Single-step Method For Synthesis Research Articles

Novel furfural-Complexed approach to synthesizing carbon-Doped ZnO with breakthrough photocatalytic efficacy

IntroductionThe efficiency of zinc oxide (ZnO) nanoparticles for environmental decontamination is limited by their reliance on ultraviolet (UV) light and rapid charge carrier recombination. Carbon doping has been proposed to address these challenges by potentially enhancing visible light absorption and charge separation. ObjectivesThis study aims to introduce a novel, single-step synthesis method for carbon-doped ZnO (C-Z) nanoparticles, leveraging the decomposition of zinc nitrate hexahydrate and furfural under a nitrogen atmosphere to improve photocatalytic activity under visible light. MethodsA series of C-Z variants (C-Z-1 to C-Z-5) and an undoped sample (ZnO-0) were synthesized. The influence of furfural on the synthesis process and doping mechanism was analyzed by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and UV–visible diffuse reflectance spectroscopy (DRS). ResultsXPS confirmed the integration of carbon within the ZnO matrix, and XRD indicated increased lattice dimensions owing to doping. DRS revealed bandgap narrowing, suggesting enhanced charge separation. Among the variants, C-Z-3 significantly outperformed the others, showing a 12-fold increase in the photocatalytic degradation rate of Rhodamine B compared to undoped ZnO. ConclusionThe developed single-step synthesis method for C-Z nanoparticles represents a major advancement in materials engineering for ecological applications. The enhanced photocatalytic activity under visible light, as demonstrated by C-Z-3, underscores the potential of these nanoparticles for environmental decontamination.

Unlocking the magnetic potential of Fe2O3 nanoparticles by single-step synthesis of cobalt-infused nanomaterials for chromium removal

The study optimized the chromium removal capacity of Fe2O3 nanoparticles through the infusion of cobalt using a single-step synthesis method. This approach not only enhanced their magnetic properties but also employs less-chemical synthesis techniques, ultimately yielding highly magnetic CoFe2O4 nanoparticles and less impurities. The prepared materials underwent comprehensive testing, encompassing examinations of their optical properties, structure, chemical composition, and surface characteristics using various analyticals methods. In a span of 90 min under visible light exposure, CoFe2O4 nanoparticles exhibit the ability to remove more that 90% of chromium. This was corroborated through analysis using Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). Moreover, the study illustrates that increased temperatures amplify the endothermic process of chromium adsorption. Positive ΔH°, negative ΔS°, and heightened Cr(IV) adsorption are linked to the temperature effects on solubility, mobility, and dissolved oxygen. Both Langmuir (R2 = 0.95, RL = 0.055) and Freundlich models (R2 = 0.98, n = 0.69) suggest favorable adsorption. The efficient Cr(IV) adsorption by CoFe2O4 nanocomposite is attributed to a rapid reaction rate and substantial capacity, following pseudo-second order kinetics (rate constant 0.01 g mg−1 min−1, R2 = 0.99).Graphical abstract

Facile synthesis of N-doped biomass derived porous carbon from Opuntia humifusa using simple solid state activation method for reversible capture of volatile iodine

The search for adsorbent materials capable of extracting and storing radioactive iodine derived from nuclear power plants has intensified owing to the growing nuclear waste concerns. Herein, we report a novel method, which is simple and effective, to synthesize biomass-derived porous carbon from an easily available biomass, Opuntia humifusa, via simple solid-state activation with zinc chloride. The resulting porous carbon exhibits a large specific surface area, with up to 1869 m2/g of micropores. The textural properties of activated carbons can be easily modified by adjusting the amount of zinc chloride and activation temperature. The optimal conditions were found to be a ZnCl2 to biomass ratio of 5 and a carbonization temperature of 500 °C. The obtained porous carbons can function as multifunctional solid sorbents for radioactive iodine because of their high porosity and advantageous hierarchical porous structure. Specifically, the obtained activated carbon exhibited high iodine affinity with an absorption of 408 wt%. Considering its global abundance and recyclability, Opuntia humifusa can be used as a new biomass source for the efficient production of highly effective porous carbon materials with potential applications in environmental restoration. Furthermore, the straightforward single-step synthesis method described in this study offers a technique for producing several unique activated mesoporous carbons from various biomasses.

