In situ synthesis of plate-like Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles in porous cellulose films with obvious magnetic anisotropy

Nanocomposite cellulose films with obvious magnetic anisotropy have been prepared by in situ synthesis of plate-like Fe₂O₃ nanoparticles in the cellulose matrix. The influence of the concentrations of FeCl₂ and FeCl₃ solutions on the morphology and particle size of the synthesized Fe₂O₃ nanoparticles as well as on the properties of the composite films has been investigated. The Fe₂O₃ nanoparticles synthesized in the cellulose matrix was γ-Fe₂O₃, and its morphology was plate-like with size about 48 nm and thickness about 9 nm, which was totally different from those reported works. The concentration of FeCl₂ and FeCl₃ solution has little influence on the particle size and morphology of the Fe₂O₃ nanoparticles, while the content of Fe₂O₃ nanoparticles increased with the increase of the concentration of the precursor solution, indicating that porous structured cellulose matrix could modulate the growth of inorganic nanoparticles. The unique morphology of the Fe₂O₃ nanoparticles endowed the composite films with obvious magnetic anisotropy, which would expand the applications of the cellulose based nanomaterials.     

Solvothermal Preparation and Effects of Mixed Solvent on the Properties of Copper Indium Diselenide Nanoalloys

We have developed a simple solvothermal method by using solvent mixtures of ethylenediamine with ethanol and deionized water to produce the CuInSe₂ nanoalloys. The phase structure, morphology, elemental composition and optical band gap (E_g) of synthesized the CuInSe₂ nanoalloys were characterized by Raman spectroscopy, X‐ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X‐ray spectroscopy (EDS) and zeta potential particle sizer measurements. The factors affecting product purity in the mixed solvent are also discussed. The results showed that CuInSe₂ nanoalloys with a chalcopyrite tetragonal structure were produced by adjusting the ratio of ethylenediamine to ethanol (1:2.33 by volume) and their corresponding energy band gap was found to be 1.27 eV. In addition, we prepared and coated the CuInSe₂ ink on the Mo substrate by the doctor blade method to produce a compact thin film. The crystallinity and the morphology of these polycrystalline CuInSe₂ films were characterized.     

Effects of CNT‐film Pretreatment on the Characteristics of NiCo2O4/CNT Core‐shell Hybrids as Electrode Material for Electrochemistry Capacitor

NiCo₂O₄/CNT nanocomposite films were fabricated by in‐situ growing ultrafine NiCo₂O₄ nanoparticles on acid‐modified carbon nanotube (CNT) films. The effects of CNT‐film pretreatment were investigated thoroughly by various characterization outfits including Fourier Transform Infrared spectroscopy (FT‐IR), X‐ray photoelectron spectroscopy (XPS), Raman spectroscopy, RTS‐9 four‐point probes resistivity measurement system, X‐ray powder diffraction (XRD), scanning electron microscopy (SEM) and CHI660D electrochemical workstation. These results suggested that carbon nanotubes were uniformly wrapped by NiCo₂O₄ nanoparticles forming a hierarchical core‐shell structure. And the crystallinity, conductivity of the CNTs and detail structure (both morphology and size) of the NiCo₂O₄ nanoparticles varied with prolonged acid treatment time which resulted in increased functional groups and defects on CNT films and further affected the electrochemical properties. The composite film composed of the CNT film pretreated by mixed acid for 12 h exhibited excellent electrochemical properties: 828 F/g at 1 A/g and 656 F/g at 20 A/g, and maintained over 99 % of its capacitance after 3000 cycles of charge/discharge at 5 A/g. Acid treatment for either too long or too short is detrimental to the electrochemical properties of the composite films. Such work should be of fundamental importance for tailoring electrochemical properties by elaborate design of acid treatment on CNTs.     

Preparation of antibacterial polyimide films containing silver nanoparticles

Polyimide/silver composite films were successfully prepared by in situ polymerization. A precursor, AgNO₃ was used as the source of the silver nanoparticles. The structure and morphology of resulting films were characterized by FTIR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). Consequently, the silver nanoparticles were well dispersed in polyimide matrix. Meanwhile, thermal properties from thermal gravimetric analyses (TGA) and mechanical properties from tensile test which confirmed composites were kept good performance as compared to pure polyimide. In addition, the antimicrobial activity of polyimide/silver composite films against three different bacteria, B. subtilis, S. aureus, and E. coil, illustrated excellent activity. This composite is potential useful as antimicrobial material with good thermal performance in a wide variety of biomedical and general use applications.     

