Synthesis of Pt/PEI-MWCNT composite materials on polyethyleneimine-functionalized MWNTs as supports

Composite materials with highly dispersed platinum (Pt) nanoparticles on multiwalled carbon nanotubes (MWCNTs), functionalized with polyethyleneimine (PEI) by a noncovalent method were prepared. The PEI-functionalization provided high density homogeneous functional groups on the MWCNTs’ sidewalls for binding Pt nanoparticles. Cationic PEI leads to homogeneous dispersion in solutions such as water and organic solvents. The effects of a reducing agent on the Pt nanoparticles that form on the surfaces of the MWCNT were studied by varying the molar ratio of NaOH to H₂PtCl₆. These composite materials were characterized with transmission electron micrograph (TEM), X-ray diffractometer (XRD) and X-ray photoelectron spectroscopy (XPS). The Pt/PEI-MWCNT catalyst exhibits excellent electrocatalytic activity and compared with Pt/PVP-MWCNT catalysts obtained with polyvinylpyrrolidone (PVP). Finally, the cyclic voltammogram of methanol electrooxidation for Pt/PEI-MWCNT shows better tolerance to CO and methanol oxidation to CO₂ than of Pt/PVP-MWCNT.     

Size-controlled synthesis of ZrO2-TiO2 nanoparticles prepared via reverse micelle method: Investigation of particle size effect on the catalytic performance in vapor phase Beckmann rearrangement

Zirconium-titanium mixed oxide nanoparticles have been synthesized using microreactors made of bis-(2-ethylhexyl) sulfosuccinate (AOT)/water/n-hexane microemulsions. The control of particle size was achieved by varying the process variables, such as water-to-surfactant molar ratio and reagent concentration. Their sizes, appearances, crystal structures, pore diameter and surface area were characterized by TEM, XRD, N₂ adsorption/desorption methods. The results revealed that samples prepared in reverse micelles had no crystalline phase. The Beckmann rearrangement of cyclohexanone oxime on ZrO₂-TiO₂ nanoparticles was carried out in a fixed-bed down flow reactor to investigate the effect of particle size on catalytic activity and selectivity. Samples synthesized in reverse micelles had better reaction performance than samples prepared via sol-gel method. A parallel relationship could be drawn between the catalytic activity and the particle size as well as the selectivity of the catalyst.     

Rapid synthesis, characterization and optical properties of TiO2 coated ZnO nanocomposite particles by a novel microwave irradiation method

A novel and rapid microwave method was used to prepare TiO₂ coated ZnO nanocomposite particles. The resulted particles were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HR-TEM) and X-ray photoelectron spectroscopy (XPS). Results show that ZnO nanoparticles were coated with 6-10 nm amorphous TiO₂ layers. In addition, zeta potential analysis demonstrated the presence of TiO₂ layer on the surface of ZnO nanoparticles. Photoluminescence (PL) spectroscopy and UV-visible spectroscopy were used to investigate the optical properties of the nanoparticles. Compared to uncoated ZnO nanoparticles, the TiO₂ coated ZnO nanoparticles showed enhanced UV emission. The UV-visible diffuse reflectance study revealed the significant UV shielding characteristics of the nanocomposite particles. Moreover, amorphous TiO₂ coating effectively reduced the photocatalytic activity of ZnO nanoparticles as evidenced by the photodegradation of Orange G with uncoated and TiO₂ coated ZnO nanoparticles under UV radiation.     

