Facile Synthesis Research Articles

Novel D-π-A hemicyanine dye as photoinitiators for insitu hydrogel formation and DLP printing.

The field of biofabrication imposes stringent requirements on the polymerization activity and biosafety of photopolymeric hydrogel systems. In this investigation, we designed and synthesized four hemicyanine dyes with a D-π-A structure specifically tailored for biofabrication purposes. These novel dyes, incorporating carbazole (CZ), triphenylamine (TPA), anthracene (AN), and benzodithiophene (BDT) as electron donors, along with heterocyclic salt (IN) as electron acceptors, were prepared using a straightforward synthesis method. The absorption maxima of ANIN, CZIN, and TPAIN exceeded 500 nm, rendering them suitable co-initiators for the free radical photopolymerization of acrylates under green-red light exposure facilitated by light-emitting diodes (LEDs) and the co-initiator iodonium salt (ION). Notably, CZIN and TPAIN, due to their robust dye absorption and efficient electron transfer to ION, functioned as high-performance photosensitizers. Meanwhile, BDTIN, with its strong and broad absorption range (400-600 nm), enhanced the accuracy of visible light photopolymerization. These dyes exhibit characteristics such as facile synthesis, heightened photo stability, and non-toxicity and also demonstrate the ability to discern the alkalinity of a solution to some extent. Furthermore, we explored the application of these hemicyanine dyes in 3D printing, showing potential to enhance printing resolution in DLP 3D printing (digital light process 3D printing).

Facile Gram-Scale Synthesis of Size-Tunable MgO Nanosheets Enclosed by (111) Surface with Remarkable Stability and Uniform Host Sites for Atom Dispersion

Facile Gram-Scale Synthesis of Size-Tunable MgO Nanosheets Enclosed by (111) Surface with Remarkable Stability and Uniform Host Sites for Atom Dispersion

Facile Synthesis and Electrochemical Analysis of Zn-Doped V2O5 Anode Materials for High-Rate Li Storage

The surging demand for Li rechargeable batteries with high energy densities and rapid rate capability has propelled research on materials that can replace the conventional anode materials like graphite. Vanadium pentoxides (V2O5) have emerged as promising anode candidates owing to their excellent rate capability. Specifically, V2O5 allows the electrochemical prelithiation process, in which three Li-ions can be inserted to form Li3V2O5, followed by reversible insertion and extraction of two Li-ions. Nevertheless, the unsatisfactory Li-ion diffusion coefficients and electrical conductivities of these materials remain major drawbacks. Here, we propose a Zn-doped V2O5 anode, fabricated using a two-step sol–gel method, for high-rate Li-ion batteries. Zn was incorporated into V2O5 to enhance the Li-ion transport kinetics through the electrode. The crystal structure (orthorhombic) of Zn-doped V2O5 was identified by X-ray diffraction analysis, and the Zn doping was confirmed by X-ray photoelectron microscopy. The effect of Zn doping was thoroughly examined using various analytical methods, such as cyclic voltammetry and galvanostatic intermittent titration technique. The Zn-doped V2O5 electrode exhibited remarkable cycling durability, enduring for 1000 cycles, while retaining an enhanced capacity, even under a high rate of 2C.

Intermolecular Forces Regulating the Phase-Transition Temperatures in Organic-Inorganic Hybrid Materials.

Organic-inorganic hybrid phase-transition materials have attracted widespread attention in energy storage and sensor applications due to their structural adaptability and facile synthesis. However, increasing the phase-transition temperature (Tc) effectively remains a formidable challenge. In this study, we employed a strategy to regulate intermolecular interactions (different types of hydrogen bonds and other weak interactions), utilizing bismuth chloride as an inorganic framework and azetidine, 3,3-difluoro azetidine, and 3-carboxyl azetidine as organic components to synthesize three compounds with different Tc values: [C3H8N]2BiCl5 (1, 234 K), [C3H6NF2]3BiCl6 (2, 256 K), and [C4H8O2N]3BiCl6 (3, 350 K). 1 is a one-dimensional chain structure and 2 and 3 are zero-dimensional structures. Analysis of the crystal structure and the Hirshfeld surface and 2D fingerprints further suggests that the intermolecular forces are efficiently modulated. These findings emphasize the efficacy of our strategy in enhancing Tc and may facilitate further research in this area.

