Synthesis Time Research Articles

Luminescent carbon nanoparticles obtained by microwave assisted hydrolysis from dextrin

Carbon nanoparticles (CNPs) were synthesized by acid hydrolysis from dextrin by the microwave-assisted method. The effect of temperature and synthesis time on morphology, size, UV–Vis absorption, and photoluminescence properties was studied. An increase in temperature from 135 to 180 °C decreases the CNPs diameter from 17.8 to 9.7 nm. Similarly, an increase in synthesis time from 2 to 5 min promotes a decrease in sizes from 13.1 to 6.7 nm. UV–Vis absorption spectroscopy and photoluminescence studies indicated that the nanoparticles have a maximum absorbance around 300 nm and when the CNPs are excited with λ close to 400 nm, λ emission occurs in the range of 500–650 nm. CNPs were synthesized maintaining synthesis conditions of 150 °C, for 5 min, varying the type of acid (H2SO4 and CH3COOH) and pH before subjecting the solution to microwave irradiation. It was observed that, when CH3COOH is used as a hydrolysis agent instead of H2SO4, the intensity of the emission increases. Regarding pH, it was observed that CNPs synthesized at alkaline pH have greater photoluminescence than those synthesized at acid pH.

Synthesis of Silver Nanoparticles (NPPs) Using Xylocarpus Granatum Fruit Extract and its Application in Heavy Metal Pollution Detection

Heavy metals are dangerous pollutants because they are toxic, non-biodegradable, and stable. Mercury (Hg) is a type of heavy metal that is often a source of pollution in the aquatic environment. The biosynthesis process of nanoparticles using Xylocarpus granatum fruit extract as a bioreductant has been carried out using the green synthesis method. The research was conducted to synthesize silver nanoparticles (NPP) from Xylocarpus granatum fruit extract to detect heavy metals. The optimum condition of NPP was obtained through the comparison of AgNO3 concentration with extract and reaction time. The optimum NPP produced was at a concentration of AgNO3 1 mM 1:1 at a synthesis time of 2 hours. The NPP formed is selective to Hg metal as can be seen from the color change of NPP from dark brown to clear and sensitive to Hg metal at a concentration of 40 ppm. The calibration curve formed obtained a linear regration value of the relationship between the concentration of Hg standard solution and absorbance, namely y = -0.01330 + 3.71658 with a coefficient of determination (R2) value of 0.99229. Based on the standard curve obtained NPP mangrove fruit extract Xylocarpus granatum has an accuracy of 99.229% in predicting the concentration of the sample.

Microwave Assisted Williamson Synthesis: A Green Approach towards the Preparation of Ethers

Introduction: Microwave-assisted reactions align with the principles of green chemistry by significantly reducing synthesis time, avoiding high temperatures, and typically yielding high product quantities. Method: A catalyst was synthesized from waste banana peels, ensuring both availability and lowcost production. Ethers were synthesized using microwave irradiation at 300W, employing two different alkyl halide variants with both substituted and unsubstituted phenols. Results: The reaction proceeded efficiently without the need for corrosive bases such as caustic soda or caustic potash. Microwave irradiation facilitated reduced reaction times for ether formation. Additionally, the supported catalyst demonstrated the advantage of reusability. Conclusion: This protocol offers several benefits, including the use of a green solvent and the exclusion of phase transfer catalysts and harsh conditions. Consequently, an efficient and green synthesis of ethers has been achieved.

Facile synthesis of SSZ-16 nanoaggregates with excellent performance in NH3-SCR reaction

