In situ synthesis of Pt nanoparticles in hyperbranched thin film for electrocatalytic reduction of dioxygen

Hyperbranched thin film (HTF) with amino and imino groups, which can accommodate PtCl₆²⁻, was synthesized with small organic molecules on gold substrate based on SN₂ displacement reaction. Platinum nanoparticles (Pt_NPs) were in situ synthesized by electrochemically reduction of precursors, PtCl₆²⁻, within HTF. The prepared films were characterized by X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS) and atomic force microscopy (AFM). It was confirmed that densely packed Pt_NPs were prepared with a narrow size distribution. EIS indicated that HTF inhibits electron transfer slightly while Pt nanoparticles in the HTF enhanced the electron-transfer ability greatly. Cyclic voltammetry (CV) indicated that HTF containing Pt_NPs exhibited a remarkable electrocatalytic activity for the electrochemical reduction of dioxygen. The quantity of Pt_NPs could be expediently controlled by the thickness of HTF. So the catalytic ability can be tailored correspondingly.     

Sulfur Nanoparticles Synthesis and Characterization from H2S Gas, Using Novel Biodegradable Iron Chelates in W/O Microemulsion

Sulfur nanoparticles were synthesized from hazardous H₂S gas using novel biodegradable iron chelates in w/o microemulsion system. Fe³⁺–malic acid chelate (0.05 M aqueous solution) was studied in w/o microemulsion containing cyclohexane, Triton X-100 and n-hexanol as oil phase, surfactant, co-surfactant, respectively, for catalytic oxidation of H₂S gas at ambient conditions of temperature, pressure, and neutral pH. The structural features of sulfur nanoparticles have been characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), energy dispersive spectroscopy (EDS), diffused reflectance infra-red Fourier transform technique, and BET surface area measurements. XRD analysis indicates the presence of α-sulfur. TEM analysis shows that the morphology of sulfur nanoparticles synthesized in w/o microemulsion system is nearly uniform in size (average particle size 10 nm) and narrow particle size distribution (in range of 5–15 nm) as compared to that in aqueous surfactant systems. The EDS analysis indicated high purity of sulfur (>99%). Moreover, sulfur nanoparticles synthesized in w/o microemulsion system exhibit higher antimicrobial activity (against bacteria, yeast, and fungi) than that of colloidal sulfur.     

Pulsed electrodeposition of Zn in the presence of surfactants

The preparation of Zn deposits has been performed by galvanostatic pulsed electrolysis, from acidic zinc sulphate solutions, on a stainless steel substrate. The influence of the surfactants (cetyl trimethyl ammonium bromide (CTAB), sodium dodecyl sulphate (SDS) and octylphenolpoly(ethyleneglycolether)_n, n = 10, Triton X-100) on the voltammetric behaviour, structural and morphological characteristics of the deposits have been investigated. The characterization of the samples was made by X-ray diffraction (XRD) and scanning electron microscopy coupled with energy dispersive X-ray spectroscopy (SEM/EDS). The experimental data shows that the presence of surfactants affects the zinc deposition process. The electrodeposits are mainly composed by Zn with different texture, crystal shape and size (grain size ranging from 40 to 20 nm). The obtained results led us to conclude that the Zn deposits prepared in the absence of surfactants and in the presence of SDS are more crystalline and with a higher grain size than the ones obtained in the presence of CTAB and Triton X-100. These facts may be justified by the increase on the overpotential deposition as the electrochemical studies confirm.The XRD results show that the deposits prepared, in the absence of surfactant and in the presence of SDS, contain ZnSO₄ and Zn₄SO₄(OH)₆ as oxidation products. ZnO is also detected on the deposits obtained in the presence of CTAB and Triton X-100.     

Ionic liquid assisted one step green synthesis of Au–Ag bimetallic nanoparticles

Au–Ag bimetallic nanoparticles have been fabricated by one-step simple electrochemical deposition method using ionic liquid as green electrolyte (1-butyl-3-methylimidazolium tetrafluoro borate). Fabricated Au–Ag bimetallic nanoparticles have been characterized using cyclic voltammetry (CV), FE-SEM, UV–vis spectroscopy, and X-ray diffraction (XRD) studies. The electrodeposited Au–Ag bimetallic nanoparticles were found in the size range of 16–30 nm, respectively. This type of Au–Ag bimetallic nanoparticles could be directly applied for the optoelectronic and biosensing applications.     

