We report a supercritical fluid (SCF)-assisted synthesis of a tightly integrated MXene/MoS2/PANI ternary heterostructure for high-performance supercapacitor applications. The SCF route enables rapid nucleation, controlled crystallization, and intimate interfacial coupling between Ti3C2Tx MXene and MoS2 nanosheets, followed by uniform in situ polymerization of polyaniline (PANI) to construct a hierarchical conductive network. This rationally engineered architecture synergistically combines electric double-layer capacitance and pseudocapacitance while minimizing charge-transfer resistance and enhancing ion transport kinetics. The optimized composite delivers a high specific capacitance of similar to 325 F g-1 along with excellent cycling durability over 10,000 cycles, exhibiting progressive capacitance activation attributed to improved electrolyte accessibility and interfacial conductivity. The study introduces a time-efficient and structurally controlled strategy for fabricating MXene-based ternary heterostructures and establishes a scalable pathway toward advanced hybrid electrode materials for next-generation energy storage systems. A novel heterostructure MXene/MoS2/PANI was successfully synthesised using the SCF (SuperCritical fluid) process.Among MoS2, MXene/MoS2, and MXene/MoS2/PANI, the ternary composite MXene/MoS2/PANI exhibited the highest electrochemical performance.The MXene/MoS2/PANI composite achieved a maximum specific capacitance of approximately 325 F g-1.The material demonstrated strong capacitance retention over 10,000 charge/discharge cycles, indicating excellent long-term stability.
Flexible and high-performance supercapacitors are emerging as pivotal components in next-generation energy storage systems. In this work, a novel ternary Cu2ZnSnS4/MoS2/CNT (CZTS/MoS2/CNT) heterostructure was synthesized via a one-pot hydrothermal method and systematically evaluated for its electrochemical performance. Structural and morphological analyses (XRD, Raman, SEM, and TEM) confirmed the formation of a well-integrated heterostructure with uniform anchoring of CZTS and MoS2 nanoparticles on conductive CNT networks, fostering enhanced charge transport and ion diffusion. The ternary composite exhibited an impressive specific capacitance of 273.2 F g(-1) at 1.25 A g(-1), significantly outperforming pristine CZTS (141.9 F g(-1)) and binary CZTS/MoS2 (154.8 F g(-1)). Furthermore, it demonstrated exceptional energy and power densities of 97.13 Wh kg(-1) and 1.076 kW kg(-1), respectively, along with 98% capacitance retention over 1000 cycles. The superior performance arises from the synergistic interplay of MoS2's redox-active surfaces and CNT's high electrical conductivity, which together enhance electrochemical reversibility and mechanical robustness. This facile, scalable, and eco-friendly synthesis approach underscores the CZTS/MoS2/CNT heterostructure as a promising electrode material for flexible and sustainable supercapacitor applications.
The preparation of a magnetically recoverable and reusable Fe3O4@benzothiazole-Cu(II) nanoparticles with their catalytic and electrochemical sensing properties are reported in this manuscript. The prepared Fe3O4@benzothiazole-Cu(II) nanoparticles are characterized using various analytical techniques, including XRD, FTIR, SEM, TEM, XPS, TGA and VSM analysis. The prepared system has shown good catalytic activity in the reduction of 2-NBA, achieving a reaction rate constant of 0.093 min−¹ in 2 min with a low catalyst loading. The synthesized catalyst also showed very high efficiency in the reduction of 4-nitro-phenol and methylene blue within 13 min and 4 min, respectively. The prepared material demonstrated good recovery yield and could be reused as a catalyst for multiple cycles without a significant loss in catalytic activity. It also exhibited a remarkable electrochemical sensing capability for the detection of ascorbic acid, H2O2, and paracetamol at various concentrations, as determined through cyclic voltammetry and impedance measurements. They exhibited clear redox transformations, indicating the electrochemical sensing ability of the prepared materials.
