磁性核壳Fe3O4/Ag纳米复合粒子的制备及性能

以硅烷偶联剂巯基丙基三甲氧基硅烷作为添加剂,甲醛作为还原剂,在Ag[(NH3)2] 溶液中制备出具有核壳结构的Fe3O4/Ag纳米复合粒子.用X射线衍射、场发射扫描电镜、差热分析、振动样品磁强计和Hall效应测试系统对样品进行了表征.结果表明:Fe3O4/Ag核壳复合粒子粒径为40～60 nm,Ag壳层厚度为10～15 nm,体积电阻率为7.757 3×10-4 Ω·cm,饱和磁化强度为26.37 A·m2/kg.     

Reduced graphene oxide supported highly porous V2O5 spheres as a high-power cathode material for lithium ion batteries

Reduced graphene oxide (rGO) supported highly porous polycrystalline V(2)O(5) spheres (V(2)O(5)/rGO) were prepared by using a solvothermal approach followed by an annealing process. Initially, reduced vanadium oxide (rVO) nanoparticles with sizes in the range of 10-50 nm were formed through heterogeneous nucleation on rGO sheets during the solvothermal process. These rVO nanoparticles were oxidized to V(2)O(5) after the annealing process in air at 350 °C and assembled into polycrystalline porous spheres with sizes of 200-800 nm. The weight ratio between the rGO and V(2)O(5) is tunable by changing the weight ratio of the precursors, which in turn affects the morphology of V(2)O(5)/rGO composites. The V(2)O(5)/rGO composites display superior cathode performances with highly reversible specific capacities, good cycling stabilities and excellent rate capabilities (e.g. 102 mA h g(-1) at 19 C).     

Studies on the synthesis of electrospun PAN‐Ag composite nanofibers for antibacterial application

We have successfully synthesized polyacrylonitrile (PAN) nanofibers impregnated with Ag nanoparticles by electrospinning method at room temperature. Briefly, the PAN‐Ag composite nanofibers were prepared by electrospinning PAN (10% w/v) in dimethyl formamide (DMF) solvent containing silver nitrate (AgNO₃) in the amounts of 8% by weight of PAN. The silver ions were reduced into silver particles in three different methods i.e., by refluxing the solution before electrospinning, treating with sodium borohydride (NaBH₄), as reducing agent, and heating the prepared composite nanofibers at 160°C. The prepared PAN nanofibers functionalized with Ag nanoparticles were characterized by field emission scanning electron microscopy (FESEM), SEM elemental detection X‐ray analysis (SEM‐EDAX), transmission electron microscopy (TEM), and ultraviolet‐visible spectroscopy (UV‐VIS) analytical techniques. UV‐VIS spectra analysis showed distinct absorption band at 410 nm, suggesting the formation of Ag nanoparticles. TEM micrographs confirmed homogeneous dispersion of Ag nanoparticles on the surface of PAN nanofibers, and particle diameter was found to be 5–15 nm. It was found that all the three electrospun PAN‐Ag composite nanofibers showed strong antibacterial activity toward both gram positive and gram negative bacteria. However, the antibacterial activity of PAN‐Ag composite nanofibers membrane prepared by refluxed method was most prominent against S. aureus bacteria. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

Visible light active Cu-doped iron oxide for photocatalytic treatment of methylene blue

In recent work, pure α-Fe₂O₃ (F-1) and series of 5% Cu doped Fe₂O₃ (CF-5) , 10% Cu doped Fe₂O₃ (CF-10) and 15% Cu doped Fe₂O₃ (CF-15) nanoparticles by facile chemical coprecipitation method were synthesized to study the effect of concentration of doping for photocatalytic activity. As prepared F-1, CF-5, CF-10, CF-15 nanoparticles were subjected to X-ray diffraction (XRD) and Fourier transform infra-red (FTIR) techniques to analyse the structural and functional groups features. These characterization techniques confirmed the successful doping of Cu ²⁺ ions in α-Fe₂O₃. The crystallite size of synthesized samples was calculated by Scherrer formula. Gradually decline in crystallite size from 18 to 15 nm was observed for undoped to doped samples. Scanning electron microscopic (SEM) analysis expressed that doping of Cu reduced the aggregation of particles and enhanced the surface area of nanoparticles. UV–Visible spectroscopic analysis of synthesized samples was used to calculate the bandgap energy of F-1, CF-5, CF-10, CF-15 nanoparticles i.e., 2.0, 1.7, 1.5, 1.4eV respectively. Narrowing bandgap energy of doped hematite supported to perform excellent photocatalytic activity. Maximum degradation of methylene blue was recorded via CF-10 within 140 min. Higher degradation rate of methylene blue by optimal concentration of CF-10 is due to effective electron trapping ability of photocatalyst.     