d6r units were proved to be crucial for the synthesis of SSZ-16 zeolite with AFX topology, and FAU zeolite owning plenty of d6r units was chosen as the essential raw material for constructing AFX frameworks. In this work, SSZ-16 zeolite was directly synthesized using colloidal silica and sodium aluminate as the raw materials in short crystallization time of 5 h. The corresponding crystallization process were carefully investigated by various characterizations, demonstrating that the key to this success was the formation of d6r units built up by a large amount of s4r units which were formed with the assistance of the appropriate organic structure directing agent (OSDA) and seeds in the synthetic media. Interestingly, the products of C-SSZ-16 zeolites presented spherical shapes consisted of relatively small particles with size range from 30 to 50 nm. Moreover, after ion-exchanged with Cu ions, the Cu-C-SSZ-16 products showed excellent performance in the selective catalytic reduction of NOx with NH3 (NH3-SCR) and better hydrothermal stability than conventional Cu-SSZ-16-con samples due to slightly higher Si/Al ratio of the Cu-C-SSZ-16. Therefore, remarkable catalytic performance and the use of low-cost raw materials as well as short period of synthesis time make AFX zeolites as potential applicants in NH3-SCR field, from an industrial viewpoint.

Rapid synthesis and enhanced microwave absorption of carbon-supported high-entropy metal oxide

Complex preparation process and long annealing time of high-entropy metal oxide (HEO) limit its extensive application as microwave absorber at civil and military fields. Herein, a rapid synthesis method of mesocarbon microbeads (MCMB)-loaded spinel structure (FeCoCrNiMnCu)O is studied via plasma flow. In the presence of extreme plasma heating rate, a nanoscale high-entropy phase can be formed while modifying the surface activity of carbon. Simultaneously, due to the short synthesis time, gaseous conversion of carbon under high temperature aerobic conditions is avoided. By appending of carbon, the dual-media absorber exhibits better absorption performance with a maximum peak (-44.7 dB), which achieves over 90 % absorption in 11.2–15.5 GHz with a thickness of only 1.9 mm. Interestingly, the real and imaginary parts of complex permittivity increase remarkably. The former change is attributed to the expansion of heterogeneous hole carrier region and the latter dues to the interfacial polarization of the strongly coupled interface. The increase of dielectric loss and conductance loss leads to great improvement of microwave absorption. Our study injects new vitality into the preparation of HEO for advanced applications and the as-prepared HEOM is promised to be high-efficient microwave absorber based on robust stability and excellent absorbing performance.

Hydrothermal synthesis of bioactive calcium silicate glass

This work presents the synthesis of bioactive glass 60SiO2-40CaO (wt.%) by the hydrothermal method without using acid catalysts in shortened synthesis time. The precursors Si(OC2H5)4 (TEOS), Ca(NO3)2.4H2O were introduced in a hydrothermal system, and heated at 150 oC for 24 hours. The resulting gel was dried at 150 oC for 24 hours, then calcined at 800 oC for 3 hours to achieve bioactive glass. Several physical-chemical methods such as TG-DSC, XRD, SEM, and ICP-OES were used to evaluate the synthetic material. The bioactivity and biocompatibility of synthetic glass were evaluated by in vitro experiments in SBF solution and in cell culture environment. The obtained results show that the synthetic glass is an amorphous material, presenting the bioactivity through the formation of a hydroxyapatite mineral layer after 10 days of soaking in SBF solution, and also showing good biocompatibility with cells L-929. Keywords: Bioactive glass, bioactivity, artificial bone, hydroxyapatite, cell viability

Microwave-Assisted Hydrothermal Synthesis of Photocatalytic Truncated-Bipyramidal TiO2/Ti3CN Heterostructures Derived from Ti3CN MXene.

TiO2/MXene heterostructure has garnered significant interest as a photocatalyst due to its large surface area and efficient charge carrier separation at the interface. However, current synthesis methods produce TiO2 without clear crystal faceting and often require complicated postprocessing step, limiting its practical applications. We demonstrate a facile and controlled microwave-assisted hydrothermal synthesis for transforming multilayered Ti3CN MXene to a truncated-bipyramidal TiO2/Ti3CN heterostructure. The resulting TiO2 nanocrystals at the Ti3CN surface exhibited crystalline anatase truncated bipyramids, exposing {001} and {101} facets. We further tailored an indirect optical band gap of the TiO2/Ti3CN heterostructure in the range of 3.17-3.23 eV by varying the hydrothermal synthesis time from 15 min to 5 h at a fixed temperature of 160 °C. Efficient charge separation allowed us to decompose 97% of methylene blue (MB) within 30 min of ultraviolet (UV) light irradiation, ∼3.9-fold faster than the benchmark P25, higher than any other TiO2/MXene heterostructures. With simulated white light, we achieved over 60% efficiency of the dye decomposition within 2 h of irradiation, which resulted in 1.5-fold faster kinetics than P25. We also observed a similar excellent performance of Ti3CN-derived TiO2 in decomposing various persistent synthetic dyes, including commercial textile dye, methyl orange, and rhodamine B. In conclusion, our study provides a strategy for utilizing MXene chemical reactivity to produce highly crystalline optically active TiO2/Ti3CN heterostructure. The developed heterostructure can serve as an efficient photocatalyst for the degradation of organic pollutants.