Synthesis of Se nanoparticles by using TSA ion and its photocatalytic application for decolorization of cango red under UV irradiation

In this study, we describe a size-controlled synthesis of selenium nanoparticles based on the reduction of selenious acid (H₂SeO₃) by UV-irradiated tungstosilicate acid (H₄SiW₁₂O₄₀, TSA) solution which serves both as reducing reagent and stabilizer. The nanoparticles are characterized by ultraviolet-visible spectroscopy (UV-vis), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction analysis (XRD), X-ray photoelectron spectroscopy (XPS), the Raman spectra, transmission electron microscopy (TEM) and Zetasizer, respectively. The characteristic catalytic behavior of the Se nanoparticles is established by studying the decolorization of cango red in the presence of UV light. It is obvious that selenium catalyzes the reaction efficiently. The results show that the rate of dye decolorization varies linearly with the nanoparticle concentration and the rate of dye decolorization decreases with the size of the Se nanoparticles increasing.     

Molecular design of nanometric zinc borate-containing polyimide as a route to flame retardant materials

Zinc borate (Zn₂B₆O₁₁·3H₂O) nanoparticles were successfully prepared by using an emulsion liquid membrane (W/O/W emulsion) to control the size of particles with Na₂B₄O₇·10H₂O, boric acid and ZnSO₄·7H₂O as raw materials. All materials were dispersed with the polyimide (PI) precursor, poly (amic acid). Using a combination of dissolving the poly (amic acid) and mixing fatty acid surfactant-coated zinc borate nanoparticles; we have demonstrated the formation of nanocomposites with uniform nanoparticles dispersion. We report the first deposition of nanocomposite polyimides from solution using spin-coating. The microstructures and morphology of the as-obtained samples were studied by X-ray diffraction (XRD), infrared spectra (IR), scanning electron microscopy (SEM) equipped with an energy-dispersive X-ray spectrometer (EDX), transmission electron microscopy (TEM) and thermogravimetric analysis (TGA).     

The synthesis and characterization of nanocrystalline Cu- and Ag-based multinary sulfide semiconductors

The novel polygonal flake like Ag₈SnS₆ crystal, Cu₂FeSnS₄ flaky, and well-dispersed Cu₂CoSnS₄ nanoparticles were successfully prepared via a convenient hydrothermal reaction route at relatively low temperature, which was avoiding the use of high temperature treatments or toxic organic solvents. The products were characterized by means of X-ray powder diffraction (XRD), transmission electronic microscopy (TEM), X-ray photoelectronic spectra (XPS) and inductively coupled plasma-atomic emission spectroscopy (ICP-AES). It was found that the reaction temperature played a key role for the formation of the target products.     

IF-WS2 nanoparticles size design and synthesis via chemical reduction

An innovative synthesis of inorganic fullerene-like disulfide tungsten (IF-WS₂) nanoparticles was developed using a chemical reduction reaction in a horizontal quartz reactor. In this process, first tungsten trisulfide (WS₃) was formed via a chemical reaction of tetra thiotungstate ammonium ((NH₄)₂WS₄), polyethylene glycol (PEG), and hydrochloric acid (HCl) at ambient temperature and pressure. Subsequently, WS₃ was reacted with hydrogen (H₂) at high temperature (1173-1373 K) in a quartz tube. The produced WS₂ nanoparticles were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray (EDAX), and transmission electron microscopy (TEM). The characterization results indicated that the high-purity (100%) IF-WS₂ nanoparticles were produced. Moreover, addition of surfactant (PEG) and higher operating temperature (1173-1373 K) decreased the particles agglomeration, and consequently led to the reduction of average diameter of WS₂ particles in the range of 50-78 nm. The developed method is simple, environmentally compatible, and cost-effective in contrast to the conventional techniques.     

A novel route to the synthesis of nanosized metallic molybdenum at moderate temperature and its catalytic properties

Nanosized metallic molybdenum could be synthesized from MoO₃ and KBH₄ by solid-state reaction at moderate temperature. The crystallinity, morphology, surface properties of as-synthesized metallic molybdenum were investigated by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectral (XPS). The results of its catalytic activity test show that the as-synthesized nanosized metallic molybdenum is superior to the noble metal catalyst 0.3% Pd/Al₂O₃ for the selective hydrogenation of alkadienes at higher temperature and pressure.     