Synthesized substituted N-acetyl-3,5-diaryl-2-pyrazolines through their chalcone intermediates and evaluated for anti-cancer activity. Chalcones were synthesized from 2,4,5-trimethoxy benzaldehyde obtained from oxidation of β-asarone ((Z)-2,4,5-trimethoxy-1-propenylbenzene) is a major active principle component found in Acorus calamus oil (70–80
In this work, 2,4,5-trimethoxy substituted 3,5-diaryl isoxazoles were synthesized via their chalcone intermediates and evaluated for antimicrobial and anticancer activities. The natural precursor 2,4,5-trimethoxy benzaldehyde (asaronaldehyde) was obtained from oxidation of β-asarone (Acorus calamus oil) and then reacted with substituted acetophenones via Claisen-Schmidt condensation yielded 2,4,5-trimethoxy substituted chalcones. These chalcones on further treatment with hydroxylamine in presence of sodium acetate and acetic acid cyclizes to give the corresponding 3,5-diaryl isoxazoles yields ranging from 65-80%. Structures were confirmed by IR, GC-MS, 1H NMR and 13C NMR. Synthesized compounds were screened for their antimicrobial activity against bacteria and fungi. The para-substituted isoxazoles (5b, 5c and 5d) exhibited good activity against Gram-negative (Escherichia coli) and (Pseudomonas aeruginosa) and Gram-positive (Bacillus subtilis) and Bacillus licheniformis bacteria and fungi (Phytophthora capsici, Sclerotirum rolfsii, Aspergillus niger and Alternaria alternate). Further, these novel analogues were evaluated for their in vitro anticancer activity against three human tumor cell lines (MCF-7, SW-982 and HeLa) using MTT assay. The anticancer results revealed that phenyl ring at C-3 position bearing electron donor groups in the para-position and 2,4,5-trimethoxy substitutent of the phenyl ring at C-5 position isoxazole showed better inhibitory activity (5b, 5c and 5d). Among synthesized isoxazoles due to the hyper conjugative effect, 2,4,5-trimethoxy 3,5-diaryl isoxazole (5g) having 3-triflouromethyl substitution showed good antimicrobial and higher inhibitory IC50 values 8.56 ± 0.32, 12.16 ± 0.86 and 10.16 ± 0.68 μg/mL (p < 0.05) respectively, when compared to natural precursor β-asarone.
Based on a multitarget-directed drug design technique, a series of new quinoxalinone-based pyrazole derivatives (4a-h) were designed and synthesized. The potency of newly synthesized molecules to inhibit the anti -proliferation of the human cancer cell lines MCF-7 (breast), HCT-116 (colon), and A549 (lung) was examined. The most effective compounds against the examined cancer cell lines were 4e, 4f, 4 g, and 4 h. Among these, compounds 4e and 4 h had a strong anticancer activity that was equivalent to sorafenib. The capacity of the potent compounds (4e, 4f, 4 g, and 4 h) to inhibit the in vitro activity of the thymidylate synthase (TS) enzyme, BRaf, and EGFR kinases was also tested. With IC50 values for the TS enzyme, BRaf kinase, and EGFR kinase ranging from 1.16 to 2.97 mu M, 1.28 to 3.69 mu M, and 1.93 to 4.28 mu M, respectively, all the investigated compounds showed a noticeable inhibitory action. Among the synthesized hybrids, compound 4 h showed IC50 value of 2.04, 2.69 and 1.93 mu M against MCF-7, HCT-116, and A549 cell line, respectively, and 1.16, 1.28 and 1.93 nM against TS, BRaf and EGFR kinase enzyme, respectively. All of the synthesized hybrids adhered to Lipinski's guidelines, which suggested that they would have favorable oral drug-like qualities. To determine the probable interaction between the potent compounds and the TS active site, molecular docking study was conducted.
In present work, a simple hydrothermal method is employed for the synthesis of silk cocoon-ZnO micro-nanocomposite and investigation of their gas sensing is reported. The ZnO nanoparticles were synthesized using hydrothermal methods and coated on the surface of silk cocoon layers using a simple doctor-blade method. The as-prepared silk cocoon-ZnO micro-nanocomposite materials were analyzed using X-ray diffractometer (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR) and IV characteristics. The results confirm the formation of pure ZnO and silk cocoon-ZnO micro-nanocomposite with rod-like morphology. The surface of silk cocoon fibers was uniformly coated with ZnO nanorods. The gas sensing property of the as-prepared silk cocoon-ZnO micro-nanocomposite was evaluated against the leakage of LPG gas at room temperature. Voltage-Time curve analysis was performed and found that with the detection of LPG gas there is an increase in the voltage. Based on the present findings, it is proposed that silk cocoon-ZnO micro-nanocomposite based devices will be suitable for light weight, biocompatible and low-cost gas sensors.
