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TEM
Kinds of TEM Terms modified by TEM Selected AbstractsSynthesis and properties of ,-Fe2O3 nanorodsCRYSTAL RESEARCH AND TECHNOLOGY, Issue 9 2010R. Ramesh Abstract We report synthesis of ,-Fe2O3 (hematite) nanorods by reverse micelles method using cetyltrimethyl ammonium bromide (CTAB) as surfactant and calcined at 300 °C. The calcined ,-Fe2O3 nanorods were characterized by X-ray diffraction (XRD), high-resolution scanning electron microscopy (HRSEM), transmission electron microscopy (TEM), energy dispersive spectrometer (EDS), fourier transform infrared spectroscopy (FTIR) and vibrating sample magnetometer (VSM). The result showed that the ,-Fe2O3 nanorods were hexagonal structure. The nanorods have diameter of 30-50 nm and length of 120-150 nm. The weak ferromagnetic behavior was observed with saturation magnetization = 0.6 emu/g, coercive force = 25 Oe and remanant magnetization = 0.03 emu/g. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Preparation of shuttle-like Sb2S3 nanorod-bundles via a solvothermal approach under alkaline conditionCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2010Ling Zhang Abstract Uniform shuttle-like Sb2S3 nanorod-bundles were synthesized via a polyvinylpyrrolidone (PVP) assisted solvothermal approach under alkaline condition, using antimony chloride (SbCl3) and thiourea (CH4N2S, Tu) as the starting materials in ethanol. The phase structure, composition and morphology of the product were characterized by means of X-ray diffraction (XRD), energy dispersive X-ray spectrometry (EDS), transmission electron microscopy (TEM), and high-resolution transmission electron microscopy (HRTEM). XRD and EDS results confirm that the synthesized Sb2S3 nanorod-bundles have an orthorhombic structure and an atomic ratio of 3:2 for S:Sb. TEM and HRTEM results show that the shuttle-like Sb2S3 bundles are composed of nanorods with a size distribution of 20-40 nm and growing along c-axis. Furthermore, experiments under different reaction conditions were carried out and the mechanism for the growth of nanorod-bundles was discussed (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis and morphology of nanosized zeolite LCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2010S. Sadegh Hassani Abstract AFM is a powerful tool for imaging nanoscale surface features; it provides two and three dimensional crystal structure images and other information about actual surface of zeolite crystallites. In this paper, nanosized zeolite L is synthesized in different crystallization times and a study of crystal growth of zeolite L is reported using atomic force microscopy (AFM). X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) techniques are used for characterization of the as synthesized samples. TEM and two-dimensional AFM images indicate that the zeolite particles are in a nano-range and they have hexagonal structure. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Hydrothermal synthesis of nano-crystalline BaMoO4 under mild conditions using simple additiveCRYSTAL RESEARCH AND TECHNOLOGY, Issue 2 2010Guangru Tian Abstract Large-scale high-quality BaMoO4 nanocrystals have been synthesized in aqueous solutions under mild conditions with citrate as a simple additive. The crystals have bone-like, spindle-like and wheatear-like morphologies assembled from nanoparticles, nanofibers and have been characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) techniques. The results showed that experimental parameters had great influences on the shape evolution of products. The adjustment of these parameters such as room temperature stirring time, reaction temperature and reaction time of hydrothermal reaction, can lead to obvious morphology changes of products, and the growth mechanism has been proposed. Room-temperature photoluminescence indicated that the as-prepared BaMoO4 nanocrystals had a strong blue emission peak at 481.5 nm. This facile route could be employed to synthesize more promising nanomaterials with interesting self-assembly structures. (© 2010 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Oxide layer dissolution in Si/SiOx/Si wafer bonded structuresCRYSTAL RESEARCH AND TECHNOLOGY, Issue 10 2009N. Zakharov Abstract The evolution of the interfaces of hydrophilic-bonded Si wafers and the corresponding low-angle twist boundary have been analysed in relation to thermal annealing and their relative crystallographic orientation. Two orientation relationships were investigated: Si<001>/Si<001> and Si<001>/Si<110>, where the interfaces are seperated by thin native SiO2 layers. The interfaces were analysed by TEM and STEM/EELS. It is found that the decomposition rate of the intermediate oxide layer and the formation of a Si(Si bonded interface depend very much on the lattice mismatch and on the twist angle. The velocity of the dissolution of the thin oxide layers and the formation of Si(Si bonds at the bonding interface depend on the orientation relations of the corresponding wafers. The processes of interface fusion and the dissolution of oxide layer are discussed. