Reflux Route Research Articles

Cerium-infused tungstate nanocrystals: Illuminating the future of solid-state lighting

Rare earth based luminescent materials have emerged as a focal point of the scientific investigation owing to their remarkable optical behaviour and potential applications. An effort has been made to develop a series of Ce3+ doped CaWO4 nano-phosphors using an ethylene-glycol assisted reflux route. The detailed structural and morphological properties have been examined through various analytical techniques. The +3-oxidation state of the activator ion Ce has been verified through the XPS study. The change in optical band gap due to the substitution is well discussed using diffuse reflectance spectroscopy. In Photoluminescence study, a broad emission centred at 465 nm is observed due to the 5D3/2→2FJ transitions (J = 7/2 and 5/2) and a significant enhancement in the emission peak is obtained for the optimized phosphor. Concentration quenching phenomenon, observed after 3 mol% of Ce3+ is mainly mediated by the electric multipole-multipole type interaction. The CIE diagram indicates the tuning of emission colour from blue to white region and the emission near white region for the optimized phosphor is further authenticated by its low colour purity value (43 %). The effective tunability of photo-physical properties and colorimetric parameters suggest the applicability of the optimized nano-phosphor in solid state lighting especially for outdoor illumination.

Submental Artery Perforator Flap Drained Solely With the Vena Comitans of Facial Artery.

The submental artery perforator flap (SMAPF) is an alternative to reconstruct oral and maxillofacial defects secondary to oral cancers. However, vascular anomalies or surgical damage often lead to vascular crises or harvest failure. Our clinical findings suggest that the vena comitans of the facial artery (cFA) very commonly exist. This study aimed to investigate the reliability of the cFA as a sole venous reflux route for the SMAPF. The patients were from the Department of Oral and Maxillofacial Surgery, Hospital of Stomatology, Jilin University. All patients were treated for oral cancer between January 2016 and September 2022. Seventeen SMAPFs were successfully raised to reconstruct the postoperative defects, of which 7 had cFA as the sole reflux route. The size of the flaps varied from 4.0×3.0cm to 12.0×3.0cm. All flaps survived. Patients were followed from 1 month to 5 years. Satisfactory restoration of contour and functional outcomes were achieved at the recipient sites. The scars were well camouflaged in the submental region. No local or regional recurrence was detected during follow-up. Patients had an overall 2-year survival rate of 100% with no suspected flaps-related recurrence. The cFA as the sole venous reflux route for SMAPF is reliable for flap harvesting and is applicable for immediate defect reconstruction secondary to cancer resection.

CuMn2O4 anchored on graphene sheets as a high-performance electrodes for sodium-ion batteries

A novel class of CuMn2O4 (CMO) nanoparticles were synthesized by the reflux route method and explored as an anode in sodium-ion batteries. This work deals with the homogenous distribution of CuMn2O4 (CMO) nanoparticles interconnected within the graphene sheet. HR-TEM deceptively evidences the homogeneous distribution and well-defined CuMn2O4 nanoparticles over graphene sheets (CMO/G). This appropriately designed architecture of CMO/G allows adequate void space to assimilate the substantial volume fluctuation during cycling, improve reaction sites, and enhance electron transport, resulting in significant electrochemical performance as an anode in sodium-ion batteries. The CMO/G anode showed a high capacity of 313 mAh g−1 at 100 mA g−1 with 70 % capacity retention after 50 cycles, and under the high current of 2 A g−1, it exhibits as high as 145 mAh g−1. Moreover, the title anode is capable of delivering stable appreciable capacity of 164 mAh g−1 for extended 300 cycles at 1 A g−1. CMO/G composite anode has been validated as a high-efficient anode for sodium-ion battery applications in this study.

