Size-controllable synthesis of catalyst of gold nanoparticles with capping agents of natural chitosan

In this study, size-controllable gold nanoparticles (NPs) are synthesized by using sonoelectrochemical methods in the presence of natural chitosan (Ch). First, positively charged Au-containing complexes were prepared in 0.1 N NaCl by using oxidation–reduction cycle (ORC) treatment to Au substrate. Then size-controllable Au NPs, ranging from 10 to 80 nm in diameter, were synthesized by varying the addition quantities of Ch from 1 to 2 g/L, respectively, in solutions under using sonoelectrochemical reduction. Experimental results indicate that the optimal molar ratio of used Ch to synthesized Au NPs is ca. 3 for obtaining the smallest Au NPs. Moreover, the catalytic activity of the size-controllable Au NPs on the decomposition of acetaldehyde in solution was examined. Au NPs with 10 nm in diameter demonstrate significantly catalytic activity. However, bigger Au NPs with 80 nm in diameter are almost inert for the decomposition of acetaldehyde.     

Structural,spectroscopic and biological investigation of copper oxides nanoparticles with various capping agents

Powder composed of copper oxides nanoparticles with various capping agents has been synthesized and characterized with the use of X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and X-ray diffraction (XRD). Polyvinyl alcohol (PVA), glycol propylene, glycerin and glycerin plus ammonia were used as capping agents. The scanning electron microscopy (SEM) studies showed that nanoparticles form agglomerates with the size from 80 to 120 nm while particles size determined from the XRD experiment was in the range from 7 to 21 nm. XPS and XRD experiments revealed that depending on capping and reducing agents used in the synthesis nanoparticles are composed of Cu₂O, CuO or a mixture of them. The biological activity test performed for a selected sample where the capping agent was glycerin plus ammonia has shown promising killing/inhibiting behavior, very effective especially for Gram negatives bacteria.     

Synthesis and characterisation of magnetite nanoparticles using gelatin and starch as capping agents

Nanoparticles of magnetite passivated with gelatin and starch were synthesised using a co‐precipitation technique. The nanoparticles were characterised using ultraviolet–visible (UV–vis), dynamic light scattering (DLS), Zeta potential, transmission electron microscope (TEM), X‐ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The UV–vis spectra showed characteristic surface plasmon resonance of magnetite nanoparticles. The DLS results showed the nanoparticles to have average hydrodynamic diameters of 138 ± 2 and 283 ± 21 nm for particles passivated with gelatin and starch, respectively. The stability in a colloidal solution was greater in nanoparticles passivated with gelatin than nanoparticles obtained with starch, as can be seen by their Zeta potential value (−31 ± 2 and −16 ± 0.5 mV, respectively). According to the TEM evaluation, the use of gelatin allowed to obtain nanoparticles with a spherical morphology and an average size of 10 ± 2 nm. However, when using starch the nanoparticles exhibited diverse morphologies with an average size of 25 ± 7 nm. The XRD results confirmed the crystalline structure of the samples, which showed crystallite sizes of 14.90 and 24.43 nm for nanoparticles passivated with gelatin and starch, respectively. FTIR analysis proved the establishment of interactions between functional groups of biopolymers and magnetite nanoparticles.Inspec keywords: crystallites, nanofabrication, ultraviolet spectra, gelatin, surface plasmon resonance, transmission electron microscopy, scanning electron microscopy, visible spectra, X‐ray diffraction, iron compounds, electrokinetic effects, particle size, colloids, nanoparticles, nanomedicine, precipitation (physical chemistry), light scattering, magnetic particles, Fourier transform infrared spectra, nanomagnetics, filled polymers, nanocompositesOther keywords: magnetite nanoparticles, gelatin, starch, characteristic surface plasmon resonance, capping agents, passivation, co‐precipitation technique, ultraviolet–visible spectra, zeta potential value, dynamic light scattering, DLS, transmission electron microscopy, TEM, X‐ray diffraction, XRD, Fourier transform infrared spectroscopy, FTIR, surface plasmon resonance, hydrodynamic diameters, colloidal solution, spherical morphology, crystalline structure, crystallite size, biopolymers, Fe₂ O₃      