Multi-stimuli (pH/thermo/redox)-responsive amphiphilic poly(cysteine methacrylamide)-block-poly(2-(dimethylamino)ethyl methacrylate)-block-polybutadiene-block-poly(2-(dimethylamino)ethyl methacrylate)-block-poly(cysteine methacrylamide) (PCysMAM-b-PDMAEMA-b-PB-b-PDMAEMA-b-PCysMAM) pentablock copolymer biohybrids, based on hydrophobic PB, ampholytic redox responsive PCysMAM and dual (pH and temperature) stimuli responsive PDMAEMA segments, are synthesized via a four-step synthesis protocol. The synthesis protocol involves: (1) in situ post polymerization modification of living polybutadiene-based carbanionic species to prepare hydroxyl terminated polybutadiene (HTPB); (2) introduction of an initiating functionality (capable of acting as an ATRP initiator) to HTPB, yielding a telechelic ATRP macroinitiator (Br-PB-Br); (3) recyclable alloy-mediated successive RDRP of DMAEMA and CysMAM, yielding a series of PCysMAM-b-PDMAEMA-b-PB-b-PDMAEMA-b-PCysMAM (A-B-C-B-A) pentablock copolymers with various chain lengths; and (4) conversion of the PDMAEMA block to poly(quaternary ammonium) (PQA) via quaternization. The stimuli responsiveness of the copolymer is investigated against changes in pH, temperature and redox. The pentablock copolymer self-assembles into spherical nanospheres, can switch between its monocationic, zwitterionic and monoanionic charged states, exhibits antifouling behaviour and is capable of removing ionic contaminants from water. These pentablock copolymers may emerge as a promising material for emerging applications.
In the work, Cu2ZnSnS4 (CZTS)/Polyaniline (PANI) nanocomposites was successfully synthesized by an in-situ supercritical water reaction from the mixture of CZTS-precursors and PANI. The synthesized samples were characterized by X-ray diffraction, TEM, thermogravimetry/differential thermal analysis (TG-DTA), scanning electron microscopy, and elemental mapping of CZTS powder. In order to evaluate the electrochemical performance of CZTS nanoparticles and CZTS/PANI nanocomposites, their supercapacitor electrodes were fabricated. The electrochemical experiment revealed that the specific capacitance of CZTS/PANI in 1 M KOH aqueous electrolyte at a current density of 2.5 A/g was 371 F/g, which was significantly more than the specific capacitance of the pure CZTS sample (271 F/g) after 1000 cycles also, the composite retained 97% of its capacitance. Thus, it can be concluded that the reduced electrolyte charge-transfer resistance and ion-diffusivity can be the cause of enhanced conductivity and a large surface of the material, which synergistically improved the capacitive performance of the electrode material.
Solar-driven photocatalytic hydrogen generation by splitting water molecules requires an efficient visible light active photocatalyst. This work reports an improved hydrogen evolution activity of visible light active TiO2-x photocatalyst by introducing reduced graphene oxide via an eco-friendly and cost-effective hydrothermal method. This process facilitates graphene oxide reduction and incorporates intrinsic defects in TiO2 lattice at a one-pot reaction pro-cess. The characteristic studies reveal that RGO/TiO2-x nanocomposites were sufficiently durable and efficient for photocatalytic hydrogen generation under the visible light spec-trum. The altered band gap of TiO2-x rationally promotes the visible light absorption, and the RGO sheets present in the composites suppresses the electron-hole recombination, which accelerates the charge transfer. Hence, the noble metal-free RGO/TiO2-x photocatalyst exhibited hydrogen production with a rate of 13.6 mmol h-1g-1cat. under solar illumination. The appreciable photocatalytic hydrogen generation activity of 947.2 mmol h-1g-1cat with 117 mAcm-2 photocurrent density was observed under visible light (>450 nm).
Preparation of chirality-defined few-walled CNT (FWCNT) is one of the major challenges in the carbon nanotube (CNT) fields. In the last two decades, significant progress has been made in preparing chirality-controlled synthesis (CCS) of FWCNT through both a direct synthesis approach and a post-synthesis separation approach due to insignificant changes in the tube diameter and twist angle. Hopefully, the present study will encourage further research on the preparation of FWCNT and also utilize key research and practical applications of FWCNTs. In this study, the SEM images of as-grown nanotubes show that applying electric field during the growth process affects the growth of the nanotubes and nanotubes properties can be achieved and altered by changing the supplied electrical DC bias. Raman spectroscopy has been used to analyze the structure and forms of grown FWCNTs samples. The Raman spectrum from all obtained CNTs samples shows the presence of major two peaks, corresponding to the 1350 cm−1 and 1570 cm−1 bands as well as characteristic Raman bands for metallic or semi-conductive CNTs and their corresponding electrochemical performance also have been performed.