In-situ synthesis of structurally oriented hierarchical UiO-66(–NH2)/CdIn2S4/CaIn2S4 heterostructure with dual S-scheme engineering for photocatalytic renewable H2 production and asulam degradation

The in-situ fabrication of dual S-scheme ternary heterostructure is a promising approach to isolate photo-induced electron-hole and boost the efficiency of a semiconductor photocatalyst. However, the dual S-scheme heterostructure based on MOFs are rarely narrated. Herein, a S-vacancy rich hierarchical UiO-66(–NH2)/CdIn2S4/CaIn2S4 ternary hybrid material is successfully fabricated by in-situ preferential growth of ultrathin CaIn2S4 nanosheets and CdIn2S4 nanorods in presence of UiO-66(–NH2) (UN) spherical nanoparticles by using a simple reflux route. The physiochemical characteristics and optoelectronic features of the developed materials are illustrated in detail. The efficacy of UiO-66(–NH2)/CdIn2S4/CaIn2S4 ternary hybrid material is explored for photocatalytic H2 evolution reaction and decontamination of asulam (ASM) herbicide. The development of S-vacancy facilitates interfacial charge carrier migration and reduces the recombination rate. The enhanced photocatalytic H2 production and ASM degradation could be ascribed to staggered band alignment between UiO-66(–NH2) (UN), CdIn2S4 (CDS) and CaIn2S4 (CAS), which support S-scheme charge channelization in the heterojunction. Due to its physio-chemical advantages, the optimal 15UN/CDS/CAS30 hybrid photocatalyst exhibits highest photocatalytic H2 evolution rate of 4931 μmol g−1h−1 with apparent conversion efficiency of 31.5% and ASM degradation > 93% (k = 0.02 min−1) under irradiation of visible light. This work furnishes a new perceptive into the in-situ construction of dual S-scheme photocatalytic systems for renewable energy production and decontamination of organic pollutants. In addition, this study for the first time illustrates mineralization of Asulam using a heterogeneous photocatalytic route.

Facile low temperature reflux synthesis of Bi self-doped Bi2MoO6 and construction of CaFe2O4/Bi2MoO6 0D QD-2D p-n heterojunction photocatalyst for efficient bisphenol A degradation and Cr(VI) reduction

In this study, a mild reflux route was developed for facile synthesis of Bi-self doped Bi2MoO6 (BMOR) with nanoplate morphology. Microstructural study revealed substitution of Bi5+ ions in the molybdate layer which resulted in partial reduction of Mo6+ to Mo5+ ions and creation of Mo vacancy. The defect engineered BMOR material exhibited improved optical and photoelectrochemical properties compared to its undoped analogue. The BMOR material was subsequently employed as host lattice for construction of CaFe2O4/Bi2MoO6 0D-2D p-n heterojunctions by using an in situ preparative strategy. Well dispersed CaFe2O4 quantum dots over BMOR nanoplates provide a strong interfacial contact conducive for fast charge mobilization. Comprehensive characterization of the composites revealed extended UV–vis response, improved charge carrier separation, prolonged excited state life time and robust radical generation efficiency compared to pure components. The CaFe2O4/Bi2MoO6 composites displayed improved photocatalytic performance for bisphenol A (BPA) degradation (kapp = 0.0132 min−1) and Cr(VI) reduction (kapp = 0.15 min−1) with reaction rates 5–9 times higher than pure components. The involvement of •OH and •O2− radicals in the photodegradation of BPA was confirmed from radical trapping study. The formation of an interfacial p-n heterojunction and a double charge migration mechanism accounted for the improved photocatalytic efficacy of the composite.