Synthesis of Ag modified vanadium oxide nanotubes and their antibacterial properties

Vanadium oxide nanotubes (VO_x-NTs) modified by highly dispersed Ag nanoparticles have been synthesized via a facile silver-mirror reaction. The crucial factors that affected the preparation of the Ag modified vanadium oxide nanotubes (Ag/VO_x-NTs) have been also studied. The dispersion and structure of Ag nanoparticles in the obtained materials were characterized by transmission electron microscopy (TEM), electron diffraction (ED) and X-ray diffraction (XRD). The results showed the distribution and size of the formed Ag particles were greatly influenced by the concentration of AgNO₃ solution. Typically, Ag nanoparticles were well dispersed on the VO_x-NTs with the size range from 3 to 10 nm. The corresponding antibacterial tests demonstrated the as-synthesized Ag/VO_x-NTs exhibited strong antibacterial activity against Escherichia coli (E. coli).     

Synthesis and characterization of supported heteropolymolybdate nanoparticles between silicate layers of Bentonite with enhanced catalytic activity for epoxidation of alkenes

A new heterogeneous catalyst (PVMo/Bentonite) consisting of vanadium substituted heteropolymolybdate with Keggin-type structure Na₅[PV₂Mo₁₀O₄₀]·14H₂O (PVMo) supported between silicate layers of bentonite has been synthesized by impregnation method and characterized using X-ray diffraction, Fourier-transformed infrared spectroscopy, scanning electron microscopy, UV–vis diffuse reflectance spectroscopy, transmission electron microscopy and elemental analysis. X-ray diffraction and scanning electron microscopy analysis indicated that PVMo was finely dispersed into layers of bentonite as support. The PVMo/Bentonite used as an efficient heterogeneous catalyst for epoxidation of alkenes. Various cyclic and linear alkenes were oxidized into the corresponding epoxides in high yields and selectivity with 30% aqueous H₂O₂. The catalyst was reused several times, without observable loss of activity and selectivity. The obtained results showed that the catalytic activity of the PVMo/Bentonite was higher than that of pure heteropolyanion (PVMo).     

Preparation of nanostructured NiFe2O4 catalysts by combustion reaction

Nanosize nickel ferrite powders (NiFe₂O₄) have been prepared by combustion reaction using nitrates and urea as fuel. The resulting powders were characterized by X-ray diffraction (XRD), nitrogen physical adsorption (BET), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and catalytic activity. The results showed nanosize nickel ferrite powders with high specific surface area (55.21 m²/g). The powders showed extensive XRD line broadening and the crystallite size calculated from the XRD line broadening was 18.0 nm. The nickel ferrite powder presented significant activity as catalyst for the water gas shift reaction, over the temperature range of 250–450 °C.     

Synthesis of acid-base bifunctional mesoporous materials by oxidation and thermolysis

A novel and efficient method has been developed for the synthesis of acid-base bifunctional catalyst SO₃H-MCM-41-NH₂. This method was achieved by co-condensation of tetraethylorthosilicate (TEOS), 3-mercaptopropyltrimethoxysilane (MPTMS) and (3-triethoxysilylpropyl) carbamicacid-1-methylcyclohexylester (3TAME) in the presence of cetyltrimethylammonium bromide (CTAB), followed by oxidation and then thermolysis to generate acidic site and basic site. X-ray diffraction (XRD) and transmission electron micrographs (TEM) show that the resultant materials keep mesoporous structure. Thermogravimetric analysis (TGA), X-ray photoelectron spectra (XPS), back titration, solid-state ¹³C CP/MAS NMR and solid-state ²⁹Si MAS NMR confirm that the organosiloxanes were condensed as a part of the silica framework. The bifunctional sample (SO₃H-MCM-41-NH₂) containing amine and sulfonic acids exhibits excellent acid-basic properties, which make it possess high activity in aldol condensation reaction between acetone and various aldehydes.     

