Soft Chemical Method Research Articles

Intercalation-type MoP and WP nanodots with abundant phase interface embedded in carbon microflower for enhanced Li storage and reaction kinetics

High discharging capacity materials with an intercalation-type mechanism are the promising anodes to replace the conventional graphite. In this work, WP and MoP nanodots encapsulated in flower-like carbon framework are prepared by a simple soft chemical method followed by phosphorization. The intercalation-type lithiation mechanisms of WP and MoP are proved by the ex situ X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). The electron conductivity and the electrode pulverization of WP@MoP are improved by carbon microflowers. The abundant phase interface facilitates the transfer and storage of Li+, revealed by the galvanostatic intermittent titration technique (GITT) and the density functional theory (DFT). These advantages result in its high discharging capacity (636 mAh g−1 at 0.1 A g−1) and ultralong cycling life (81.5% capacity retention after 1700 cycles at 1 A g−1). The outstanding performances of electrode at high mass loading and full cell further reflect its potential value in practice.

A general method to synthesize metal/N-doped carbon nanocomposites with advanced sodium storage properties

Seeking a general and facile method to prepare the nanocomposite of metal and carbon is the key to develop the metal-based anode in sodium ion battery. Here, a simple soft chemistry method followed by carbonization process is reported to prepare Bi(Sn)/N-doped carbon nanocomposites (denoted as Bi/NC and Sn/NC). The conductive carbon layer effectively hinders the volume effect during sodiation/desodiation process. Thus, Bi/NC and Sn/NC exhibit an outstanding rate capability of 220 and 158 mAh g−1 at 3.0 A g−1 and a long cyclic stability (negligible capacity fading after 2000 cycles for Bi/NC and 86.4% capacity retention after 1000 cycles for Sn/NC at 1.0 A g−1).

Structural, Optical and Photocatalytic Properties of PVC/CdS Nanocomposites Prepared by Soft Chemistry Method

This work investigates the preparation of cadmium sulfide nanoparticles (CdS) embedded in the polymeric polyvinylchloride (PVC) matrix. PVC/CdS nanocomposite films were prepared via sol–gel method with deposition by spin-coating on glass substrates. Effects of CdS nanoparticles on the structural, morphological, optical and photocatalytic properties of the synthetized nanocomposite were studied. Results of XRD and Raman analysis confirm the formation of CdS nanoparticles with hexagonal phase in the PVC matrix, with average crystallite size between 17 to 69 nm. The UV–vis spectroscopy reveals that the transmission is between 80 and 95% in the visible region, and a direct energy bandgap between 4.07 eV for 3.85 eV. The PL emission spectra indicate the interstitial cadmium defect states. In addition, the surface modifier (PVC) exert great influence not only on the optical performance of the particles themselves but also on the size distribution of the particle in the PVC matrix. The photocatalytic study shows a good potential of PVC/CdS nanocomposites films for MB degradation under UV light irradiation.

Understanding Gas Phase Ion Chemistry Is the Key to Reliable Selected Ion Flow Tube-Mass Spectrometry Analyses.

Ion-molecule reactions (IMR) are at the very core of trace gas analyses in modern chemical ionization (CI) mass spectrometer instruments, which are increasingly being used in diverse areas of research and industry. The focus of this Perspective is on the ion chemistry that underpins gas-phase analytical CI methods. Special attention is given to the soft chemical ionization method known as selected ion flow tube-mass spectrometry (SIFT-MS). The processes involved in the ion chemistry of the reagent cations, H3O+, NO+, and O2+•, and the anions, O-•, O2-•, OH-, and NO2-, are discussed in some detail. Stressed throughout is that an understanding of these processes is mandatory to obtain reliable analyses of humid gaseous media such as ambient air and exhaled breath. It is indicated that further research is needed to understand the consequences of replacing helium in some situations by the more readily available nitrogen as the carrier gas in SIFT-MS.

