Hydrothermal Research Articles

Synthesis of Nd2Sn2O7 pyrochlore with different lattice disorder degrees and oxygen vacancy contents

In this study, a series of Nd2Sn2O7 pyrochlores with different lattice disorder degrees and oxygen vacancy contents were prepared via simple methods, including the sol–gel (SG) technique, glycine–nitrate combustion (GNC), coprecipitation (CP), and the hydrothermal (HT) method. Raman spectroscopy proved the most effective in identifying the lattice disorder degree and lattice defects of the pyrochlore-type composite oxides, followed by XRD, with FTIR spectroscopy as the least sensitive technique. For pure phase Nd2Sn2O7, the content of oxygen vacancies and adsorbed oxygen species follow the sequence CP > GNC > SG, which is well consistent with the lattice disorder degrees. This is because that the higher the lattice disorder of Nd2Sn2O7 pyrochlore, the weaker the Sn-O bond, making it easier to break and form oxygen vacancies. Although the HT sample exhibits the lowest disorder degree, its synergistic effect with residual SnO2 on the surface is beneficial for further enriching oxygen vacancies.

Platelet Ceria Catalysts from Solution Combustion and Effect of Iron Doping for Synthesis of Dimethyl Carbonate from CO2.

Solution combustion (SC) remains among the most promising synthetic strategies for the production of crystalline nanopowders from an aqueous medium, due to its easiness, time and cost-effectiveness, scalability and eco-friendliness. In this work, this method was selected to obtain anisometric ceria-based nanoparticles applied as catalysts for the direct synthesis of dimethyl carbonate. The catalytic performances were studied for the ceria and Fe-doped ceria from SC (CeO2-SC, Ce0.9Fe0.1O2-SC) in comparison with the ceria nanorods (CeO2-HT, Ce0.9Fe0.1O2-HT) obtained by hydrothermal (HT) method, one of the most studied systems in the literature. Indeed, the ceria nanoparticles obtained by SC were found to be highly crystalline, platelet-shaped, arranged in a mosaic-like assembly and with smaller crystallite size (≈6 nm vs. ≈17 nm) and higher surface area (80 m2 g-1 vs. 26 m2 g-1) for the undoped sample with respect to the Fe-doped counterpart. Although all samples exhibit an anisometric morphology that should favor the exposition of specific crystalline planes, HT-samples showed better performances due to higher oxygen vacancies concentration and lower amount of strong basic and acid sites.

Hydrothermal Growth Zinc Oxide Nanorods for pH Sensor Application

The aim of this work is to apply synthesized zinc oxide (ZnO) Nanorods using hydrothermal (HTL) growth technique for pH sensor application. The highly crystallite of ZnO Nanorods was obtained by anneal the growth ZnO Nanorods in furnace at 200 °C for 2 hours. Besides that, XRD analysis shows the produced ZnO Nanorods belonged to the (002) plane. Furthermore, Scanning Electron Microscope (SEM) images confirm that the ZnO Nanorods with hexagonal-faceted structural were successfully produced by HTL growth technique. In addition, Ultraviolet–visible (UV-Vis) spectrophotometer analysis shows that the synthesized ZnO belongs to the wide band gap semiconductor material. The growing ZnO Nanorods were then subjected to electrical measurement with various pH levels. The outcome demonstrates that the current rises as the solution changes from acidic to alkaline. Overall, our study shows a relationship between the electrical as well as the structural characteristics of ZnO Nanorods at various pH levels.

Oil palm frond leaves (OPFLs), a high recalcitrant biomass as an alternative cellulose source for glucose conversion