Synthesis of Indole‐2‐carboxylates via Condensation of Nitroacetic Esters and 2‐Dimethylbenzaldehydes

AbstractA new operationally simple single step method for synthesis indole‐2‐carboxylates from 2‐dimethylaminobenzaldehydes and nitroacetic acid esters in 22–59 % yields has been developed.

Single-Step Synthesis of Ag Hexagonal Nanoplate-Decorated Reduced Graphene Oxide and Its Cytotoxicity Studies.

Graphene-based Ag nanocomposites are of specific interest because of their unique properties and applications, especially in the field of cytotoxicity. However, developing a simple method to synthesize reduced graphene oxide (rGO)/silver hexagonal nanoplate (Ag HNPT) (rGO-Ag HNPT) nanocomposites with well-defined morphology has been believed to be a major challenge. In this work, a facile, robust, and single-step synthesis method was developed to prepare silver-graphene (rGO-Ag HNPT) nanocomposites with hexagonal-structured silver nanoplates without any templates. The primary characterizations of the synthesized nanocomposite were done using a UV-visible spectrophotometer, X-ray diffraction (XRD), and Raman spectroscopy. The formation of uniformed hexagonal-shaped Ag nanoplates was confirmed by high-resolution transmission electron microscopy (HR-TEM), and the elemental composition was confirmed using energy dispersive X-ray analysis (EDX). With SiHa cervical cancer cells, the short-term in vitro cytotoxicity of the as-synthesized rGO-Ag HNPTs was evaluated by the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide (MTT) assay. The anticancer response of the rGO-Ag HNPTs was investigated using an MTT assay.

Nitrogen-Doped Graphene Oxide as Efficient Metal-Free Electrocatalyst in PEM Fuel Cells

Nitrogen-doped graphene is currently recognized as one of the most promising catalysts for the oxygen reduction reaction (ORR). It has been demonstrated to act as a metal-free electrode with good electrocatalytic activity and long-term operation stability, excellent for the ORR in proton exchange membrane fuel cells (PEMFCs). As a consequence, intensive research has been dedicated to the investigation of this catalyst through varying the methodologies for the synthesis, characterization, and technologies improvement. A simple, scalable, single-step synthesis method for nitrogen-doped graphene oxide preparation was adopted in this paper. The physical and chemical properties of various materials obtained from different precursors have been evaluated and compared, leading to the conclusion that ammonia allows for a higher resulting nitrogen concentration, due to its high vapor pressure, which facilitates the functionalization reaction of graphene oxide. Electrochemical measurements indicated that the presence of nitrogen-doped oxide can effectively enhance the electrocatalytic activity and stability for ORR, making it a viable candidate for practical application as a PEMFC cathode electrode.

Novel Carbidopa Functionalised Silver Nanoparticles a Selective Detection for Lead and Levodopa

Novel approaches to engineer nanoparticles with desired chemical characteristics open new opportunities to utilize such materials for assorted applications. In this context, various methods have been developed to prepare metal nanoparticles. In the present work, we report a single-step synthesis method to prepare silver nanoparticles by using Carbidopa which is useful in treating Parkinson's disease to increase the dopamine level of the brain. Here we used the Carbidopa drug as a capping agent. Nanoparticles were characterized by Uv-Visible spectroscopy, Particle size Analyzer (PSA), dynamic light scattering (DLS), Powder X-ray Diffractometry (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Transmission electron microscopy (TEM). Then amino acid detection study was performed with all 24 amino acids, which provides the successful data for sensing the amino acid L-dopa. These prepared nanoparticles were further applied for metal analyte studies which reveal that lead can be sensed successfully by using these nanoparticles. Nanoparticle also shows radical scavenging activity against 2,2-diphenyl-1-picrylhydrazyl (DPPH).