Enhanced Photoreduction Activity in BiOI1‐xFx Nanosheet for Efficient Removal of Pollutants from Aqueous Solution

AbstractBismuth oxyhalide compounds have similar electronic configurations and crystal structures. Due to high electronegativity, they can be used for synthesizing solid solutions that have a number of advantages, which are enhanced charge separation, efficient adsorption, and high photoreduction potential. Solid solutions of the general formula BiOI1‐xFx (X=0 to 0.5) were prepared using the soft chemical method. The investigation of the optical properties of the considered solid solutions revealed a blue shift in wavelength. The solid solution BiOI0.7F0.3 exhibited an excellent adsorption coefficient and optimum photodegradation performance with RhB dye. Compared to pure BiOI, it showed higher adsorption and caused twice more efficient photodegradation. The different density functional theory (DFT) methods calculations revealed that the shift in band gap in the considered solid solutions mainly took the form of up‐shifting in the conduction band; thus, it was predicted that the reduction potential would increase with the increase in fluorine content. The results thus suggest that BiOI1‐xFx solid solutions are a viable alternative for the use in photocatalytic removal of toxic Pb2 ions from aqueous solutions.

Synthesis, characterization of polystyrene-phosphate films and their application as heterogeneous catalyst for Knoevenagel condensation in solvent-free conditions

Novel film catalysts of the polystyrene (Ps) and trimethyl phosphate (P) nanoparticles were synthesized on glass substrates by soft chemistry using doctor blade method. Subsequently, the prepared Ps–P film catalysts were characterized by various techniques, including fourier transform infrared spectroscopy (FTIR), nuclear magnetic resonance (NMR), density (d), polarizing microscope (PM), X-ray diffraction (XRD) and thermal analysis. According to the results, the structure and morphology of film catalysts were confirmed by all analyses. The Ps–P films, as heterogeneous solid catalysts, have demonstrated strong activity for Knoevenagel condensation, producing alkenes of high purity. The recovered yields are excellent, up to 96% in solvent-free conditions at room temperature. Further, the film catalysts have showed high stability, good reusability (up to five times) while maintaining their efficiency and productivity. In the present study, the polystyrene/phosphate film catalysts were characterized and synthesized by soft chemistry method. These film catalysts were show an excellent catalytic activity for Knoevenagel condensation reaction. Further, they have demonstrated high yields, in solvent-free at room temperature, with a good reusability and high stability.

Impact of Different Set of Precipitants on the Formation of BaFe12O19 Phase Nanomaterials.

This work deals with the preparation of BaFe12O19 materials by soft chemical co-precipitation method using a different set of precipitants namely, (i) NaOH and Na₂CO₃, (ii) NH₂CONH₂ and NH₄OH, and (iii) NH₄HCO₃ and NH₄OH. The influence of these precipitants on the different properties is also investigated by various characterizations. The precipitants used in this work considerably affected the phase formation of BaFe12O19 materials. The thermal analyses reveal the thermal decomposition of the intermediate phase as well as the crystallization of BaFe12O19 phase. Due to the amorphous nature, all the co-precipitated products were annealed for 2 h at 1000 °C. Among the different annealed samples, the NaOH and Na₂CO₃ set of precipitant derived materials exhibit nearly single hexagonal phase of crystalline BaFe12O19 nanomaterials with an average crystalline size of ˜48 nm with a = 0.5888(4) nm and c = 2.320(2) nm. The particle size observed in micrograph was rather much higher than the average crystalline size obtained from XRD for the best sample. The BaFe12O19 nanomaterials studied in the present work have been found potential applications in magneto-optic recording media, biomolecular separations, magnetic carriers for drug targeting, permanent magnet, chip inductors, microwave absorbers, and hyperthermia cancer treatment.

Facile soft chemical synthesis and physico-chemical characterisation of ceria based novel ceramic nanocomposite electrolyte for LTSOFC application

ABSTRACT The current study is mainly focused on the preparation of new ceramic electrolyte material based on doped cerium oxide nanocomposite for low-temperature solid oxide fuel cell (LTSOFC) application. The nanocomposite material with composition Ce0.95Nd0.05O2-δ-Ce0.95Gd0.05O2-δ (CNO-CGO) was prepared by a simple cost effective soft chemical precipitation method. The structural, morphological properties and thermal properties of the synthesised nanocomposite material were studied. The mass variation and heat flow rate of CNO-CGO precursor were studied using TGA-DSC analysis. A single fluorite cubic phase structure was revealed by XRD. The surface was studied using SEM resulting in a uniform spherical shape with the agglomerated tightly packed structure without any pores. The presence of a single crystalline phase and the distorted cubic structure was observed by HR-TEM. The nanocomposite was uniaxially pressed and sintered to study the microstructural characteristics. The obtained results were discussed in order to use the material as an efficient electrolyte for LTSOFC application.