Structural,optical, morphological properties of silver doped cobalt oxide nanoparticles by microwave irradiation method

The synthesis of silver doped cobalt oxide nanoparticles by microwave-assisted method and their structural, optical, antibacterial activities are presented in this study. The doping concentrations were chosen as 5, 10, 15, and 20 wt percentages. The sample was undergone powder X-ray diffraction studies and the result shows the good crystalline nature of the sample. Also, the average crystallite size increases from 13.95 nm, 21.26 nm, 26.13 nm, and 28.35 nm with different doping concentrations. The transmission electron microscopy image shows cubic and spherical morphology. The optical properties were tested by UV–vis–NIR absorption spectrum. It indicates the decrease of band gap value. From the antibacterial activity studies, the 20 wt % Ag doped nanoparticles exhibit better activity.     

Plasmon enhanced upconversion luminescence of NaYF(4):Yb,Er@SiO(2)@Ag core-shell nanocomposites for cell imaging

NaYF(4):Yb,Er@SiO(2)@Ag core-shell nanocomposites were prepared to investigate metal-enhanced upconversion luminescence. Two sizes (15 and 30 nm) of Ag nanoparticles were used. The emission intensity of the upconversion nanocrystals was found to be strongly modulated by the presence of Ag nanoparticles (NPs) on the outer shell layer of the nanocomposites. The extent of modulation depended on the separation distance between Ag NPs and upconversion nanocrystals. The optimum upconversion luminescence enhancement was observed at a separation distance of 10 nm for Ag NPs with two different sizes (15 and 30 nm). A maximum upconversion luminescence enhancement of 14.4-fold was observed when 15 nm Ag nanoparticles were used and 10.8-fold was observed when 30 nm Ag NPs were used. The separation distance dependent emission intensity is ascribed to the competition between energy transfer and enhanced radiative decay rates. The biocompatibility of the nanocomposites was significantly improved by surface modification with DNA. The biological imaging capabilities of these nanocomposites were demonstrated using B16F0 cells.     

纳米铁酸锰吸附去除Cr(Ⅵ)的研究

分别采用水热法和溶剂热法制备了两种不同形貌的纳米铁酸锰样品,研究了其吸附去除Cr6+的效果.以FeCl3和MnCl2为反应原料,以乙醇胺为沉淀剂采用水热法180℃保温8 h制备得到粒径为10~20 nm的铁酸锰纳米颗状,颗粒间团聚现象严重.采用溶剂热法以FeCl3、MnCl2和无水乙酸钠为反应原料,以乙二醇为溶剂200℃保温12 h制备得到粒径400~700 nm的铁酸锰多孔球.利用XRD、TEM和N2吸附-脱附等对铁酸锰样品进行了表征,研究了吸附剂用量、Cr(Ⅵ)初始浓度、pH值及吸附时间对Cr(VI)吸附性能的影响.实验结果表明,采用溶剂热法制备的铁酸锰多孔球具有较好的Cr(Ⅵ)去除效果.     

One-pot fabrication of Ag–SrTiO3 nanocomposite and its enhanced thermoelectric properties

Ag–SrTiO₃ ceramic nanoparticles were fabricated by doping SrTiO₃ with various contents (0.5, 1, 3, and 5%, in mass ratio) of Ag. Composite samples were prepared through a one-pot solvothermal method and sintering process. The temperature-dependent thermoelectric properties of these sample were measured from 300 K to 500 K. The maximum power factor (843.3 μ·W/m·K²) at 500 K, which is ∼3.96 times higher than that of the pristine SrTiO₃ ceramics, was obtained for the Ag–SrTiO₃ composite sample with 1% of Ag. In addition, the thermal conductivity of the composites decreased due to the phonon scattering effect. The maximum thermoelectric figure of merit (ZT), i.e., ∼0.09, which was achieved with 1% of Ag at 500 K, yielded an enhanced power factor and a reduced thermal conductivity. This ZT value was ∼4.27 times larger than that of pristine SrTiO₃ at the same temperature.     