Morphology and Vibrational Modes of Lanthanum Oxide (La2O3) Nanoparticles Prepared with Reflux Routes at Different Reaction Times

Morphology and Vibrational Modes of Lanthanum Oxide (La2O3) Nanoparticles Prepared with Reflux Routes at Different Reaction Times

Preparation and characterization of Co doped TiO2 for efficient photocatalytic degradation of Ibuprofen

Photocatalytic degradation of Ibuprofen (IBU) which is an anti-inflammatory drug was investigated in aqueous solution by Co-doped TiO2 and bare TiO2 synthesized by reflux route. The prepared catalyst powders were fully characterized using X-ray diffraction (XRD), FT-IR spectroscopy, scanning electron microscopy (SEM), BET surface areas, X-ray Fluorescence Spectroscopy (XRF), dynamic light scattering (DLS). Efficiency of photocatalytic activity for synthesized Co-doped and bare TiO2 was evaluated for the degradation of IBU under UV-C and visible irradiation by investigating the effects of cobalt doping percentage, amount of catalyst, irradiation time, initial IBU concentration, pH and also the effect of organic and inorganic matrix. At optimum degradation conditions under UV-C light and visible light, photocatalytic degradation rates were monitored using UV/Vis spectrophotometer, HPLC and Total Organic Carbon (TOC) analysis. The results showed up the degradation of IBU was improved upon Co doping. It was detected that complete removal was achieved within 240 min of irradiation under UV-C and 98% of IBU was decomposed under visible light in 300 min.

Enhanced E. coli Capturing Efficacy Over Magnetic Dextrin–Cobalt Sulfide Nanohybrid as a Promising Water Disinfection System

The aim of this research is synthesis of a promising bacterial elimination nanohybrid for water disinfection. Hence dextrin, a carbohydrate polymer composed of linear α-(1,4)-linked d-glucose, is used as an intermediate to prepare Fe3O4–dextrin–CoS nanohybrid. At the first step magnetic dextrin was prepared by one step ultrasound assisted route using Fe2+ as iron source and dextrin as capping agent. At the second step functional groups of dextrin was employed to trap Co2+ ions for decorating CoS at the biosorbent structure through refluxing route. The structure of the magnetic dextrin and nanohybrid was studied by XRD, EDX, FESEM, TGA and zeta potential measurement. EDX and TGA results confirmed that the CoS has been decorated with high density onto magnetite dextrin structure. The prepared nanohybrid has been employed to capture Escherichia coli as a sample pathogen from water solution. Effective parameters on bacterial elimination, i.e., pH, contact time, nanohybrid dosage and presence of anions have been studied. Results showed that at pH of 3.5, contact time of 15 min and nanohybrid dosage of 20 mg E. coli capturing efficacy was more than 99% which confirmed high efficiency of the nanosystem in bacteria elimination from water solution.

A sensitive electrochemical sensor based on functionalized graphene oxide/SnO2 for the determination of eugenol

A nanocomposite of functionalized graphene oxide decorated tin oxide (APTMS-GO@SnO2) nanoparticles was successfully synthesized using a refluxing route. The carbon paste electrode (CPE) modified with an APTMS-GO@SnO2 nanocomposite showed good electrocatalytic activity for eugenol oxidation in a 0.1 M phosphate buffer solution (PBS) pH 3.0. The oxidation of eugenol by the APTMS-GO@SnO2/CPE was controlled by the diffusion process and exhibited a higher anodic current response than when unmodified. The differential pulse voltammetry (DPV) was used to determine the optimal electrode parameters and the purposed sensor showed good stability, sensitivity, and selectivity with a low limit of detection at 0.02 μM (3σ) and a wide linear range of 0.05–440 μM. The developed sensor was successfully applied for determining the eugenol content in clove and capsule products. These results exhibited that the sensor has good precision with a %recovery > 95% and good agreement results with other methods at a confidence level of 95%.

Enhanced photocatalytic activity and hydrogen evolution of CdS nanoparticles through Er doping

Generation of hydrogen fuel via the photocatalytic water splitting mechanism using semiconductor nanoparticles under sunlight irradiation is highly important. Moreover, the development of nanophotocatalysts for polluted water treatment is significant. In this regard, we synthesized CdS, CdS:Er (2 at%), and CdS:Er (4 at%) nanoparticles by a simple reflux route. According to the comprehensive structural analysis, Er3+ ions were incorporated into the CdS host lattice at the substitutional and interstitial sites, without altering the original structure. Photocatalytic measurements revealed that the degradation efficiency of 2 at% Er-doped CdS nanoparticles reached 100% within 100 min of visible light irradiation. In addition, CdS:Er (2 at%) nanoparticles exhibited enhanced photocatalytic hydrogen generation ability under simulated sunlight irradiation. Hence, from the obtained results, we concluded that CdS:Er (2 at%) nanoparticles are promising semiconductor photocatalytic materials for wastewater treatment as well as hydrogen fuel generation.