Self-activated, urea modified microporous carbon cryogels for high-performance CO2 capture and separation

Conventionally, porous carbons were synthesized using corrosive chemical activating agents. On contrary, we designed a single-step synthesis method for the preparation of a series of self-activated heteroatom (N)-doped carbon cryogels from potassium hydrogen phthalate (KHP) and urea at various temperatures (700–1000 °C), in the absence of any activating agent. To highlight the effectiveness of N-doping in porosity generation and CO2 adsorption/separation, a comparative analysis was drawn with a series of undoped carbon cryogels. Notably, the N-doped cryogels exhibit a highly porous structure with remarkable specific surface area (SSA; 2084 m2 g−1), micropore volume (1.1806 cm3 g−1), well-defined pore size distribution, and abundant narrow micropores (<1.04 nm). Additionally, a considerable mechanical strength (compressive strength = 0.621 MPa and compressive modulus = 8.86 MPa) was also observed. Moreover, the porous cryogel endowed with sufficient pyrrolic nitrogen content (≈51.4 at %) lead to high CO2 adsorption (280.57 mg/g at 273 K and 171.31 mg/g at 298 K at 1 bar) and an excellent ideal adsorbed solution theory (IAST)-based CO2/N2 selectivity (≈115) at 273 K, surpassing the CO2 adsorption/separation performance of previously reported N-doped carbons and resorcinol-based carbon gels. Furthermore, the moderate heat of adsorption (36.109 kJ mol−1) and stable cyclic behavior of CO2 adsorption-desorption under flue gas conditions (i.e., 15% CO2/85% N2) unveils the physisorption nature of adsorption which governs the energy-effective regeneration process. Summarizing, the present work demonstrates the successful fabrication of highly porous carbon cryogels as efficient CO2 adsorbents, thereby opening new synthetic avenues for self-activating porous carbon formation.

Novel single-step synthesis and shape transformation of Au/CuO micro/nanocomposites using plasma-liquid interaction

We report a novel single-step synthesis method of metal/metal oxide composites and transformation of the shape of the oxide material by Plasma-Liquid Interaction. Considering the potential applications of noble metal nanoparticle decorated copper oxide composites, we synthesize Au/CuO micro/nanocomposites by generating plasma between two copper electrodes inside a gold precursor (HAuCl4) solution. Simultaneous synthesis of CuO and Au nanoparticles from the electrode material and from the precursor solution respectively is possible due to the interaction of energetic electrons and other active species formed in the plasma zone. Moreover, the process does not require any external stabilizing and reducing chemical agents. The method provides a remarkable tunability of the materials’ physical and chemical properties by only controlling the precursor solution concentration. By controlling process parameters, the shape of CuO particles can be transformed from spindles to sheet-like and the size of Au nanoparticles can also be varied. It influences the particles’ specific surface area and total pore volume. Plasmonic property of Au nanoparticles is also observed i.e. optical tunability can be achieved. The process is found to be effective for synthesis of desired nanomaterials having various energy storage and solar light-driven photocatalytic applications.

Single-step metal-catalyzed synthesis of hybrid planar graphene–orbicular graphitic carbon structures using an amorphous carbon thin film as a precursor

Graphene is one of the strongest and most electrically and thermally conductive materials in nature; therefore, incorporating even traces of graphene into other materials can significantly enhance their mechanical, electrical, and thermal properties. Such graphene-based materials can be used in many applications, including flexible displays, batteries, supercapacitors, solar panels, and mobile devices. However, developing graphene-based 2D materials is challenging. In this study, a facile single-step synthesis method for fabricating thin layers of amorphous carbon (a-C) containing planar graphene (PG) and orbicular graphitic carbon (OGC) nanostructures was developed by thermal annealing in inert atmosphere using an sp3-rich a-C thin film as a precursor. By annealing thin-film stacks of Si/NiFe/a-C, a thin layer with a hybrid a-C-PG-OGC structure was produced with OGC nanostructures forming on top of PG nanostructures and pyramidal NiSix nanocrystals extending into the Si substrate due to the diffusion of nickel during elevated-temperature annealing. Raman spectroscopy and cross-sectional transmission electron microscopy confirmed the transformation from amorphous to graphitic structure in the a-C film during thermal annealing. The obtained results demonstrate that the development of this 2D material with a hybrid a-C-PG-OGC microstructure is due to a metal-catalyzed PG nucleation mechanism and a mismatch-induced OGC growth mechanism. The present method for synthesizing graphene-containing thin-film structures paves the way toward the fabrication of complex micro-assemblies where high strength and good thermoelectric properties are of paramount importance.