General and facile synthesis of Co/CoO nanoparticals supported by nitrogen-doped graphenic networks as efficient oxygen electrocatalyst forZn-air batteries.

Reasonable design of low-cost, high-efficiency and stable bifunctional oxygen electrocatalysts is of great significance to improve the reaction efficiency of Zn-air batteries, which is still a huge challenge. Here, we report a highly efficient bifunctional oxygen electrocatalyst with three-dimensional (3D) N-doped graphene network-supported cobalt and cobalt oxide nanoparticles (Co/CoO-NG), which can be in situ synthesized by inducing metal ions on metal plates via graphene oxide as an inducer. This 3D network structure and open active center show excellent bifunctional oxygen electrocatalytic activity under alkaline conditions, and can be used as an air electrode in rechargeable Zn-air batteries, with significantly better power density (244.28 mW cm-2) and stability (over 340 h) than commercial Pt/C + RuO2mixtures. This work is conducive to advancing the practical application of graphene-based materials as air electrodes for rechargeable zinc-air batteries.

A Facile Synthesis of MgO Decorated Spinel Magnetic Nanoparticles Using Terminalia catappa Leaf Extract: Its Application in EBT Dye Removal

A Facile Synthesis of MgO Decorated Spinel Magnetic Nanoparticles Using Terminalia catappa Leaf Extract: Its Application in EBT Dye Removal

Extending the Scope of the C-Functionalization of Cyclam via Copper(I)-Catalyzed Alkyne-Azide Cycloaddition to Bifunctional Chelators of Interest.

Cyclam, known for its potent chelation properties, is explored for diverse applications through selective N-functionalization, offering versatile ligands for catalysis, medical research, and materials science. The challenges arising from N-alkylation, which could decrease the coordination properties, are addressed by introducing a robust C-functionalization method. The facile two-step synthesis proposed here involves the click chemistry-based C-functionalization of a hydroxyethyl cyclam derivative using Cu(I)-catalyzed alkyne-azide cycloaddition (CuAAC). Boc-protecting groups prevent undesired copper coordination, resulting in compounds with a wide range of functionalities. The optimized synthesis conditions enable C-functional cyclams to be obtained easily and advantageously, with high application potential in the previously cited fields. The methodology has been extended to trehalose-based Siamese twin amphiphiles, enabling efficient gene delivery applications.

Facile synthesis of MgO-carbon nanocomposites for advanced capacitive electrode materials

Facile synthesis of MgO-carbon nanocomposites for advanced capacitive electrode materials

Siloxane-Functionalized Eugenol-Based Novolacs: from Facile Synthesis to Their Cured Bisphenol A Epoxy Thermosets with Superb Toughness and Thermal Stability

Siloxane-Functionalized Eugenol-Based Novolacs: from Facile Synthesis to Their Cured Bisphenol A Epoxy Thermosets with Superb Toughness and Thermal Stability

Unlocking the Power of Acyl Fluorides: A Comprehensive Guide to Synthesis and Properties

AbstractAcyl fluorides have emerged as versatile reagents in various synthetic endeavors, offering a range of advantages over their counterparts, acyl chlorides. This study delves into the properties and reactivity of acyl fluorides, particularly their reaction with amines and alcohols, to elucidate their distinct characteristics. We also introduce a facile and practical synthesis of acyl fluorides from a stable solution of CF3O− salt. Additionally, we establish an efficient one‐pot process for the direct preparation of amides or esters from corresponding acids and amines or alcohols, showcasing the remarkable efficiency of acyl fluorides in these transformations.