Synthesis of Ag-SiO2 composite nanospheres and their catalytic activity

A simple,mild,and time-saving method is employed to synthesize Ag-SiO2 composite nanospheres with Ag nanoparticles uniformly distributed on the surface of SiO2 nanoparticles.The chemical elements and the morphology of Ag-SiO2 composite nanospheres were analyzed with transmission electron microscopy(TEM),X-ray power diffraction(XRD),and X-ray photoelectron spectroscopy(XPS).On the surface of Ag-SiO2 composite nanospheres,silane coupling agent(KH-550)is introduced as an intermediary to connect the surfaces of SiO2 nanospheres and Ag nanoparticles,which is also helpful for avoiding the aggregation of Ag nanoparticles.It is found that Ag-SiO2 composite nanospheres have very good catalytic properties for the reduction of organic dyes,which may have potential application in wastewater treatment.     

Preparation and properties of cellulose/silver nanoparticle composites with in situ-generated silver nanoparticles using Ocimum sanctum leaf extract

In the present work, silver nanoparticles were in situ-generated in cellulose matrix using Ocimum sanctum leaf extract as a reducing agent. Regenerated wet cellulose films were first immersed in O. sanctum leaf extract and then it was allowed to diffuse into the films. The leaf extract–diffused wet films were dipped in different concentrated aq.AgNO₃ solutions. The leaf extract inside the wet films reduced AgNO₃ into nanosilver. The dry composite films were black in color. Some of the nanoparticles were also formed outside the film in the solution. The nanoparticles were viewed by transmission electron microscopy and scanning electronic microscopy techniques. The composite films showed good antibacterial activity. The cellulose, matrix, and the composite films were characterized by Fourier transform infrared spectroscopy, X-ray diffraction, and thermogravimetric analysis techniques. The tensile properties of the composite films were higher than those of the matrix. These biodegradable films can be used for packaging and medical purposes.     

Photosensitive layers of TiO2/polythiophene composites prepared by electrodeposition

We adopted an electrophoretic deposition method for the preparation of thin layers of insoluble composite nanoparticles composed of TiO₂ core and about 2 nm thick shell of polythiophene, prepared by oxidative polymerization of thiophene. The reduced form of TiO₂-polythiophene composite material was deposited on the conductive surface from an ultrasonically generated microdispersion. Varying the dispersion media, applied voltage and the electrode arrangement made it possible to control the quality and morphology of the films. Compact semitransparent films deposited on ITO electrodes, suitable for photoelectrical measurements, were obtained within short deposition times.     

Effect of the solvent on growth and properties of polyaniline-based composite films

In this study, we report on the electrosyntheses of polyaniline (PAni) and PAni/magnetite nanoparticle (PAni/Fe₃O₄-NP) composite films by a potentiodynamic method from water and ethanol solutions. The aim of the study is to evaluate the effect of the solvent on the electrochemical growth of these films. The growth cyclic voltammograms and the mass change variation (Δm), determined by the electrochemical quartz crystal microbalance technique, show that the polymer growth rate is lower in ethanol than in water (Δm in water is ca. 50% higher than in ethanol after 30 voltammetric cycles). As a consequence, the films grown from ethanol show a more compact and uniform morphology, as we observed with scanning electron microscopy. Furthermore, the formation of oxidation products is inhibited in ethanol. The PAni/Fe₃O₄-NP composite films electrosynthesized in ethanol showed enhanced electrochemical response than the composite films grown from water. This is attributed to the better dispersion of the nanoparticles in this solvent and consequently in the polymer matrix, as confirmed by the Δm value and the spectroscopic characterization. We conclude that electropolymerization from ethanol solution provides high-quality PAni and PAni/Fe₃O₄-NP composite films; the electrochemical and morphological properties of these films suggest that their use for corrosion protection is promising.     