N-alkylthioureacadmium (II) complexes as novel precursors for the synthesis of CdS nanoparticles

The cadmium(II) complexes of thiourea and N-alkylthioureas (with alkyl group methyl or ethyl) have been used as precursors for the preparation of TOPO-capped CdS nanoparticles. The precursors are air-stable, easy to prepare and inexpensive. These compounds decompose cleanly to give good quality crystalline materials. The nanoparticles obtained showed quantum confinement effects in their optical spectra and close-to-band-edge emission in luminescence experiments. The broad diffraction patterns and the diffuse rings observed in the SAED patterns are typical of nanometric particles. The TEM images showed agglomerates of needle-like plates of particles. The presence of a strong phosphorus peak in the EDAX spectra is indicative of TOPO bound to the surface.     

Facile microwave-combustion synthesis of wurtzite CdS nanoparticles

In this study we first report microwave-combustion synthesis of faceted CdS nanoparticles by using cadmium thiocyanate complex as a single source precursor. This is the first example of a metal-thiocyanate (M-SCN) complex being used as a source for metal sulfides (M-S) preparation in a microwave-combustion process. The synthesized CdS was characterized using X-ray diffraction (XRD), field mission scanning electron microscopy (FE-SEM), and high-resolution transmission electron microscopy (HR-TEM). The by-product assisted combustion synthesis yields CdS nanoparticles with the mixtures of octahedral geometries, hexagonal, and triangle plate morphologies and the sizes were found to be 100 nm to 5 microm. The XRD patterns imply the formation of well crystallized wurtzite CdS. The influence of cadmium and sulfur precursors and microwave irradiation time on the morphology of CdS nanoparticle was also investigated. The cadmium and sulfur precursors strongly influenced the CdS morphology and increasing the microwave irradiation time and intensity has no effect on the CdS morphology. In addition, a plausible mechanism of CdS nanoparticle formation has been proposed in this research.     

CdS纳米颗粒的合成方法研究及比较

CdS纳米颗粒在太阳能转化、非线性光学、光电子化学电池和光催化等方面具有广泛的应用,因此其合成方法的研究近年来受到人们的青睐.按照反应物的状态,将纳米硫化镉的制备方法分为固相法、液相法和气相法.本文详细介绍了各种制备方法,分析比较了它们的优点和缺点.     

Novel synthesis and characterization of cobalt titanate nanoparticles: investigation of capping agents effect and its photocatalyst application

This work has provided a general, simple, and effective method to control the composition and morphology of CoTiO₃ nanoparticles, which revealed potential new insight into inorganic synthesis methodology. CoTiO₃ nanoparticles were synthesized via a novel route based on the reaction between cobalt salt and tetra-n-butyl titanate (TNBT) in ethanol. Results of this investigation demonstrate that CoTiO₃ with very uniform sphere-like shape, small grain size and pure rhombohedral phase could be synthesized by different capping agents such as asparagine, alanine, and leucine. XRD, SEM, EDS, and UV–vis spectroscopy were employed to characterize structural, morphological, and optical properties of CoTiO₃ nanoparticles. According to the vibrating sample magnetometer (VSM) result, CoTiO₃ nanoparticles indicated a paramagnetic behavior at room temperature. Furthermore, the photocatalytic properties of as synthesized CoTiO₃ were evaluated by degradation of methyl orange (MO) as water contaminant.     

