Search Results (69)

Spent fluid catalytic cracking catalysts (E-cat) are a challenging waste from the petroleum refining industry, enriched with heavy metals such as nickel, vanadium, and iron. This study proposes a circular valorization strategy by incorporating E-cat into a chemically bonded iron phosphate ceramic matrix, known for its excellent waste stabilization properties. Composites were synthesized at room temperature using E-cat, hematite, and phosphoric acid, with E-cat contents from 0% to 35%. Characterization by XRF, XRD, SEM, compressive strength, and water absorption tests identified an optimal formulation containing 16% E-cat, achieving a maximum compressive strength of 16.6 MPa, 35% higher than the control. This improvement can be attributed to the dual function of E-cat, acting both as a micro-aggregate that promotes matrix densification and as a pozzolanic component that enhances mechanical reinforcement. These results demonstrate that iron phosphate ceramics represent a low-energy and sustainable strategy for the immobilization of spent catalysts and the production of durable construction composites. Full article

Enhancing the flame retardancy of polymeric materials by adding only eco-friendly ammonium polyphosphate (APP) while simultaneously maintaining high-temperature resistance has become a challenge. Talcum has been introduced as a cooperative agent into the silicone rubber/APP system to investigate the effect of talcum on flame retardancy, thermal stability, and high-temperature resistance. The machining process induces the orientation of talcum in the system. The ceramifiable silicone rubber blends containing oriented talcum (e.g., sample SA₆T₄) exhibited superb flame retardancy, including an LOI of 29.4%, a UL-94 rating of V-0, and a peak heat release rate (PHRR) of 250.2 kW·m⁻². More importantly, the blends present excellent thermal stability and high-temperature resistance, characterized by outstanding self-supporting properties and dimensional stability. Based on the structural analysis of the blends and their residues, the made of action for the improved flame retardancy may be attributed to the formation of a compact barrier layer. This layer is formed by oriented talcum platelets combined with phosphoric acid, from the thermal decomposition of APP, promoting crosslinking, thereby achieving a good inhibition barrier to inhibit heat feedback from the condensation zone. The excellent thermal stability and high-temperature resistance of the ceramifiable silicone rubber blends may be ascribed to a cooperative effect between APP and talcum at high temperatures, which facilitates the formation of ceramic structures. The novel ceramifiable silicone rubber composite has potential applications as flame-retardant sealing components for rail transit equipment and encapsulation materials for new energy battery modules. Full article

The objective of this study was to evaluate whether any coating material would have a beneficial influence on maintaining color stability and surface roughness and to what extent an uncoated resin composite can keep its original color. The study evaluated three direct composite resins (Gradia Direct Anterior A2, Tetric EvoCeram A2, Filtek Z550 A2) using 30 samples per material (1 mm thick, 14 × 10 × 1 mm). Samples were prepared in 3D-printed molds, light-cured for 40 s, and initially smoothed with abrasive paper (grit 400–2000). The surface treatments applied were as follows: group 1—polished with a brush and Compo + polishing paste, group 2—conditioned with 37% phosphoric acid, ScotchBond adhesive applied, light-cured. All samples were cleaned ultrasonically for 5 min. Initial surface roughness and color were measured with a profilometer and spectrophotometer. Samples were then immersed in distilled water (control at 37 °C), Coca-Cola and red wine (at 10 °C) with surface roughness and color changes measurements taken on days 1, 7, 14 and 90. Immersion media were refreshed weekly. The most notable color changes after immersion in coloring solutions were observed in the groups treated with Coca-Cola and red wine compared with the control group in distilled water. Tetric EvoCeram sealed and Gradia sealed maintained the greatest resistance to perceptible coloration over 90 days, while Filtek Z550 performed the poorest. Tetric EvoCeram sealed maintained the greatest color stability (ΔE < 3.5 at 90 days), whereas Filtek Z550 sealed showed early degradation. Roughness is often decreased by surface sealing. As immersion time rises, unsealed surfaces often become noticeably rougher than sealed ones. This study simulates the oral environment and the exposure of restorative materials to staining agents. As the loss of esthetic properties over time is a continuous problem, the clinical significance of this research lies in demonstrating how a restorative material could resist pigmentation, when in contact with well-known high staining beverages, in order to maintain its esthetic properties and remain suitable for long-term use in the oral cavity. Moreover, the hypothesis that a coating material would protect the resin composite surface and reduce discoloration and surface roughness was tested. Full article