Among the oil palm biomass, oil palm frond leaves (OPFLs) are under-valued since they can be classified as a high recalcitrance feedstock due to the high lignin and hemicellulose content. This work proposes a new way of using OPFLs as alternative cellulose sources for glucose conversion by an application of various pre-treatments at varying parameters. From green pre-treatment, steam explosion (SE) is much more effective in disrupting the OPFLs structure in contrast to hydrothermal (HT) pre-treatment, by a vast dissolution of hemicellulose and depolymerization of lignin. The pre-impregnation with H2SO4 prior to steam explosion was beneficial to enhance the hemicellulose removal up to 89.94 %. The 2D-HSQC NMR analysis divulged the reduction of ß-O-4 linkage and S/G value after the SE and HT pre-treatment, verifying the degradation of lignin-carbohydrate linkage in OPFLs. Meanwhile, the dilute NaOH pre-treatment enhanced the delignification by 87.14 %. SEM analysis revealed a well-disrupted structure of pre-treated OPFLs exposing a higher cellulosic fraction, whereas SEC analysis divulged a decreasing pattern of degree of polymerization of cellulose. The enzymatic analysis revealed that pre-treated OPFLs yielded higher glucose ranging from 29.81 % to 49.98 % w/w, which was ∼3-fold higher than raw OPFLs (14.31 % w/w). A maximum cellulose digestibility (100 %) was achieved by steam-exploded OPFLs after 72 h of enzymatic hydrolysis. This suggests the potency of various pre-treatments to enhance enzymatic saccharification of OPFLs producing a higher glucose yield.

Application of nano-urea in conventional flood-irrigated Boro rice in Bangladesh and nitrogen losses investigation

Bangladesh stands third in global rice production while complete modernization of rice production is not fully enforced. The boon of nano agriculture might circumvent the challenge of increasing the yield with minimal ecological damage. Nanofertilizer might be one of the solutions to address the problem of modern agriculture confronting environmental hazards owing to the excessive use of synthetic fertilizers by farmers in Bangladesh. We synthesized nanourea by chemical co-precipitation (CP) and hydrothermal (HT) methods in an attempt to develop environmentally friendly nanofertilizers. We characterized the nanourea and confirmed the functionalization of nanohydroxyapatite (nHAP) with urea by scanning transmission electron microscopy (STEM)/EDS mapping. The CP method produced particle dimensions of 45.62 nm for length and 14.16 nm for width. In comparison, the readings obtained through the HT method were around 74.69 nm and 20.44 nm for length and width, respectively. The field application of nanourea demonstrated impressive results, indicating a significant relationship between the particle size of nanourea and its impact on several agricultural factors. The grain yield using traditional synthetic fertilizer (urea) ranged from 6.47 to 6.52 t ha−1 with a very low NUE of 35.8–36.34 %. Contrarily, the grain yield was found from 6.52 to 6.84 t ha−1 and the obtained NUE ranged from 57.58 to 71.0 % using nanourea of the same concentration calibrated with traditional urea by two methods. Additionally, nanourea treatments having 25 % less nitrogen (N) provided higher total N (TN) in grain suggesting possible nutritional enrichment while checking the yield penalty and substantial increase in N use efficiency (NUE). However, further upscaling of this research on a field scale is necessary to confirm the findings.

Mechanical degradation of Longmaxi shale exposed to water-based fluids and supercritical carbon dioxide

Mechanical alterations in shale formations due to exposure to water-based fracturing fluids and supercritical carbon dioxide (ScCO2) significantly affect the performance of shale gas exploration and CO2 geo-sequestration. In this study, a hydrothermal (HT) reaction system was set up to treat Longmaxi shale samples of varying mineralogies (carbonate-, clay-, and quartz-rich) with different fluids, i.e. deionized (DI) water, 2% potassium chloride (KCl) solution, and ScCO2 under HT conditions expected in shale formation. Statistical micro-indentation was conducted to characterize the mechanical property alterations caused by the shale-fluid interactions. An in situ morphological and mineralogical identification technique that combines scanning electron microscopy (SEM) and backscattered electron (BSE) imaging with energy-dispersive X-ray spectroscopy (EDS) was used to analyze the microstructural and mineralogical changes of the treated shale samples. Results show no apparent changes in the Young’s modulus, E, and hardness, H, after treatment with DI water under room temperature (20 °C) and atmospheric pressure for 7 d. In contrast, E and H were decreased by 31.2% and 37.5% at elevated temperature (80 °C) and pressure (8 MPa), respectively. The addition of 2% KCl into DI water mitigated degradation of the mechanical properties. Quartz-rich shale specimens are the least sensitive to the water-based fracturing fluids, followed by the clay-rich and carbonate-rich shale formations. Based on in situ morphological and mineralogical identification, the primary factors for the mechanical degradation induced by water-based fluids include carbonate dissolution, clay swelling, and pyrite oxidation. Slight increases in the measured E and H and compression of porous clay aggregates were observed after treatment with ScCO2. The major factor contributing to the mechanical changes resulting from the exposure to scCO2 appears to be the competition between swelling caused by adsorption and compression of shale matrix.

