Single-source Precursor Method Research Articles

Fabrication of Nanobioengineered Interfaces Utilizing Quaternary Nanocomposite for Highly Efficient and Selective Electrochemical Biosensing of Urea.

Nanobioengineered interfaces have gained attention owing to their small size and high surface area-to-volume ratio for utilization as a platform for highly selective and sensitive biosensing applications owing to the integration of biological molecules with engineered nanomaterials/nanocomposites. In this work, a novel Ag-complex, [(PPh3)2Ag(SCOf)]-based quaternary Ag-S-Zn-O nanocomposites (NCs), was synthesized through an environmentally-friendly process. The results revealed the formation of the NCs with an average crystallite size and particle size of 36.08 and 40.22 nm, respectively. In addition, this is the first study to utilize such NCs synthesized via a single-source precursor method, offering enhanced sensor performance due to their unique structural properties. Further, these NCs were used to fabricate a urease (Ur)/Ag-S-Zn-O NCs/ITO nanobioengineered electrode for precise and sensitive electrochemical biosensing of urea. The interfacial kinetic studies revealed quasi-reversible processes with high electron transfer rates and linear current responses, indicating efficient reaction dynamics. A high diffusion coefficient and low surface concentration suggested a fast diffusion-controlled process, affirming the electrode's potential for rapid and sensitive urea detection. The biosensor demonstrated notable sensing properties such as high sensitivity (12.56 μA mM-1 cm-2) and a low detection limit (0.54 mM). The fabricated bioelectrode was highly selective and reproducible and demonstrated stability for up to 60 days. These results validate the potential of this nanobioengineered interface for next-generation biosensing applications, paving the way for advanced point-of-care diagnostics and real-time health monitoring.

Sleuthing the performance of the sustainable mixed metal trichalogenide BaS:Sn2S3:LaS from single source route as an electrode material for charge storage

A novel ternary transition and lanthanide metal composite sulfide (Ba, Sn, and La) has been developed using a single-source precursor method with diethyldithiocarbamate ligand. The resulting BaS:Sn2S3:LaS chalcogenide exhibits a finely tuned band gap of 3.88 eV, reflecting its superior optical performance. This eco-friendly sulfide features an average crystalline size of 17.93 nm and displays a mix of phases. Vibrational analysis reveals distinct transmission peaks corresponding to metal-sulfur bonds. Morphologically, BaS:Sn2S3:LaS composite is characterized by irregularly shaped particles forming a randomly agglomerated mass. The electrochemical charge storage properties of the semiconducting trichalcogenide BaS:Sn2S3:LaS have been investigated using cyclic voltammetry, galvanostatic charge-discharge, and impedance spectroscopy. BaS:Sn2S3:LaS electrode demonstrated impressive performance, storing electrical charge efficiently with a specific capacity of 659.6 F g⁻1 and achieving a power density of up to 3661.65 W kg⁻1. Additionally, the electrode exhibited low resistance, with an equivalent series resistance (Rs) of just 0.43 Ω, indicating efficient ion diffusion across the interface. Given its excellent redox activity and low resistance, BaS:Sn2S3:LaS shows strong potential as an electrode material for supercapacitors and batteries.

Constructing Phase-Transitional NiSx@Nitrogen-Doped Carbon Cathode Material with High Rate Capability and Cycling Stability for Alkaline Zinc-Based Batteries.

Alkaline zinc-based batteries are becoming promising candidates for green and economical energy-storage systems, thanks to their low cost and high energy density. The exploitation of the stable cathode materials with high rate capability and cycling stability is crucial for their further development. Herein, a series of NiSx coated with nitrogen-doped carbon (denoted as NiSx@NC) compounds (x = 0.5-1.0) are synthesized using the facile single-source precursor method. Benefiting from the unique phase-transitional NiSx@NC with high activity and enhanced conductivity from the well-balanced conductive metal nickel and carbon layer, the alkaline zinc-nickel batteries with a phase-transitional NiSx@NC cathode deliver a high capacity of 148 mA h g-1 at a high current density of 100 mA cm-2 and demonstrate a long lifespan of over 500 cycles with a high capacity retention of 98.8%. This work provides a significant guideline for the structural design and optimization of nickel-based materials in alkaline energy-storage devices.

