Preparation of silica hollow fibers by surface-initiated atom transfer radical polymerization from electrospun fiber templates

Silica hollow fibers were produced by surface-initiated atom transfer radical polymerization (ATRP) from poly(methyl methacrylate-co-vinylbenzyl chloride) (P(MMA-co-VBC)) electrospun fibers combined with sol-gel process and subsequent calcination. Fourier-transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) were used to characterize the intermediate products and the silica hollow fibers. The resulting silica hollow fibers are of high purity with amorphous morphology. The thickness of the hollow fibers is approximately 0.25 µm.     

Fabrication of hollow silver spheres by MPTMS-functionalized hollow silica spheres as templates

In this study, we provide a strategy to prepare the hollow silver spheres by accumulating the silver nanoparticles on the surface of 3-mercaptopropyltrimethoxysilane (MPTMS)-functionalized silica as templates, which was accomplished by the chemisorption between silver nanoparticles and thiol groups. Then, the resulting hollow silver spheres were obtained through the chemical wet etching process with 10 M HF solution. In conventional method, the fabrication of hollow silver spheres from core-shell spheres was not easy due to the difficulties in retaining the shell structures during core removal. The method in this paper could overcome this limitation. The major focus of study is on understanding the mechanism of formation of the hollow silver spheres through the self-assembly behavior by chemisorption between silver nanoparticles and thiol groups. The silver-coated silica and hollow silver spheres were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), high-resolution TEM (HR-TEM), and X-ray photoelectron spectroscopy (XPS).     

Coprecipitation-assisted hydrothermal synthesis of PLZT hollow nanospheres

Lanthanum-modified lead zirconate titanate Pb_1−xLa_x(Zr_1−yTi_y)O₃ (PLZT) hollow nanospheres have been successfully prepared via a template-free hydrothermal method using the well-mixed coprecipitated precursors and the KOH mineralizer. The structure, composition, and morphology of the PLZT hollow nanospheres were characterized by XRD (X-ray diffraction), ICP (inductive coupled plasma emission spectrometer), FTIR (Fourier transform infrared spectra), TG/DTA (thermogravimetric analysis and differential thermal analysis), TEM (transmission electron microscopy) and SEAD (selected area diffraction). The results show that the composition and the morphology control of the PLZT products are determined by the KOH concentration. The PLZT hollow nanospheres with uniform size of about 4 nm were synthesized in the presence of 5 M KOH. The crystalline nanoparticles can be prepared at dilute KOH, in contrast to the amorphous powders prepared at concentrated KOH. Formation mechanisms of the PLZT hollow nanospheres are also discussed.     

Synthesis of dendrimer-stabilized gold-polypyrrole core-shell nanoparticles

Core-shell composite nanoparticles consisting of a gold core and polypyrrole shell were prepared and stabilized with the poly(amidoamine) dendrimer. An in situ redox polymerization technique was used in which pyrrole reduced Au3+ to Au and then oxidized to polypyrrole. The presence of gold nanoparticles as a core was characterized by its surface plasmon absorption peak at 534 nm. Fourier transform infrared spectroscopy confirmed the presence of polypyrrole on the nanoparticle surfaces. The average diameter of the core-shell nanoparticle is 8.7 +/- 1.8 nm with a shell thickness of approximately 1.5-2.0 nm as estimated from the transmission electron microscopy image. Dissolution of the Au core using KCN enabled the formation of hollow polymer nanospheres.     

Self-assembly directed synthesis of poly(ortho-toluidine)-metal(gold and palladium) composite nanospheres

Poly(ortho-toluidine) (POT)-gold (Au) and palladium (Pd) composite nanospheres were successfully synthesized by the reaction of o-toluidine with the corresponding metal (Au or Pd) colloidal solution through self-assembly process in the presence of dodecylbenzenesulfonic acid (DBSA), which acts as both a dopant and surfactant, and ammonium peroxydisulfate as an oxidizing agent. The composites (POT-DBSA/Au or Pd) were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), Fourier transform infrared (FTIR) spectroscopy, UV-Visible (UV-Vis) spectroscopy, and electrical conductivity measurements. TEM images of the nanocomposites reveal that metal (Au or Pd) nanoparticles were well dispersed on POT spheres. TGA and XRD results show that the composites exhibit high thermal stability and are more crystalline compared with pristine POT. It was found that the electrical conductivity of the POT-DBSA/Au or Pd composites is 2 orders of magnitude higher than that of pristine polymer. Also, the POT-DBSA/Pd composite exhibits magnetic property. The formation mechanism of the POT-DBSA/Au or Pd composite nanosphere is discussed.     