This study evaluated the influence of different surface treatments and composite materials on the microtensile bond strength (μTBS) of repaired aged bulk-fill resin composite restorations, aligning with the principles of minimal intervention dentistry. Seventy-two specimens of bulk-fill resin composite (Tetric EvoCeram) were prepared, sectioned into bars (1 × 1 × 5 mm), and subjected to thermocycling to simulate aging. Specimens were randomly allocated into six groups (n = 12) based on surface treatment and repair material: phosphoric acid etching followed by repair with either Tetric EvoCeram (Group 1) or Filtek Z350 XT (Group 2); diamond bur roughening followed by repair with Tetric EvoCeram (Group 3) or Filtek Z350 XT (Group 4); and air abrasion followed by repair with Tetric EvoCeram (Group 5) or Filtek Z350 XT (Group 6). μTBS testing was performed using a universal testing machine, and failure patterns were examined under a stereomicroscope at 40× magnification. The highest bond strength values were observed in Groups 5 and 6 (air abrasion), followed by Group 3 (diamond bur). Groups 1, 2, and 4 showed significantly lower bond strength values (p < 0.05). No significant differences in failure modes were reported across groups. These findings suggest that air abrasion is a superior surface treatment for repairing aged bulk-fill resin composites, as it significantly enhanced μTBS compared to phosphoric acid etching and diamond bur roughening. Full article

The aim of this study was to investigate the possibility of Ag nanoparticle crystallization in B₂O₃–Bi₂O₃ glass using a heat treatment method and to investigate the possible influence of the obtained nanoparticles on the emission intensity of Eu³⁺ ions. Borate–bismuth glasses with different B₂O₃:Bi₂O₃ molar ratios of 50:50, 60:40 and 70:50 with Ag and Eu³⁺ ions were successfully synthesized. The structure of the glasses was studied using XRD and FTIR methods. The XRD results exhibited a characteristic amorphous halo, confirming the absence of long-range order in the samples. The glass transition temperatures of various compositions, required to select the annealing temperature, were measured using DTA analysis. The strong maximum in the UV–Vis spectrum of the sample with the highest Bi₂O₃ content clearly indicated the presence of Ag nanoparticles in the glass. Moreover, a color change was observed for this sample, from slightly yellow to red. The presence of Ag nanoparticles was further confirmed via TEM and XPS studies. However, with a high content of Ag nanoparticles in the matrix, their positive effect on luminescence intensity was not observed. The obtained results show that B₂O₃–Bi₂O₃ glass and glass ceramics, with Ag nanoparticles and rare-earth (Re) ions, could be considered as a new phosphor for light-emitting diodes (LEDs). Full article

The ancient site of Olympia is located on the northern fringe of the Basin of Makrisia at the confluence of the Kladeos and Alpheios rivers (western Peloponnese, Greece) and was used as a venue for the Panhellenic Games from Archaic times until the 4th century AD. Geophysical prospection (frequency domain electromagnetic induction and electrical resistivity tomography) was carried out as a basis for detailed geoarchaeological investigations. In doing so, we identified a previously unknown building structure adjacent to the Altis, the inner part of the sanctuary at Olympia. Situated south of the Southwest Thermae, this structure measures at least 100 m (WSW-ENE) by 80 m (NNW-SSE). Its external orientation is in line with the orientation of the Southwest Thermae and the Leonidaion. We retrieved sediment cores from 17 different locations in combination with high-resolution direct push sensing from inside the newly found structure. All cores revealed distinct units of organic-rich limnic sediments dominated by clay and fine silt. Geochemical and micropaleontological analyses of selected sediment samples indicate highly eutrophic conditions, as evidenced by elevated phosphorous concentrations and the dominance of the ostracod species Cyprideis torosa, which is able to live under low-oxygen conditions. Moreover, molecular biomarker analyses show a significant input of lipid fecal markers, implying strong anthropogenic pollution. Further, the limnic sediments include numerous charcoal remains and abundant diagnostic artifacts such as ceramic fragments and building material. Radiocarbon dating documents that these limnic conditions persisted within the building structure from at least the 5th century BC to the 6th century AD. The identified building structure lies in the immediate proximity to the Lake of Olympia, which was recently found to have existed from the mid-Holocene to the Medieval period. Its characteristic filling with fine-grained sediments and multiple indications for a strongly polluted and heavily used standing water environment let us hypothesize that it was possibly used as a harbor installation. A harbor at ancient Olympia could have been used to reach the sanctuary by boat and to transport goods of all kinds. Full article

