Kinetics and mechanism of the formation of silver nanoparticles by reduction of silver (I) with maltose in the presence of some active surfactants in aqueous medium

The kinetics and mechanism of the formation of silver nanoparticles by reduction of Ag⁺ with maltose were studied spectrophotometrically by monitoring the absorbance change at 412 nm in aqueous and micellar media at a temperature range 45–60 °C. The reaction was carried out under pseudo-first-order conditions by taking the [maltose] (>tenfold) the [Ag⁺]. A mechanism of the reaction between silver ion and maltose is proposed, and the rate equation derived from the mechanism was consistent with the experimental rate law. The effect of surfactants, namely cetyltrimethylammonium bromide (CTAB, a cationic surfactant) and sodium dodecyl sulfate (SDS, an anionic surfactant), on the reaction rate has been studied. The enthalpy and the entropy of the activation were calculated using the transition state theory equation. The particle size of silver sols was characterized by transmission electron microscopy and some physiochemical and spectroscopic tools.     

Nucleation and growth kinetics of silver nanoparticles prepared by glutamic acid in micellar media

The title reaction in the presence of cetyltrimethylammonium bromide (CTAB) has been followed spectrophotometrically at 325 nm. In the process of reduction, characteristic surface resonance plasmon absorption peaks appear for the silver nanoparticles (NP) and the intensities increase with reaction time. UV–visible spectra suggest that [CTAB] and glutamic acid influence the morphology of the silver NP and act as shape‐directing agents, whereas [Ag⁺] has no effect. The effects of the total [glutamic acid], [CTAB], and [Ag⁺] on the apparent rate constants of silver NP formation are determined. The sigmoidal curve of absorbance versus reaction time indicates an autocatalytic path involved in the growth process. The α‐amino and ? COOH groups undergo chemical transformation (oxidative deamination and decarboxylation). The particles are spherical in shape with average diameters ranging between 12 and 25 nm, and their size distribution is wide. A plausible mechanism has been proposed with the following rate law: (d[silver sol])/dt = k[Ag⁺][Glutamic acid]_T. © 2012 Wiley Periodicals, Inc. Int J Chem Kinet 44: 680–691, 2012     

Effect of Poly(Vinyl Alcohol) on the Size,Shape, and Rate of Silver Nanoparticles Formation

The kinetics of cetyltrimethylammonium bromide (CTAB) stabilized silver nanoparticles have been studied spectrophotometrically at 425 nm (λ_max of silver sol) in the absence and presence of water soluble polymer (poly(vinyl alcohol); PVA). Transmission electron microscopy (TEM), ultraviolet-visible spectroscopy, and viscosity measurements were used to determine the size, shape, and the size distribution of the silver nanoparticles. The reaction follows the same behavior with respect to [CTAB], [tri-sodium citrate], and [Ag⁺] in both the media indicating the silver nonoparticles were formed through the same reaction path. The sigmoid nature of the kinetic curves suggests an autocatalytic path in the growth of nanoparticles. The reaction rate is increased by increasing [CTAB]. The presence of PVA inhibits nucleation and retards the rate of particle growth, absorbance and size of the particles. Polymer-surfactant interactions were analyzed based on the viscosity of the reaction mixture.     

Preparation and Antibacterial Effect of Bamboo Charcoal/Ag on Staphylococcus Aureus and Pseudomonas Aeruginosa

Bamboo charcoal supporting silver (BC/Ag) was prepared by activation and chemical reduction. The BC/Ag composites were characterized by silver particle size and distribution, silver ion (Ag⁺) release and antibacterial properties. Scanning and transmission electron microscopy (SEM and TEM) showed that the Ag particles were distributed uniformly on the BC matrix. The Ag particle size was found to be less than 150 nm based on TEM. The Ag⁺ release increased initially which was followed by a marginal increase between the 8th and 24th hour. Composites contained higher amounts of silver exhibited a further rise in Ag⁺ release from the 24‐hours of storage in water. The antibacterial effects of the BC/Ag composite powders against Pseudomonas aeruginosa and Staphylococcus aureus were assessed from the minimum inhibitory concentrations (MICs) and minimum bactericidal concentrations (MBCs) method, and an excellent antibacterial performance was discovered.     