Cysteine-Encapsulated Liposome for Investigating Biomolecular Interactions at Lipid Membranes

The development of a strategy to investigate interfacial phenomena at lipid membranes is practically useful because most essential biomolecular interactions occur at cell membranes. In this study, a colorimetric method based on cysteine-encapsulated liposomes was examined using gold nanoparticles as a probe to provide a platform to report an enzymatic activity at lipid membranes. The cysteine-encapsulated liposomes were prepared with varying ratios of 1,2-dimyristoyl-sn-glycero-3-phosphocholine (DMPC) and cholesterol through the hydration of lipid films and extrusions in the presence of cysteine. The size, composition, and stability of resulting liposomes were analyzed by scanning electron microscopy (SEM), dynamic light scattering (DLS), nuclear magnetic resonance (NMR) spectroscopy, and UV-vis spectrophotometry. The results showed that the increased cholesterol content improved the stability of liposomes, and the liposomes were formulated with 60 mol % cholesterol for the subsequent experiments. Triton X-100 was tested to disrupt the lipid membranes to release the encapsulated cysteine from the liposomes. Cysteine can induce the aggregation of gold nanoparticles accompanying a color change, and the colorimetric response of gold nanoparticles to the released cysteine was investigated in various media. Except in buffer solutions at around pH 5, the cysteine-encapsulated liposomes showed the color change of gold nanoparticles only after being incubated with Triton X-100. Finally, the cysteine-encapsulated liposomal platform was tested to report the enzymatic activity of phospholipase A₂ that hydrolyzes phospholipids in the membrane. The hydrolysis of phospholipids triggered the release of cysteine from the liposomes, and the released cysteine was successfully detected by monitoring the distinct red-to-blue color change of gold nanoparticles. The presence of phospholipase A₂ was also confirmed by the appearance of a peak around 690 nm in the UV-vis spectra, which is caused by the cysteine-induced aggregation of gold nanoparticles. The results demonstrated that the cysteine-encapsulated liposome has the potential to be used to investigate biological interactions occurring at lipid membranes.     

CO2 Hydrogenation Studies on Co and CoPt Bimetallic Nanoparticles Under Reaction Conditions Using TEM, XPS and NEXAFS

Cobalt and platinum?Ccobalt bimetallic alloy nanoparticles of uniform size distribution where prepared and supported on MCF-17 to produce a controlled and well-characterized model catalyst which was studied under reaction conditions during CO₂ hydrogenation. Near edge X-ray absorption fine structure (NEXAFS) spectroscopy was used to elucidate the oxidation state of the catalyst under reaction conditions while the effect of reducing H₂ gas on the composition and structure of the bimetallic PtCo nanoparticles was measured using ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and environmental transmission electron microscopy (ETEM). NEXAFS indicates that Pt aids the reduction of Co to its metallic state under relevant reaction conditions, while AP-XPS and ETEM indicate that Pt is enriched at the surface by exchange with subsurface layers which become Pt deficient??in agreement with the ??Pt-like?? selectivity seen during catalytic testing of these materials.     

Effect of Triton X-100 in water-added electrolytes on the performance of dye-sensitized solar cells

The performance of a Ru(II) dye-sensitized nanocrystalline TiO₂ solar cell (DSSC) with both Triton X-100 and water as additives in 3-methoxypropionitrile solutions is described. In the presence of these additives, the open-circuit voltage (V_oc), fill factor and stability of the cell increased, while the short-circuit photocurrent density decreased compared to those found in their absence. Based on these changes, the DSSC yielded a higher solar-to-electricity conversion efficiency of 5.9%, compared to 5.3% for the cells fabricated without the additives. Furthermore, the addition of Triton X-100 to the water-added electrolyte was found to render the Ag metal corrosion resistant.     