航空煤油在不同孔径的Ag基介孔材料吸附剂上深度吸附脱硫的研究

以3种不同孔径的介孔材料MCM-41,SBA-15,大孔SBA-15(SBA-15-L)为载体,采用离子交换法制备了Ag/Al-MCM-41,Ag/Al-SBA-15和Ag/Al-SBA-15-L介孔材料吸附剂。利用XRD,N2吸附,SEM-EDS,ICP-MS等手段对所制备的吸附剂进行了表征,并在固定床上对航空煤油进行了吸附脱硫研究。结果表明,交换Ag+所制备的吸附剂依然保持介孔材料的特性,并可将含S量为150×10-6的航空煤油中的硫化物,选择性的吸附脱除到S含量低于1.0×10-6。其中,在Ag/Al-MCM-41,Ag/Al-SBA-15和Ag/Al-SBA-15-L吸附剂上,可分别得到8.0,9.0和17.0mL的清洁航空煤油(含硫量小于1.0×10-6)。实验结果也表明,所制备的吸附剂吸附脱硫性能主要取决于介孔材料载体的孔径大小,载体的孔径越大,Ag+的利用率越高,吸附剂的吸附脱硫性能越强。将吸附饱和的Ag/Al-SBA-15-L吸附剂,于空气中在350℃进行再生5h,吸附剂的吸附性能可以100%的恢复。     

Silver nanoparticles synthesized from mesoporous Ag/SBA-15 composites

Silver nanoparticles were prepared by removing silica from mesoporous Ag/SBA-15 composites. The results of nitrogen adsorption–desorption isotherms, X-ray diffraction, transmission electron microscopy and UV–vis spectroscopy indicated that Ag nanoparticles existed in the pore channels of SBA-15. Ag nanoparticles with diameters in the range of 2.5–5.5 nm and a narrow size distribution were confirmed by atomic force microscope images and energy-dispersive X-ray spectroscopy. UV–vis spectroscopy showed a broad emission peak of Ag nanoparticles centered at ca. 438 nm.     

A sweet killer: mesoporous polysaccharide confined silver nanoparticles for antibacterial applications

Silver nanoparticles (AgNP) confined within porous starch have been prepared in a simple, green and efficient manner, utilising the nanoporous structure of predominantly mesoporous starch (MS) to act as nanoparticle stabiliser, support and reducing surface. MS/AgNP materials present high surface areas (S(BET) > 150 m(2) g(-1)) and mesopore volumes (V(meso) > 0.45 cm(3) g(-1)). The interaction of the AgNP precursor and forming nanoparticle nuclei with the mesoporous domains of the porous polysaccharide, direct porosity to increasingly narrower and more defined pore size distributions, indicative of a degree of cooperative assembly. Transmission electron microscopy images indicated the presence of spherical AgNP of a size reflective of the porous polysaccharide mesopore diameter (e.g., 5-25 nm), whilst XPS analysis confirmed the metallic Ag(0) state. Materials were prepared at relatively low Ag loadings (<0.18 mmol g(-1)), demonstrating excellent antimicrobial activity in solid and liquid phase testing against Gram negative (E. coli) and positive (S. aureus) model bacteria. The resulting materials are biocompatible and present a useful solid porous carbohydrate-based polymer vehicle to control the AgNP size regime and facilitate transference to a biological environment.     

Eu~(3+)掺杂浓度对NaYF_4:Eu~(3+)晶体荧光强度的影响

在乙醇和乙二醇的混合溶剂中,用溶剂热法,150℃,反应12 h,成功合成了NaYF4:Eu3+晶体。室温下,用X射线衍射对材料的组成进行了表征,JCPDS号为16-0334。荧光光谱分析表明,在395 nm(7F0→5L4)紫外光激发下,其发射峰在476 nm、540~578 nm、718 nm分别对应着Eu3+的5DJ(J=0,1,2,3)→7FJ(J=1,2,3,4)能级跃迁。并讨论了离子Y3+:Eu3+不同浓度掺杂比对荧光性质的影响。结果表明,Eu3+的最佳掺杂浓度比为5%,当掺杂浓度为10%时,出现荧光猝灭。     