Electrochemical Detection of H2O2 Using Bi2O3/Bi2O2Se Nanocomposites.

The development of high-performance hydrogen peroxide (H2O2) sensors is critical for various applications, including environmental monitoring, industrial processes, and biomedical diagnostics. This study explores the development of efficient and selective H2O2 sensors based on bismuth oxide/bismuth oxyselenide (Bi2O3/Bi2O2Se) nanocomposites. The Bi2O3/Bi2O2Se nanocomposites were synthesized using a simple solution-processing method at room temperature, resulting in a unique heterostructure with remarkable electrochemical characteristics for H2O2 detection. Characterization techniques, including powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM), confirmed the successful formation of the nanocomposites and their structural integrity. The synthesis time was varied to obtain the composites with different Se contents. The end goal was to obtain phase pure Bi2O2Se. Electrochemical measurements revealed that the Bi2O3/Bi2O2Se composite formed under optimal synthesis conditions displayed high sensitivity (75.7 µA µM-1 cm-2) and excellent selectivity towards H2O2 detection, along with a wide linear detection range (0-15 µM). The superior performance is attributed to the synergistic effect between Bi2O3 and Bi2O2Se, enhancing electron transfer and creating more active sites for H2O2 oxidation. These findings suggest that Bi2O3/Bi2O2Se nanocomposites hold great potential as advanced H2O2 sensors for practical applications.

Time-Dependent Hydrothermal Synthesis of La2O3 NPs for Effective Catalytic Activity of Ionic Dye.

Lanthanum oxide was successfully synthesized by hydrothermal method by varying the reaction time such as 6, 12, and 24 h. In XRD, study confirms the presence of a hexagonal structure, and the phase remains the same at different times; the main goal is to assess the average crystallite size of prepared La2O3 nanoparticles, which was found in the range of 6 to 8 nm. An interesting observation from the XRD data was the apparent increase in crystalline nature as the synthesis time was extended. The UV-Vis spectroscopic studies show a change in the band gap when the reaction time is changed. The morphology analysis shows that the image revealed that the particles formed were agglomerated and formed a spherical shape, with diameters ranging between 35 and 86 nm. When tested for photocatalytic activity, the La2O3 nanoparticles show a degradation of methylene blue dye when the time varies. Remarkably, the nanoparticles synthesized exhibited a profound ability to degrade the dye, with an efficiency rate hitting as high as 89% under halogen light illumination.

Synthesis of Ternary Layered Double Hydroxides and Application for Wastewater Treatment

AbstractThis study systematically investigates the optimization of synthesis parameters for ternary layered double hydroxide (LDH) to achieve a pure phase and high crystallinity. The , LDH is synthesized using the coprecipitation method and applied for wastewater treatment. The ternary LDH is synthesized at 60 °C for 24 h and exhibited maximum crystallinity with a crystallite size of 4 nm. The crystallinity index (CI) is a quantitative indicator of crystallinity, which is calculated using the X‐ray diffraction (XRD) method. The influence of reaction time on the structural characteristics of this LDH was thoroughly investigated, mainly focusing on achieving well‐crystalline LDH. Experimental results revealed a direct correlation between reaction time and crystallinity. This study highlights the significant influence of controlled synthesis and reaction time on producing high crystalline ternary LDH. The role of different parameters, such as solution pH, adsorbent dosage, contact time, and dye concentration, has been investigated. The adsorption isotherm data is analyzed using different isotherm models, which shows this material having a significant adsorption capacity of 82.92 mg/g for Congo Red dye.