Structural and optical characterization of Ag-doped TiO2 nanoparticles prepared by a sol–gel method

Undoped and silver-doped TiO₂ nanoparticles (Ti_1?x Ag _x O₂, where x?=?0.00?C0.10) were synthesized by a sol?Cgel method. The synthesized products were characterized by X-ray diffraction (XRD), particle size analyzer (PSA), scanning electron microscope (SEM), and UV?CVisible spectrophotometer. XRD pattern confirmed the tetragonal structure of synthesized samples. Average crystallite size of synthesized nanoparticles was determined from X-ray line broadening using the Debye?CScherrer formula. The crystallite size was varied from 8 to 33?nm as the calcination temperature was increased from 300 to 800?°C. The incorporation of 3 to 5% Ag⁺ in place of Ti⁴⁺ provoked a decrease in the size of nanocrystals as compared to undoped TiO₂. The SEM micrographs revealed the agglomerated spherical-like morphology of particles. SEM, PSA, and XRD measurements show that the particles size of the powder is in nanoscale. Optical absorption measurements indicated a red shift in the absorption band edge upon silver doping. Direct allowed band gap of undoped and Ag-doped TiO₂ nanoparticles measured by UV?CVis spectrometer were 3.00 and 2.80?eV, respectively, at 500?°C.     

Green synthesis of silver nanoparticles using different volumes of <Emphasis Type="Italic">Trichodesma indicum</Emphasis> leaf extract and their antibacterial and photocatalytic activities

Silver nanoparticles (Ag NPs) were prepared by a green synthesis process, using Trichodesma indicum (T. indicum) leaf extract at different (5, 10 and 15 mL) concentrations. The formation of Ag NPs was confirmed by UV–Vis spectrophotometry with surface plasmon resonance at 443 nm. After this confirmation, the influence of leaf extract concentrations on the structural and surface morphological properties was studied. Along with their physical properties, antibacterial activity against pathogenic (B. cereus and E. coli) bacteria and photocatalytic de-colorization of methylene blue (MB) were examined. The XRD studies revealed that all the nanoparticles exhibited preferential orientation along the (111) plane of silver. The crystallite size decreases as the extract concentration is increased. From SEM images, it was found that the particles are spherical in shape and the size of the particles decreased drastically when the leaf extracts concentration is greater than 10 mL. The images strongly support the result observed from the SEM studies. FT-IR analysis showed that the plant compounds are involved in the reduction of Ag⁺ ions to Ag⁰. Ag NPs synthesized in 15 mL of leaf extract greatly resist the growth of both species and decomposed 82% of MB within 210 min. This ability of Ag NPs can be due to the small spherical-shaped particles and larger Ag⁺ ion release.     

Ag2O-Bi2MoO6:制备及光催化降解富里酸

以钼酸铵、硝酸铋和硝酸银为原料, 以十六烷基三甲基溴化铵(CTAB)为辅助活性剂, 采用水热法合成了Ag₂O-Bi₂MoO₆光催化剂。用X射线粉末衍射、扫描电镜及紫外-可见吸收光谱等进行表征, 并对水中天然有机物富里酸进行了光催化氧化研究。结果表明:未掺杂钼酸铋表面平滑, Ag₂O-Bi₂MoO₆表面有明显的小块颗粒存在, 分布集中, 且其XRD图出现Ag₂O的衍射峰。与未掺杂样品相比, 掺杂Ag₂O后Bi₂MoO₆的可见光催化活性提高, 当掺银量为1.5%时活性最高。实验最佳催化剂浓度为0.6 g·L^-1, 在溶液pH值减小、富里酸初始浓度减小时有助于富里酸的去除。富里酸降解过程符合一级反应动力学方程, 拟合方程为y=-0.019 5x。对富里酸降解产物进行发光菌生物毒性测试, 发现光催化2 h后降解产物比处理前毒性降低约90%。     

Crystalline Vanadium Pentoxide with Hierarchical Mesopores and Its Capacitive Behavior