Synthesis of Phthalimide Imine Derivatives as a Potential Anticancer Agent

The outstanding evidence of phthalimide pharmacophore in securing enhanced biological activities had encouraged further research and development into phthalimide-based derivatives as potential new drugs. In this study, phthalimide core was hybridized with aldehydes giving integrated imines displaying different types of functionalities and at alternating positions. The resulting compounds, therefore, provide an innovative window to explore possible differential biological effects as antioxidants and anticancer agents. A total of sixteen compounds were synthesized, and each was verified by FT-IR, H NMR, C NMR, and MS characterization. Herein, a facile single-step synthesis method was employed substituting the conventional two-step chemical production routes. Among the sixteen tested compounds, the H7 compound with hydroxyl phenolic group has shown an eminent antioxidant activity with a 19.52% decrease to the IC50 value compared to that of the control standard BHT antioxidant. On the other hand, the halogenated H6 Schiff base structure was successful in securing effective cancer inhibition to both colon and breast cancer cell lines, while maintaining selective action toward normal tissues. Results have collectively indicated the importance and impactful effects of functional groups position and types within similar basic structures, in directing different biological outcomes.

Single-step synthesis of novel chloroaluminate ionic liquid for green Friedel–Crafts alkylation reaction

Friedel–Crafts alkylation reactions constitute a very important class of reactions which are usually catalysed in the liquid phase using Lewis acids at the industrial scale. Diphenyl methane synthesised by Friedel–Crafts alkylation from benzene with benzyl chloride has been interesting in organic synthesis, perfumes and dyes. The new environmental legislation recommends a green and reusable catalyst system that is environmentally benign which leads to minimal pollution and waste generation. Chloroaluminate ionic liquids (ILs) have been used immensely as homogeneous catalyst in the organic synthetic processes. Though these ILs have multiple advantages, their synthesis process involves certain disadvantages like multiple step synthesis, viz. use of solvents and its removal after reaction, removal of precursors, solvent washing for removal of trace impurities and drying of salt/adduct. We have established a novel single-step synthesis method of chloroaluminates from tributylamine and aluminium chloride via amine–aluminium chloride adduction using suitable solvent or one of the reactants as reaction medium. The process improved the atom economy, reduced the use of volatile organic chemicals and drastically minimised the generation of wastes. Formation of chloroaluminate ILs was confirmed by FTIR, 27Al NMR and mass spectroscopy (ESI–MS), and other physicochemical properties were also determined. The chloroaluminate IL was used as catalyst for Friedel–Crafts benzylation of benzene. The performance of the ILs as catalyst showed higher catalytic activity and could be recycled twice for benzylation reaction. Reaction parameters were also optimised to achieve higher yields of diphenyl methane. Tributylamine can be easily recovered by hydrolysis of spent IL which would moderate the chemical oxygen demand in generated effluent.

DNA-Templated Strontium-Doped Calcium Phosphate Nanoparticles for Gene Delivery in Bone Cells.

Calcium phosphates (CaPs), constituents of the inorganic phase of natural bone, are highly biocompatible and biodegradable. Strontium (Sr) regulates the formation and resorption of bone. Incorporation of Sr into CaPs may target genes of interest to bone cells while regulating their function. In this work, we developed a single-step synthesis method to prepare Sr-doped CaP nanoparticles (SrCaP-DNA NPs) by using DNA as a template for controlling the mineralization and the stability of the colloidal solution. The resulting nanoparticles were monodispersed with well-controlled size, morphology, and composition. By using this method, we were able to fabricate CaP NPs with varying contents of Sr2+. We demonstrated that the stability of CaP NPs in extracellular environments increased when Sr2+ partially replaced Ca2+ in CaP NPs. We showed that the cellular uptake of SrCaP-DNA NPs and the efficiency of gene transfer and alkaline phosphatase activity in human fetal osteoblastic cell line (hFOB1.19) were dependent on the content of Sr2+ in NPs. Together with other studies, our results suggest SrCaP-DNA NPs can be optimized for targeted gene transfer to regulate function of bone cells, enabling applications such as bone tissue engineering and treating bone diseases.