Magnetic graphene oxide incorporated with Fe2O3 for the removal of lead (II) ions

The objective of this research work is to synthesise graphene oxide (GO) with iron oxide (Fe2O3) nanoparticles as a magnetic adsorbent for lead ion (Pb2+) removal. In this work, the effect of synthesis parameters of GO/Fe2O3 (Fe2O3 loading weight ratio, synthesis time and calcination temperature) and adsorption parameters (initial Pb2+ concentration, adsorption temperature and contact time) on Pb2+ removal were investigated. The adsorption experiment was carried out in a batch system, and the synthesised GO/Fe2O3 adsorbent was characterised using TGA and N2 sorption-desorption analyses. The adsorption characteristics of Pb2+ using GO/Fe2O3 adsorbent were analysed using adsorption isotherms and kinetic study. The optimal synthesis parameters were found to be a 1:0.5 ratio for GO/Fe2O3, a synthesis time of 60 min and a calcination temperature of 400°C, resulting in a Pb2+ removal rate of 96% and adsorption capacity of 49.85 mg Pb2+/g adsorbent. The GO/Fe2O3 adsorbent synthesised at 400°C and a 1:0.5 ratio exhibits a larger surface area and smaller pore diameter, 98.20 m2/g and 15.67 nm, respectively, compared to other samples. Increasing the synthesis temperature decreases the growth and formation of GO/Fe2O3, reducing the surface area. Experimental results revealed that the adsorption of Pb2+ using GO/Fe2O3 adsorbent fitted the pseudo-second-order kinetic and was best described by the Langmuir isotherm with a high correlation coefficient (R2 >0.99).

FEATURES OF THE INTERACTION AND FORMATION OF NANOSTRUCTURED CHITOSAN SYSTEMS DURING IONOTROPIC GELATION

Bombyx mori chitosan nanoparticles (ChS NPs) were obtained and the kinetic aspects of their size distribution depending on the degree of nonequilibrium of the synthesis by ionotropic gelation using sodium tripolyphosphate (TPP) were studied. The size of ChS NPs was greatly influenced by the ChS concentration, which varied from 0.5 to 10 mg/ml. The size of the NPs increased from 100 to 300 nm when the ChS concentration increased from 0.5 to 10 mg/ml and while maintaining all other parameters of the reaction. An increase in the ChS to-TPP ratio corresponded to a lower cross-linking density and thus ensured slower kinetics for NP formation alongside the formation of large chitosan/TPP aggregates. There was an almost threefold increase in the particle size when the pH of the medium increased from 3.8 to 4.7; thus, the size of ChS NPs depends on the pH of the solution. There was a slight agglomeration of NPs from 363 to 642 nm with an increase in the NP synthesis time from 4 to 24 h. According to calculations, the maximum interaction energy is 50.4 and 69.4 kcal/mol for deprotonated TPP (P3O105-); after adiabatic transfer of the proton, the value decreases to 32.9–33.5 kcal/mol. The maximum interaction energy is –12.8 kcal/mol for the initially protonated TPP (H4P3O10-).

Comprehensive Evaluation of Process Parameters in the Green Synthesis of Iron Oxide Nanoparticles Using Moringa olifera extract.

This study investigates the green synthesis of iron oxide nanoparticles using Moringa olifera ethanolic extract and evaluates the impact of various process parameters on their physicochemical characteristics. The parameters examined include synthesis time, temperature, pH, stirring speed (RPM), and the ratio of extract to iron precursors. The findings reveal that a lower proportion of the extract increases the entrapment efficiency of the nanoparticles. Specifically, batch ME3 (3:1 ratio) produced the smallest nanoparticles at 117.8 nm, with a drug release of 75.54% and the highest entrapment efficiency at 60.28%. Extending the synthesis time to three hours in batch TM3 resulted in a drug release of 74.23% and a particle size of 116.3 nm. Batch TEM1, synthesized at 70°C, showed the highest entrapment efficiency and a favorable drug release profile of 71.09%, with the smallest particle size of 105.24 nm, suggesting that higher synthesis temperatures favor smaller particle sizes. Adjusting the pH to 10 in batch PM3 achieved a drug release efficiency of 76.02%. Batch RM5, synthesized with a stirring speed of 750 RPM, demonstrated a particle size of 95.7 nm and a drug release of 78.26%, indicating that higher stirring rates produce smaller nanoparticles and enhance drug release. These results highlight the significance of optimizing synthesis conditions to produce nanoparticles with desired properties. The use of M. olifera extract as a sustainable reducing and stabilizing agent presents an environmentally friendly approach to nanotechnology. This method has potential applications in drug delivery systems and various other industries, emphasizing the importance of green synthesis in creating sustainable and efficient nanomaterials.