The antioxygen radiation properties of the nanocomposite film consisted of hydrogenated amorphous carbon (a-C:H) and MoS2

MoS₂/a-C:H multilayer film and MoS₂/a-C:H composite film exhibit excellent tribological properties in vacuum, which can be used as the potential space lubricant. The radiation-protective properties of these two films in atomic oxygen (AO) are evaluated. The influences of AO radiation on structure, morphology, and tribological properties of the films were investigated. The results show that AO radiation mainly causes oxidation and increases sp² C content in both of the films. Furthermore, the MoS₂ sublayer on the surface of the multilayer film is oxidized heavily, whereas both the MoS₂ and the a-C:H matrix on the surface were oxidized in the composite film. As a result of this, the multilayer film exhibits high friction coefficient and short sliding lifetime in vacuum after AO radiation. Compared with that, the composite film exhibits lower friction and longer sliding time more than 3600 seconds in vacuum, which illustrates it has a good AO radiation protection. This indicates that MoS₂/a-C:H composite film is more likely to be used as a potential space lubricant.     

Recent Developments in Colloidal Synthesis of CuInSe2 Nanoparticles

Ternary semiconductor nanocrystals, such as CuInSe₂, are of high interest for photovoltaic application due to their relatively low toxicity and unique properties. During the last decades great success has been achieved in the colloidal synthesis of binary nanoparticles, but for ternary compounds this research is still in an early stage of development. These materials are a challenge for synthetic chemistry, because the interaction between the three components (copper, indium, and selenium) plays a major role for the production of high quality material. The purpose of this Minireview is to provide a summary of the achievements in colloidal synthesis of CuInSe₂ nanoparticles—in particular, details of reaction mechanism and its characterization possibilities, which might be useful also for the colloidal synthesis of other multicomponent systems.     

帽状铜纳米粒子的制备及表面增强拉曼散射活性研究

采用真空热蒸发法在SiO₂纳米粒子自组装单层膜上沉积铜薄膜制备了帽状铜纳米粒子。用扫描电镜、原子力显微镜和紫外-可见-近红外分光光度计对帽状复合纳米粒子的表面形貌和光学性质进行了表征。以亚甲基蓝和吡啶-(2-偶氮-4)间苯二酚为探针分子,研究了该复合纳米粒子的表面增强拉曼散射(SERS)活性。通过比较吸附在不同基底上的吡啶-(2-偶氮-4)间苯二酚的谱峰强度,探讨了SERS效应与表面等离子体共振(SPR)的关系。     

电沉积-退火工艺制备铜铟硒太阳能电池薄膜及表征

CuInSe₂ (CIS) films with good crystalline quality were synthesized by electrodeposition followed by annealing in Se vapor at 530 oC. The morphology, composition, crystal structure, optical and electrical properties of the CIS films were investigated by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction, Raman spectroscopy, UV-VIS-NIR spectroscopy, and admittance spectroscopy. The results revealed that the annealed CIS films had chalcopyrite structure and consisted of relatively large grains in the range of 500-1000 nm and single grain of films extend usually through the whole film thickness. The band gap of CIS films was 0.98 eV and carrier concentration was in the order of 10¹⁶ cm^-3 after etching the Cu-Se compounds on the film surface. Solar cells with the structure of AZO/i-ZnO/CdS/CIS/Mo/glass were fabricated. Current density vs. voltage test under standard reported condition showed the solar cells with an area of 0.2 cm² had a conversion efficiency of 0.96%. The underlying physics was also discussed.     

Investigations on the structural,mechanical, thermal,and electrical properties of Ce-doped TiO2/poly(n-butyl methacrylate) nanocomposites

This study focused on the fabrication of poly(n-butyl methacrylate) (PBMA) nanocomposites with various concentrations of cerium-doped titanium dioxide (Ce–TiO₂) nanoparticles via in situ polymerization technique. The structural characterization and the material properties of all the composites were analyzed by UV–visible, FTIR, XRD, SEM, DSC, TG, and tensile strength measurements. The UV–visible and FTIR studies confirmed the effective inclusion of Ce–TiO₂ nanoparticles into the PBMA matrix. The change in amorphous morphology of PBMA to a crystalline structure was observed from the XRD pattern. The SEM morphology revealed the attachment of nanoparticles in the polymer matrix. The inclusion of Ce–TiO₂ nanoparticles enhanced the glass transition temperature, and thermal stability of the PBMA matrix was revealed from DSC and TG, respectively. The tensile strength of PBMA was greatly enhanced by the addition of Ce–TiO₂ nanoparticles. The AC conductivity, dielectric constant, and dielectric loss studies were also performed in the frequency range 10²–10⁶ Hz, and it was observed that addition of Ce–TiO₂ nanoparticles greatly enhanced the electrical properties of PBMA. The change in dielectric constant with the addition of nanoparticles was correlated with a theoretical modeling study. This work also extended to study the role of Ce–TiO₂ nanoparticles in the reinforcing mechanism of the nanocomposite by comparing the actual tensile strength of the composite with different theoretical modeling. The high dielectric constant and tensile strength of composite are beneficial in designing lightweight and highly efficient nanoelectronic materials based on the family of polybutyl acrylates.