High-performance Platinum-free oxygen reduction reaction and hydrogen oxidation reaction catalyst in polymer electrolyte membrane fuel cell

The integration of polymer electrolyte membrane fuel cell (PEMFC) stack into vehicles necessitates the replacement of high-priced platinum (Pt)-based electrocatalyst, which contributes to about 45% of the cost of the stack. The implementation of high-performance and durable Pt metal-free catalyst for both oxygen reduction reaction (ORR) and hydrogen oxidation reaction (HOR) could significantly enable large-scale commercialization of fuel cell–powered vehicles. Towards this goal, a simple, scalable, single-step synthesis method was adopted to develop palladium-cobalt alloy supported on nitrogen-doped reduced graphene oxide (Pd3Co/NG) nanocomposite. Rotating ring-disk electrode (RRDE) studies for the electrochemical activity towards ORR indicates that ORR proceeds via nearly four-electron mechanism. Besides, the mass activity of Pd3Co/NG shows an enhancement of 1.6 times compared to that of Pd/NG. The full fuel cell measurements were carried out using Pd3Co/NG at the anode, cathode in conjunction with Pt/C and simultaneously at both anode and cathode. A maximum power density of 68 mW/cm2 is accomplished from the simultaneous use of Pd3Co/NG as both anode and cathode electrocatalyst with individual loading of 0.5 mg/cm2 at 60 °C without any backpressure. To the best of our knowledge, the present study is the first of its kind of a fully non-Pt based PEM full cell.

Zero- and two-dimensional hybrid carbon phosphors for high colorimetric purity white light-emission.

Carbon nanomaterials are promising phosphors for white light emission. A facile single-step synthesis method has been developed to prepare zero- and two-dimensional hybrid carbon phosphors for the first time. Zero-dimensional carbon dots (C-dots) emit bright blue luminescence under 365 nm UV light and two-dimensional nanoplates improve the dispersity and film forming ability of C-dots. As a proof-of-concept application, the as-prepared hybrid carbon phosphors emit bright white luminescence in the solid state, and the phosphor-coated blue LEDs exhibit high colorimetric purity white light-emission with a color coordinate of (0.3308, 0.3312), potentially enabling the successful application of white emitting phosphors in the LED field.

Study on Single Step Method for Synthesis of Nano Fluids

Study on Single Step Method for Synthesis of Nano Fluids

Synthesis of nanocrystalline TaC powders via single-step high temperature spray pyrolysis from solution precursors

Nanocrystalline powders for high temperature ceramics (HTC) and ultrahigh temperature ceramics (UHTC) are important materials for aerospace and other important industrial applications. In this study, a low cost, single-step synthesis method for nanocrystalline HTC and UHTC powders is reported, which is based on high temperature spray pyrolysis (HTSP) process. The synthesis starts with solution of oxide and carbon precursors dissolved in common organic solvents, which are broken into fine droplets (e.g., via nebulizer). The droplets then go through processes of solvent removal, thermolysis, and rapid in situ carbothermal reduction (CTR), all in one single pass in a tube furnace operated at high temperature. The synthesis method was demonstrated successfully using the example of tantalum carbide (TaC) from precursors of tantalum chloride (TaCl5) and phenolic resin in a single-step HTSP process with maximum temperature of 1650°C in one pass that finished within minutes, yielding agglomerated nanocrystalline TaC UHTC powders.

A simple single-step method for the synthesis of recombinant non-homologous competitor cDNA and its implications for quantitative PCR in biological sciences and molecular diagnostics.

In recent years there has been great interest in quantitative polymerase chain reaction. Consequently, a large number of assays have been developed, of which the one using non-homologous competitors is arguably the most precise. Despite widespread applications, currently there is no simple method to synthesize such competitors. Here a facile and cost-effective, single-step method for synthesis of recombinant, non-homologous, competitor complementary DNA is described. The method can be adapted to generate competitors of any size and sequence. The entire procedure is quick, straightforward and does not require any specialized equipment except a standard thermocycler.