Facile Synthesis of Bumpy-Structured ZnO-ZnS Core-Shell Microspheres with Enhanced Photocatalytic Performance

Zinc oxide is considered an outstanding photocatalyst candidate, but its low photo-corrosion resistance is a problem to be solved. In the ZnO-ZnS core-shell structure, ZnS acts as a protective layer for the ZnO core, and thus, it can enhance stability and long-term performance. The ZnO-ZnS core-shell structure is synthesized into various nanoscale morphologies with high specific surface areas to improve photocatalytic efficiency. However, they are easily agglomerated and are hard to separate from reaction media. In this study, micro-sized bumpy spheres of ZnO-ZnS core-shell structure were prepared via facile chemical transformation of as-prepared ZnO. After sulfurization of the ZnO template, it was confirmed through SEM, TEM, EDS, and XPS analysis that a uniform ZnS shell layer was formed without significant change in the initial ZnO morphology. The ZnO-ZnS core-shell microsphere has shown superior efficiency and stability in the photocatalytic degradation of Rhodamine B compared with pristine ZnO microspheres

Facile synthesis of cobalt-nickel oxide nanocomposites for trifunctional application towards antioxidant, anticancer and electrochemical performance

Transition metallic mixed oxides have received a lot of curiosity due to their exceptional electrochemical performance and incredibly low cost for hybrid supercapacitors. Herein, we report a facile synthetic approach of cobalt nickel oxide (CNC) composites from Carica papaya leaf extract. The synthesized mixed oxide composite was analyzed by various spectroscopic techniques (IR, UV–Vis, Powder XRD, SEM-EDAX, TEM and XPS). The electrochemical behavior of CNC was investigated by cyclic voltammetry (CV) and galvanostatic charge–discharge (GCD) method in 2 M KOH solution. The composites exhibit specific capacitance of 289.28 F g−1 at 1 A g−1 demonstrating improved charge storage. The electrode retains 81 % of its specific capacitance from the initial value after repeated charge–discharge processes for 2000 cycles. In addition to the electrochemical studies, biological activities such as anti-oxidant and anti-cancer activities of the CNC were examined. The radical scavenging activity of CNC was assessed with different radicals such as DPPH•, ABTS+., NO–, OH•, O2– and the acquired results showed that the composites possessed substantial activity. Anticancer activity of CNC was studied against HepG2 and MM2 cancer cells and the CNC possessed significant activity with the IC50 value of 45.8 and 38.3 µg/ml respectively compared with the standard drug cisplatin. Further apoptogenic nature of the CNC was confirmed with DAPI staining assay.

Facile Synthesis and Li-Electroactivity of Cobalt Oxide Based on Resources Recovered from Waste Lithium-Ion Batteries

In this study, cobalt oxide (Co3O4) powder was prepared by simple precipitation and heat-treatment process of cobalt sulfate that is recovered from waste lithium-ion batteries (LIBs), and the effect of heat-treatment on surface properties of as-synthesized Co(OH)2 powder was systematically investigated. With different heat-treatment conditions, a phase of Co(OH)2 is transformed into CoOOH and Co3O4. The result showed that the porous and large BET surface area (ca. 116 m2/g) of Co3O4 powder was prepared at 200°C for 12 h. In addition, the lithium electroactivity of Co3O4 powder was investigated. When evaluated as an anode material for LIB, it exhibited good electrochemical performance with a specific capacity of about 500 mAh g–1 at a current density of C/5 after 50 cycles, which indicates better than those of commercial graphite anode material.

Capacitive-Controlled Prussian White with a Nickel Iron Hexacyanoferrate Composite Cathode for Rapid Sodium Diffusion.