Crystalline vanadium pentoxide with hierarchical mesopores was synthesized by using a CTAB/BMIC cotemplate (CTAB=cetyltrimethylammonium bromide, BMIC=1‐butyl‐3‐methylimidazolium chloride). The material was fully characterized by SEM, TEM, N₂ adsorption–desorption, XRD, XPS, and CV methods. By elaborate adjustment of the template proportions, the distribution and size of the hierarchical pores were tuned successfully. CTAB cationic surfactant contributed more to the larger mesopores, whereas BMIC ionic liquid was beneficial in forming the smaller nanopores. The vanadium‐containing anions combined with CTA⁺ micelles and BMI⁺ rings through electrostatic interactions. The CTA⁺–O(VO)O^?–BMI⁺ entities built up an orderly array, which finally formed the hierarchical mesoporous framework during thermal treatment. The mesoporous vanadium pentoxide directed by the cotemplate of CTAB/BMIC=1:1 showed many orderly crystalline structures and demonstrated a large capacitance (225 F g^?1); it is thus a promising material for electrochemical capacitors. Two alternative solutions to the disappearance of capacitance due to insertion of K⁺ are proposed in view of possible future applications.     

A Green Approach for the Synthesis of Silver Nanoparticles Using Root Extract of <Emphasis Type="Italic">Chelidonium majus:</Emphasis> Characterization and Antibacterial Evaluation

In this study, silver nanoparticles (Ag-NPs) have been synthesized using extract of Chelidonium majus root in aqueous solution at room temperature. The root extract was able to reduce Ag⁺ to Ag⁰ and stabilized the nanoparticles Different physico-chemical techniques including UV–Vis spectroscopy, transmission electron microscopy and powder X-ray diffraction (PXRD) were used for the characterization of the biosynthesized Ag-NPs obtained. The surface plasmon resonance band appeared at 431 nm is an evidence for formation of Ag-NPs. TEM imaging revealed that the synthesized Ag-NPs have an average diameter of around 15 nm and with spherical shape. Moreover the crystalline structure of synthesized nanoparticles was confirmed using XRD pattern. Furthermore antimicrobial activities of synthesized Ag-NPs were evaluated against Escherichia coli -ATCC 25922 and Pseudomonas aeruginosa ATCC 2785 bacteria strain.     

Synthesis of MCM-48 from silatrane via sol–gel process

High-quality cubic MCM-48 is successfully synthesized using a new silica source known as silatrane and cetyltrimethylammonium bromide (CTAB) as the structure-directing agent via sol–gel process. The effects of synthesis parameters, viz. crystallization temperature, crystallization time, surfactant concentration, quantity of NaOH, and silica source, on the product structure are investigated. The synthesized samples are characterized using X-ray diffractometer (XRD), N₂ adsorption–desorption isotherms, and electron microscopy. Optimally, this product is synthesized from samples crystallized at 140°C for 16 h with a CTAB/SiO₂ ratio of 0.3 and NaOH/SiO₂ ratio of 0.5. The XRD result exhibits a well-resolved pattern, corresponding to the Ia3d space group of MCM-48. The BET surface area of this product is as high as 1,300 m²/g with a narrow pore-size distribution of 2.86 nm. The scanning electron microscopic (SEM) images also show the truncated octahedral shape and well-ordered pore system of MCM-48 particles.     

CTAB-assisted synthesis of mesoporous F-N-codoped TiO2 powders with high visible-light-driven catalytic activity and adsorption capacity

This article describes the preparation of mesoporous rod-like F-N-codoped TiO₂ powder photocatalysts with anatase phase via a sol-gel route at the temperature of 373 K, using cetyltrimethyl ammonium bromide (CTAB) as surfactant. The as-prepared photocatalysts were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and UV-visible diffuse reflectance spectra (UV-vis DRS). The results showed that the photocatalysts possessed a homogeneous pore diameter and a high surface area of 106.3-160.7 m³ g⁻¹. The increasing CTAB reactive concentration extended the visible-light absorption up to 600 nm. The F-N-codoped TiO₂ powders exhibited significant higher adsorption capacity for methyl orange (MO) than that of Degussa P25 and showed more than 6 times higher visible-light-induced catalytic degradation for MO than that of P25.     