Self-growth of graphene nanosheets on a crystalline nanodiamond substrate using NixZnxO catalyst and their efficient photodetection properties

The correlation of structure-properties in material chemistry has stimulated the synthesis of innovative materials with unique nanostructures. At the same time, these new kinds of nanostructures can be fascinating building blocks for future photodetection platforms. Here, we report on the self-growth of fine-edged graphene oxide sheets on crystalline nanodiamond (CND) substrates using NixZnxO as a catalyst and a simple soft chemical method. In this novel strategy, one-dimensional (1D) NixZnxO nanostructures are converted into two-dimensional (2D) nanostructures, with the self-growth of graphene on a CND substrate, as evidenced from Raman, XRD and TEM measurements. It is envisioned that these self-assembled 2D graphene sheets on NixZnxO/CND will promote the performances of broadband spectrum NixZnxO photodetectors. Then, Ag electrodes is used to fabricate the present hybrid nanostructure (graphene/ NixZnxO nanopellets/CND substrate) and utilized for photodetection studies. The as-fabricated hybrid structure exhibited remarkable photo-detection properties compared to those of pristine NixZnxO and ZnO/CND based photodetectors. Specifically, the presented hybrid device shows an enhanced on/off current ratio (~6037), a rapid response/recovery speed (39/32 s), and decent photoresponsivity (3 mA/W), which are superior to those reported to date for crystalline nanodiamond based photodetector studies. In addition, the synergistic effects between graphene and NixZnxO/CND greatly improve the broad range absorption. The enhanced photodetection properties of this hybrid device can be ascribed to the formation of multiple depletion regions and intermediate energy levels. It is hoped that these results will inspire the design and fabrication of innovative nanostructures for high-performance optoelectronic applications.

MnxCo3-xO4 spinel oxides as efficient oxygen evolution reaction catalysts in alkaline media

The design of efficient electrocatalysts for oxygen evolution reaction (OER) is an essential task in developing sustainable water splitting technology for the production of hydrogen. In this work, manganese cobalt spinel oxides with a general formula of MnxCo3-xO4 (x = 0, 0.5, 1, 1.5, 2) were synthesised via a soft chemistry method. Non-equilibrium mixed powder compositions were produced, resulting in high electrocatalytic activity. The oxygen evolution reaction was evaluated in an alkaline medium (1 M KOH). It was shown that the addition of Mn (up to x ≤ 1) to the cubic Co3O4 phase results in an increase of the electrocatalytic performance. The lowest overpotential was obtained for the composition designated as MnCo2O4, which exhibited a dual-phase structure (∼30% Co3O4 + 70% Mn1.4Co1.6O4): the benchmark current density of 10 mA cm−2 was achieved at the relatively low overpotential of 327 mV. The corresponding Tafel slope was determined to be ∼79 mV dec−1. Stabilities of the electrodes were tested for 25 h, showing degradation of the MnCo2O4 powder, but no degradation, or even a slight activation for other spinels.

A facile synthesis of mesoporous Mo–Al oxides for desulfurization of dibenzothiophene in the extractive catalytic oxidative desulfurization system

In order to obtain the deep desulfurization in the extractive catalytic oxidative desulfurization (ECODS) system, the evaporation-induced self-assembly (EISA) assisted by cash (combined assembly by soft and hard chemistry) method was applied to prepare mesoporous Mo–Al oxides with the stable catalytic performance when the acetonitrile as the extractant and H2O2 as the oxidant. Their physical chemical properties were also characterized by XRD, N2 sorption, FT-IR, SEM–EDX, H2-TPR, and Raman techniques. The characterization results indicated that tetrahedral molybdenum species can be highly dispersed into the meso-structure of γ-Al2O3, and the stronger interactions would be formed for 25Mo–Al catalyst than the 25Mo–Al–C catalyst prepared by impregnation method resulting in their superior physical chemical properties although the molybdenum species is the same. The 25Mo–Al catalyst showed higher desulfurization ratio than other xMo–Al catalysts and its value can be reached up to 100% at the molar ratio of H2O2 to dibenzothiophene (DBT) 2.3, volume ratio of oil phase to acetonitrile 3, catalyst dosage 0.012 g/mL, reaction temperature 60 °C and reaction time 30 min. The 25Mo–Al catalyst also showed good stability even after reaction for 10 recycles.