Deposition of copper sulfide hollow nanospheres in aqueous solution at room temperature

Uniform copper sulfide hollow nanospheres were obtained in high yield by reacting copper nitrate with thioacetamide in water at room temperature under the assistance of sodium dodecyl sulfate (SDS). The spheres (average diameter of ca. 200 nm) displayed big cavity while their surface were constructed by randomly stacked nanoflakes. The products were characterized by X-ray diffraction (XRD), energy-dispersive X-ray spectrometry (EDX), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM). SDS was found to play a key role in the synthesis process while a four-step mechanism was proposed to explain the formation of hollow nanospheres. The influence of SDS concentration on the size and shape of the product has also been investigated in detail.     

Facile synthesis and characterization of ZnFe2O4/α-Fe2O3 composite hollow nanospheres

ZnFe₂O₄/α-Fe₂O₃ composite hollow nanospheres were successfully fabricated via a facile one-pot solvothermal method, utilizing polyethylene glycol as soft template. X-ray diffraction and scanning electron microscopy analysis revealed that the prepared nanospheres with cubic spinel and rhombohedra composite structure had a uniform diameter of about 370 nm, and the hollow structure could be further confirmed by transmission electron microscopy. Energy dispersive X-ray, X-ray photoelectron spectroscopy and Fourier transform infrared techniques were also applied to characterize the elemental composition and chemical bonds in the hollow nanospheres. The ZnFe₂O₄/α-Fe₂O₃ composite hollow nanospheres show attractive light absorption property for potential applications in electronics, optics, and catalysis.     

Preparation of hollow CdSe nanospheres

Cadmium selenide (CdSe) hollow nanospheres (approximately 40–50 nm) have been successfully synthesized by γ-irradiating polyacrylamide (PAM) hydrogel template which contains CdCl₂ and Na₂SeO₃ aqueous solution at room temperature. The nanospheres were characterized by energy dispersive spectrum (EDS), field emission scanning electron micrograph (FESEM), transmission electron microscopy (TEM) and high-resolution transmission electron micrograph (HRTEM), respectively. EDS showed that nanospheres were composed of Cd and Se (atomic ratio, 1.15:1). A possible formation mechanism of CdSe hollow nanospheres through two-steps was presented.     

Solvothermal synthesis of solid and hollow CoO nanospheres and their electrochemical properties in lithium-ion battery

Solid and hollow CoO nanospheres were synthesized by solvothermal method with oleic acid as reactant and SiO₂ as template. Each sample of high-purity CoO was characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy and X-ray photoelectron energy spectroscopy, respectively. Both solid and hollow CoO nanospheres as anode for lithium-ion battery were tested by galvanostatic discharge–charge experiments. The first discharge capacity of 1598 and 1640 mAh g^?1 was obtained at 0.1C for solid and hollow CoO nanospheres, respectively. Hollow CoO nanospheres showed better cycle performance.     

SnO2纳米空心球的合成及在锂离子电池正极方面的应用

采用锡盐溶液浸渍-煅烧锯末法,制备了SnO2纳米空心球.分别用X射线衍射(XRD)、透射电子显微镜(TEM)、高分辨透射电子显微镜(HRTEM)及恒流充放电技术对产品的结构形态和电化学性质进行了表征.结果表明,SnO2空心球的尺寸在50～120nm之间,壳层厚度约为5nm.在作为锂离子电池正极使用时,初始放电容量为607.7 mAh g-1.     