Electron Beam Synthesis and Characterization of Poly Vinyl Alcohol/Poly Acrylic Acid Embedded Ni and Ag Nanoparticles

Electron beam irradiation was applied to prepare poly (vinyl alcohol) and poly (acrylic acid) P (PVA/AAc) containing nickel and silver nanoparticles. The prepared P (PVA/AAc)–Ni and P (PVA/AAc)–Ag nanoparticles were characterized by Fourier-transform infrared, UV–Visible spectroscopy, X-ray diffraction (XRD) and transmission electron microscope (TEM). The electrical conductivity and thermal gravimetrical analysis (TGA) have been investigated. Bacterial sensitivity toward nickel and silver nanoparticles was studied. The XRD and TEM confirmed that by increasing the Ni or Ag contents from 10 to 150?mmol in the copolymers, the metal particle size increases from 27.6 to 45.6?nm for Ni and from 14.8 to 37.4?nm for Ag. Meanwhile, the mean size particle increases from 33.02 to 45.05?nm for Ni and from 15.5 to 44.03?nm for Ag. The electrical conductivity of the polymer containing Ag is higher than that of Ni and it increased by increasing the metal content. The TGA studies confirmed that, the thermal stability increase by the introduction of metal into polymeric complex. Bacterial sensitivity to metal nanoparticles was found to vary depending on the microbial species. Disc diffusion studies with P. aeruginosa, E. coli and K. pneumoniae revealed greater effectiveness of the silver nanoparticles compared to the nickel nanoparticles, S. aureus depicted the highest sensitivity to nanoparticles compared to the other strains and was more adversely affected by the nickel nanoparticles.     

A simple aqueous solution based chemical methodology for synthesis of Ag nanoparticles dispersed on mesoporous silicate matrix

A simple chemical method has been developed for preparation of Ag nanoparticles dispersed on mesoporous silicate matrix, SBA-15. Ag nanoparticles were uniformly dispersed on SBA-15 matrix by using the reduction reaction of AgNO₃ with trisodium citrate. The synthesized materials were characterized by using room temperature powder XRD analysis, N₂ adsorption-desorption isotherm, high resolution TEM and SEM. It was observed that the synthesized SBA-15 and Ag-SBA-15 have a surface area of 778 and 151 m²/g respectively. The synthesized materials have long range ordering of pores with narrow pore size distribution centered at ∼ 7 nm. Pore structure of SBA-15 remains preserved even after deposition of Ag nanoparticle. This chemical route reported here offers a simple method for preparation of Ag-SBA-15, where unagglomerated Ag nanoparticles (∼ 20 nm) are uniformly dispersed on SBA-15.     

Photocrosslinkable acid urethane dimethacrylates from renewable natural oil and their use in the design of silver/gold polymeric nanocomposites

Castor oil-based acid urethane macromers were prepared and employed for obtaining Ag/Au/polymer nanocomposites. Structure and UV induced photopolymerization of the macromers were investigated by spectral methods. The polymerization rate and the degree of conversion decreased with about 10% in the presence of 2.5 wt.% silver nanoparticles (Ag NPs). For the diacid macromer, the surface plasmon intensity increased with irradiation time (the optical density of the absorption maximum (430 nm) attained 2.3 after 600 s), whereas a diminished efficiency was found for Ag NPs in situ generated. Transmission electron microscopy and X-ray photoelectron spectroscopy confirmed uniform distribution of the spherical nanoparticles (0.6 nm (Ag NPs); 5 nm (Au NPs)) and the appearance of Ag 3d_3/2, Ag 3d_5/2, Au 4f_7/2 and Au 4f_5/2 peaks corresponding to Ag (0) or Au (0). Environmental scanning electron microscope with energy-dispersive X-ray detector, contact angle and mechanical parameters measurements complemented the above observations.     