Chemical Syntheses of Two-Dimensional Boron Materials

In this issue of Chem, Kondo and co-workers report a facile soft-chemical method for the preparation of layered, electrically conductive hydrogen boride, which is short-range order but amorphous as a result of the geometrical frustration of the terminal B–H bonds. This work offers an alternative route to two-dimensional (2D) boron materials.

Anti-diabetic activites of ZnO doped with Ce (5 at %) nano particles (NPs)

In general nano materials and nano crystals are widely used in material applications and they have some special properties when compared to bulk materials. For nano powder, PXRD is used. But here nano particles of ZnO doped with Ce 5at % are synthesis directly into nano form by soft chemical method. In this ZnO doped with Ce 5 at % nano particles have anti diabetic activities and the nano particles have the inhibition values are increased with proper increase in the value of concentration (10–80), IC50 values are 28.45 for nano particles of ZnO doped with Ce5 at %.

Anti-diabetic activities of ZnO doped with Ce (3 at %) nano particles

The cerium doped zinc oxide nano particles were successfully synthesized by soft chemical method. The ZnO nano particles doped with cerium has 3 at % is reported here for AD activity. In this study, the inhibition values are increased with proper increase in the value of concentration. We have IC 50 value of 28.97, because of this; these nano particles are confined to be anti-diabetic activities. We take ZnO doped Ce at 3 atomic percent only but we are also in the process doping at 5 and 7 atomic percent too. If the value of atomic percent is varied, corresponding IC 50 values will also varied.

Synthesis and evaluation of antibacterial properties of magnesium oxide nanoparticles

In this paper we studied the efficiency of magnesium oxide (MgO) nanoparticles with an average size of 27 nm synthesized by a simple soft chemical method, in killing both Gram negative and Gram positive pathogenic bacteria. The antibacterial activity was determined by a minimum inhibitory concentration technique, agar cup method and live count technique. These nanoparticles show the maximum antibacterial activity towards Bacillus sp. in comparison with Escherichia coli. Transmission electron microscopy analyses of the treated-bacterial strains showed a morphological deformation with increased cell wall disruption. From the analysis of the antibacterial activity of MgO nanoparticles it is revealed that $$6\,\upmu \hbox {g ml}^{-1}$$ of dose is sufficient for killing Bacillus sp. whereas it is $$7.5\,\upmu \hbox {g ml}^{-1}$$ for E. coli. These doses may be used in medical application. MgO nanoparticles could be used as antibacterial agents after completion of successful in vivo trials.

Novel route for simplified and efficient synthesis of spiky-like copper sulfide nanoballs by soft chemistry method and their basic physicochemical characterizations

Growth of copper sulfide nanoparticles using two different methods is reported in the present investigation. The first reaction was carried out by applying half an hour of heating in constant temperature water bath while in the second case the mixture was sonicated. As copper and sulfur sources, copper nitrate and thiourea solutions were used respectively. Main physicochemical properties of the synthesized samples were studied using various characterization techniques. Formation of copper sulfide with hexagonal crystalline structure was corroborated, coinciding with previously reported values for covellite. The most relevant results corresponded to the un sonicated sample, which exhibited spiky-like nanoballs morphology and better size distribution. Optical tests revealed band gaps of 1.69 and 2.05 eV, while photoluminescence emissions at 421 and 430 nm, showing promising possibilities for applications in solar cells, catalysis and optoelectronic devices.

Soft-Chemical Method for Synthesizing Intermetallic Antimonide Nanocrystals from Ternary Chalcogenide.