Optimization of cerium-based metal–organic framework synthesis for maximal sonophotocatalytic tetracycline degradation

Wastewater treatment is inevitably required to alleviate the pollution of water resources by various contaminants such as antibiotics. MOFs are novel materials with photocatalytic activities. In this study, sonophotocatalytic degradation of tetracycline (TC) by the Cerium-based MOF (Ce-MOF) is optimized by modification of its synthesis route. Ce-MOF synthesis by room temperature (RT), hydrothermal (HT), and sonochemical synthesis (SC) are studied. TC degradation experiments revealed the superiority of SC synthesis. The interplay of main synthesis parameters, namely, initial ligand concentration, ultrasound (US) power and time on sonophotocatalytic activity of Ce-MOF, were investigated by response surface methodology model (RSM) utilizing the central composite experimental design (CCD). The optimum SC synthesis conditions are an initial ligand concentration of 8.4 mmol/L, a sonication power of 50 amplitude, and a US time of 60 min. The optimally synthesized Ce-MOF was characterized by infrared spectroscopy, FTIR, XRD, FE-SEM, TEM, zeta potential analysis, diffuse reflectance spectroscopy, particle size analysis, Mott-Schottky analysis, photocurrent analysis, electrochemical impedance spectra, and photoluminescence spectroscopy. The findings indicate that the removal efficiency of TC can reach up to 81.75% within 120 min in an aqueous solution containing an initial TC concentration of 120 ppm and 1 g/L Ce-MOF at pH of 7. Mineralization efficiency of the process is 71% according to COD measurements. The Ce-MOF catalyst retained its chemical stability and remained active upon TC degradation which makes it a promising candidate for wastewater treatment.

Synthesis of surface-engineered SrFe2O4 for efficient catalytic partial oxidation of methane

In this study, a series of platinum (Pt)-doped strontium iron oxide (SrFe2O4) catalysts with varying particle sizes were synthesized through the four different catalysis synthesis methods such as solution combustion synthesis (SCS), co-precipitation (Co-PPT), oxalic acid assisted sol-gel (OXA) and, hydrothermal (HT). The objective was to investigate the impact of particle size on the catalytic activity and long-term stability of these four catalysts. The XRD and Raman results confirmed the formation of the SrFe2O4 perovskite structure. HRTEM, SEM, and other characterizations revealed a clear correlation between the synthesis conditions and the resulting particle sizes. The highest%CH4 conversion was around 95 % for the catalyst prepared through Solution combustion synthesis and the catalyst was found to be thermally stable up to. 100 h at 800 °C with a negligible variation of conversion while maintaining the H2/CO ratio at 2.0. To gain insight into catalytic activity, stability, and selectivity of catalysts we have performed Temperature-programmed surface reaction (TPSR) at a controlled temperature ramping program. This study also includes the study of coke deposition on the spent catalysts through different characterization techniques. Furthermore, we have performed a kinetic study to find the initial rate of the reaction and the activation energy of the Pt-doped SrFe2O4 catalyst and it has been found that activation energy was 35 KJ/mol for the catalyst Pt/SrFe2O4 synthesis through the solution combustion method.

Unusual emission from 2F5/2 two lowest excited levels of Yb3+-doped LuPO4 nano/micro-crystalline materials

Yb3+-doped inorganic materials are constantly in demand due to a strong interest in fundamental and applied research. The simplicity of the 4f1³ electronic structure minimizes de-excitation processes and enables a quasi-three-level laser emission scheme at 1 μm employed for IR laser devices.In this work, we present an unusual simultaneous emission from two of the lowest levels of the 2F5/2 excited state observed at 77 K, measured for the first time and confirmed by the barycenter law for Yb3+-doped tetragonal LuPO4 revealing the lowest crystal field among Yb3+ ion-activated oxide crystals.Three series of tetragonal lutetium orthophosphate powders, containing various concentrations of Yb3+ ions (0.5–5 mol %), were analyzed in nano and micro-crystalline forms. The ionic liquid-assisted (IL) hydrothermal (HT) method was used for the nano-powders' preparation. This route enabled the fabrication of fine nano-powders with particle sizes of 15 nm in an ethylene glycol (GE) reaction medium and 30 nm in a water (W) medium, each exhibiting the desired well-crystallized single-phase phosphate. For comparative studies, the micro-crystalline samples were synthesized via reaction in the solid phase at a relatively high temperature.The Yb3+ ion also served as a structural probe, its spectroscopy i.e., absorption at 4.2 K, selectively excited luminescence at 77 K, and fluorescence decays were used to assign Yb3+ energy levels in only one D2d center precisely. This assignment was based on exceptional features due to the unique emissions observed from the two lowest levels of the 2F5/2 excited state, split only by 27 cm−1, confirmed by calculation of the crystal field parameters from Zeeman spectra.