Synthesis and photochemical performance of CdS nanoparticles photocatalysts for photodegradation of organic dye

Large scale CdS nanoparticles are synthesized by a facile and effective route. The as-prepared CdS product was characterized by X-ray diffraction, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electronmicroscopy, photoluminescence spectroscopy, X-ray photoelectron spectroscopy and UV–Vis diffuse reflectance spectroscopy. The CdS nanoparticles showed higher photocatalytic activity for the discoloration of methyl orange under UV light irradiation for 90 min. Significantly, the stability and recycling of the photocatalyst was also investigated. This study may provide a new insight into the design and prepared of visible-light photocatalytic materials.     

Influence of organic polymers as capping agent on structural and optical properties of ZnS:Mn2+ and CdS nanocrystals

We have synthesized the luminescent ZnS:Mn2+ and bare CdS nanocrystals by employing polyvinyl alcohol (PVA), citric acid (CA) and biotin as organic capping agents by chemical co-precipitation route. The synthesized materials were characterized by X-ray diffraction, small angle X-ray scattering and transmission electron microscopy for the structural analysis, while UV-Visible spectroscopy and photoluminescence (PL) for optical properties. The results show that all the three organic polymers have the same effect and are capable of controlling the growth of the nanoclusters. From UV-Visible absorption spectra, it was observed that different capping agents do not affect the band gap of ZnS:Mn2+ system as well, while capping effect clearly observed on PL properties of ZnS:Mn2+ system. We have observed a novel result that capping with biotin show excellent photoluminescence as compared to capping of PVA and CA on ZnS:Mn2+ -systems. On the other hand, the annealing of these systems leads to degradation of luminescence intensity.     

Chemical synthesis of CdS nanoparticles and their optical and dielectric studies

Cadmium sulphide nanoparticles were synthesized by chemical displacement reaction method using cadmium nitrate as cadmium source and ammonium sulphide as sulphur source. The CdS samples are characterized using X-ray diffraction, UV–Vis spectroscopy, FTIR spectroscopy, scanning electron microscopy and impedance spectroscopy. CdS nanoparticles are found to possess cubic structure with the crystallite size ~10 nm. The absorption spectra of synthesized CdS nanoparticles revealed the blue shift in excitonic transitions with respect to CdS bulk material, clearly confirming the formation of nanoparticles. The dielectric properties of CdS nanoparticles are studied in the frequency range 10³–10⁷ Hz at room temperature. The dielectric properties of CdS nanoparticles are found to be significantly enhanced specially in the low frequency range due to confinement.     

Fluorescent CdS nanoparticles for cell imaging

Fluorescent cadmium sulfide nanoparticles stabilized by an organic shell based on ethylenediaminetetraacetic acid have been prepared by chemical condensation in an aqueous solution. The nanoparticle concentration in aqueous solutions has been optimized and it has been shown that such hybrid nanoparticles can be used to image cell cultures and explore the cell structure. Not only the nanoparticle concentration but also the incubation time of the nanoparticle solution with the cell culture are essential for observing structural details.     

The effect of capping agents on the structural and magnetic properties of cobalt ferrite nanoparticles

Microwave-assisted co-precipitation method was adopted to analyze the effect of polyethylene glycol (PEG) and urea concentrations on the properties of cobalt ferrite nanoparticles (NPs). The average crystallite size of single phase cubic spinel cobalt ferrite NPs was controlled within 10–14 nm with the effect of PEG, urea and the combination of them. The transmission electron micrographs revealed that the morphology of cobalt ferrites was not significantly influenced by the different concentration of capping agents but almost uniform morphology with nearly narrow size distribution was obtained. The interaction of PEG and urea molecules on the surface of nanoparticles was mediated through –OH hydroxyl group affected the crystal growth rate. The possible interaction mechanism was proposed with the help of IR vibrational spectra. All the samples exhibited ferromagnetism at room temperature and it was found that the capping agents showed an effect on the magnetic properties. The maximum saturation magnetization of 58 emu/g was achieved when the urea of 60 mg was used and the maximum coercivity of 311 Oe was attained when the mixture of PEG (40 mg) and urea (20 mg) were used. Ultrafine and hydrophilic cobalt ferrite NPs that showed appreciable magnetic properties obtained in the present experimental procedure would be of great interest in various biomedical applications.     

