Synthesis of modified vermiculite by interaction with aromatic heterocyclic amines

Vermiculite of general formula [Si_6.85Al_1.15][Mg_4.68Al_0.51Fe_0.63]O₂₀(OH)₄Ca_0.128Na_0.032K_0.094 reacted with heteroaromatic amines α-, β-, and γ-picolines from aqueous solution. The products were characterized by elemental analysis, infrared spectroscopy, and X-ray diffraction. The intercalated nanocompounds maintained the crystallinity and changed the original interlayer distance of 1422 pm to 1474, 1456, and 1474 pm, for the sequence of the guest picoline molecules. Natural and intercalated vermiculite can remove copper at the solid/liquid interface; removal 0.40 mmol g⁻¹ was obtained for the original matrix, and 1.10, 0.92, and 1.33 mmol g⁻¹ for the intercalated forms. These values are near the capacity of cation exchange (CEC) of this clay mineral, which can be possibly used as source of copper removal from aqueous solution.     

Latex-mediated synthesis of ZnS nanoparticles: green synthesis approach

A low-cost, green synthesis of ZnS nanoparticles is reported using 0.3 % latex solution prepared from Jatropha curcas L. ZnS nanoparticles were characterized by X-ray diffraction, selected area electron diffraction, transmission electron microscopy, energy dispersive analysis of X-rays, UV–vis optical absorption and photoluminescence techniques. Fourier Transform Infrared Spectroscopy was performed to find the role of cyclic peptides namely curcacycline A (an octapeptide), curcacycline B (a nonapeptide) and curcain (an enzyme) as a possible reducing and stabilizing agents present in the latex of J. curcas L. The average size of ZnS nanoparticles was found to be 10 nm. Latex of J. curcas L. itself acts as a source of sulphide (S⁻²) ions that are donated to Zn ions under present experimental conditions. Source of sulphide (S⁻²) ions is still unclear, but we speculate that cysteine or thiol residues present in enzyme curcain may be donating these sulphide (S⁻²) ions.     

Observation of green emission from Ce-doped gadolinium oxide nanoparticles

Green emission at around 500 nm is observed in Gd₂O₃:Ce³⁺ nanoparticles and the intensity is highly dependent on the concentration of Ce³⁺ in the nanoparticles. The luminescence of this emission displays both picosecond (ps) and millisecond (ms) lifetimes. The ms lifetime is over four orders of magnitude longer than typical luminescence lifetimes (10-40 ns) of Ce³⁺ in traditional Ce³⁺ doped phosphors and therefore likely originates from defect states. The picosecond lifetime is shorter than the typical Ce³⁺ value and is also likely due to defect or surface states. When the samples are annealed at 700 °C, this emission disappears possibly due to changes in the defect moieties or concentration. In addition, a blue emission at around 430 nm is observed in freshly prepared Gd₂O₃ undoped nanoparticles, which is attributed to the stabilizer, polyethylene glycol biscarboxymethyl ether. On aging, the undoped particles show similar emission to the doped particles with similar luminescence lifetimes. When Eu³⁺ ions are co-doped in Gd₂O₃:Ce nanoparticles, both the green emission and the emission at 612 nm from Eu³⁺ are observed.     

Electrochemical synthesis of magnetic iron oxide nanoparticles with controlled size

We present a novel and facile method enabling synthesis of iron oxide nanoparticles, which are composed mainly of maghemite according to X-ray diffraction (XRD) and Mössbauer spectroscopy studies. The proposed process is realized by anodic iron polarization in deaerated LiCl solutions containing both water and ethanol. Water seems to play an important role in the synthesis. Morphology of the product was studied by means of transmission electron microscopy and XRD. In the solution containing almost 100% of water a black suspension of round shaped maghemite nanoparticles of 20–40 nm size is obtained. Regulating water concentration allows to control nanoparticle size, which is reduced to 4–6 nm for 5% of water with a possibility to reach intermediate sizes. For 3% or lower water concentration nanoparticles are of a needle-like shape and form a reddish suspension. In this case phase determination is problematic due to a small particle size with the thickness of roughly 3 nm. However, XRD studies indicate the presence of ferrihydrite. Coercivities of the materials are similar to those reported for nanoparticle magnetite powders, whereas the saturation magnetization values are considerably smaller.     