Rapid fabrication and optical properties of zinc sulfide nanocrystallines in a heterogeneous system

ZnS nanoparticles about 3 nm in size were prepared by a simple, rapid and reliable route under microwave irradiation in a heterogeneous system, using ZnAc₂·2H₂O (AcCH₃COO) and Na₂S·9H₂O as the starting materials, ethylene glycol (EG) as the medium. The product was characterized with X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and ED, respectively. The optical properties of ZnS nanoparticles were studied.     

CeO2 nanocrystals: Seed-mediated synthesis and size control

This work reports on seed-mediated synthesis and size control of monodispersed CeO₂ nanoparticles. CeO₂ nanoparticles of mean size smaller than 2 nm were first prepared by a simple mixing of aqueous solution of cerium (IV) sulfate and ammonia solution at ambient conditions. Using these as-prepared fine particles as the tiny seeds, tunable sizes of CeO₂ nanoparticles were achieved via a facile hydrothermal treatment. All samples were characterized by X-ray diffraction (XRD), infrared (IR) spectroscopy, UV-vis spectroscopy, and thermogravimetric analysis (TGA). It is shown that in comparison with other inorganic cerium salts such as cerium (III) nitrates, cerium (IV) sulfate appears more suitable for forming CeO₂ nanoparticles at room temperature. Sulfate groups are strongly thermodynamically adsorbed on CeO₂ nanoparticle surfaces. The formation mechanism, surface hydration and sulfation characteristics of the resulting CeO₂ nanoparticles are also discussed.     

Synthesis and structure characterization of Ru nanoparticles stabilized by PVP or γ-Al2O3

Uniform and stable Ru nanoparticles were synthesized by reduction of RuCl₃ in ethylene glycol (EG) in the presence of poly(N-vinyl-2-pyrrolidone) by using microwave-assisted solvothermal method. The obtained materials were characterized by UV-vis, FT-IR, XPS, XRD and TEM techniques, and used as precursors of heterogeneous metal colloid catalysts. Characterization by TEM showed that as-prepared PVP-stabilized Ru nanoparticles have small average diameters (below 2 nm) and narrow size distributions (1-3 nm). Diffraction data confirmed that a crystallite size is around 2.0 nm. A colloidal Ru/γ-Al₂O₃ catalyst was obtained by two different methods: immobilization of the PVP-stabilized Ru colloid on the support or by in situ deposition of Ru colloid, e.g., reduction of RuCl₃ with EG in the presence of the γ-alumina. It was found that both synthesis methods produced the Ru/γ-Al₂O₃ catalysts with narrow size distributions of metallic nanoparticles, that are distributed uniformly over the support. However, only in situ preparation of the colloidal Ru/γ-Al₂O₃ catalyst results in chlorine free system with high activity for hydrogen chemisorption. The H₂ uptake on the Ru(PVP)/γ-Al₂O₃ catalyst was very low because the ruthenium surface was strongly occluded with a thin layer of polymer molecules.     

Highly dense and uniformly dispersed platinum nanoparticles on poly(acrylic acid) modified multi-walled carbon nanotubes for methanol oxidation

Poly(acrylic acid) modified multi-walled carbon nanotubes (PAA-MWNTs) were synthesized through in situ radical polymerization in acetone and the PAA-MWNTs were used as supporting material for platinum nanoparticles. Platinum nanoparticles were deposited on the surface of PAA-MWNTs with high loading and high dispersion through ethylene glycol reduction. The size of Pt nanoparticles on PAA-MWNTs can be tuned by the water content in the reaction system and the loading amount can be adjusted by the mass ratio of H₂PtCl₆ to PAA-MWNTs. The electrocatalytic properties of the Pt/PAA-MWNTs catalyst were evaluated by methanol oxidation. The results of cyclic voltammetry show that the Pt/PAA-MWNTs composite possesses high electrocatalytic activity, good long-term stability and storage property, which can be attributed to the small particle size and high dispersion of Pt nanoparticles as well as the nature of MWNTs.     