Cobalt ferrite decorated multiwalled carbon nanotubes as the electrode for efficient field electron emission

In the present study, Cobalt Ferrite (CF) nanoparticles with different weight concentrations were successfully decorated on Multi-Walled Carbon nanotubes (MWCNT) using a simple glycol assisted chemical route. The physicochemical and electronic properties of CF decorated MWCNTs (MWCNT-CF) were accomplished with the help of different techniques such as X-ray Diffraction (XRD), Raman Spectroscopy , Transmission Electron Microscopy (TEM), X-ray Photo-electron Spectroscopy (XPS) and Fourier Transform Infrared Spectroscopy (FTIR). Further, the effect of CF concentration on Field Emission (FE) characteristics of MWCNT-CF is investigated. The FE studies revealed that, CF decorated MWCNT emitter (MWCNT-CF; 1:1) exhibits lower turn on (0.52 V/μm, at 10 μA/cm 2 ) and threshold fields (0.62 V/μm, at 100 μA/cm 2 ) in contrast to pristine CF, MWCNT, and MWCNT-CF (1:0.5 and 1:2). Interestingly, from the MWCNT-CF (1:1) emitter, very high emission current density ~10,408 μA/cm 2 has been extracted at a relatively lower applied field of 1.18 V/μm. The enhancement in FE characteristics of MWCNT-CF emitters is attributed to lowering of work function measured from the UPS analysis and increased number of emitting sites. The results imply that very high current density field emitters can be fabricated using a simple strategy based on the decoration of MWCNT's with CF nanoparticles. • Hierarchical MWCNT-CF heterostructure by varying CF concentration is synthesized using reflux route. • All the characterization tools shows formation of CF decorated MWCNT heterostructure. • Enhanced FE behavior explained on the basis of modulation of work function, high aspect ratio and number of emitting sites. • MWCNT-CF exhibits superior FE performance shows potential emitter for vacuum based devices.

Structural and Electrochemical Behaviour of Cucurbita Seed Like Zinc Oxide Nanoparticles by Chemical Reflux Route

Cucurbita seed like zinc oxide (ZnO) nanoparticle is synthesised via chemical reflux method. The phase, size and structure of ZnO elucidates by X-ray diffraction method. Infrared spectrum is revealed its functional groups which are present in the synthesised nanoparticles. The cucurbita seed like morphology of prepared zinc oxide nanoparticles were examined by SEM analysis. Optical absorption property and bandgap of synthesized ZnO nanoparticles are investigated. The electrochemical activity of Cucurbita seed like ZnO nanoparticles measurement carry out through electrochemical impedance analysis, galvanostatic charge discharge and cyclic voltammetry results

Physico-Chemical Properties of Nickel Promoted Sulfated Zirconia Powder Prepared using Different Procedures

In this work, nickel promoted sulfated zirconia (Ni/SZ) as catalyst was prepared by either by reflux (Ni/SZ-R) or hydrothermal Ni impregnation (Ni/SZ-H) routes. The aim of this study was to evaluate the influences of two preparative methods on the physico-chemical properties of prepared catalysts. Both the catalysts were characterized by XRD, FTIR, ammonia adsorption, SEM-EDX, TEM-SAED, AAS and BET. It was found that the presence of sulfate and nickel could enhance the Brønsted and Lewis active acid sites. In relation to the effect of Ni impregnation method, acidity, amount of sulfate and Ni found in Ni/SZ-R were higher than those in Ni/SZ-H. Unfortunately, higher impregnated sulfate and nickel on zirconia support led to a decrease in surface area and pore volume and an increase in crystallite size of grainy aggregated mesoporous nickel promoted sulfated zirconia (Ni/SZ).