Reverse micelle synthesis of perovskite oxide nanoparticles

La_0.6Sr_0.4Co_xFe_1−xO_3−δ (LSCF), La_0.6Sr_0.4Cu_0.2Fe_0.8O_3−δ, Ba_0.5Sr_0.4Co_0.8Fe_0.2O_3−δ and LaFeO_3−δ nanoparticles were synthesized by a reverse micelle procedure. Controlling the size of the micelles through the water:oil phase ratio enabled synthesis of phase pure perovskite particles with average sizes from 14 nm to 50 nm. Small amounts of an impurity phase, likely cobalt oxide, were detected in the XRD spectrum of high cobalt content samples of LSCF (x = 0.8). La_0.6Sr_0.4Co_0.2Fe_0.8O_3−δ nanoparticles were utilized to coat the surface of a dense thin-film La_0.6Sr_0.4Co_0.2Fe_0.8O_3−δ solid oxide fuel cell cathode. The polarization resistance of the nanoparticle coated electrode, measured at open circuit in air at 973 K, was 20% lower than an equivalent un-coated electrode.     

Controlled synthesis and characterization of layered manganese oxide nanostructures with different morphologies

Layered manganese oxide nanostructures with different morphologies, such as nanowire bundles, cotton agglomerates, and platelikes were successfully fabricated by a simple and template-free hydrothermal method based on a reaction of KMnO₄ and KOH solutions with different concentrations. The obtained nanowire bundles were assembled by nanowires with diameters of 10 to 200 nm and lengths up to 5–10 μm. The cotton agglomerates were composed of manganese oxide layers with a thickness of about 10 nm. Both the concentration of KOH solutions and the reaction temperature played an important role in the formation of layered manganese oxide nanostructures with different morphologies. XRD, SEM, TEM, HRTEM, SAED, TG-DTA, and chemical analysis were employed to characterize these materials. On the basis of the experimental results, a possible formation mechanism of layered manganese oxide nanostructures with different morphologies was presented. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Chemical synthesis and characterization of manganese oxide coated Ni particles

Nanosized Ni particles with an average diameter of about 8 nm were prepared by reducing of NiCl 2 with sodium borohydride (NaBH 4 ) in aqueous solution. By moderate annealing in protective atmosphere, the composite grew up to be 15-20 nm particles. Both of the as-prepared and annealed Ni particles were coated by a layer of manganese oxide via decomposition reaction in aqueous KMnO4 solution. Hysteresis loops of as-prepared samples show a large increase in the magnetization with decreasing temperature and an unsaturated component at high magnetic field. In contrast, the ferromagnetic characteristics of annealed one are much stronger with large magnetization and coercivity. The thermomagnetic curves verified the coexistence of ferromagnetic Ni and antiferromangetic Mn oxide phases. But there exists no exchange bias behavior in the samples, even though the interface structure between the ferromagnetic Ni core and the antiferromagnetic manganese oxides has been distinctly formed. The absence of exchange bias probably originates from the weak ferromagnetic characteristic of Ni cores.     

Formation of fractal aggregates during green synthesis of silver nanoparticles

The aggregation behavior of silver nanoparticles (AgNPs) prepared by a green synthesis procedure using starch as the stabilizer was studied by the small angle X-ray scattering (SAXS) technique. The protecting ability of starch was affected by the presence of NaOH leading to different aggregation behaviors. In all the samples, mass as well as surface fractal regimes were observed. Assuming spherical form, the radii of nanoparticles were in the range of 11–17 nm.     

Laser ablation synthesis of indium oxide nanoparticles in water

Colloidal solutions of Indium oxide nanoparticles have been produced by means of laser ablation in liquids (LALs) technique by simply irradiating with a second harmonic (532 nm) Nd:YAG laser beam a metallic indium target immersed in distilled water and varying the laser fluence up to 10 J cm⁻² and the ablation time up to 120 min. At all the investigated fluences the vaporization process of the indium target is the dominant one. It produces a majority (>80%) of small size (<6 nm) nanoparticles, with a very limited content of larger ones (size between 10 and 20 nm). The amount of particles increases regularly with the ablation time, supporting the scalability of the production technique. The deposited nanoparticles stoichiometry has been verified by both X-ray photoelectron spectroscopy (XPS) and Energy Dispersive X-ray (EDX) analysis. Optical bandgap values of 3.70 eV were determined by UV-vis absorption measurements. All these results confirm the complete oxidation of the ablated material.     