Evaluation of an automated synthesis method for [18F]Fluoromisonidazole using a Scintomics GRP® module

There is limited information on utilizing commercially supplied [18F]Fluoride from an off-site cyclotron for the synthesis of radiopharmaceuticals. This study explored the production of the PET hypoxia marker [18F]FMISO, using the Scintomics® GRP module and distantly produced [18F]Fluoride, which lacks published data. A radiochemical yield of 27.4 ± 3.6% (n = 5) and high radiochemical purity were achieved in synthesis time of 48 min. The [18F]FMISO met all Ph. Eur. standards, demonstrating the consistency and reliability of the module in generating a clinical-grade radiopharmaceutical using off-site produced [18F]Fluoride, but available patient doses were severely limited.

One-step microwave-assisted synthesis of metal-free heteroatom-doped carbon catalyst for H2O2 electrosynthesis

This study reports on a one-step conversion of polyaniline into a metal-free heteroatom-doped carbon electrocatalyst through microwave heating. A high surface area carbonaceous structure forms after a total synthesis time of only 140 s, with the presence of nitrogen and oxygen functional groups, as confirmed by thorough spectroscopic analysis. This catalyst exhibits high activity (onset potential of 0.73 V vs. RHE), selectivity (82 %), and stability (over a 7.5-hour test period) for the electrochemical oxygen reduction reaction towards hydrogen peroxide in alkaline media. Microwave synthesis reduces heating time by 29-fold and energy consumption by 77-fold, while producing materials with high electrocatalytic efficiency comparable to those conventionally prepared at 700°C. The microwave and the conventionally synthesized heteroatom-doped carbon catalysts show similar electrochemical performances, which can be attributed to the presence of nearly identical nitrogen functional groups and surface area in the two samples. In contrast, the microwave and conventionally synthesized samples exhibit significant variations in their oxygen functional groups. These results suggest that nitrogen functional groups are the main active sites for alkaline hydrogen peroxide formation, while oxygen functional groups play a minor role in the catalytic activity. Our work brings a solid contribution to the debate regarding the active centers for hydrogen peroxide formation.

Effect of synthesis time on the photocatalytic performance of aggregated CuBO₂ microstructures for photo induced hazardous dye removal

Effect of synthesis time on the photocatalytic performance of aggregated CuBO₂ microstructures for photo induced hazardous dye removal

Portable Electrochemical Immunosensor Based on a Gold Microblobs-Optimized Screen-Printed Electrode for SARS-CoV-2 Diagnosis

The development of biosensors for determining the most diverse biomolecules is a constant focus of many research groups. There is a latent need to propose sensors that combine portability, simple measurements, and good analytical performance. Here, we propose an electrochemical immunosensor that is fully portable and energy-independent for diagnosing antibodies against SARS-CoV-2 (the virus that causes COVID-19). Initially, disposable screen-printed carbon electrodes (SPEs) were covered by gold microblobs (AuMBs), which were synthesized amperometrically from Au3+ ions. Then, the SPE-AuMBs were coated with cysteamine, which allowed the N-hydroxysuccinimide-activated SARS-CoV-2 antigen (spike protein) to be immobilized. The antigen-activated electrode was used to detect COVID-19 antibodies from current measurements obtained by differential pulse voltammetry. The AuMBs synthesis time was optimized, and the presence of gold structures improved the electrochemical responses of the SPE. It was possible to quantitatively determine antibodies in the concentration range of 0.25 to 10 µg mL−1. This range includes concentrations found in biological fluids from patients at any stage of the disease. An analysis took approximately the same time as traditional rapid nasal tests (20 min) and costed less, considering all the steps necessary to prepare a disposable antigen-functionalized SPE.