Reductant-free synthesis of magnetoplasmonic iron oxide-gold nanoparticles

Stable suspensions of spherical 10–15 nm superparamagnetic iron oxide nanoparticles (SPIONs) have been synthetized by co-precipitation, stabilized with citric acid, surface functionalized with aminopropyltriethoxysilane (APTES) and finally decorated with ultra-small gold nanoparticles (GNPs) by in situ reduction of a soluble gold salt (HAuCl₄), obtaining well dispersed SPIONs-GNPs colloids.The morphology, size and stability of the SPIONs-GNPs suspensions have been controlled by adjusting the molar ratio of the reagents (Fe/HAuCl₄ and Fe/APTES). The synthesis route differs from that typically found in literature, using tunable chelating layer modifications (such as citric acid and –NH₂ groups) of the magnetic core, depositing GNPs on the amine-functionalized iron oxide surface without the use of a specific reducing agent, and tuning the process pH and temperature. An explanation of how the different chemical species involved in the synthesis route could be responsible for the reducing action has been provided. The SPIONs-GNPs colloids have been characterized after each synthesis step by Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM), energy-dispersive X-ray spectroscopy (EDXS), Fourier transform infrared spectroscopy (FTIR), ζ Potential measurements, magnetic measurements with a vibrating-sample magnetometer (VSM) and UV–VIS spectroscopy. The SPIONs-GNPs colloids showed magnetoplasmonic behaviors since they maintained the plasmonic properties of GNPs and the superparamagnetic response of iron oxide NPs.     

Synthesis of nanoscale hydroxyapatite particles using triton X-100 as an organic modifier

Nano-sized rod like hydroxyapatite (HA) particles were synthesized using Ca(NO₃)₂·4H₂O and (NH₄)₂HPO₄ as precursors with varying contents of non-ionic surfactant viz., p-(1,1,3,3-tetramethylbutyl)phenoxypoly(oxyethylene)glycol (triton X-100) as organic modifer. The crystalline phase, chemical composition, surface area and morphology of the prepared samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET surface area analysis, high resolution scanning electron microscopy (HRSEM) and transmission electron microscopy (TEM). The above studies indicate the presence of nanoscale hydroxyapatite (HA) phase. Triton X-100 does not appear to affect the crystallinity of the samples. Increase of BET surface area and the consequent decrease in particle size of HA were observed as a function of surfactant content. Probable mechanism for the role of the surfactant in the synthesis of nanoscale HA has also been discussed.     

双微乳液法制备纳米硫酸钡颗粒

在水溶液/TritonX-100/正己醇/环己烷组成的反相微乳液中,以氯化钡和硫酸钠为原料,通过沉淀反应,制备出类球形BaSO₄纳米颗粒,并通过XRD、SEM、TEM、FTIR对其进行表征。考察了三种反应方式、水/TritonX-100摩尔比（R）、反应物浓度以及助表面活性剂/表面活性剂摩尔比（P）对纳米BaSO₄颗粒大小和形貌的影响。同时考察了R对微乳液液滴大小和粒径分布的影响,并通过动态光散射技术（DLS）对微乳液液滴进行测定。实验结果表明：室温条件下,采用双微乳液法,R=17.97,P在2.11～4.22之间是纳米BaSO₄颗粒合成的最佳反应条件,反应物浓度对BaSO₄颗粒的大小和形貌几乎没有影响。在该反应条件下,合成出的类球形BaSO₄粒径为18～22 nm,产率可达87.5%。     

Facile Synthesis of Calcium Borate Nanoparticles and the Annealing Effect on Their Structure and Size

Calcium borate nanoparticles have been synthesized by a thermal treatment method via facile co-precipitation. Differences of annealing temperature and annealing time and their effects on crystal structure, particle size, size distribution and thermal stability of nanoparticles were investigated. The formation of calcium borate compound was characterized by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and Thermogravimetry (TGA). The XRD patterns revealed that the co-precipitated samples annealed at 700 °C for 3 h annealing time formed an amorphous structure and the transformation into a crystalline structure only occurred after 5 h annealing time. It was found that the samples annealed at 900 °C are mostly metaborate (CaB₂O₄) nanoparticles and tetraborate (CaB₄O₇) nanoparticles only observed at 970 °C, which was confirmed by FTIR. The TEM images indicated that with increasing the annealing time and temperature, the average particle size increases. TGA analysis confirmed the thermal stability of the annealed samples at higher temperatures.     

Self-assembled gold nanoparticles modified ITO electrodes: The monolayer binder molecule effect

The fabrication of gold attached organosilane-coated indium tin oxide Au_NPs-MPTMS/ITO and Au_NPs-APTES/ITO electrodes [MPTMS = 3-(mercaptopropyl)-trimethoxysilane, APTES = 3-(aminopropyl)-triethoxysilane, ITO = indium tin oxide] was carried out making use of a well-known two-step procedure and the role played by the -SH and -NH₂ functional groups in the two electrodes has been examined and compared using different techniques. Information about particle coverage and inter-particle spacing has been obtained using trasmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM) whereas, bulk surface properties have been probed with UV-vis spectroscopy, CV and electrochemical impedance spectroscopy (EIS). The catalytic activity of the two electrodes has been evaluated studying the electrooxidation of methanol in alkaline conditions. The results obtained show that the NH₂ functionality in the APTES binder molecule favours the formation of isle-like Au nanoparticle aggregates that lead to both a higher electron transfer and electrocatalytic activity.     