The synthesis of intermetallic antimonides usually depends on either the high-temperature alloying technique from high-purity metals or the flux method in highly poisonous Pb-melt. In this paper, we introduced a soft-chemical method to synthesize intermetallic antimonides from ternary chalcogenide precursors under an argon atmosphere below 200 °C. Powder X-ray diffraction and compositional analysis clearly indicate that a new phase of the Ag3Sb nanocrystal was synthesized from the Ag3SbS3 precursors. Three types of trialkylphosphines (TAPs) were applied as desulfurization agents, and the transformation mechanism was elucidated. The capability of the desulfurization agent follows the sequence of triphenylphosphine (TPP) > tributylphosphine(TBP) > trioctylphosphine(TOP). Besides, this TAP-driven desulfurization route to synthesize the intermetallic phase could also be possible for AgSbSe2 and Sb2S3. Therefore, this paper provides an efficient and mild technique for the fabrication of intermetallic nanocrystals.

Methyl Orange Degradation using TiO2 Powder and Immobilized TiO2 Photocatalysts

Methyl orange is one of the anionic dyes and is a major pollutant from textile industry that enters both aquatic and atmospheric systems. In this research, methyl orange was degraded using TiO2 powder and immobilized TiO2 on glass. Titanium tetra-isopropoxide (TTIP) was used for preparation of TiO2 powder using soft chemistry method, and it was immobilized on glass via paste-gel coating method. The prepared photocatalysts were characterized by XRD and SEM. Highly crystalline anatase TiO2 powder photocatalyst was obtained. Meanwhile, immobilized TiO2 was less crystalline and agglomerated onto the glass surface. TiO2 powder had higher degradation rate (71%) compared to immobilized TiO2 (52%) due to its chemical stability and larger amount of photocatalyst contacted with methyl orange during the degradation process.

Synthesis and characterization of novel organic–inorganic hybrid nanocomposites of phosphate–benzimidazole by soft chemistry route in aqueous media

In this work, novel organic–inorganic hybrid nanocomposites M+/PO3− (M = 2,2′-dibenzimidazolyl butane) were prepared by soft chemistry method. The synthesis was done by ion exchange method between sodium metaphosphate anions (yNaPO3) and 2,2′-dibenzimidazolyl butane dichlorhydrates cations (xMCl2) in aqueous media. The MCl2 organic salt and the M+/PO3− hybrid nanocomposites were characterized by using spectroscopic and microscopic analyses. The FTIR and Raman spectroscopy are showed new bands in the hybrid nanocomposites structure, which proved the interactions between PO3 and NH of MCl2 molecules. The UV–Vis results of MCl2 and M+/PO3− materials showed a broad absorption band in 200–300 nm regions, originating from phosphate and benzimidazole molecules. The X-ray diffraction was showed the appearance of new peaks attributed to the phosphate (PO3) and a reduction of the intensity of the benzimidazole peaks. The TEM images are showed changes in appearance and size of hybrid materials. Moreover, the surface of hybrids became less dark and the size of M+/PO3− nanocomposites diameter was < 50 nm. The EDX analysis results revealed the presence of carbon, oxygen, and phosphate, confirming the interactions between phosphate and MCl2 organic salt.

Customized unique core-shell Fe2N@N-doped carbon with tunable void space for microwave response

Here, we report a unique core-shell nanocomposite of Fe2N@N-doped carbon that coats dopamine-derived carbon shells on porous Fe2N nanoparticles via a facile and effective soft chemical method. The feasibility of preparing core-shell structure in the process of polymerization is realized by utilizing the fact that affluent amino and hydroxyl groups in dopamine endow the formidable chelation ability with metal ions. Temperature-dependent volume shrinkage effect of Fe2N originates from the lattice transformation in nitridation process, which is the key factor to control the void space inside carbon nanocubes and optimize the electromagnetic performance. Consequently, the as-prepared samples achieve excellent reflection loss (RL) values and effective absorption bandwidth at an even thin thickness of 1.4 mm. The balance between the temperature-dependent conduction loss and the optimization of hole structure impedance matching may be responsible for the excellent microwave behaviors. This work offers an attractive core-shell Fe2N@carbon with controllable void space as a promising candidate to handle the electromagnetic interface (EMI) issues.