     

Synthesis and characterization of FePt nanoparticles and FePt nanoparticle/SiO2-matrix composite films

Superparamagnetic face-centered cubic (fcc) FePt nanoparticles were synthesized using a polyol process. The effect of reaction temperature and molar ratio of Fe(CO)₅ to Pt(acac)₂ on the structure, composition and morphology of nanoparticles has been investigated. The optimum processing condition has been obtained for producing well-monodisperse fcc-phase FePt nanoparticles with the 2:1?molar ratio of Fe-Pt at 220?°C. In order to circumvent the problem of FePt particle coalescence during high temperature annealing for the L1₀ ordering, FePt nanoparticle/SiO₂-matrix composite films have been fabricated by sol?Cgel method. The experimental results confirm that the amorphous SiO₂ matrix effectively inhibits the grain growth and particle aggregation during 700?°C annealing for 1?h. Well-monodisperse face-centered tetragonal (fct) FePt particles embedded in the SiO₂ matrix can be obtained with the long-range chemical order parameter S of ~0.74, indicating partially ordered L1₀ phase transition in FePt/SiO₂ composite films. The FePt/SiO₂ system exhibits a hysteretic behavior with smaller coercive field of 1,450 Oe. The incomplete phase transition from cubic deredat height maxsium (A ₁-disordered phase to tetragonal L1₀-ordered phase) might be responsible for it.     

Formation of polyaniline/Pt nanoparticle composite films and their electrocatalytic properties

Polyaniline (PANI) thin films modified with platinum nanoparticles have been prepared by several methods, characterised and assessed in terms of electrocatalytic properties. These composite materials have been prepared by the in situ reduction of a platinum salt (K₂PtCl₄) by PANI, in a variety of solvents, resulting in the formation of platinum nanoparticles and clusters of different sizes. The further deposition of platinum clusters at spin cast thin films of PANI/Pt composites from a neutral aqueous solution of K₂PtCl₄ has also been demonstrated. Thin-film electrodes prepared from these materials have been investigated for their electrocatalytic activity by studying hydrazine oxidation and dichromate reduction. The properties of the composite materials have been determined using UV–visible spectroscopy, atomic force microscopy and transmission electron microscopy. The nature of the material formed is strongly dependent on the solvent used to dissolve PANI, the method of preparation of the PANI/Pt solution and the composition of the spin cast thin film before subsequent deposition of platinum from the aqueous solution of K₂PtCl₄.Dedicated to Professor Dr. Alan Bond on the occasion of his 60th birthday.     

Trigonal pyramidal CuInSe2 nanocryastals derived by a new method for photovoltaic applications

Copper indium selenide (CuInSe₂) nanocrystals with trigonal pyramidal shape are synthesized by a two-step process for photovoltaic applications. Structural, morphological and optical properties of the as-synthesized CuInSe₂ nanocrystals are characterized by using powder X-ray diffraction analysis, transmission electron microscopy, X-ray photoelectron spectroscopy and UV-Vis absorption spectroscopy. Results indicate that the monodispersed nanocrystals show a single phase polycrystalline and the size of the trigonal pyramid is in the range of 10-12 nm, and the average composition ratio of the Cu/In/Se is measured to be 1.0:1.2:2.0. It is also investigated that the size and morphology of the CuInSe₂ nanocrystals can be tuned through a manipulation of the reaction time. Under an illumination of the simulated AM 1.5, the as-fabricated hybrid solar cell based on the P3HT/CuInSe₂ nanocrystals blends exhibits a promising open circuit voltage (V_oc) of 0.42 V and its energy conversion efficiency is as 3 times as that of the solar cell fabricated by only the naked P3HT polymer.     