Improving hypercrosslinked polymer CO2/N2 selective separation through tuning polymer's porous properties: Optimization using RSM-BBD

This study investigates the effect of synthesis and operating parameters on the adsorption of CO2 and N2 and the CO2/N2 selectivity of a hypercrosslinked adsorbent based on waste-expanded polystyrene. Six factors were examined, including synthesis time, crosslinker and catalyst amounts, adsorption temperature and pressure, and CO2 percentage in the mixture. The response surface methodology (RSM) and ideal adsorbed solution theory (IAST) were employed to design the experiment. After synthesizing 19 adsorbents under different conditions, characterization tests were conducted. Results indicate that the specific surface area and micropore volume initially increase and then decrease with increased synthesis time, crosslinker, and catalyst amounts. The highest specific surface area and micropore volume were 803.84 m2/g and 0.1355 cm3/g, respectively. CO2/N2 selectivity and the adsorption of CO2 and N2 also increase and decrease with increased synthesis parameters. Furthermore, it was observed that CO2 adsorption and CO2/N2 selectivity increased with an increase in pressure and CO2 percentage and a decrease in temperature, while N2 adsorption decreased. The adsorbents were optimized using RSM to maximize CO2 adsorption and CO2/N2 selectivity with a target of 15 % CO2 in the gas mixture. The optimal synthesis parameters for the hypercrosslinked adsorbent, including synthesis time, crosslinker, and catalyst amounts, were determined to be approximately 13 hours, 30 mmol, and 30 mmol, respectively. Under optimal conditions for flue gas applications (CO2:N2/15:85), the adsorbent demonstrated a CO2/N2 selectivity of 11.05, making it suitable for flue gas capture.

Synthesis, characterization, and catalytic activity of zinc-isonicotinic acid MOF

The synthesis and characterization of Zn (INA) microcrystalline MOF was conducted, revealing its high catalytic activity in the production of substituted benzyl alcohol (BzOH) to substituted benzaldehyde (BzA). The MOF was found to be cost-effective and efficient, with a short synthesis time and moderate reaction conditions. The MOF's structure was confirmed through XRD, SEM, and TEM imaging, and its purity was confirmed through EDS analysis. The TGA investigation revealed significant thermal stability with minimal weight loss and BET studies shows the substantial surface area and pore volume, suggesting potential for various industrial uses. The MOF's efficiency under mild reaction conditions, low cost, and absence of noble metals makes it a promising candidate for sustainable catalytic applications.

Energy-efficient removal of trace VOCs from humid air using metal-organic gel derived porous carbon

The development of granular adsorbents for the efficient capture of low-concentration volatile organic compounds (VOCs) from humid air are highly desirable. Herein, we report the synthesis of granular ZIF-8 monolith (monoZIF-8) featuring high surface area (2312 m2/g) and mesoporous structure by shortening the synthesis time and optimizing the reactant concentrations, which was further carbonized at 1000 °C to obtain porous granular carbon. As-prepared ZIF-8-C1000 exhibited high surface area (1623 m2/g), hierarchical porous structure (0.5–10 nm) and hydrophobicity (water contact angle 145.8°), thus it showed very high adsorption performance for trace VOCs like toluene and hexanal under both dry and humid conditions (relative humidity 30 %-80 %) at 25 °C, much higher than commercial activated carbon (AC) such as BPL-AC, coconut shell AC, and representative MOFs including HKUST-1, monoHKUST-1, monoMIL-100(Fe), MIL-101(Cr) and MOF-235. Additionally, ZIF-8-C1000 could be rapidly regenerated under mild temperatures (60 °C to 80 °C), while BPL-AC requires a higher desorption temperature and more time due to disordered porosity. The exceptional adsorption and desorption performance of granular ZIF-8-C1000 over BPL-AC can be attributed to its interconnected micropores and mesopores.