Sub-2 nm SnO2 nanocrystals: A reduction/oxidation chemical reaction synthesis and optical properties

A simple reduction/oxidation chemical solution approach at room temperature has been developed to synthesize ultrafine SnO₂ nanocrystals, in which NaBH₄ is used as a reducing agent instead of mineralizers such as sodium hydroxide, ammonia, and alcohol. The morphology, structure, and optical property of the ultrafine SnO₂ nanocrystals have been characterized by high-resolution transmission electron microscopy (HRTEM), X-ray powder diffraction (XRD), differential scanning calorimetry and thermogravimetric analysis (DSC-TGA), X-ray photoelectron spectroscopy (XPS) and UV-vis absorption spectroscopy. It is indicated that the uniform tetragonal ultrafine SnO₂ nanocrystals with the size below 2 nm have been fabricated at room temperature. The band gap of the ultrafine SnO₂ nanocrystals is about 4.1 eV, exhibiting 0.5 eV blue shift from that of the bulk SnO₂ (3.6 eV). Furthermore, the mechanism for the reduction/oxidation chemical reaction synthesis of the ultrafine SnO₂ nanocrystals has been preliminary presented.     

Synthesis and characterization of polyaniline nanorods/Ce(OH)3-Pr2O3/montmorillonite composites through reverse micelle template

Polyaniline (PANI) nanorods/Ce(OH)₃-Pr₂O₃/montmorillonite (MMT) nanocomposites were synthesized via in situ polymerization of aniline monomer through reverse micelle template (RMT) in the presence of montmorillonite and Ce(OH)₃, Pr₂O₃. In the experiment, sulphosalicylic acid was used as dopant, aniline was designated as oil phase and the aqueous solution comprising Ce³⁺ and Pr³⁺ as water phase. The nanocomposites were characterized by scanning electron microscope (SEM), X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy and thermogravimetry-differential thermal analysis (TG-DTA). The results showed that PANI nanorods were synthesized in the interlayer spaces of MMT with uniform spherical rare earth nanoparticles. The thermal stability of the nanocomposites prepared was enhanced drastically compared with pure polyaniline.     

Preparation of Pt-Ru-Ni ternary nanoparticles by microemulsion and electrocatalytic activity for methanol oxidation

Ternary platinum-ruthenium-nickel nanoparticles are prepared by water-in-oil reverse microemulsions of water/Triton X-100/propanol-2/cyclohexane. Nanoparticles formed in the microemulsions are characterized by transmission electron microscopy (TEM), electron diffraction (ED), X-ray diffractometry (XRD), energy dispersive X-ray analysis (EDX). These resulting materials showed a homogenous alloy structure, the mono-dispersion and an average diameter of 2.6 ± 0.3 nm with a narrow particle size distribution. The composition and particle size of ternary Pt-Ru-Ni nanoparticles can be controlled by adjusting the initial metal salt solution and preparation conditions. Pt-Ru-Ni ternary metallic nanoparticles showed an enhanced catalytic activity towards methanol oxidation compared to Pt-Ru bimetallic nanoparticles.     

Formation of NiFe2O4 nanoparticles by mechanochemical reaction

Preparation of nanosized NiFe₂O₄ particles by mechanochemical reaction(NiO+α-Fe₂O₃) and subsequent thermal treatment was investigated using X-ray diffraction (XRD). Thermal treatment of the as-milled powder at 700 °C for 1 h led to the formation of NiFe₂O₄ nanoparticles with an average crystal size of about 23 nm. Effect of thermal treatment temperature on the crystal size of the nanoparticles was studied. The mechanism of nanoparticles growth was primarily discussed. The activation energy of NiFe₂O₄ nanoparticle formation during calcination was calculated to be 16.6 kJ/mol.