In this study, a silk cocoon layer (SCL) was surface coated with polyaniline (PANI), which serves asan electrode for thermoelectric generator (TEG) application. Here, the PANI was synthesized usingthe sol-gel method and coated on both sides of SCL using doctor-blade method. The efficiency ofconverting thermal energy into electrical energy was analyzed with a temperature range from 30 to 60ºC. The TG-DTA analysis was performed to evaluate thermal stability. An evident change in theresistance was noticed for both cold (~5 °C) and heat (60 ºC) respective temperatures. Thus, this studyprovides a new biomaterial-based TEG electrode for waste heat recovery system/thermal management.
Photocatalytic activity of hydrothermally synthesized CZTS-MWCNT hetero structured NCs was investigated here. The CZTS NPs and CZTS-MWCNT NCs of varying MWCNT contents (3 wt%, 6 wt% and 9 wt%) were characterized by XRD, SEM, TEM, Raman and UV-Vis spectroscopy. The TEM image confirmed that the CZTS NPs are anchored to MWCNTs. From the UV-Vis spectroscopy, the optimum optical band gap of CZTS-6 wt% MWCNT NCs was found 1.4 eV and exhibited higher absorption than CZTS NPs. Under visible light radiation, photocatalytic dye degradation of methylene blue studies revealed a 19% higher photodegradation efficiency for CZTS-6 wt% MWCNT NCs than CZTS NPs. CZTS-6 wt% MWCNT NCs achieved a reaction rate constant of 0.012 min (-1), which is twice that of CZTS NPs. Because of the optimal bandgap of CZTS and the rapid charge carrier mobility of MWCNTs, CZTS-MWCNT NCs have the advantage of enhancing photocatalytic activity over CZTS NPs.
A series of tacrine-2-amide derivatives were synthesized and biologically evaluated for their acetylcholinesterase (AChE) inhibition studies. All synthesized compounds showed a good potency less than 100 nM. Of 11 analogues compounds 7b, 8a and 8c were found to exhibit good potency of 23.66 nM, 20 nM and 24.33 nM towards inhibition of acetylcholinesterase, respectively. Insilico study revealed that these compounds can bind strongly in catalytic active site (CAS) as well as peripheral active site (PAS) of enzyme. The docking results stated that the π-π stacking interaction, have a significant role in the protein-ligand binding and provide information about the binding enthalpy. The compound 7b shows good affinity with AChE, and possess a glide score of −10.38 kcal/mol and having a binding energy of −24.03 kcal/mol. The compound 7b showed interaction with Tyr341 and forming π-π stacking with Trp86. The compound 8a shows a glide score of −11.22 kcal/mol with a binding energy of −30.88 kcal/mol which is contributed by π-π stacking interaction with Trp86, and a hydrogen bond with amino group of tacrine with His447. The compound 8c showed a better glide score of −12.81 with binding affinity of −59.90 kcal/mol.
Layered 2D transition metal dichalcogenides (TMD’s) have been considered as an important class ofmaterials in the field of energy and environmental applications. Therefore, it is desirable to fabricate2D hybrid TMD’s materials in simple solution processing methods. In this study, MoS2-RGO hybrid2D few layered sheets are produced by supercritical fluid process (SCF) by using ethanol as solvent at250 ºC in a short duration of 0.5 h. Atomic force microscopy (AFM), transmission electron microscope(TEM) and scanning electron microscope (SEM) images confirmed the formation of 2D hybrid fewlayered sheets. The electrochemical impedance measurement indicates fivefold increase in conductivityof bulk MoS2. This work presents rapid and one pot exfoliation of MoS2 and simultaneous reductionof GO that can facilitate the production of 2D hybrid materials.
In present study, the synthesis of spinel MnFe2O4 nanoparticles using a facile one-pot super critical fluid method and their application for Mg-ion battery application as anode materials is reported. The synthesized MnFe2O4 nanoparticles were well characterized for their structure and morphology using XRD, SEM, TEM and EDS analysis. The average particle size of materials was less than 50 nm with spinel structure. The main feature of magnesium ion battery is its high specific capacity and large volumetric energy density, which makes it a promising alternative to Li-ion batteries. The spinel MnFe2O4 material has been used as an anode material for Mg-ion batteries. At different C-rates (0.05C to 2C), electrochemical charge-discharge behaviour has been observed. In first cycle of the phase-pure spinel structured anode, an initial specific capacity of 195.82 mAh/g, 139.70 mAh/g, 25.04 mAh/g and 14.16 mAh/g were obtained at C rate of 0.05C, 0.1C, 1C and 2C, respectively. A possible phase conversion reaction of the anode resulted in a decrease in specific capacity with increasing C-rate.