Template-free synthesis of Se-nanorods-rGO nanocomposite for application in supercapacitors

AbstractBoth selenium and reduced graphene oxide have low specific capacitance due to their chemical nature. Nevertheless, their specific capacitance could be enhanced by hybridizing Se nanomaterials with reduced graphene oxide via formation of electrochemical double layer at their interfacial area. Therefore, novel Se-nanorods/rGO nanocomposite was successfully synthesized by template free hot reflux route starting with graphene oxide and selenium dichloride. The composite of rGO decorated by Se-nanorods is characterized using X-ray diffractometry (XRD), Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and nitrogen adsorption– desorption. The unique architecture of the composite exhibits high specific capacitance of 390 F/ g at 5 mV/s scan rate in 1.0 M KOH solution with ~ 90% cyclic stability after 5000 cycles making it very promising electrode material for supercapacitor applications.

In situ supported VOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

The vanadium oxide/carbon nanotube (VOx/CNTs) composite catalyst was prepared by in-situ growth of VOx nanoparticles on CNTs with a cetylpyridinium chloride (CPC) assisted reflux route. The in-situ prepared catalysts exhibit better NH3-SCR activity in a broader temperature window at low temperature than those prepared by impregnation or a mechanically mixed method. The structural characterizations show that vanadium oxide nanoparticles have a good dispersion on the CNTs surface, with much lower valence vanadium species and chemisorbed oxygen species. The physics-chemistry properties indicate that there is a strong interaction between the VOx and CNTs, and the catalysts present a larger amount of stronger acid. The abovementioned reasons have eventually led to the enhancement of NH3-SCR activity.

Influenced of Ni loading on SBA-15 synthesized from oil Palm ash silica for syngas production

The nickel loading (1-3wt.%) effect on SBA-15 prepared via sol-gel method for dry reforming of methane (DRM) was investigated. Silica source of sodium silicate-oil palm ash (Na2SiO3-OPA) was obtained from extraction of OPA using mass ratio Na2SiO3/P123~2.9. The SBA-15 was synthesized via hydrothermal treatment reflux route at treatment temperature of 80 °C. A vertical stainless steel fixed-bed reactor was applied for catalytic DRM process at 800 °C, atmosphere pressure and ratio CH4:CO2 is 1:1 for 30 h. Characteristic of structure SBA-15 was successfully analyzed by TEM, indicates to the positive role of Na2SiO3-OPA as silica sources. XRD, BET and FTIR results revealed that 2Ni/SBA-15 exhibited high surface area (460.89 m2/g) and pore diameter (6.53 nm), small NiO particle (14.71 nm) which assist good metal dispersion and led to better metal-support interaction. The increase of Ni loading from 1 to 3wt.% results in lowering the surface area and pore volume of catalyst as more Ni particles tend to agglomerate and positioning on the SBA-15 pores. The performance of Ni/SBA-15 catalyst in DRM decrease with the trend of 2Ni/SBA-15>3Ni/SBA-15>1Ni/SBA-15 whereby the H2/CO followed the order of 2Ni/SBA-15≈3Ni/SBA-15>1Ni/SBA-15.These studies revealed the Ni loading influences the metal-support interaction and significantly affect the H2/CO production.