Assessment of two recent hot dry rock thermal energy production projects

In this paper, we present analyses of laboratory and field data indicating that the current two-well, injection-production system, connected with multiple hydraulic fractures, is a very promising method for extracting heat from hot dry rock (HDR) systems to generate electricity. The current two-well system could be expanded to a three-well system consisting of one injection well and two symmetric producing wells connected via the central hydraulic fracture emanating from the injection well. To improve a uniform distribution of the injected fluid among all hydraulic fracture stages in the injection well, we advocate for field implementation of a newly designed well stimulation technique, the GeoThermOPTIMAL.We first present an analysis of the post-fracturing flow data obtained from an HDR geothermal injection well at the Utah FORGE Enhanced Geothermal System (EGS) research field site. The site is adjacent to the Roosevelt hydrothermal (HT) field. The objective of the study is to assess the effectiveness of well stimulation in extracting heat from the low-permeability, hot dry granitoid rock in the Utah FORGE research site. The study includes interpreting pressure falloff data obtained during the well stimulation process and employing laboratory-measured core data as a major input in the interpretation of the field falloff data. As a confirmation of the robustness of our analysis in Utah FORGE, we reviewed and analyzed the flow test results published for an injection-production doublet at the Blue Mountain EGS (Project Red) commercial site in Nevada. From the analyses of these two field tests, we have concluded that the interpretation and findings of the Blue Mountain EGS pilot test are consistent with the interpretation and findings from the Utah FORGE field research project test results.In summary, our engineering assessments began with laboratory experiments conducted on various core samples, including those from a granite outcrop and the Utah FORGE geothermal reservoir. These experiments aimed to measure key parameters such as matrix and fracture permeabilities, and porosities (km≈10−18m2, kf,eff≈10−15m2,ϕm≈10−1,andϕf≈10−4). These data served as guides and inputs for analytical and numerical solutions used to match the field pressure response of the geothermal wells. While we did not have core samples from the Blue Mountain EGS wells, we successfully applied the Utah FORGE analysis approach to the Blue Mountain site with cautious optimism.

New insight of combined hydrothermal and ultrasonic pretreatment for methane production from anaerobic digestion of food waste

ABSTRACT Food waste (FW) biotransformation into bioenergy has garnered a lot of scientific interest as a way to address the energy crisis and trash disposal issues. FW is converted into biogas, a gaseous combination of biomethane and carbon dioxide. In order to valorize FW, anaerobic digestion (AD) with combined pretreatment (hydrothermal (HT) and ultrasonic (US)) is used as a potential method. Three digesters were investigated: the control (unpretreated), HT(121°C) + US, and HT(134°C) + US, respectively. Based on changes in the combined pretreatment conditions, the paper assessed the methane productivity. Furthermore, kinetic modeling was evaluated with six kinetic models. The results show that the HT pretreatment at 121°C combined with US improves the volatile solid (VS) removal to 73 ± 5% and the methane yield to 529.7 ± 11 NmL/gVS. Both the Transference model and the first order have the greatest fits in terms of R2, and they also have the best fits in terms of relative errors, and methane production rate, respectively. The combined pretreatment has a positive impact on increasing methane yield as well as stabilizing the anaerobic digestion process.