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Solvothermal production of CdS nanorods using polyvinylpyrrolidone as a templateCRYSTAL RESEARCH AND TECHNOLOGY, Issue 8 2009Titipun Thongtem Abstract CdS nanorods were solvothermally produced using Cd(NO3)2 and S powder in ethylenediamine containing different amounts of polyvinylpyrrolidone (PVP). The phase with hexagonal structure was detected using X-ray diffraction (XRD) and selected area electron diffraction (SAED). Their SAED patterns were in accordance with those of the simulations. Scanning and transmission electron microscopies (SEM and TEM) revealed the presence of CdS nanorods with their lengths influenced by different amounts of PVP. The nanorods were also characterized using high resolution TEM (HRTEM). They grew in the [001] direction normal to the (002) parallel crystallographic planes composing the nanorods. Raman spectra showed the 1LO (first harmonic) and 2LO (second harmonic) modes at the same wavenumbers although the products were produced under different conditions. (© 2009 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Synthesis and characterization of fine lithium niobate powders by sol- gel methodCRYSTAL RESEARCH AND TECHNOLOGY, Issue 4 2007L. H. Wang Abstract Lithium niobate (LN) nanocrystal powders were prepared by low-temperature sol-gel method. Dihydrate lithium acetate as lithium source, and niobium chloride as niobium source were used as starting materials. The gel and powders were characterized by thermogravimetry and differential scanning calorimetry (TG/DSC), X-ray diffraction (XRD), transmission electronmicroscopy (TEM) and Fourier transform infrared (FTIR) spectra. The results show that when the gel was heat-treated at 600°C, the fine LN nanocrystals with the size of 40-60 nm were obtained, and the size of the powders become larger with the heat-treated temperature increasing. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Solvothermal growth of single-crystal hexagonal prismatic SrCO3 microrodsCRYSTAL RESEARCH AND TECHNOLOGY, Issue 3 2007Fanglin Du Abstract Single-crystal hexagonal prism SrCO3 microrods have been prepared by a simple solvothermal route. The effects of the reaction time, the content of 1,2-propanediol and the reactants mass on the products have been investigated, respectively. The as-synthesized microrods were characterized by X-ray powder diffraction (XRD), field-emission scanning electron microscopy (FE-SEM) and transmission electron microscopy (TEM). The results reveal that the products have uniform shape and excellent monodispersity. (© 2007 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim) [source] Centrioles are freed from cilia by severing prior to mitosis,CYTOSKELETON, Issue 7 2010Jeremy D.K. Parker Abstract Cilia are necessary for normal tissue development and homeostasis and are generally present during interphase, but not in mitosis. The precise mechanism of premitotic ciliary loss has been controversial, with data supporting either sequential disassembly through the transition zone or, alternatively, a severing event at the base of the cilia. Here we show by live cell imaging and immunofluoresence microscopy that resorbing flagella of Chlamydomonas leave remnants associated with the mother cell wall. We postulated that the remnants are the product of severing of doublet microtubules between the basal bodies and the flagellar transition zone, thereby freeing the centrioles to participate in spindle organization. We show via TEM that flagellar remnants are indeed flagellar transition zones encased in vesicles derived from the flagellar membrane. This transition zone vesicle can be lodged within the cell wall or it can be expelled into the environment. This process is observable in Chlamydomonas, first because the released flagellar remnants can remain associated with the cell by virtue of attachments to the cell wall, and second because the Chlamydomonas transition zone is particularly rich with electron-dense structure. However, release of basal bodies for spindle-associated function is likely to be conserved among the eukaryotes. © 2010 Wiley-Liss, Inc. [source] A New Amperometric Hydrazine Sensor Based on Prussian Blue/Single-walled Carbon Nanotube NanocompositesELECTROANALYSIS, Issue 16 2010Cong Wang Abstract A slow reaction process has been successfully used to synthesize Prussian blue/single-walled carbon nanotubes (PB/SWNTs) nanocomposites. Electrochemical and surface characterization by cyclic voltammetry (CV), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis absorption spectroscopy, Fourier transform infrared (FTIR) spectroscopy and X-ray diffraction (XRD) confirmed the presence of PB nanocrystallites on SWNTs. PB/SWNTs modified glassy carbon electrode (GCE) exhibits efficient electron transfer ability and high electrochemical response towards hydrazine. The fabricated hydrazine sensor showed a wide linear range of 2.0×10,6,6.0×10,3,M with a response time less than 4,s and a detection limit of 0.5,,M. PB/SWNTs modified electrochemical sensors are promising candidates for cost-effective in the hydrazine assays. [source] Electrocatalytic Oxidation of Glucose by the Glucose Oxidase