Cr2S3(Et2DTC) complex and [Cr2S3-MoS2(Et2DTC)] bilayer thin films: single source stationed fabrication, compositional, optical, microstructural and electrochemical investigation

ABSTRACT Current investigation has for the first time synthesized chromium sulphide diethyldithiocarbamate [Cr2S3(Et2DTC)] complex utilizing diethyldithiocarbamate (DDTC) utilizing single source precursor method. Thin films of bilayer chromium sulphide diethyldithiocarmate and molybdenum disulphide [Cr2S3-MoS2(Et2DTC)] were deposited on the fluorine doped tin oxide (FTO) substrate by physical vapour deposition (PVD). Synthesized complex and bilayer were characterized by Xray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), ultraviolet-visible spectrophotometry (UV-Vis), and scanning electron microscopy (SEM) for exploration of the compositional, optical, crystalline and morphological parameters, respectively. FT-IR peaks expressed the chelation of [Cr2S3(Et2DTC)] expressing interactions between chromium sulphide and the ligand. The band gaps obtained from Tauc plot were 3.89 (direct) and 3.38 eV (indirect), respectively for Cr2S3(Et2DTC) complex. The direct and indirect band gap of 3.75 and 3.35 eV, respectively, were obtained for [Cr2S3-MoS2(Et2DTC)] bilayer thin films. Average crystallite size of 13 (hexagonal orientation) and 13.4 (orthorhombic orientation) nm and for Cr2S3(Et2DTC) complex and [Cr2S3-MoS2(Et2DTC)] bilayer thin films expressed from XRD. SEM micrographs expressed cannular and rod protrusions for Cr2S3-DDTC complex and smoother and unvarnished surficial characteristics for [Cr2S3-MoS2(Et2DTC)] bilayer thin films corresponding to compactness and uniformity of the films. Furthermore, [Cr2S3-MoS2(Et2DTC)] also expressed remarkable electrochemical aspects of the current generation and operational stability of analysed through 5760 s at 100 mA analysed via linear sweep voltammetry and chronoamperometry. The fabricated films can be efficiently used in optoelectronic devices. Current work can be extended to the optimization of bilayer thin films fabrication for achieving an alleviation in the band gaps.

Analysis of dopant concentration effect on optical and morphological properties of PVD coated Cu-doped Ni3S2 thin films

Current research has commenced the synthesis of Nickel-Diethyl dithiocarbamate Ni (S2CN (Et) 2) n]) and Copper diethyldithiocarbamate Cu (S2CN(Et)2) complex by single source precursor method. These complexes were utilized for deposition of pure and Cu-doped Ni3S2 thin films on glass substrate by physical vapor deposition technique. FTIR peaks of Copper and Nickel complex confirmed the formation of dithiocarbamate complex depicted by vibrational frequencies of M–S bond. Thermo-gravimetric analysis (TGA) of Nickel diethyl dithiocarbamate depicted decomposition of complex into corresponding metal sulphides. Different phases were observed by XRD in which predominant phase is Ni3S2 and crystalline size was about 90.8 nm calculated by Debye Scherrer equation. Fabrication of thin film is confirmed by UV–vis-Spectroscopy indicating the band gap of 2.1 eV for pure nickel sulphide which decreases to an appreciable extent of 1.89 eV for 6% doping of Copper while a slight decrease (i.e., 1.63 eV) upon 10% doping. The SEM showed homogeneous covering with Ni3S2 spherical particles at a few distance apart and grain size was 450 μm. Energy dispersive X-ray (EDX) have shown the proper deposition of Nickel Sulphide on glass substrate with subsequent doping of Copper. To the best of our knowledge, optical and structural analysis of PVD deposited doped and undoped Ni3S2 thin films were examined for the first time in this study.

Synthesis of MnS from Single- and Multi-Source Precursors for Photocatalytic and Battery Applications

Nanomaterials have been shown to possess exclusive properties in heterogeneous catalysis as evidenced by studies dedicated to the synthesis of transition-metal-containing nanomaterials. However, the series of nanomaterials which have been synthesized are mostly oxides. A ligand, 1-(2-chloro-4-nitrophenyl)-3,3-chlorobenzoyl (Tu), has been created through which MnS nanoparticles (NPs) and nanosheets (NSs) have been successfully synthesized, initially from a single-source precursor (SS) and then from multi-source precursors, respectively. The main objective of this article was to identify the differences in the morphologies of the materials synthesized from the two different sources, with photodegradation and battery applications performed just with MnS NPs (synthesized by the SS method). A preliminary study has been carried out on the photocatalytic properties and battery applications of the recently synthesized MnS employing the SS method. MnS NPs demonstrated higher activity than their bulk sheet for the photocatalytic degradation of four different dyes, methyl violet, methylene green, methylene blue, and rhodamine B, under visible-light irradiation. More significantly, the preparation method in the present work might be applied to other metal chalcogenide nanomaterials for various new applications. More notably, battery applications have been evaluated for MnS NPs (synthesized by the SS method) by testing their electrochemical discharge/charge at voltage limits of − 0.2 to 3.2 V versus Li/Li+.