Boosting photocatalytic water splitting of TiO2 using metal (Ru, Co, or Ni) co-catalysts for hydrogen generation

The photocatalytic activity of titanium dioxide (TiO2) nanoparticles toward hydrogen generation can be significantly improved via the loading of various metals e.g., Ru, Co, Ni as co-catalysts. The metal co-catalysts are loaded into TiO2 nanoparticles via different deposition methods; incipient wet impregnation (Imp), hydrothermal (HT), or photocatalytic deposition (PCD). Among all of the tested materials, 0.1 wt% Ru–TiO2 (Imp) provided the highest initial hydrogen catalytic rate of 23.9 mmol h−1 g−1, compared to 10.82 and 16.55 mmol h−1 g−1 for 0.3 wt% Ni–TiO2 (Imp) and 0.3 wt% Co–TiO2 (Imp), respectively. The loading procedures, co-catalyst metals type, and their loading play a significant role in elevating the photocatalytic activity of pristine TiO2 semiconductors toward hydrogen generation. Redox transition metals e.g., Co and Ni exhibit comparable photocatalytic performance to expensive elements such as Ru.

Comparing magnetic characteristics of CoSe3xFe2–4xO4 (x ≤ 0.10) spinel ferrite nanoparticles synthesized via Sol-Gel and hydrothermal approaches

In this study, Se substituted Co spinel ferrite nanoparticles (CoSe3xFe2–4xO4 (x ≤ 0.10), CoSe SFNPs) have been synthesized via sol-gel (SG) and hydrothermal (HT) routes and their structural, magnetic and morphological features have been compared. The effect of both the Se substitution and the method of synthesis on the structural, morphological and magnetic features of the host CoFe2O4 have been investigated. The structure and morphology of the SFNPs were examined using XRD, EDX, SEM, TEM and HR-TEM methods. XRD analysis confirmed the single-phase formation of CoSe SFNPs for both HT and SG routes. A TEM study for the HT process demonstrated the development of spherical nanoparticles with uniform size, whereas the SG procedure produced NPs with an indeterminate shape. By examining the hysteresis loops at 300 and 20 K and analysing the temperature-dependent changes in magnetization (M), the magnetic characteristics of CoSe (x ≤ 0.10) SFNPs prepared by the SG and HT methods were investigated. CoSe SFNPs possess magnetically soft and hard natures at 300 and 20 K, respectively. Under each synthesis condition, at 20 K, the SQR values are above 0.5, which signifies well-ordered magnetic domains at this temperature. Across all the materials, as the temperature decreases, zero field cooling (ZFC) branches exhibit a non-linear decline in magnetization which becomes nearly stable in the field cooling (FC) branches. The deviation of the ZFC curve with respect to FC one is more pronounced in the case of SFNPs prepared by the HT process. Our findings demonstrate that by employing the desired synthesis method, Se dopants can be applied to achieve particular magnetic characteristics of CoFe2O4 NPs.

Enhancing Transparency in Non-Cubic Calcium Phosphate Ceramics: Effect of Starting Powder, LiF Doping, and Spark Plasma Sintering Parameters

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.

Preparation of HT/PLA coatings on Zn-Mn-Mg alloy surface for biomaterials in bone tissue engineering

Zinc, as a promising biodegradable metal, has received the attention of many researchers in the medical field. However, zinc-based implants release excessive zinc ions when degraded in the human physiological environment, which in turn leads to high cytotoxicity and low osteogenic capacity. This study aims to further enhance the biocompatibility of zinc alloys while improving their osteogenic properties. For this purpose, calcium-containing phosphate (CaP) interlayer and polylactic acid (PLA) composite layers with different sealing degrees are prepared on Zn–Mn–Mg alloys by hydrothermal (HT) and dip-coating methods. Results show that the PLA layer is tightly bonded to the CaP intermediate layer, and it can effectively prevent early damage at the bone implantation site of the CaP layer on the surface of the zinc alloy. Electrochemical and immersion tests show that the composite layer improves the corrosion resistance of the zinc alloy and that the HT/PLA (12 w/v) coatings show a large CaP deposition on the surface, which suggests that the composite layer obtained from the preparation has good bioactivity. The HT/PLA (12 w/v) composite layer is the most cytocompatible and more suitable for the attachment of MC3T3-E1 cells among all tested samples. This superiority is manifested by increased survival of MC3T3-E1 cells, good attachment morphology, and highest spreading density. This study provides a certain reference value for surface modification of zinc-based materials, which is favorable for future application in degradable orthopedic surgery.