Ag2S/Ag3PO4/Ni复合薄膜的制备及其光催化性能

采用电化学方法制备Ag_2S/Ag_3PO_4/Ni复合薄膜,以扫描电子显微镜(SEM)、X射线衍射(XRD)、紫外-可见漫反射光谱(UVVis DRS)对薄膜的表面形貌、晶相结构、光谱特性及能带结构进行了表征,以罗丹明B为模拟污染物对薄膜的光催化活性和稳定性进行了测定,采用向溶液中加入活性物种捕获剂的方法对薄膜的光催化机理进行了探索。结果表明:最佳工艺制备的Ag_2S/Ag_3PO_4/Ni是由均匀的球形纳米颗粒构成的薄膜,其光催化活性明显优于纯Ag_3PO_4/Ni薄膜和纯Ag_2S/Ni薄膜,且在保持薄膜光催化活性基本不变的前提下可循环使用6次。提出了可见光下Ag_2S/Ag_3PO_4/Ni复合薄膜光催化降解罗丹明B的反应机理。     

Enhanced photocatalytic activities of ZnO thin films: a comparative study of hybrid semiconductor nanomaterials

Nanostructure single ZnO, SnO₂, In₂O₃ and composite ZnO/SnO₂, ZnO/In₂O₃ and ZnO/SnO₂/In₂O₃ films were prepared using sol?Cgel method. The obtained composite films were characterized with X-ray diffraction (XRD), scanning electron microscopy (SEM), and UV?CVis spectroscopy. The photocatalytic activities of composite films were investigated using phenol (P), 2,4-dichlorophenol (2,4-DCP), 4-chlorophenol (4-CP) and 4-aminophenol (4-AP) as a model organic compounds under UV light irradiation. Hybrid semiconductor thin films showed a higher photocatalytic activity than single component ZnO, SnO₂ and In₂O₃ films. The substituted phenols degrade faster than phenol. The ease of degradation of phenols is different for each catalyst and the order of catalytic efficiency is also different for each phenol. The use of multiple components offered a higher control of their properties by varying the composition of the materials and related parameters such as morphology and interface. It was also found that the photocatalytic degradation of phenolic compounds on the composite films and single films followed pseudo-first order kinetics.     

Ag2S/Ag3PO4/Ni复合薄膜的制备及其光催化性能

采用电化学方法制备Ag₂S/Ag₃PO₄/Ni复合薄膜,以扫描电子显微镜（SEM）、X射线衍射（XRD）、紫外-可见漫反射光谱（UV-Vis DRS）对薄膜的表面形貌、晶相结构、光谱特性及能带结构进行了表征,以罗丹明B为模拟污染物对薄膜的光催化活性和稳定性进行了测定,采用向溶液中加入活性物种捕获剂的方法对薄膜的光催化机理进行了探索。结果表明：最佳工艺制备的Ag₂S/Ag₃PO₄/Ni是由均匀的球形纳米颗粒构成的薄膜,其光催化活性明显优于纯Ag₃PO₄/Ni薄膜和纯Ag₂S/Ni薄膜,且在保持薄膜光催化活性基本不变的前提下可循环使用6次。提出了可见光下Ag₂S/Ag₃PO₄/Ni复合薄膜光催化降解罗丹明B的反应机理。     

Synthesis and characterization of polyaniline/silicon dioxide composites and preparation of conductive films

The focus of this study was to synthesize the inherently conductive polymer polyaniline using an optimized process to prepare polyaniline/silicon dioxide (PANI/SiO₂) composites by in situ polymerization and ex situ solution mixing. PANI and PANI/SiO₂ composite films were prepared by drop‐by‐drop and spin coating methods. The electrical conductivities of HCl doped PANI film and PANI/SiO₂ composite films were measured according to the standard four‐point‐probe technique. The composite films exhibited an increase in electrical conductivity over neat PANI. PANI and PANI/SiO₂ composites were also investigated by spectroscopic methods including UV‐Vis, FT‐IR, and Photoluminescence. UV‐Vis and FT‐IR studies showed that SiO₂ particles affect the quinoid units along the polymer backbone and indicate strong interactions between the SiO₂ particles and the quinoidal sites of PANI (doping effect). The photoluminescence properties of PANI and PANI/SiO₂ composites were studied and the PANI/SiO₂ composites showed increased intensity as compared to neat PANI. The increase of conductivity of PANI/SiO₂ composite may be partially due to the doping or impurity effect of SiO₂ where the silicon dioxides compete with chloride ions. The morphology of particles and films were examined by a scanning electron microscope (SEM). SEM measurements indicated that the SiO₂ were well dispersed and isolated in composite films. Copyright © 2009 John Wiley & Sons, Ltd.