Prussian blue analogues receive tremendous attention owing to their spacious three-dimensional skeleton, high theoretical specific capacity, facile synthesis procedure, and high cost-effectiveness as among the most promising candidates for cathode materials in sodium-ion batteries (SIBs). Nonetheless, the practical specific capacity, especially under high current, is particularly frail due to the sluggish ion diffusion. In this study, the strategy of Ni substitution and formation of water-coordinated Fe is applied to lower the crystal field energy and elevate the active low-spin (LS) Fe content, which leads to a capacitive sodium storage mechanism, resulting in a substantial specific capacity under high current density. The delivered specific capacity of PW-325@2NiFe-55 is 95 mAh g-1 at 50 C, which is 72.5% capacity retention of the one at 0.5 C. Also, it maintains 80.2% of its initial specific capacity after 500 cycles at 5 C. Furthermore, a hypothesis of a joint diffusion-controlled and capacitive mechanism for high-spin (HS) Fe and a mere capacitive mechanism for LS Fe is put forward and verified through potentiastatic tests, operando 57Fe Mössbauer spectroscopy, and ex situ XRD, which provides a new horizon to enhance the electrochemical performance for SIBs.

Kilogram scale facile synthesis and systematic characterization of a Gd-macrochelate as T1-weighted magnetic resonance imaging contrast agent

To overcome the problems of commercial magnetic resonance imaging (MRI) contrast agents (CAs) (i.e., small molecule Gd chelates), we have proposed a new concept of Gd macrochelates based on the coordination of Gd3+ and macromolecules, e.g., poly(acrylic acid) (PAA). To further decrease the r2/r1 ratio of the reported Gd macrochelates that is an important factor for T1 imaging, in this study, a superior macromolecule hydrolyzed polymaleic anhydride (HPMA) was found to coordinate Gd3+. The synthesis conditions were optimized and the generated Gd-HPMA macrochelate was systematically characterized. The obtained Gd-HPMA29 synthesized in a 100 L of reactor has a r1 value of 16.35 mM−1 s−1 and r2/r1 ratio of 2.05 at 7.0 T, a high Gd yield of 92.7% and a high product weight (1074 g), which demonstrates the feasibility of kilogram scale facile synthesis. After optimization of excipients and sterilization at a high temperature, the obtained Gd-HPMA30 formulation has a pH value of 7.97, osmolality of 691 mOsmol/kg water, density of 1.145 g/mL, and viscosity of 2.2 cP at 20 ℃ or 1.8 cP at 37 ℃, which meet all specifications and physicochemical criteria for clinical injections indicating the immense potential for clinical applications.Graphical

Graphene Oxide‐Assisted Molecular Crystal Co‐Assembly for Large‐Scale Freestanding 2D Photoresponse Heterostructures with Synaptic Plasticity

Abstract2D van der Waals heterostructures (2D vdWHs) have been gaining significant attention in neuromorphic electronics. However, the facile synthesis of large‐scale, high‐quality freestanding 2D vdWHs remains challenge, particularly for organic counterparts due to susceptible nucleation behaviors and weak intermolecular interactions. Here, the study reports a graphene oxide (GO)‐assisted molecular crystal co‐assembly method for one‐step growth of centimeter‐scale freestanding heterostructures. This co‐assembly involves the simultaneous assembling of organic and GO precursors at the liquid–liquid interface, where the amphiphilic nature of GO nanosheets facilitates the diffusion of organic molecules and 2D nucleation of organic crystals, and the nanosheets also become enriched to grow a quasi‐solid film for the bilayer formation. Owing to integrated photosensitive and charge‐trapping properties as well as type II band structure, this heterostructure exhibits exceptional photonic synaptic behaviors, with a paired‐pulse facilitation index of 141% and image recognition of 91%.

Facile synthesis and application of hyperbranched TiO2 hollow spheres for enhancement of power conversion efficiency of CdSeTe quantum dot-sensitized solar cells

Facile synthesis and application of hyperbranched TiO2 hollow spheres for enhancement of power conversion efficiency of CdSeTe quantum dot-sensitized solar cells

Biological metal–organic frameworks for natural gas purification and MTO product separation