Sustainable Valorization of Coffee Silverskin: Extraction of Phenolic Compounds and Proteins for Enzymatic Production of Bioactive Peptides.

Coffee silverskin (CS), a by-product of the coffee roasting process, has high protein content (16.2-19.0%, w/w), making it a potential source for plant protein and bioactive peptide production. This study aims to develop innovative extraction methods for phenolic compounds and proteins from CS. The conditions for hydrothermal (HT) extraction of phenolic compounds from CS were optimized by varying CS loading (2.5-10%, w/v), temperature (110-130 °C), and time (5-30 min) using a one-factor-at-a-time (OFAT) approach. The highest TPC of 55.59 ± 0.12 µmole GAE/g CS was achieved at 5.0% (w/v) CS loading and autoclaving at 125 °C for 25 min. Following hydrothermal extraction, CS protein was extracted from HT-extracted solid fraction by microwave-assisted alkaline extraction (MAE) using 0.2 M NaOH at 90 W for 2 min, resulting in a protein recovery of 12.19 ± 0.39 mg/g CS. The CS protein was then subjected to enzymatic hydrolysis using protease from Bacillus halodurans SE5 (protease_SE5). Protease_SE5-derived CS protein hydrolysate had a peptide concentration of 0.73 ± 0.09 mg/mL, with ABTS, DPPH, and FRAP values of 15.71 ± 0.10, 16.63 ± 0.061, and 6.48 ± 0.01 µmole TE/mL, respectively. Peptide identification by LC-MS/MS revealed several promising biological activities without toxicity or allergenicity concerns. This study's integrated approach offers a sustainable and efficient method for extracting valuable compounds from CS, with potential applications in the food and pharmaceutical industries.

Multi-color polymer carbon dots synthesized from waste polyolefins through phenylenediamine-assisted hydrothermal processing

The large accumulation and low recycling rates of polyolefin waste have posed a threat to the environment and human health. The shortage of chemical recycling methods for polyolefins strongly demands the development of new and sustainable treatment technologies for hydrocarbon plastics to improve their waste management. In this study, polyethylene (PE) and polypropylene (PP) were utilized for the preparation of multi-color polymer carbon dots (PCDs) via a two-step hydrothermal (HT) synthesis involving (i) thermo-oxidative degradation of polyolefins to precursors containing plentiful oxygen-based functional groups, and (ii) modification with phenylenediamine (PDA). The fluorescence of PCDs depends on the structure of isomeric PDA and PCDs modified by ortho-, meta-, and para-PDA emit blue, green, and yellow color fluorescence, respectively. The formation mechanism of PCDs, involving dehydrative condensation and amination of PE or PP-derived precursors by PDA, was proposed. The obtained PCDs were utilized for the detection and quantification of Fe3+ ions at ppm concentrations. The proposed strategy here aims to broaden the scope of the chemical recycling methods for polyolefin plastic waste as well as to develop a conversion route of polyolefin to value-added materials.

Functionalized magnesium alloys obtained by superplastic forming process retain osteoinductive and antibacterial properties: An in-vitro study

ObjectivesThis study aimed to investigate the biocompatibility, osteogenic and antibacterial activity of biomedical devices based on Magnesium (Mg) Alloys manufactured by Superplastic Forming process (SPF) and subjected to Hydrothermal (HT) and Sol-Gel Treatment (Sol-Gel). MethodsMg-SPF devices subjected to Hydrothermal (Mg-SPF+HT) and Sol-Gel Treatment (Mg-SPF+Sol-Gel) were investigated. The biocompatibility of Mg-SPF+Sol-Gel and Mg-SPF+HT devices was observed by indirect and direct cytotoxicity assays, whereas the colonization of sample surfaces was assessed by confocal microscopy. qRT-PCR analysis and microbial growth curve analyses were employed to evaluate the osteogenic and antibacterial activity of both SPF-Mg treated devices, respectively. ResultsMg-SPF+HT and Mg-SPF+Sol-Gel showed a high degree of biocompatibility. Analysis of mRNA expression of osteogenic genes in cells cultured on Mg-treated devices revealed a significant upregulation of the expression levels of BMP2 and Runx-2. Furthermore, the bacterial growth in strains developed in contact with both the Mg-SPF+HT and Mg-SPF+Sol-Gel devices was lower than that observed in the control. SignificanceHydrothermal and Sol-Gel Treatments of Mg alloys obtained through the SPF process demonstrated bioactive, osteogenic and antibacterial activity, offering a promising alternative to conventional Mg-based devices. The obtained Mg-based materials may have the potential to enhance the tunability of temporary devices in maxillary reconstruction, eliminating the need for second surgeries, and ensuring a good bone reconstruction and a reduced implant failure rate due to bacterial infections.