Silver nanoparticles with gelatin nanoshells: photochemical facile green synthesis and their antimicrobial activity

In the current study, a facile green synthesis of silver-gelatin core–shell nanostructures (spherical, spherical/cubic hybrid, and cubic, DLS diameter: 4.1–6.9 nm) is reported via the wet chemical synthesis procedure. Sunlight-UV as an available reducing agent cause mild reduction of silver ions into the silver nanoparticles (Ag-NPs). Gelatin protein, as an effective capping/shaping agent, was used in the reaction to self-assemble silver nanostructures. The formation of silver nanostructures and their self-assembly pattern was confirmed by SEM, AFM, and TEM techniques. Further investigations were carried out using zeta-potential, UV–Vis, FTIR, GPC, and TGA/DTG/DTA data. The prepared Ag-NPs showed proper and acceptable antimicrobial activity against three classes of microorganisms (Escherichia coli Gram-negative bacteria, Staphylococcus aureus Gram-positive bacteria, and Candida albicans fungus). The antibacterial and antifungal Ag-NPs exhibit good stability in solution and can be considered as promising candidates for a wide range of biomedical applications.     

Copper-assisted shape control in colloidal synthesis of indium oxide nanoparticles

Indium oxide is an important n-type transparent semiconductor, finding application in solar cells, sensors, and optoelectronic devices. We present here a novel non-injection synthesis route for the preparation of colloidal indium oxide nanocrystals by using oleylamine (OLA) as ligand and as solvent. Indium oxide with cubic crystallographic structure is formed in a reaction between indium acetate and OLA, the latter is converted to oleylamide during the synthesis. The shape of the nanocrystals can be influenced by the addition of copper ions. When only indium (III) acetate is used as precursor flower-shaped indium oxide nanoparticles are obtained. Addition of copper salts such as copper (I) acetate, copper (II) acetate, copper (II) acetylacetonate, or copper (I) chloride, under otherwise identical reaction conditions changes the shape of nanoparticles to quasi-spherical or elongated. The anions, except for chloride, do not influence the shape of the resulting nanocrystals. This finding suggests that adsorption of copper ions on the In₂O₃ surface during the nanoparticles growth is responsible for shape control, whereas changes in the reactivity of the In cations caused by the presence of different anions play a secondary role. X-ray diffraction, transmission electron microscopy, nuclear magnetic resonance, energy dispersive X-ray analysis, and UV–Vis-absorption spectroscopy are used to characterize the samples.     

Mesoporous silica nanoparticles in an efficient solvent-free transamidation of carboxamides with amines: an exhibition of a green recyclable nanocatalyst

A protocol is described for an efficient transamidation of amides with amines in the presence of mesoporous silica nanoparticles (MSNs). The latter is used as a green, heterogeneous, and recyclable nanocatalyst, under solvent-free conditions. Following this protocol, a wide range of aromatic, aliphatic, and cyclic/acyclic primary or secondary amines are used in synthesis of a series of amides with good to excellent yields (65–96%). MSNs is characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), small-angle powder X-ray diffraction (XRD), nitrogen adsorption-desorption analysis, and FT-IR spectroscopy. The metal/solvent-free condition, easy work up, high purity of the products, recyclability, and environmentally-friendly nature of the catalyst are the attractive features of this methodology.

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Graphical abstract An efficient transamidation of carboxamides was achieved via the use of mesoporous nanoparticles as green nanocatalyst. The metal/solvent-free condition, easy work up, high purity of the products, recyclability, and environmentally-friendly nature of the catalyst are the attractive features of this methodology.

     

Fluctuation mediated interaction and phase separation of nanoparticles in a liquid crystal solvent

Water-in-oil microemulsions of nanodroplets in the isotropic phase of a thermotropic liquid crystal exhibit, with decreasing temperature and in anticipation of a demixing transition, enhanced correlation in fluctuations of both molecular orientation and droplet concentration. Mean field modeling of this pretransition behavior, on the basis of a lattice in which the nanodroplets are introduced as holes, shows that the observed interdroplet attractive interaction is produced by the disordering effect of the droplets on the liquid crystal and mediated solely by paranematic fluctuations.     