Green and gentle synthesis of Cu2O nanoparticles using lignin as reducing and capping reagent with antibacterial properties

In this work, Cu₂O nanoparticles of a particular shape were prepared by an eco-friendly, gentle and low-cost synthetic method using lignin as a reducing and capping reagent. Structure and morphology of the Cu₂O nanoparticles were characterised by high-resolution transmission electron microscopy, X-ray photoelectron spectroscopy, X-ray diffraction (XRD) and Fourier-transform (FT-IR) spectroscopy. The results established that Cu₂O nanoparticles coated by lignin showed a particular shape. The morphology of Cu₂O nanoparticles presented as some loose accumulation of particles just like broccoli, and the particle size range was between 100 and 200 nm. And, the XRD revealed the structure of crystalline of the Cu₂O nanoparticles. In addition, the sterilisation of Cu₂O nanoparticles on Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) was also investigated. The Cu₂O nanoparticles showed effective bactericidal activity against E. coli and S. aureus. The antibacterial rate could get 100% after 30 min with 4.0 g/L Cu₂O nanoparticles. Furthermore, the Cu₂O nanoparticles were confirmed to have low cytotoxicity.     

Surface-modified CdS nanoparticles as a fluorescent probe for the selective detection of cysteine

We present a novel method for the selective detection of cysteine, a sulfur-containing amino acid, which plays a crucial role in many important biological functions such as protein folding. Surface-modified colloidal CdS nanoparticles have been used as a fluorescent probe to selectively detect cysteine in the presence of other amino acids in the micromolar concentration range. Cysteine quenches the emission of CdS in the 0.5-10?μM concentration range, whereas the other amino acids do not affect its emission. Among the other amino acids, histidine is most efficient in quenching the emission of the CdS nanoparticles. The sulfur atom of cysteine plays a crucial role in the quenching process in the 0.5-10?μM concentration range. Cysteine is believed to quench the emission of the CdS nanoparticles by binding to their surface via its negatively charged sulfur atom. This method can potentially be applied for its detection in biological samples.     

Structural characterization of CdS nanoparticles grown in polystyrene matrix by thermolytic synthesis

Cadmium sulfide nanoparticles embedded in a polystyrene matrix (CdS/PS) were successfully prepared by in situ thermolysis of a cadmium thiolate precursor dispersed in the polymer. The heat-induced formation of cadmium sulfide was studied by thermogravimetric analysis and differential thermal analysis, while the chemistry of the reaction forming the CdS/PS compound was investigated by nuclear magnetic resonance and X-ray photoelectron spectroscopy. The structural characterization was performed by X-ray diffraction and transmission electron microscopy. The CdS nanocrystals are single crystals of cubic phase (zincblende structure) of spherical shape. The average diameter of the nanocrystals embedded in the polystyrene matrix achieved by our synthesis process is as small as 2.5 ± 0.5 nm. Room temperature UV–VIS absorption spectra exhibit a shoulder at 412 nm that is consistent with the presence of CdS nanocrystals of ∅ ≈ 2 nm. The role of the polymer on the nanoparticle growth was also discussed.     

One-pot morphology-controlled synthesis of various shaped mesoporous silica nanoparticles

A simple synthetic method has been developed for synthesis of mesoporous silica nanoparticles with versatile morphologies by adopting CTAB and C₁₂–OH as dual soft templates. In such a simple method, only by regulating the dose of C₁₂–OH and temperature, we can well-realize the silica nanoparticle morphological transformation from sphere to shell-like, rugby-like, peanut-like, hollow, and complex yolk–shell structures. These as-fabricated silica nanoparticles were characterized by scanning electron microscopy, transmission electron microscopy, Brunauer–Emmett–Teller (BET), and small-angle powder X-ray diffraction. The as-prepared mesoporous silica nanoparticles with versatile morphologies possessing varying BET surface areas, pore diameter, and pore distributions have some potential applications in separation, sensing, and heterogeneous catalysis.     