Microwave-Assisted Hydrothermal Synthesis of Pure-Phase Sodalite (>99 wt.%) in Suspension: Methodology Design and Verification.

Despite numerous studies focused on the hydrothermal (HT) synthesis of fly ash zeolites (FAZs), this method still has many limitations, the main of which is the low yield of zeolites. Hydrothermally synthesized zeolites are typically multiphase and exhibit low purity, which limits their applicability. Pure-phase zeolites have been primarily prepared from filtrates after alkaline mineralization of fly ashes, not directly in suspension. In addition, the published methodologies have not been tested in a wider set of samples, and thus their reproducibility is not confirmed. The aim of the study is to propose a reproducible methodology that overcomes the mentioned limitations. The influence of the Si/Al ratio (1.3:1-1:2), the type and concentration of the activator (2/4 M NaOH/KOH/LiOH), the reagent (30% LiCl), the duration (24-168 h), and the temperature (50-180 °C) of the synthesis phases were studied. The sequence of the synthesis phases was also optimized, depending on the type of heat transfer. The fly ashes were analyzed by wavelength-dispersive X-ray fluorescence (WD XRF), flame atomic absorption spectrometry (F-AAS), and X-ray diffraction (XRD). The energy intensity of the synthesis was reduced through the application of unique microwave digestion technology. Both microwave and combined (microwave and convection) syntheses were conducted. FAZs were identified and quantified by XRD analysis. This study presents a three-stage (TS) hydrothermal synthesis of pure-phase sodalite in suspension. Sodalite (>99 wt.%) was prepared from nine fly ashes under the following conditions: I. microwave phase: 120 °C, 150 min, solid-to-liquid ratio (S/L) 1:5, Si/Al ratio 1:1.5, and 4 M NaOH; II. convection phase: 120 °C, 24 h, S/L 1:40, and the addition of 30 mL of 30% LiCl; and III. crystallization: 70 °C for 24 h. The formation of rhombododecahedral sodalite crystals was confirmed by scanning electron microscope (SEM) images.

Strong green upconversion emission from submicron spindle-shaped SrMoO4:Yb3+,Er3.

Upconversion luminescence (UCL) is a fluorescence process where two or more lower-energy photons convert into a higher-energy photon. Lanthanide (Ln3+)-doped UCL materials often suffer from weak luminescence, especially when directly synthesized by a hydrothermal (HT) process due to the existing hydroxyl group and undesirable arrangement of dopants within host lattices which quench luminescence and limit energy transfer. Therefore, additional heat treatment processes are required to enhance their UCL emission, even though direct hydrothermal synthesis without further heat treatment has the advantages of low energy consumption, fast synthesis, and wide applicability to generate UCL materials. In this study, via a HT process without annealing, we have produced Yb3+ and Er3+ co-doped SrMoO4 submicron spindles with a strong green UCL emission which can be seen with the naked eye, which HT produced oxide-based UCL materials often fail to demonstrate. We have investigated different HT synthesis conditions, such as temperature, time, pH and dopant composition, which control the nucleation, growth, lattice structure arrangement, and ultimately their UCL properties through XRD, SEM, EDS and UCL measurements. The bright green UCL from the SrMoO4:Yb,Er submicron spindles is further enhanced by post-synthesis annealing within a molten NaNO3/KNO3 system to prevent particle size growth. The green UCL intensity from the annealed SrMoO4:Yb,Er submicron spindles surpasses samples produced by the solid-state method and is comparable to that from the commercial NaYF4:Yb,Er sample. We have further studied the temperature-dependent luminescence of both the HT-prepared and molten-salt annealed SrMoO4:Yb,Er submicron spindle samples. The strong UCL from our SrMoO4:Yb,Er submicron spindles could warrant their candidacy for bioimaging and anticounterfeiting applications.