The use of porous solid adsorbents is an effective and excellent approach for the separation and purification of methanol-to-olefins product and methane (CH4). In this particular study, a series of adenine (AD)-based biological metal–organic frameworks (Bio-MOFs) {Their general formula is Cu 2 (AD) 2 (X) 2 [X = formic acid, acetic acid (AA), and propionic acid]} were proposed, which exhibited remarkable efficiency in the purification of CH4 and the separation of C3H6 from methanol-to-olefins product, ultimately yielding purified C2H4. The experimental findings demonstrate that different terminal ligands induce alterations in the pore microenvironment, consequently leading to variations in adsorption capacities and stability. Specifically, Cu-AD-AA exhibits the highest adsorption capacity and selectivity among the three MOFs, as confirmed by static adsorption isotherm testing and theoretical evaluation using ideal adsorbed solution theory (IAST) simulation. At 298 K and 1 bar, Cu-AD-AA exhibits 786 and 10.9 selectivity for C3H8/CH4 and C3H6/C2H4, respectively, surpassing the majority of MOFs materials. Furthermore, breakthrough experiments conducted in ambient conditions reveal that Cu-AD-AA possesses commendable separation capabilities, enabling one-step purification of C2H4 at varying proportions (C2H4/C3H6 = 50:50, 50:20, and 90:10), along with satisfactory recycling performance. Importantly, the synthesis of Cu-AD-AA utilizes simple and easily obtainable raw materials, thereby offering advantages such as cost-effectiveness, low toxicity, and facile synthesis that enhance its potential for industrial applications.

Fe3O4@SiO2@CSH+VO3− as a novel recyclable heterogeneous catalyst with core–shell structure for oxidation of sulfides

Iron nanoparticles, with low toxicity and many active sites, are among the materials that not only reduce waste along with green chemistry but also increase the separation power and recover the catalyst from the reaction environment. In this study, first, the surface of iron nanoparticles was silanized, and in the next step, the complex of chitosan HCl.VO3 was placed on the surface of Fe3O4 (Fe3O4@SiO2@CSH+VO3−). This nanocatalyst is a novel, recoverable, and potent nanocatalyst with high selectivity for the oxidation of sulfides to sulfoxides. Various physicochemical techniques such as IR, XRD, TGA, SEM, EDX, mapping, TEM, and VSM were used to affirm the well synthesis of the catalyst. Oxidation of sulfides in the presence of hydrogen peroxide as a green oxidant and in ethanol was catalyzed by the Fe3O4@SiO2@CSH+VO3−. All sulfoxides were achieved with high efficiency and in a short time. The notable privileges of this method include facile and economic catalyst synthesis, proper catalyst durability, great performance, simple catalyst isolation, good recovery capability, at least up to 5 times without an index drop in catalytic power.

High‐Efficiency Iridium‐Yttrium Alloy Catalyst for Acidic Water Electrolysis

AbstractProton exchange membrane (PEM) water electrolysis holds great promise in revolutionizing clean energy production by enabling the efficient generation of hydrogen. Nevertheless, a formidable challenge persists in the realm of designing electrocatalysts that are both highly active and acid‐resistant during the oxygen evolution reaction (OER), thereby mitigating the substantial kinetic barrier. In this study, the facile synthesis of iridium‐yttrium (IrY) alloy nanocatalysts via a thermal shock method is introduced, which exhibits exceptional activity in the context of acidic water oxidation. Through the strategic incorporation of dispersed Y into the lattice of Ir metal, the IrY catalyst demonstrates a notably low overpotential of 255 mV at a current density of 10 mA cm−2 and showcases remarkable catalytic stability in acidic electrolytes, enduring for over 500 h with a high current density of 100 mA cm−2. Through a comprehensive set of in situ characterizations and analytical methods, the formation of a surface Ir‐based oxide layer, induced by deprotonation and electrochemical oxidation is unveiled, which is notably stabilized by the presence of Y dopants. This stabilization of the active site imparts enhanced resistance to over‐oxidation and dissolution, underpinning the exceptional stability of the catalyst. Theoretical calculations suggest that the incorporation of Y into the catalyst structure has a significant impact on enhancing the reactivity of the oxygen intermediate (O*) at adjacent Ir sites, thus lowering the overpotential and promoting OER activity. The alloying approach presents a straightforward method for achieving atomic‐level modifications in catalyst design and can pave the way for the development of more effective and economically viable OER catalysts and beyond.