Eco-friendly green synthesis of silver nanoparticles and their potential applications as antioxidant and anticancer agents

Abstract

Eco-friendly green synthesis of nanoparticles using medicinal plants gained immense importance due to its potential therapeutic uses. In the current study, silver nanoparticles (AgNPs) were synthesized using water extract of Jurinea dolomiaea leaf and root at room temperature. MTT assay was used to study anticancer potential of AgNPs against cervical cancer cell line (HeLa), breast cancer cell lines (MCF-7), and mouse embryonic fibroblast (NIH-3 T3) cell line for toxicity evaluation. The antioxidant potential was evaluated using stable DPPH radicals. In addition, the apoptotic nuclear changes prompted by AgNPs in more susceptible HeLa cells were observed using fluorescence microscope through DAPI and PI staining. Physiochemical properties of biosynthesized AgNPs were characterized using various techniques. AgNPs were formed in very short time and UV–vis spectra showed characteristic absorption peak of AgNPs. SEM and TEM showed spherical shape of AgNPs and XRD revealed their crystalline nature. EDX analysis revealed high percentage of silver in green synthesized AgNPs. FTIR analysis indicated involvement of secondary metabolites in fabrication of AgNPs. In vitro cytotoxic and antioxidant study revealed that herb and biosynthesized AgNPs exhibited significant dose-dependent and time-dependent anticancer and antioxidant potential. Furthermore, study on normal cell line and microscopic analysis of apoptosis revealed that AgNPs exhibited good safety profile as compared to cisplatin and induces significant apoptosis effect. Based on the current findings, it is strongly believe that use of J. dolomiaea offers large scale production of biocompatible AgNPs that can be used as alternative anticancer agents against cancer cell lines tested.     

Crystallization kinetics and densification of YAG nanoparticles from various chelating agents

Yttrium aluminium garnet (YAG, Y₃Al₅O₁₂) nanoparticles were prepared using sonochemical sol-gel method with three different chelating agents and the effect of crystallization kinetics was investigated with differential scanning calorimetry-thermogravimetry (DSC-TG). The activation energy values of crystallization for the as-synthesized YAG nanoparticles using citric acid (CA), glycine (G) or a mixture of citric acid-glycine (CA-G), as chelating agents were found to be 160.5, 142.2 and 140.4 kJ mol⁻¹ and the corresponding Avarami constants were 2.2, 2.1 and 1.9, respectively. Samples produced with the mixed chelating agent under sonification, could be crystallized to single phase YAG nanoparticles (10-65 nm) after annealing at 1100 °C. Pellets made from the annealed YAG particles could be sintered to a relative density greater than 99% at 1500 °C with a grain size of 4.5 μm, made up of secondary particles formed from primary nano-crystals within the grains. Grain size and relative density increased with different chelating agents from CA to G and CA-G in the increasing order when YAG samples were sintered. Grain growth and densification occurred at a relatively low temperature of 1500 °C as compared to over 1800 °C in solid-state reactions.     

Chitosan as template for the synthesis of ceria nanoparticles

Cerium oxide (CeO₂), nanoparticles were prepared using chitosan as template, cerium nitrate as a starting material and sodium hydroxide as a precipitating agent. The resultant ceria–chitosan spheres were calcined at 350 °C. The synthesized powders were characterized by, XRD, HRTEM, UV–vis, FTIR, and TG-DTA. The average size of the nanoparticles obtained was ∼4 nm and BET specific surface area ∼105 m² g⁻¹. Blueshifts in the ultraviolet absorption spectra have been observed in cerium oxide nanocrystallites. The band-gap was found to be 4.5 eV. The blueshifts are well explained for diameters down to less than a few nanometers by the change in the electronic band structure.