In the fabrication of soft magnetic composites, the lattice mismatch between the inorganic insulation layer and the iron matrix often leads to the formation of cracks during the molding process, which significantly impairs the operational performance of the materials. Consequently, it is imperative to develop novel strategies for inorganic insulation coatings that offer high electrical resistivity and thermal stability and are less susceptible to cracking during formation. This paper presents a new structure for soft magnetic composites that incorporates FePO₄ as an intermediate transition layer between the iron-based soft magnetic particles and the inorganic ceramic insulation layer. This configuration is designed to provide insulation coatings with superior voltage and thermal resistance, as well as high electrical resistivity. The research details the processes forming the FePO₄ intermediate transition layer and the SiO₂ insulation layer on the iron powder surface, along with their interaction mechanisms. An analysis comparing the scenarios with and without the FePO₄ intermediate transition layer shows its beneficial impact on the magnetic properties and mechanical strength of the soft magnetic composites. Further investigations reveal that at a phosphoric acid concentration of 1 wt.%, the FePO₄ layer significantly enhances the interface compatibility between the Fe powder matrix and the SiO₂ insulation layer. Under these conditions, the Fe@ FePO₄/SiO₂ soft magnetic composites demonstrate outstanding overall performance: the saturation magnetization stands at 215.60 emu/g, effective permeability at 83.2, resistivity at 57.42 Ω·m, power loss at 375.0 kW/m³ under 30 mT/100 kHz, and radial compressive strength at 15.95 Kgf. These findings offer novel insights and practical approaches for advancing inorganic insulation coating strategies and provide vital scientific support for further enhancing the magnetic and mechanical properties of soft magnetic composites. Full article

Tunable blue/red dual-emitting Eu³⁺-doped, Bi³⁺-sensitized SrF₂ phosphors were synthesized utilizing a solvothermal-microwave method. All phosphors have cubic structure (Fm-3m (225) space group) and well-distinct sphere-like particles with a size of ~20 nm, as examined by X-ray diffraction and transmission electron microscopy. The diffuse reflectance spectra reveal a redshift of the absorption band in the UV region as the Bi³⁺ concentration in SrF₂: Eu³⁺ phosphor increases. Under the 265 nm excitation, photoluminescence spectra show emission at around 400 nm from the host matrix and characteristic orange ⁵D₀ → ⁷F_1,2 and deep red ⁵D₀ → ⁷F₄ Eu³⁺ emissions. The red emission intensity increases with an increase in Bi³⁺ concentration up to 20 mol%, after which it decreases. The integrated intensity of Eu³⁺ red emission in the representative 20 mol% Bi³⁺ co-doped SrF₂:10 mol% Eu³⁺ shows twice as bright emission compared to the Bi³⁺-free sample. To demonstrate the potential application in LEDs for artificial light-based plant factories, the powder with the highest emission intensity, SrF₂: 10Eu, 20 Bi, was mixed with a ceramic binder and placed on top of a 275 nm UVC LED chip, showing pinkish violet light corresponding to blue (409 nm) and red (592, 614, and 700 nm) phosphors’ emission. Full article

A novel five-surface phosphor-in-glass (FS-PiG) structure for high illumination and excellent color uniformity in large-view scale LEDs for sensor light source application is demonstrated. YAG phosphor (Y₃Al₅O₁₂:Ce³⁺) was uniformly mixed with ceramic and sintered at 680 °C to form a phosphor wafer. Sophisticated laser engraving was employed on the phosphor wafer to form saddle-shaped large-view scale FS-PiG LEDs. The performance of the FS-PiG LEDs exhibited an illumination of 401 lm, average color temperature (CCT) of 5488 K ± 110 K, and color coordinates (CIE) of (0.3179 ± 0.003, 0.3352 ± 0.003). In contrast to convention single-surface phosphor-in-glass (SS-PiG) LEDs, the performance exhibited an illumination of 380 lm, average CCT of 5830 K ± 758 K, and CIE of (0.3083 ± 0.07, 0.3172 ± 0.07). These indicated that the performance of the FS-PiG LEDs was higher than the SS-PiG LEDs for illumination, CCT, and CIE by 1.7, 7, and 23 times, respectively. Furthermore, the FS-PiG LEDs demonstrate a lower lumen loss of 2% and a reduced chromaticity shift of 5.4 × 10⁻³ under accelerated aging at 350 °C for 1008 h, owing to the high ceramic melting temperature of up to 510 °C. In this study, the proposed FS-PiG large-view scale LEDs with excellent optical performance and high reliability may be promising candidates to replace the conventional phosphor-in-organic silicone material used in high-power LEDs for the next generation of sensor light sources, display, and headlight applications. Full article

