crystalline ASA, with good reproducibility. Conclusions: Vertical HME provides a compact, cleanable, and modular platform that supports the development of stable amorphous dispersions with controlled release. It represents a robust and versatile solution for pharmaceutical innovation, with strong potential for cost-efficient continuous manufacturing and industrial-scale adoption. Full article

The objective of this work was the synthesis and characterization of novel, insensitive high explosives. 1-hydroxy-5-methyltetrazole served as both a scaffold and anion for preparing various nitrogen-rich energetic salts. The compounds were characterized using ¹H and ¹³C NMR spectroscopy, high-resolution mass spectrometry, elemental analysis, low-temperature single-crystal X-ray diffraction, and IR spectroscopy. Thermal stability was investigated via differential thermal analysis (DTA). Sensitivities towards mechanical stimuli were measured using a BAM drop hammer for impact sensitivity and a BAM friction apparatus for friction sensitivity, employing one of six testing procedures. Energetic performance parameters were calculated using the EXPLO5 code, incorporating room-temperature X-ray densities and solid-state heats of formation obtained via CBS-4M calculations using the Gaussian 16 program. Full article

Background/Objectives: Chronic lung diseases are among the leading causes of death worldwide. In the treatment of these diseases, non-steroidal anti-inflammatory drugs can be effective. We have previously developed an excipient formulation alongside a modern manufacturing protocol, which we aim to further investigate. We have chosen two new model drugs, meloxicam (MX) and its water-soluble salt, meloxicam-potassium (MXP). The particles in dry powder inhaler (DPI) formulation were expected to have a spherical shape, fast drug release, and good aerodynamic properties. Methods: The excipients were poloxamer-188, mannitol, and leucine. The samples were prepared by spray drying, preceded by solution preparation and wet grinding. Particle size was determined by laser diffraction, shape by scanning electron microscopy (SEM), crystallinity by powder X-ray diffraction (PXRD), interactions by Fourier-transform infrared spectroscopy (FT-IR), in vitro drug dissolution by paddle apparatus, and in vitro aerodynamic properties by Andersen cascade impactor and Spraytec^® device. Results: We achieved the proper particle size (<5 μm) and spherical shape according to laser diffraction and SEM. The XRPD showed partial amorphization. FT-IR revealed no interaction between the materials. During the in vitro dissolution tests, more than 90% of MX and MXP were released within the first 5 min. The best products exhibited an aerodynamic diameter of around 4 µm, a fine particle fraction around 50%, and an emitted fraction over 95%. The analysis by Spraytec^® supported the suitability for lung targeting. Conclusions: The developed preparation process and excipient system can be applied in the development of different drugs containing DPIs. Full article

High-energy ball milling for different durations was used to synthesize nanocrystalline Mg₆₀Ni₂₅Cu₁₀Ce₅ powders. The morphology and microstructure of the milled powders were investigated by scanning electron microscopy and X-ray diffraction, respectively. It was found that different milling times result in considerably different phase composition. The powder milled for 1 h is characterized by elemental Mg, Ni, Cu and Ce with some minor content of intermetallics. In total, 3 h milling promotes the intensive formation of intermetallic compounds, while 10 h of powder processing results in a partially amorphous state coupled with compound phases. Isothermal hydrogenation and dehydrogenation experiments were conducted in a Sieverts’-type apparatus. It was found that all powders absorb H₂ reversibly, while the shortest milling time provides the best overall capacity. Excellent kinetics without any activation cycle were obtained for the 3 h milled composite, releasing and absorbing 50% of the total hydrogen content within 120 s. Each kinetic measurement has satisfactorily been fitted by the Johnson–Mehl–Avrami function. X-ray diffraction analysis on the dehydrided powders confirmed the complete desorption. Full article

The objective of this study is to explore the high-temperature rheological properties and microscopic interaction mechanisms of styrene–butadiene–styrene (SBS) composite-modified asphalt with hydroxylated multi-walled carbon nanotubes (MWCNT-OH). SBS-modified asphalt, MWCNT-modified asphalt and MWCNT/SBS composite-modified asphalt were prepared with high-speed shearing apparatus and machine mixer. Physical property tests, dynamic shear rheological (DSR) tests, multiple stress creep recovery (MSCR) tests, X-ray diffraction (XRD) and Raman spectroscopy analyses were carried out to systematically compare the differences in macroscopic performance and changes in microscopic structure of different types of asphalts. According to the results of physical property tests, DSR tests and MSCR tests, the composite-modified asphalt was superior to the single-component-modified asphalt in terms of complex modulus (G*) and rutting factor (G*/sin δ). Its creep recovery rate (R) and unrecoverable compliance (Jnr) exhibited better anti-deformation ability under high temperatures, verifying the synergistic effect of SBS and MWCNTs-OH. XRD analysis showed that composite modification reduced the disorder degree of the crystalline phase of asphalt. Raman spectroscopy confirmed that there were changes in the vibration of chemical bonds between the modifier and asphalt, indicating that the modifier and asphalt acted on the asphalt system through physical dispersion and chemical cross-linking. Full article