Folic acid modified Pluronic F127 coating Ag2S quantum dot for photoacoustic imaging of tumor cell-targeting

In this study, an oil-soluble Ag2S quantum dot (QD) was synthesized through thermal decomposition using the single-source precursor method, and Pluronic F127 (PF127), a triblock copolymer functionalized with folic acid (FA), was deposited on the surface of the QD, then a water-soluble PF127-FA@Ag2S nanoprobe with targeting ability was fabricated. The as-prepared PF127-FA@Ag2S exhibited spheroidal morphology and high dispersibility, with average diameters of 115 ± 20.7 nm (as observed by transmission electron microscopy). No obvious toxicity of the PF127-FA@Ag2S nanoprobe was found in standard 3-(4, 5-dimethylthiazol-2-yl)-2, 5-diphenyltetrazolium bromide assay and colony-formation assay, indicating good biocompatibility and safety. The resulting PF127-FA@Ag2S exhibited excellent stability between 4 °C–40 °C. Additionally, the capacity of the tumor cell-targeting high contrast enhanced photoacoustic imaging of PF127-FA@Ag2S was verified in comparison with A547 and HeLa cells. In other words, the excellent properties of PF127-FA@Ag2S show great potential in further research for targeting and photoacoustic imaging.

Designing the morphology of PbS nanoparticles through a single source precursor method

The synthesis and characterization of lead sulphide nanoparticles using complexes as single sources of both lead and sulphur are reported. A cubic phase of galena perfectly matched all synthesized nanoparticles confirming that no secondary product was generated. The complexes prepared from thiosemicarbazide materials and lead bromide reacted differently in oleylamine to produce PbS nanoparticles. Smaller cubic shapes and quantum dots with a blue-shifted absorption were yielded from cinnamaldehyde thiosemicarbazide and benzophenone thiosemicarbazide complexes due to larger ligands and the symmetrical position of the thiosemicarbazide group in benzophenone complex. Relatively larger particles were obtained from acetophenone thiosemicarbazide complex. The temperature of synthesis also affected the shape and size of PbS nanoparticles.

Synthesis and characterization studies of NiO nanorods for enhancing solar cell efficiency using photon upconversion materials

We report the effect of calcination on the structural and optical properties of nanocrystalline NiO nanoparticles were successfully synthesized by virtue of a single source precursor method at mild reaction conditions between nickel nitrate and sodium hydroxide. Composition, structure and morphology of the products were analyzed and characterized by X-ray powder diffraction (XRD). The ultra-violet visible (UV–vis) absorption peaks of NiO exhibited a large blue shift and the luminescent spectra had a strong and broad emission band centered at 328nm. The intense band gap was also observed, with some spectral tuning, to give a range of absorption energies from 2.60 to 3.41eV. The various functional groups present in the NiO nanorods were identified by FTIR analysis. High resolution transmission electron microscopy (HRTEM) and the chemical composition of the samples the valence states of elements were determined by X-ray photoelectron spectroscopy (XPS) in detail. The electrochemical response of NiO proved that the nano-nickel has a high level of functionality due to its small size and higher electrochemical activity without any modifications. The above studies demonstrate the potential for the utilization of NiO nanoparticles as a promising material for opto-electronics applications.