Synthesis and luminescence properties of Eu(III)-doped silica nanorods based on the sol–gel process

Uniform Eu³⁺-doped SiO₂ nanorods were synthesized through a simple sol–gel method using cetyltrimethylammonium bromide (CTAB) as surfactant template and tetraethylorthosilicate as silicon source. X-ray diffraction, energy-dispersive X-ray spectroscopy, Fourier transform infrared spectrum, scanning electron microscope (SEM), transmission electron microscopy, and photoluminescence spectra were employed to characterize the products in detail. The nanorods have good uniformity and their diameters and lengths are in the range of 200–300 and 500–700 nm through the SEM images, respectively. The formation of the nanorods was studied by taking SEM images after different aging time. The experimental results indicate that CTAB plays a crucial role in the formation of the silica nanorods. The luminescence of Eu³⁺-doped SiO₂ nanorods is dominated by red-emission around 612 nm due to intra-atomic 4f → 4f (⁵D₀ → ⁷F₂₎ transition of Eu³⁺ ions. Furthermore, the effect of doping concentrations of Eu³⁺ ions on the luminescence was investigated.     

Microwave-assisted synthesis of ZnO and its photocatalytic activity in degradation of CTAB

Nanosized zinc oxide (nano-ZnO) was prepared by a microwave irradiation method using zinc nitrate and triethanolamine as starting materials and distilled water as a solvent. The as-prepared powder was characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The photocatalytic degradation of cetyltrimethylammonium bromide (CTAB) using the prepared material under UV irradiation was studied.The effects of ZnO dosage and initial pH on the photodegradation of CTAB were investigated. As the ZnO load increased, the CTAB degradation first increased and then decreased. The optimum ZnO dosage was 3 g L^–1. Photodegradation of CTAB is more efficient in slightly alkaline media (pH 9).     

Bicontinuous nanodisc and nanospherical titania materials prepared by sol-gel process in reverse microemulsion

TiO₂ nanoparticles with different shapes and sizes were synthesised by the sol-gel route in Water/Brij78/Hexane reverse microemulsions. The aqueous cores of these microemulsions were used as nanoreactors to control sol-gel reactions. We studied the effect of water/surfactant mole ratio (W ₀) on the morphology, and textural properties of the final products. The materials thus obtained were characterised by different techniques. Thermogravimetric and differential thermal analysis (TG-DTA) was used to study the thermal behaviour of the products and X-ray diffraction (XRD) to identify the crystalline phases. The morphological and textural properties of the products were determined by scattering electron microscopy (SEM) and the Brunauer-Emmett-Teller (BET) method, respectively. We also studied the influence of thermal treatment on the structure and size of the TiO₂ particles. The effect of W ₀ on the anatase-rutile phase transition temperature was investigated.     

Ag2O-Bi2MoO6:制备及光催化降解富里酸

以钼酸铵、硝酸铋和硝酸银为原料,以十六烷基三甲基溴化铵(CTAB)为辅助活性剂,采用水热法合成了Ag₂O-Bi₂MoO₆光催化剂。用X射线粉末衍射、扫描电镜及紫外-可见吸收光谱等进行表征,并对水中天然有机物富里酸进行了光催化氧化研究。结果表明:未掺杂钼酸铋表面平滑,Ag₂O-Bi₂MoO₆表面有明显的小块颗粒存在,分布集中,且其XRD图出现Ag₂O的衍射峰。与未掺杂样品相比,掺杂Ag₂O后Bi₂MoO₆的可见光催化活性提高,当掺银量为1.5%时活性最高。实验最佳催化剂浓度为0.6g·L^-1,在溶液pH值减小、富里酸初始浓度减小时有助于富里酸的去除。富里酸降解过程符合一级反应动力学方程,拟合方程为y=-0.0195x。对富里酸降解产物进行发光菌生物毒性测试,发现光催化2h后降解产物比处理前毒性降低约90%。     

Influence of surfactants on the morphologies of CaCO3 by carbonation route with compressed CO2

Three surfactants, sodium dodecyl sulfate (SDS), cetyltrimethylammonium bromide (CTAB) and polyoxyethylene-80-sorbitan monooleate (Tween 80), were used to control the growth of CaCO₃ crystals by carbonation route using Ca(OH)₂ and compressed CO₂. The obtained CaCO₃ particles were characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) techniques. The effects of surfactants on the morphology of the particles were studied. It was demonstrated that Tween 80 and SDS have obvious effect on the morphology of CaCO₃ particles, while CTAB does not affect morphology considerably. The possible mechanism has been discussed on the basis of the binding of the surfactants to the certain face of the crystals.     