Optimisation of aqueous synthesis of iron oxide nanoparticles for biomedical applications

Iron oxide nanoparticles (IONPs) were prepared via aqueous synthesis which combines alkaline co-precipitation (CP) of ferric and ferrous precursors with mild hydrothermal (HT) treatment without cupping agents (CA). In this novel synthesis route, CP + HT, we found the optimal synthesis conditions to obtain IONPs without a second phase and with the size larger than in standard CP: the equal number of Fe(II) and Fe(III) ions are co-precipitated with 6 M ammonia and further HT treated in mild conditions (120 °C for 24 h) without CA. The IONPs obtained by novel CP + HT route had faceted rectangular morphology, a mean TEM diameter of 21.5 ± 6.3 nm, a hydrodynamic diameter of 30.2 ± 9.1 nm and a zeta potential at pH 4 of 48.2 ± 0.6 mV. After the subsequent oxidation step, the final product (IONPs) was studied by XRD, FTIR and XPS, which confirmed the desired structure of γ-Fe₂O₃. Importantly, this synthesis was especially planned for the preparation of IONPs for biomedical applications. Thus, our novel synthesis was designed to be compliant with the regulations of nano-safety: no special atmosphere, no complex multistep size separation, no organic solvents or solvent exchange, no CA and their washing and the use of low temperature in the final optimised conditions. In addition, this simple synthesis route combines the CP and HT methods, which are both proven to be scalable. Moreover, repeatability and reproducibility of the optimal CP + HT synthesis were confirmed on the lab-scale; more than 100 repetitions with different dishes, different operators and different batches of chemicals were performed.     

醇热反应低温合成锰钴镍热敏薄膜

锰钴镍复合氧化物是一种具有半导体性质的热敏材料. 本文采用金属有机沉积技术于室温条件下、在Si衬底上沉积一定 厚度的Mn_1.74Co_0.72Ni_0.54O₄金属 有机化合物薄膜, 并通过醇热反应进行低温结晶化合成, 可得到Mn_1.74Co_0.72Ni_0.54O₄结晶薄膜. 通过X 射线衍射、场发射扫描电子显微镜 (FESEM) 以及阻温特性等测试方法表征, 讨论了醇热反应对锰钴镍热敏薄膜的物相结构、微观形貌以及电学性能的影响. X射线衍射图显示薄膜已出现尖晶石结构的特征峰. 电镜照片说明结晶薄膜的表面较为平整、孔隙率低. 阻温特性关系表明薄膜具有明显的负温度系数效应, 室温(≈27°) 电阻率约为303.13 Ω·cm. 关键词： 醇热反应 锰钴镍薄膜 热敏电阻 低温合成     

Simulation of interaction of radiation with nanoparticles

Enhancement of microwave radiation at wavelength λ ∼ 10 cm in a cavity is simulated using the system of constituent equations derived earlier. It is shown that a radiation energy density of W ∼ 1000 J/m³ can be attained. Pumping of the medium containing conducting nanoparticles is carried out with a stationary electric field. The required mass concentration of nanoparticles and pumping field are estimated. A method of obtaining active medium using a statitionary electric field for enhancement of microwave radiation in a wavelength range of λ ∼ 10 cm is proposed. In this method, extended conducting nanoparticles should be sputtered.     

Low-temperature first-order reversal curves and interaction effects on assemblies of iron oxide nanoparticles

We present the synthesis and magnetic properties of high quality uncoated and gold-coated iron oxide magnetic nanoparticles. The structural properties of these nanoparticles are investigated by transmission electron microscopy, UV-visible spectroscopy and X-ray diffraction. Experimental results and theoretical simulations indicate that the synthesized nanoparticles present a very good monodispersity, and well defined size and shape. The coercive field of these particles is identified by low-temperature first-order reversal curves and the results used in order to fit zero-field-cooled magnetization processes with theoretical models. The identification of the parameters in this analysis suggests that the coating process hardly affects the morphology and the overall magnetic properties of the cores inside coated particles.     

Ultrasonic activated efficient method for the cleavage of epoxides with aromatic amines

An improved protocol for the cleavage of epoxides with aromatic amines in the presence of FeCl₃ promoted by ultrasonic irradiation. This new methodology provides excellent yields in short reaction times (15–25 min) at room temperature.