Effects of surfactants on the preparation of TiO<Subscript>2</Subscript> nanoparticles in microwave-assisted sol-gel process and their photocatalytic activity

Nanosized TiO₂ particles were prepared through facile sol-gel reaction by using microwave-assisted method. To investigate the effects of surfactants on the formation of TiO₂, various additives (PVP, Triton X-100 and P123) were employed. The diameter of synthesized titania spheres could be controlled from 105 to 380 nm. The TiO₂ particles prepared with P123 triblock copolymer showed large surface area and high pore volume. It was attributed to the fact that the pore site, where the surfactant template initially existed, was generated upon calcination process. The characteristics of prepared TiO₂ nanoparticles were analyzed by using FE-SEM, TEM, XRD, FT-IR and N₂ adsorption-desorption. As an application of prepared composites for water treatment, their photocatalytic performances for the degradation of methylene blue dye were examined by using UV-vis spectrophotometer under room light irradiation. The prepared TiO₂ particles with Triton X-100 and P123 exhibited higher performance for methylene blue photo-degradation than that of P25. It was attributed to the effects of large specific surface area and high porosity.     

Effects of annealing on the structural and magnetic properties of flame spray pyrolyzed MnFe2O4 nanoparticles

In this study, manganese ferrite (MnFe₂O₄) nanoparticles were produced through flame spray pyrolysis (FSP). To investigate the effects of heat treatment, the nanoparticles were annealed between 400 and 650°C for 4 h in air in a comparative manner. The structural, chemical, morphological, and magnetic properties of the nanoparticles were evaluated using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), dynamic light scattering (DLS), and vibrating sample magnetometry (VSM), respectively. The XRD results showed that the nanoparticles synthesized by the FSP method exhibited the MnFe₂O₄ spinel ferrite structure. The annealing process led to the decomposition of MnFe₂O₄ into various phases. According to the morphological analysis, the as-synthesized particles were hemispherical–cubic in shape and had an average particle size of less than 100 nm. In addition, the chemical bond structures of the nanoparticles were confirmed in detail by XPS elemental analysis. The highest saturation magnetization was recorded as 33.50 emu/g for the as-produced nanoparticles. The saturation magnetization of the nanoparticles decreased with increasing annealing temperature, while coercivity increased.     

Hollow mesoporous silica spheres supported Ag and Ag–Au catalyzed reduction of 4-nitrobenzo-15-crown

Hollow mesoporous silica (HMS) spheres of size within the range 120–220 nm have been prepared using propanol–water solvent as template and cetyltrimethylammonium bromide (CTAB) as stabilizer. HMS supported silver and silver–gold catalysts were prepared by impregnating metal nanoparticles on HMS and were characterized by ultraviolet–visible spectroscopy (UV–vis), dynamic light scattering (DLS), optical microscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), inductive coupled plasma optical emission spectroscopy (ICP-OES) and N₂ adsorption–desorption. The reduction of 4-nitrobenzo-15-crown (4-NB-15-C) was compared using HMS supported silver and silver–gold nanocatalysts varying experimental parameters. Bimetallic Ag–Au/HMS nanocatalysts was found to be more active than monometallic Ag/HMS nanocatalyst.     

Templated Synthesis of Gold Nanorods (NRs): The Effects of Cosurfactants and Electrolytes on the Shape and Optical Properties

Seeded growth of gold nanorods (NRs) has been accomplished in a micellar medium containing mixed surfactants or a high salt concentration. Cetyl trimethylamoniumbromide (CTAB) forms micelles upon which the growth of rod shaped gold nanoparticles occurs. AgNO₃ is introduced into the growth solution to enhance the formation of NRs. The roles of non-ionic surfactants such as Tween and Triton, and of electrolytes such as sodium chloride and potassium chloride have been examined. As the concentration of these additives in the growth solution is increased, the aspect ratio of the NRs increases to a critical limit, after which it decreases again. Upon carefully controlling the content of Triton X-100 or Tween 20 in the growth solution, these non-ionic surfactants assisted in fine-tuning the shape of gold NRs (e.g. rectangular or “dogbone”). The growth pattern of the NRs fits into the model of a soft template formed by the mixture of CTAB and non-ionic surfactants.     