Selective synthesis of copper microsheets and ultralong microwires via a surfactant assisted hydrothermal process

The surfactant assisted hydrothermal process for selective preparation of copper nanosheets and ultralong microwires by reducing Cu²⁺ with 2-(bis-phosphonomethylamino)propionic acid (dpc) under the action of cetyltrimethylammonium bromide (CTAB) or polyvinyl pyrrolidine (PVP) is presented. X-ray powder diffraction (XRD) and energy dispersive X-ray analysis (EDX) indicate that the products are pure Cu of cubic phase. The effects of starting material concentration and reaction time on morphology of nanosheets have been studied by scanning electron microscopy (SEM). The presence of CTAB and PVP as capping agents is identified by EDX, transmission electron microscopy (TEM) and FT-IR. The possible growth process for ultralong microwires was studied by stopping the growth at a series of intermediate morphology stages based on SEM observations. Optical properties of Cu nanosheets and ultralong microwires were studied by UV-Vis spectrophotometry.     

Size-controlled synthesis of CuO–ZrO<Subscript>2</Subscript> nanoparticles prepared through reverse micelle method

In this research, CuO–ZrO₂ nanoparticles are synthesized using microreactors made of surfactant/water/cyclohexane microemulsions. The effect of different microemulsion variables on the particle size and its distribution, such as water-to-surfactant molar ratio (W ₀) and different surfactants are discussed. Three different surfactant types including cationic (CTAB), anionic (AOT), and nonionic (Brij56) are used. Also a different amount of water to surfactant in nano composite synthesis is used. The powders were characterized by DTA/TG, XRD, SEM, EDS, TEM and BET techniques and their physical properties are compared. The results show a decrease of particles size in presence of cationic surfactant. Narrow particles size distribution of the resultant CuO–ZrO₂ nanocomposite in presence of cationic surfactant, anionic and nonionic surfactant is compared. Also for AOT surfactant, by raising water to surfactant molar ratio the particles size is increased and the optimum ratio is H₂O: Surfactant = 0.32:0.055, respectively.     

Kinetics and mechanism of the redox reaction between malachite green and iron(III) in aqueous and micellar media

The kinetics of the oxidation of malachite green (MG⁺) by Fe(III) were investigated spectrophotometrically by monitoring the absorbance change at 618 nm in aqueous and micellar media at a temperature range 20–40 °C; I = 0.10 mol dm^?3 for [H⁺] range (2.50–15.00) × 10^?4 mol dm^?3. The rate of reaction increases with increasing [H⁺]. The reaction was carried out under pseudo-first-order conditions by taking the [Fe(III)] (>10-fold) the [MG⁺]. A mechanism of the reaction between malachite green and Fe(III) is proposed, and the rate equation derived from the mechanism was consistent with the experimental rate law as follows: Rate = (k ₄ + K ₁ k ₅[H⁺]) [MG⁺][Fe(III)]. The effect of surfactants, such as cetyltrimethylammonium bromide (CTAB, a cationic surfactant) and sodium dodecylsulfate (SDS, an anionic surfactant), on the reaction rate has been studied. CTAB has no effect on the rate of reaction while SDS inhibits it. Also, the effect of ligands on the reaction rate has been investigated. It is proposed that electron transfer proceeds through an outer-sphere mechanism. The enthalpy and the entropy of the activation were calculated using the transition state theory equation.     

One‐step Hydrothermal Synthesis and Assembly of Copper and Silver Nanoparticles to Aggregates in Glyoxal Reduction System

A simple hydrothermal process has been developed for the synthesis and assembly of copper and silver nanoparticles to aggregates. The reduction of Cu²⁺ and Ag⁺ ions to the zerovalent metal was performed by glyoxal in the absence of any external agent. The produced glyoxylic acid (GA) in the redox process stabi‐ lized metallic copper and silver particles and rendered them oxidation resistant for several months and dispersible in polar organic solvents and water. Detailed nanostructures of synthesized products were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and X‐ray diffraction (XRD). The results demonstrated that assembly of nanoparticles to aggregates and their regularity were dependent on the reaction conditions such as temperature and concentration of the starting material. The Ostwald ripening process was proposed to explain the formation of copper nanoparticles by TEM observation at several times during the reaction. The existence of the surface stabilizing agent was identified by Fourier Transform infrared spectroscopy (FT‐IR) and thermogravimetric analyses (TGA).