Composite phosphor ceramics for warm white LED lighting were fabricated with K₂SiF₆:Mn⁴⁺ (KSF) as both a narrowband red phosphor and a translucent matrix in which yellow-emitting Y₃Al₅O₁₂:Ce³⁺ (YAG) particles were dispersed. The emission spectra of these composites under blue LED excitation were studied as a function of YAG loading and thickness. Warm white light with a color temperature of 2716 K, a high CRI of 92.6, and an R9 of 77.6 was achieved. A modest improvement in the thermal conductivity of the KSF ceramic of up to 9% was observed with the addition of YAG particles. In addition, a simple model was developed for predicting the emission spectra based on several parameters of the composite ceramics and validated with the experimental results. The emission spectrum can be tuned by varying the dopant concentrations, thickness, YAG loading, and YAG particle size. This work demonstrates the utility of KSF/YAG composite phosphor ceramics as a means of producing warm white light, which are potentially suitable for higher-drive applications due to their increased thermal conductivity and reduced droop compared with silicone-dispersed phosphor powders. Full article

This work explores the effects of rigid (0.1, 0.25, and 0.5 wt. %) and semi-flexible (0.5, 1.0, and 2.5 wt. %) all-aromatic polyelectrolyte reinforcements as rheological and morphological modifiers for preparing phosphate geopolymer glass–ceramic composites. Polymer-modified aluminosilicate–phosphate geopolymer resins were prepared by high-shear mixing of a metakaolin powder with 9M phosphoric acid and two all-aromatic, sulfonated polyamides. Polymer loadings between 0.5–2.5 wt. % exhibited gel-like behavior and an increase in the modulus of the geopolymer resin as a function of polymer concentration. The incorporation of a 0.5 wt. % rigid polymer resulted in a three-fold increase in viscosity relative to the control phosphate geopolymer resin. Hardening, dehydration, and crystallization of the geopolymer resins to glass-ceramics was achieved through mold casting, curing at 80 °C for 24 h, and a final heat treatment up to 260 °C. Scanning electron microscopy revealed a decrease in microstructure porosity in the range of 0.78 μm to 0.31 μm for geopolymer plaques containing loadings of 0.5 wt. % rigid polymer. Nano-porosity values of the composites were measured between 10–40 nm using nitrogen adsorption (Brunauer–Emmett–Teller method) and transmission electron microscopy. Nanoindentation studies revealed geopolymer composites with Young’s modulus values of 15–24 GPa and hardness values of 1–2 GPa, suggesting an increase in modulus and hardness with polymer incorporation. Additional structural and chemical analyses were performed via thermal gravimetric analysis, Fourier transform infrared radiation, X-ray diffraction, and energy dispersive spectroscopy. This work provides a fundamental understanding of the processing, microstructure, and mechanical behavior of water-soluble, high-performance polyelectrolyte-reinforced geopolymer composites. Full article

The surface treatment of zirconia prior to bonding remains controversial and unclear. This study aimed to compare the shear bond strength (SBS) of metal brackets to zirconia under surface treatments with either 4% HF or 37% PA in both immediate loading (IML) and artificial aging by thermocycling (TMC). Methods: Eighty-four zirconia were randomly assigned to six groups based on the surface treatment and artificial aging by TMC: (1) No surface treatment (NT); (2) NT + TMC; (3) HF (4% HF for 2 min); (4) HF + TMC; (5) PA (37% PA for 2 min); and (6) PA + TMC. After bracket bonding, only the TMC groups were thermocycled for 5000 cycles. The SBS and adhesive remnant index (ARI) of all groups were analyzed (p < 0.01). Results: TMC significantly lowered the SBS more than the IML in all acid surface treatment groups (p < 0.01). The ARI score after TMC was significantly higher than the IML in all acid surface treatment groups (p < 0.001). No significant differences in the SBS values or ARI scores were observed among the surface treatments (p > 0.01). Conclusions: Two-minute simple etching methods, using either 4% HF or 37% PA, showed an insufficient SBS of metal orthodontic brackets to zirconia after TMC. Full article