One dimensional well-aligned CdO nanocrystal by solvothermal method

Cadmium oxide (CdO) is a category of the practical semiconductor metal oxides, which is widely applied in various scientific and industrial fields because of its catalytic, optical, and electrical properties. CdO nanocrystal was successfully synthesized by a virtue of a single source precursor method at mild reaction conditions between cadmium oxide, and element iodine by a solvothermal route. X-ray powder diffraction (XRD), ultraviolet spectroscopy studies (UV–vis), Fourier Transform Infrared analysis (FTIR), scanning electron microscopy (SEM), μ-Raman spectroscopy and cyclic voltammogram (CV) were used to characterize the CdO nanocrystals. The ultra-violet visible absorption peaks of CdO exhibited a large blue shift and the luminescent spectra had a strong and broad emission band centered at 228nm. The various functional groups present in the CdO nanocrystals were identified by FTIR analysis. Intense PL was also observed with some spectral tuning possibly giving a range of emission photon energies approximately spanning from 2.5 to 3.4eV. Scanning electron microscopy and μ-Raman microscopy images indicated that the morphology of the product is spherical nanoparticles with an average particle size of 46nm with standard deviation. The electrochemical response of CdO which is proved the nano-cadmium has high functionality due to the small size and it has higher electrochemical activity without any modifications. The above studies demonstrate the potential for the utilization of cadmium nitrite nanocrystal in visible opto-electronics applications.

Synthesis and characterization of MnS and MnSe nanoparticles: Morphology, optical and magnetic properties

Herein, we report on the synthesis of manganese chalcogenide nanoparticles using mild synthetic methods. The MnS nanoparticles were synthesised using a single-source precursor method with tetramethylthiuram disulfide as a ligand, whilst the MnSe nanoparticles were synthesised by reacting reduced elemental selenium with manganese. These synthetic methods resulted in crystalline MnS nanoparticles with wire-like morphology with high aspect ratio and MnSe nanorods that were nearly mono-dispersed. The absorption band-edges of both MnS and MnSe were blue-shifted from the reported bulk band-edges indicative of quantum confinement effects seen in nanoparticles. Furthermore, both MnS and MnSe showed paramagnetic characteristics with the ESR spectra showing broad single resonance peaks with g-values of 2.0064 and 2.0068 respectively.

Controlled synthesis of AgInS2 nanocrystals and their application in organic–inorganic hybrid photodetectors

High quality AgInS2 nanocrystals (NCs) are synthesized using a simple single-source precursor method, in which the size and morphology of the products can be precisely controlled from heliotrope seed-like NCs of 6 × 12 nm to heliotrope seed-like dimer NCs of 8 × 16 nm by tuning the composition of the coordinating solvents of oleic acid and 1-dodecanethiol. The results show that 1-dodecanethiol plays a dominant role in determining the morphology of AgInS2 NCs due to its strong absorption onto the {001} crystal plane of AgInS2 NCs. The photoelectric properties of the as-prepared AgInS2 NCs have been characterized using AgInS2-poly(3-hexylthiophene) hybrid nanodevices. The results illustrate that the AgInS2 NCs present very high photosensitivity and photostability to outside illumination. The high sensitivity and stability of the hybrid nanodevice indicate a broad spectrum of applications in the photoelectric nanodevices.

Single-source precursor synthesis of colloidal CaS and SrS nanocrystals

Colloidal CaS and SrS nanocrystals were prepared by thermal decomposition of calcium- and strontiumdiisopropyldithiocarbamate complexes in oleylamine. The diameter of the nanocrystals was 8–10nm with a narrow size distribution, showing that this single source precursor method gives access to monodisperse nanocrystals of small size.

Controllable synthesis of MnS nanocrystals from a single-source precursor

A facile single-source precursor method has been applied for the selective synthesis of MnS nanocrystals (NCs) with well-defined shapes and crystal structures such as hexapod, octahedral, hexagonal shaped α-MnS NCs, and pencil-shaped γ-MnS NCs. The effects of the composition of precursor, reaction temperature, and the heating rate on the morphologies, and crystal structures of MnS NCs were systematically studied for the first time.

Preparation of Gd2O2S:Yb,Ho Phosphor via Thermolysis of Sulfur-Contained (Gd,Yb,Ho)[S2CN(C4H8)]3 Phen Complexes

A novel handy single-source precursor method is adopted to prepare Gd2O2S:Yb,Ho up-conversion phosphors. Pure Gd2O2S:Yb0.06Ho0.02 phosphors are prepared via thermolysis of the air-stable ternary solid complexes RE[S2CN(C4H8)]3phen (RE=Gd, Yb, Ho) in a nitrogen atmosphere with certain amount of oxygen at 600–1100°C. The as-prepared Gd2O2S:Yb0.06Ho0.02 exhibits a strong green up-conversion luminescence under 980 nm IR excitation. The intensity of the green emission component is 37.4 and 53.4 times more than that of the red and NIR emissions, respectively. It is indicated that the material is of excellent color purity. Under an IR excitation density of 34.75 mW/mm2 with a laser beam diameter of 1 mm, the material exhibits an up-conversion luminescence brightness of 43.68 Cd/m2.