Magnetic properties and magnetoresistance effect of SnFe2O4 spinel nanoparticles: Experimental,ab initio and Monte Carlo simulation

In this contribution, SnFe₂O₄ nanoparticles were prepared by the solvothermal method, the structural properties were performed using X-Ray Diffraction (DRX) to prove the success of tin ferrite formation and to determine de crystals parameters. The size and morphological study were build using Scanning Electron Microscopy (SEM) and Transmission Electron microscopy (TEM), the results showed that the size of particles is uniform with a range of particles (5–7 nm). The magnetic properties were carried out using the SQUID device, the SnFe2O4 nanoparticles have a magnetic transition at 750 K. In addition, the hysteresis loops at low temperature displayed Ms and Mr equals to 23 emu/g and 6 emu/g, respectively. The magnetoresistance properties were investigated, the SnFe₂O₄ nanoparticles present a large magnetoresistance effect (80%). The experimental results are supplemented by model calculations utilizing density functional theory and Monte-Carlo simulations.     

One-pot synthesis of mesoporous CuOx/CeO2 co-loaded ZrO2–TiO2 nanocomposites via surfactant-free solvothermal method for catalytic removal of soot under NO/O2

A novel porous CuO_x/CeO₂ co-loaded ZrO₂–TiO₂ (ZT) nanocomposite with tunable pore structure and high surface area was prepared by a simple surfactant-free solvothermal method. The pore structure could be well controlled by adjusting the ratio of ethanol to H₂O during the solvothermal process. Both copper oxides and ceria species could be homogeneously loaded into porous ZT nanocomposite by either incorporation into ZT framework or dispersion into the pore channels. Two kinds of novel catalysts with different pore structures have been synthesized and exhibit excellent soot catalytic combustion performance, owing to the porous structure and the active components of CuO_x/CeO₂.     

The gadolinium effect on crystallization behavior and luminescence of β-NaYF4:Yb,Er phase

Single phase β-NaY_0.8-xGd_xYb_0.18Er_0.02F₄ nanoparticles with different concentrations of gadolinium ions were prepared via PVP-assisted solvothermal treating at 200°C (PVP- polyvinylpyrrolidone). With the increase in Gd³⁺ concentration, size of the nanoparticles decreased. The up-converting spectra recorded upon 980 nm irradiation showed the green (510-560 nm) and red (640-690 nm) emissions, due to ²H_11/2, ⁴S_3/2 → ⁴I_15/2 and ⁴F_9/2 → ⁴I_15/2 transitions, respectively. The strongest up-conversion luminescence was detected in 15 mol% Gd³⁺-doped nanoparticles obtained after 20 hours of solvothermal treating. With the rise of Gd³⁺ content up-conversion emission decreased due to increased defect concentration in the NaYF₄ matrix. Fourier transform infrared spectroscopy proved in situ generation of hydrophilic nanoparticles as a result of PVP ligands retention at the particle surface.     

(Ag)_核·(Au)_壳复合纳米粒子的制备

以银原子团簇作晶种,采用微波高压液相合成法制备了分散性好、规则球形的(Ag)核·(Au)壳复合纳米粒子。研究了(Ag)核·(Au)壳复合纳米粒子的紫外可见吸收光谱和共振散射光谱特性。结果表明,液相(Ag)核·(Au)壳复合纳米粒子和高压微波合成的液相金纳米粒子的最强共振散射峰均在580nm处,它们的吸收光谱图相似,最大吸收分别在518.5nm和524.8nm。     

Effect of TeO2 on Near‐Infrared Emission from Bismuth Centers in Borogermanate Glasses

Bi‐doped xTeO₂–(60?x)GeO₂–15B₂O₃–20MgO–5Al₂O₃ glasses were prepared by the conventional melt‐quenching method and their absorption and fluorescence spectra were characterized. Broadband near‐infrared (NIR) emission from Bi centers centered around 1240 nm with a full width at half maximum (FWHM) of 250 nm was observed, and the position of the emission peak strongly depends on the excitation wavelength. Increasing TeO₂ concentration results in the strong coloration of the glass, leading to the reduction and finally, complete quenching of the NIR emission. Based on Raman, X‐ray photoelectron spectroscopy and transmission microscopy observation, the coloration of the glass at high TeO₂ concentration can be ascribed to the precipitation of elemental Te nanoparticles of around 3–8 nm, which effectively suppresses the NIR emission by reabsorption. The precipitation of Te nanoparticles in an oxide glass may find novel applications in photonics and relevant fields.