水热微乳液法制备锂离子阳极材料CoS2纳米空心球

通过自制的纳米苯丙乳液粒子为吸附载体,以CoCl·6H2O和CS2为原料,在100℃水热条件下,于微乳液粒子表面反应6h制备出了CoS2空心纳米球.利用X射线粉末衍射仪(XRD)、透射电子显微镜(TEM)和扫描电子显微镜(SEM)对产物进行了表征.结果表明,所得产物为纯相的立方晶系CoS2空心纳米球,直径约120nm....     

Biosynthesis and stabilization of Au and Au–Ag alloy nanoparticles by fungus,Fusarium semitectum

Abstract

Crystallized and spherical-shaped Au and Au–Ag alloy nanoparticles have been synthesized and stabilized using a fungus, F . semitectum in an aqueous system. Aqueous solutions of chloroaurate ions for Au and chloroaurate and Ag⁺ ions (1 : 1 ratio) for Au–Ag alloy were treated with an extracellular filtrate of F . semitectum biomass for the formation of Au nanoparticles (AuNP) and Au–Ag alloy nanoparticles (Au–AgNP). Analysis of the feasibility of the biosynthesized nanoparticles and core–shell alloy nanoparticles from fungal strains is particularly significant. The resultant colloidal suspensions are highly stable for many weeks. The obtained Au and Au–Ag alloy nanoparticles were characterized by the surface plasmon resonance (SPR) peaks using a UV-vis spectrophotometer, and the structure, morphology and size were determined by Fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), and transmission electron microscopy (TEM). Possible optoelectronics and medical applications of these nanoparticles are envisaged.     

Ultrasmall hollow gold-silver nanoshells with extinctions strongly red-shifted to the near-infrared

Hollow gold-silver nanoshells having systematically varying sizes between 40 and 100 nm were prepared. These particles consist of a hollow spherical silver shell surrounded by a thin gold layer. By varying the volume of the gold stock solution added to suspensions of small silver-core templates, we tailored the hollow gold-silver nanoshells to possess strong tunable optical extinctions that range from the visible to the near-IR spectral regions, with extinctions routinely centered at ～950 nm. The size and morphology of these core/shell nanoparticles were characterized by dynamic light scattering (DLS), field emission scanning electron microscopy (FE-SEM), and transmission electron microscopy (TEM). Separately, X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) were used for measuring their elemental composition; UV-vis spectroscopy was used to evaluate their optical properties. Given their relatively small size compared to other nanoparticles that absorb strongly at near IR wavelengths, these easy-to-synthesize particles should find use in applications that require ultrasmall nanoparticles with extinctions comfortably beyond visible wavelengths (e.g., medicinal therapies, diagnostic imaging, nanofluidics, and display technologies).     

The facile synthesis of CdSe hollow nanoparticles and necklace-like nanowires from a CdO sacrificial template via chemical reaction in aqueous solution

This paper describes a powerful and facile synthesis of CdSe hollow nanostructures via a sacrificial template method employing the Kirkendall diffusion effect for void formation and an anion exchange reaction for selenization. The CdSe hollow nanowires and nanoparticles were easily transformed from a sacrificial template of CdO nanowires that were formed by thermal Ostwald ripening. The distinctive structures of CdO sacrificial templates were developed through thermodynamically spontaneous process. The morphology of each CdSe nanostructure could be controlled by one of each CdO sacrificial template which was calcined at several different temperatures. Their microstructure was analyzed by field-emission scanning electron microscopy, transmission electron microscopy, and X-ray diffraction, and their optical properties were compared using light absorption. The suggested process for synthesis of hollow nanostructures could also be applied to the formation of other hollow chalcogenide compounds.     

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.     