Morphological and optical properties of MnS/polyvinylcarbazole hybrid composites

Abstract This communication describes two methods for the synthesis of manganese sulfide/polyvinylcarbazole (MnS/PNVC) nanocomposites. The first method (method 1) involves initially the removal of the Hexadecylamine (HDA) molecules in the HDA-capped MnS nanoparticles, followed by the dispersion of the bare MnS (3 wt%) into PNVC. The FE-SEM and FT-IR established a strong interaction between the nanoparticles and the polymer while the absorption and photoluminescence spectra showed improved properties. The second method (method 2) is an in situ synthesis of MnS/PNVC composite. The method is similar to the single source precursor method but utilizes PNVC as the capping agent. The FE-SEM micrograph, EDX and FT-IR confirmed the formation of the composite. The optical properties confirm the role of PNVC to be that of a capping agent.

A Facile Route for the Synthesis of Poly(N-vinylcarbazole)/Manganese Sulphide Quantum Dots Nanocomposites with Enhanced Optical Properties

This communication describes a facile route for the synthesis of manganese sulphide (MnS) quantum dots (QDs) contained in poly(N-vinyl carbazole) (PNVC) nanocomposites. MnS QDs were synthesized using the single-source precursor method by thermolysing tetramethylthiuram disulfide manganese complex in hexadecylamine (HDA). Two different methods were used for the synthesis of MnS QD incorporated PNVC nanocomposites. The first method entailed the stirring of a mixture of MnS QDs and PNVC in chloroform (CHCl3) at room temperature and the second method was the refluxing of MnS QDs and PNVC solution in CHCl3 at an elevated temperature. A field emission electron microscope (FESEM) study revealed that the dispersion of MnS QDs in a PNVC matrix was improved in the case of nanocomposites prepared by the second method. The optical properties of pure PNVC were significantly altered for the case of nanocomposite prepared by the second route.

Size Control of Monodisperse Copper Sulfide Faceted Nanocrystals and Triangular Nanoplates

High-quality faceted nanocrystals and triangular nanoplates of copper sulfide have been successfully synthesized by using the single source precursor method in the presence of oleylamine. The obtained faceted copper sulfide nanocrystals have an average size of 9.8 ± 0.3 nm, showing the regularly hexagonal closely packed nanostructure. The resulting triangular copper sulfide nanoplates have an average side length of 12.3 ± 0.6 nm, thickness of 0.8 nm, forming the six-leave flowerlike nanostructure due to their size uniformity. We also demonstrate that the shape, size, and even the phase forms of copper sulfide nanocrystals can be controlled systematically by adjusting certain reaction parameters, such as the carbon number of the substitute alkyl (n), the reaction temperature, and the concentration of the precursor.

Size-controlled synthesis of orderly organized cube-shaped lead sulfide nanocrystals via a solvothermal single-source precursor method

Monodisperse cube-shaped lead sulfide (PbS) nanocrystals were successfully synthesized by virtue of a solvothermal single-source precursor method at mild reaction conditions. These resulted PbS nanocrystals have the average size in a range of 10 nm and a uniform cubic shape, shown by TEM and HRTEM, respectively. Due to their narrow size distribution, orderly self-organized arrays on a large scale can be easily obtained. Experimental results indicate that several factors, such as coordinating ability of the solvent, carbon number of the substitute alkyls ( n), reaction temperature, and concentration of the precursor, play key roles in the final size and size distribution of PbS nanocrystals. This finding will enhance our understanding for the formation mechanism of nanostructured materials with special shapes.

Synthesis and Characterization of Eu-Doped Cadmium Selenide Nanocrystals

Substitution of Cd(II) sites by Eu ions in 5.0 nm ± 0.25 nm CdSe, Cd1-xEuxSe (x = 0−0.374), can be achieved by modification of a lyothermal, single source precursor method. The Eu guest ion occupies a tetrahedral lattice site as a Eu(III) defect ion based on analysis of the XPS and XAS data. XRD and XAS measurements show a linear contraction of the lattice parameters for increasing Eu(III) concentration consistent with statistical substitution at both core and surface sites in the lattice by a random ion displacement mechanism. On the basis of a Vegard's law analysis, the Eu(III) ion is substituted in the tetrahedral cationic lattice site without formation of vacancies or phase segregation of the Eu ion in the lattice.