Flame-made Alumina Supported Pd–Pt Nanoparticles: Structural Properties and Catalytic Behavior in Methane Combustion

Bimetallic palladium–platinum nanoparticles supported on alumina were prepared by flame spray pyrolysis. The as-prepared materials were characterized by scanning transmission electron microscopy (STEM), CO chemisorption, nitrogen adsorption (BET), X-ray diffraction (XRD), temperature programmed reduction (TPR), thermogravimetric analysis (TGA) and extended X-ray absorption fine structure (EXAFS) spectroscopy. The materials were tested for the catalytic combustion of methane with a focus on the thermal stability of the noble metal particles. After flame synthesis the noble metal components of the materials were predominantly in oxidized state and finely dispersed on the alumina matrix. Reduction afforded small bimetallic Pd–Pt alloy particles (< 5 nm) supported on Al₂O₃ ceramic nanoparticles. The addition of small amounts of platinum made the palladium particles more resistant against sintering at high temperatures and further lowered the deactivation observed during methane combustion.     

Apparent electrocatalysis on 3D nanoporous platinum film electroplated from hexagonal lyotropic liquid crystalline phase of Triton X-100

Electrocatalytic effect of nanoporous interface between platinum (Pt) and electrolyte was investigated in terms of direct electrochemical oxidation of glucose. A Pt film with 3D nanopores was electroplated from the hexagonal (H₁) lyotropic liquid crystal (LLC) phase of t-octylphenoxypolyethoxyethanol (Triton X-100), a nonionic surfactant with a phenyl group in a hydrophobic tail. This Pt film, which was electroplated from H₁-LLC of Triton X-100 (ePt-H₁-TX100), comprised closely stacked crystalline (face centered cubic) nanoparticles (diameter, 4-7 nm) with 3D nanopores (width, 1-2 nm) developed among the particles. The ePt-H₁-TX100 showed high surface roughness and selective enhancement of a sluggish redox reaction, that is, kinetic-controlled reaction such as glucose oxidation. Nonenzymatic glucose sensing can be achieved by using discriminatively enhanced sensitivity to glucose over redox active interfering molecules.     

Biomimetic Synthesis of Gelatin Polypeptide-Assisted Noble-Metal Nanoparticles and Their Interaction Study

Herein, the generation of gold, silver, and silver–gold (Ag–Au) bimetallic nanoparticles was carried out in collagen (gelatin) solution. It first showed that the major ingredient in gelatin polypeptide, glutamic acid, acted as reducing agent to biomimetically synthesize noble metal nanoparticles at 80°C. The size of nanoparticles can be controlled not only by the mass ratio of gelatin to gold ion but also by pH of gelatin solution. Interaction between noble-metal nanoparticles and polypeptide has been investigated by TEM, UV–visible, fluorescence spectroscopy, and HNMR. This study testified that the degradation of gelatin protein could not alter the morphology of nanoparticles, but it made nanoparticles aggregated clusters array (opposing three-dimensional α-helix folding structure) into isolated nanoparticles stabilized by gelatin residues. This is a promising merit of gelatin to apply in the synthesis of nanoparticles. Therefore, gelatin protein is an excellent template for biomimetic synthesis of noble metal/bimetallic nanoparticle growth to form nanometer-sized device.     

Triton X-100 directed synthesis of mesoporous γ-Al2O3 from coal-series kaolin

Mesoporous γ-Al₂O₃ has been successfully synthesized by using calcined coal-series kaolin as raw material and Triton X-100 (TX-100) as template. The effect of TX-100/Al^3 + ratio on the structural and textural properties of mesoporous γ-Al₂O₃ was investigated. Physical properties of obtained samples were characterized by X-ray diffraction (XRD), N₂ adsorption–desorption, transmission electron microscopy (TEM), thermogravimetric analysis (TG), scanning electron microscopy (SEM) with energy-dispersive X-ray analysis (EDAX) and Fourier transform infrared spectroscopy (FTIR). The results indicated that the amount of TX-100 influenced the structure and porous properties of mesoporous γ-Al₂O₃ significantly. When TX-100/Al^3 + ratio was in the range of 0.03–0.15, all samples had mesoporous structures with BET surface area of 193.0–261.0 m²/g and pore size of 5.04–6.71 nm. In addition, the reaction mechanism involved in the process was proposed and discussed.