In this study, the photoluminescence (PL) behavior of two aluminosilicate glass series containing alkali-niobates ranging from 0.4 to 20 mol% was investigated. The glasses exhibit an intense visible emission centered at ~18,400 cm⁻¹ for the peralkaline series and at higher energies (~19,300 cm⁻¹) for the metaluminous glasses. However, the photoluminescence emission intensity varies significantly with the niobate content and the bulk chemistry. PL and fluorescence lifetime measurements indicate that the broad emission bands result from the overlap of different niobate populations, whose distribution changes with niobate content. The distinct PL behavior in the two glass series was related to the structural evolution of the niobate units upon niobium addition. An enhancement of the visible emission was observed for a higher fraction of distorted [NbO₆] units. Eu-doping was carried out as a structural probe of the glass network, and also to determine if these glasses could be used as potential rare earth element (REE) activators. The crystal field strength around Eu ions is strongly dependent on the bulk chemistry and the niobate content. Furthermore, the peralkaline series showed energy transfer from the host [NbO₆] to Eu³⁺, confirming the feasibility of exploring niobate glasses and glass-ceramics as lanthanide ion-activated luminescent materials. In addition, glass-ceramics (GCs) containing alkali-niobate phases with a perovskite-like structure were developed and studied to verify the optical performance of these materials. It was verified that the bulk chemistry influences crystallization behavior, and also the photoluminescence response. The transparent GC from the metaluminous series exhibits a quenching of the Eu³⁺ emission, whereas an enhanced emission intensity is observed for the peralkaline GC. The latter shows a strong excitation-dependent PL emission, suggesting energy transfer and migration of electronic excitation from one Eu population to another. Additionally, Eu³⁺ emissions arising from the $D_1_5^{}$ and $D_2_5^{}$ excited states were observed, highlighting the low phonon energy achievable in niobo-aluminosilicate hosts. Full article

Our objective is to achieve a new good-quality and mechanically durable high-transparency material that, when activated by rare earth ions, can be used as laser sources, scintillators, or phosphors. The best functional transparent ceramics are formed from high-symmetry systems, mainly cubic. Considering hexagonal hydroxyapatite, which shows anisotropy, the particle size of the initial powder is extremely important and should be of the order of several tens of nanometers. In this work, transparent micro-crystalline ceramics of non-cubic Ca₁₀(PO₄)₆(OH)₂ calcium phosphate were fabricated via Spark Plasma Sintering (SPS) from two types of nanopowders i.e., commercially available (COM. HA) and laboratory-made (LAB. HA) via the hydrothermal (HT) protocol. Our study centered on examining how the quality of sintered bodies is affected by the following parameters: the addition of LiF sintering agent, the temperature during the SPS process, and the quality of the starting nanopowders. The phase purity, microstructure, and optical transmittance of the ceramics were investigated to determine suitable sintering conditions. The best optical ceramics were obtained from LAB. HA nanopowder with the addition of 0.25 wt.% of LiF sintered at 1000 °C and 1050 °C. Full article

To address the issue of the lack of red light in traditional Ce³⁺: YAG-encapsulated blue LED white light systems, we utilized spark plasma sintering (SPS) to prepare spinel-based Cr³⁺-doped red phosphor ceramics. Through phase and spectral analysis, the SPS-sintered ZnAl₂O₄: 0.5%Cr³⁺ phosphor ceramic exhibits good density, and Cr³⁺ is incorporated into [AlO₆] octahedra as a red emitting center. We analyzed the reasons behind the narrow-band emission and millisecond-level lifetime of ZAO: 0.5%Cr³⁺, attributing it to the four-quadrupole interaction mechanism as determined through concentration quenching modeling. Additionally, we evaluated the thermal conductivity and thermal quenching performance of the ceramic. The weak electron-phonon coupling (EPC) effects and emission from antisite defects at 699 nm provide positive assistance in thermal quenching. At a high temperature of 150 °C, the thermal conductivity reaches up to 14 W·m⁻¹·K⁻¹, and the 687 nm PL intensity is maintained at around 70% of room temperature. Furthermore, the internal quantum efficiency (IQE) of ZAO: 0.5%Cr³⁺ phosphor ceramic can reach 78%. When encapsulated with Ce³⁺: YAG for a 450 nm blue LED, it compensates for the lack of red light, adjusts the color temperature, and improves the color rendering index (R9). This provides valuable insights for the study of white light emitting diodes (WLEDs). Full article