A simple approach for facile synthesis of Ag,anisotropic Au and bimetallic (Ag/Au) nanoparticles using cruciferous vegetable extracts

We present a simple and straightforward approach for the synthesis and stabilization of relatively monodisperse Ag, Au and bimetallic (Ag/Au) nanoparticles by using cruciferous vegetable (green/red) extracts by simply adjusting the pH environment in the aqueous medium. The vegetable extracts act both as reducing and capping agents. The monometallic and bimetallic nanoparticles of Ag and Au so obtained were characterized by UV–visible spectroscopy, X-ray diffraction (XRD), dynamic light scattering (DLS) and transmission electron microscopy (TEM). It is shown that red cabbage extract can be used for the preparation of anisotropic Au nanoparticles. The formation of Au anisotropic nanoparticles was found to depend on a number of environmental factors, such as the pH of the reaction medium, reaction time, and initial reactant concentrations. Additionally, it is shown that these extract-stabilized Au and Ag nanoparticles can be used as a seed for preparation of bimetallic Au/Ag nanoparticles. For bimetallic alloy nanoparticles the absorption peak was observed between the two maxima of the corresponding metallic particles. The surface plasmon absorption maxima for bimetallic nanoparticles changed linearly with increasing Au mole ratio content in various alloy compositions. It has been shown that the formation of hollow Au spheres depends on the experimental conditions.     

Synthesis of Eu2O3 hollow submicrometer spheres through a sol–gel template approach

Submicrometer-sized hollow Eu₂O₃ spheres with a shell thickness of about 75 nm and inner diameter about 690 nm have been synthesized through a sol–gel method using PS/PE microspheres as templates. X-ray powder diffraction (XRD), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), Field emission scanning electron microscopy (FESEM), and photoluminescence (PL) spectroscopy have been used for the characterization of the obtained hollow Eu₂O₃ spheres. The PL peak is obviously broadened compared with that of bulk Eu₂O₃. The mechanism of the formation of the hollow Eu₂O₃ spheres was discussed.     

Microwave-assisted hydrothermal synthesis and characterizations of PrF3 hollow nanoparticles

PrF₃ hollow nanoparticles were synthesized by the microwave-assisted heating hydrothermal treatment of the corresponding colloidal rare earth fluorides precipitates. The products were characterized by X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and high-resolution transmission electron microscopy (HRTEM). The TEM imaging showed that the PrF₃ nanoparticles prepared in this way had hollow sphere-like morphology with the mean particle size of about 31 nm. XRD showed that the PrF₃ hollow nanoparticles had high purity and high crystallinity.     

Hollow Carbon Nanospheres with Tunable Hierarchical Pores for Drug,Gene, and Photothermal Synergistic Treatment

Design and synthesis of porous and hollow carbon spheres have attracted considerable interest in the past decade due to their superior physicochemical properties and widespread applications. However, it is still a big challenge to achieve controllable synthesis of hollow carbon nanospheres with center‐radial large mesopores in the shells and inner surface roughness. Herein, porous hollow carbon nanospheres (PHCNs) are successfully synthesized with tunable center‐radial mesopore channels in the shells and crater‐like inner surfaces by employing dendrimer‐like mesoporous silica nanospheres (DMSNs) as hard templates. Compared with conventional mesoporous nanospheres, DMSN templates not only result in the formation of center‐radial large mesopores in the shells, but also produce a crater‐like inner surface. PHCNs can be tuned from open center‐radial mesoporous shells to relatively closed microporous shells. After functionalization with polyethyleneimine (PEI) and poly(ethylene glycol) (PEG), PHCNs not only have negligible cytotoxicity, excellent photothermal property, and high coloading capacity of 482 µg of doxorubicin and 44 µg of siRNA per mg, but can also efficiently deliver these substances into cells, thus displaying enhanced cancer cell killing capacity by triple‐combination therapy.     

Sonochemical fabrication and characterization of ceria (CeO2) nanowires

Ceria (CeO2) nanowires have been successfully synthesized by a sonochemical method in ambient air and alkali aqueous solution from CeO2 nanoparticles without using any templates. The results showed that both alkali concentration and ultrasonic irradiation played critical roles in the formation of the nanowires. The crystalline structure and dimensions of the nanowires were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM) and selected area electron diffraction (SAED). The UV-visible absorption spectrum result showed that the products had conspicuous shape-specific effect. Microstructural analysis in HRTEM revealed that the preferential growth direction of CeO2 nanowires was [110]. Moreover, the catalytic activity of Au/CeO2 using CeO2 nanowires as support for CO conversion was higher than that obtained using bulk CeO2 as support.