An efficient protocol for the reductive carbonylation of (hetero) aryl halides and triflates under CO gas-free conditions using Pd/Co2(CO)8 and triethylsilane has been developed. The mild reaction conditions, enhanced chemoselectivity and, easy access to heterocyclic and vinyl carboxaldehydes highlights its importance in organic synthesis.
The vital role played by microtubules in the cell division process, marks them as a potential druggable target to decimate cancer. A novel furan-2-carboxamide based small molecule, is a selective microtubule stabilizing agent (MSA) with IC50 ranging from 4 mu M to 8 mu M in different cancer cell lines. Inhibition of tubulin polymerization or stabilization of tubulin polymers abrogates chromosomal segregation during cell division, results in cell cycle arrest and leads to cell death due to the delayed repair mechanism. A novel furan-2-carboxamide based small molecule exhibited potent anti-proliferative and anti-metastatic property In-Vitro against the panel of cancer cells. Annexin V-FITC/PI, double staining reveals potent cytotoxic effect of SH09 against HeLa cells. FACS analysis displays induction of G2/M arrest and accumulation of subG1 population of cells upon treatment with SH09. Molecular docking study unveils SH09 binding affinity to the Taxol binding pocket of tubulin proteins and MM-GBSA also confirms strong binding energies of SH09 with tubulin proteins.
Application of brown titanium dioxide (TiO2-x) and its modified composite forms in the photocatalytic decomposition of organic pollutants in the environment is a promising way to provide solutions for environmental redemption. Herein, we report the synthesis of effective and stable TiO2-x nanoparticles with g-C3N4, RGO, and multiwalled carbon nanotubes (CNTs) using a simple hydrothermal method. Among all the as-synthesized samples, excellent photocatalytic degradation activity was observed for RGO-TiO2-x nanocomposite with high rate constants of 0.075 min(-1), 0.083 min(-1) and 0.093 min(-1) for methylene blue, rhodamine-B, and rosebengal dyes under UV-Visible light irradiation, respectively. The altered bandgap (1.8 eV) and the large surface area of RGO-TiO(2-x )nanocomposite impacts on both absorption of visible light and efficiency of photogenerated charge electron (e(-))/hole (h(+)) pair separation. This resulted in enhanced photocatalytic property of carbon-based TiO2-x nanocomposites. A systematic study on the influence of different carbon nanostructures on the photocatalytic activity of brown TiO2-x is carried out.
Background: Novel carboxamides and thioureas of 2,3-dihydro-5,6-dimethoxy-2-((piperidin- 4-yl)methyl) inden-1-one were synthesized and their potential anticholinesterase activities were evaluated. The inhibition potency of the compounds 17a-j and 19a-j against AChE was measured and evaluated using Ellman’s spectrophotometric method. Among carboxamides series, compound 17f, 17i, 17j and among thiourea series, compound 19a, 19b were found to be the most active. Methods: The scaffold 2,3-dihydro-5,6-dimethoxy-2-((piperidin-4-yl)methyl) inden-1-one 16, key intermediate of drug donepezil has been synthesised in three steps and derivatised as carboxamides and thioureas for SAR studies. Compounds 17a-j and 19a-j were characterised by 1H NMR and LCMS. The inhibitory activity and antiamnesic effect were studied using different sources such as electric eel AChE, human serum AChE and rat brain homogenate AChE. Results: The results of bioassays indicated that among all the synthesized compounds tested, five compounds 17f, 17i, 17j, 19a and 19b shows IC50 at a dose of 67, 42, 64, 52 and 63 nM respectively against electric eel, human serum and rat brain homogenate, which lead to the suggestion that compound 17i might be considered to be a potent AChE inhibitor. Conclusion: Derivatives of 2,3-dihydro-5,6-dimethoxy-2-((piperidin-4-yl)methyl)inden-1-one with different substitutions were synthesised and tested for their AChE activity. The order of potency is 17i>17j>17f and 19a>19b. The other compounds screened failed to elicit any inhibition of acetyl cholinesterase from rat brain homogenate. It may be concluded from this study that, for effective binding and blocking the AChE activity, molecule needs to bind with peripheral site and active site of the enzyme. Therefore, it can be summarized that by changing the functional group and substitution in the scaffold 2,3-dihydro-5,6-dimethoxy-2-((piperidin-4-yl)methyl)inden-1-one needs to be studied for better AChE inhibitory activity in future research.