Controlled synthesis of tubular ferrite MFe2O4 (M = Fe, Co, Ni) microstructures with efficiently electrocatalytic activity for water splitting

Ferrite MFe2O4 (M = Fe, Co, Ni) tubular microstructures were successfully synthesized through a simple two-step strategy. The tubular FeOOH microstructures were first obtained by a heating reflux route. Then, tubular ferrite MFe2O4 (M = Fe, Co, Ni) microstructures were produced by a solvothermal method. The as-prepared products were characterized by the powder X-ray diffraction (XRD), the field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and EDS mapping. Experiments showed that as-obtained ferrite catalysts demanded the overpotentials of −201∼-359 mV or ∼340–432 mV to afford the current density of −/+10 mA cm−2 for hydrogen evolution reaction (HER) or oxygen evolution reaction (OER) with long-term durability for 50 h in 1.0 M KOH solution. Among them, NiFe2O4 tubular microstructures presented the best electrocatalytic activities for HER and OER due to the largest BET specific surface area, the highest electrochemical active surface area and the smallest charge-transfer resistance. Obviously, the present ferrite tubular microstructures have potential application as a bifunctional electrocatalyst for full water splitting.

A role of annealing temperature on the properties of lanthanum oxide (La2O3) microplates by reflux routes

The morphology controlled the synthesis of La2O3 is important for their application in the fields of semiconductors. In this work nanostructured La2O3 has been synthesized by reflux method using lanthanum nitrate, urea and double distilled water as starting materials. The approximate band gap of the as-prepared and calcined samples was calculated from the absorption spectrum are 5.8 and 5.9 eV respectively. The as-prepared and calcined products were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier transform infrared (FT-IR), Bandgap was calculated by UV–visible spectroscopy.

Carbon Cloth Modified with Metal‐Organic Framework Derived CC@CoMoO4‐Co(OH)2 Nanosheets Array as a Flexible Energy‐Storage Material

AbstractDue to the urgent demand for portable electronics, enormous research efforts are devoted for the development of flexible, wearable and lightweight supercapacitors. Herein, we report a cost‐effective chemical liquid process followed with a refluxing route to grow CC@CoMoO4‐Co(OH)2 nanosheets with Co‐based MOF as precursor. The resulting CC@CoMoO4‐Co(OH)2‐4 electrode delivers a significantly enhanced specific capacitance of 2028 F g−1 at 1 A g−1 and capacitance of 1581.8 F g−1 at 20 A g−1. Furthermore, the flexible all‐solid‐state asymmetric supercapacitor (CC@CoMoO4‐Co(OH)2//AC) is assembled, displays a high energy density of 61 Wh kg−1 at power density of 800 W kg−1, with an excellent cycle stability. These exceptional electrochemical performances could be ascribed to the unique structure and multi‐metal ion combination contributes to the ideal synergistic effects, which also signify that the potential application of CC@CoMoO4‐Co(OH)2 nansheets in high‐performance supercapacitors.

Photocatalytic degradation of amoxicillin using Co-doped TiO2 synthesized by reflux method and monitoring of degradation products by LC–MS/MS

Photocatalytic degradation of Amoxicillin (AMX) in aqueous solution by Co-doped TiO2 and undoped TiO2 synthesized by reflux route was investigated. The catalysts were characterized using X-ray diffractometry, FT-IR spectroscopy, UV-Vis absorption spectroscopy, scanning electron microscopy and X-ray Fluorescence Spectroscopy, and using specific surface area, particle size and zeta potential measurements. Photocatalytic efficiency of Co-doped and undoped TiO2 was compared for degradation of AMX under UV-C and visible irradiation by investigating the effects of the parameters such as percentage of the cobalt doped, amount of catalyst, irradiation time, initial AMX concentration and pH of the medium. Effects of organic and inorganic ions in the aqueous solution were also studied. Results showed that degradation of AMX is improved by Co doping to TiO2. It was detected that complete removal is achieved within 240 min of irradiation under UV-C and 300 min under visible irradiation. 94%, 21% and 16% degradation efficiencies were achieved after 300 min of photocatalysis under visible light in the presence of Co-doped TiO2, undoped TiO2 and Degussa P25 TiO2, respectively. Degradation products were determined and followed using LC–MS/MS technique to describe the evolution of AMX. An attempt was made to estimate the photocatalytic cleavage pathway of AMX by LC-MS/MS