Immobilized in Graphene-Au-Nafion BiocompositeELECTROANALYSIS, Issue 3 2010Kangfu Zhou Abstract Graphene was successfully prepared and well separated to individual sheets by introducing SO3,. XRD and TEM were employed to characterize the graphene. UV-visible absorption spectra indicated that glucose oxidase (GOx) could keep bioactivity well in the graphene-Au biocomposite. To construct a novel glucose biosensor, graphene, Au and GOx were co-immobilized in Nafion to further modify a glassy carbon electrode (GCE). Electrochemical measurements were carried out to investigate the catalytic performance of the proposed biosensor. Cyclic voltammograms (CV) showed the biosensor had a typical catalytic oxidation response to glucose. At the applied potential +0.4,V, the biosensor responded rapidly upon the addition of glucose and reached the steady state current in 5,s, with the present of hydroquinone. The linear range is from 15,,M to 5.8,mM, with a detection limit 5,,M (based on the S/N=3). The Michaelis-Menten constant was calculated to be 4.4,mM according to Lineweaver,Burk equation. In addition, the biosensor exhibits good reproducibility and long-term stability. Such impressive properties could be ascribed to the synergistic effect of graphene-Au integration and good biocompatibility of the hybrid material. [source] Electrochemical Properties of Ordered Mesoporous Carbon Film Adsorbed onto a Self-Assembled Alkanethiol Monolayer on Gold ElectrodeELECTROANALYSIS, Issue 2 2009Dan Zheng Abstract A stable ordered mesoporous carbon (OMC) film electrode was successfully constructed by adsorbing OMC onto a self-assembled monolayer (SAM) of C18H37SH chemisorbed on the Au electrode. Transmission electron microscopy (TEM), atomic force microscopy (AFM), and electrochemical methods were used to characterize the properties of the OMC film electrode. The adsorbed OMC can restore the heterogeneous electron transfer almost totally blocked by the alkanethiol monolayer. Nyquist plots show a sharply decrease of the charge transfer resistance (Rct) of the Fe(CN) couple at the OMC film electrode. Furthermore, the OMC film electrode is found to possess a significantly reduced interfacial capacitance and largely enhanced current response of hydrogen peroxide. This novel approach to the fabrication of stable OMC film electrode with excellent electrochemical properties is believed to be very attractive for electrochemical studies and electroanalytical applications. [source] Synthesis and Characterization of MWNTs/Au NPs/HS(CH2)6Fc Nanocomposite: Application to Electrochemical Determination of Ascorbic AcidELECTROANALYSIS, Issue 16 2008Jian-Ding Qiu Abstract In this article, a detailed electrochemical study of a novel 6-ferrocenylhexanethiol (HS(CH2)6Fc) self-assembled multiwalled carbon nanotubes-Au nanoparticles (MWNTs/Au NPs) composite film was demonstrated. MWNTs/Au NPs were prepared by one-step in situ synthesis using linear polyethyleneimine (PEI) as bifunctionalizing agent. HS(CH2)6Fc, which acted as the redox mediator, was self-assembled to MWNTs/Au NPs via Au-S bond. Transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDX), Fourier transformed infrared absorption spectroscopy (FT-IR), UV-visible absorption spectroscopy, and cyclic voltammetry were used to characterize the properties of the MWNTs/Au NPs/HS(CH2)6Fc nanocomposite. The preparation of the nanocomposite was very simple and effectively prevented the leakage of the HS(CH2)6Fc mediator during measurements. The electrooxidation of AA could be catalyzed by Fc/Fc+ couple as a mediator and had a higher electrochemical response due to the unique performance of MWNTs/Au NPs. The nanocomposite modified electrode exhibited excellent catalytic efficiency, high sensitivity, good stability, fast response (within 3,s) and low detection limit toward the oxidation of AA at a lower potential. [source] On-Off PVC Membrane Based Potentiometric Immunosensor for Label-Free Detection of Alpha-FetoproteinELECTROANALYSIS, Issue 11 2007Lu Zhou Abstract A poly(vinylchloride) (PVC) membrane based potentiometric immunosensor for the direct detection of alpha-fetoprotein (AFP) has been developed. First, Au colloid particle was chemisorbed upon amino groups of o -phenylenediamine, which were dissolved in plasticized PVC membrane. Then alpha-fetoprotein antibody (anti-AFP) was immobilized upon the surface of the Au colloid particle to prepare a potentiometric AFP immunosensor. The Au colloid particle modified PVC membrane was characterized by digital photo and transmission electron microscope (TEM). The immunosensor exhibited fast potentiometric response (,4,min) and showed specific response to AFP in the range of 4.9 to 158.5,ng/mL with a correlation coefficient of 0.9971 and a detection limit of 1.6,ng/mL. The factors influencing the performance of the immunosensor were also studied in detail. Moreover, the proposed method is economical and efficient as well as potentially attractive for clinical immunoassays. [source] Open-tubular capillary electrochromatography using a capillary coated with octadecylamine-capped gold nanoparticlesELECTROPHORESIS, Issue 4 2008Qishu Qu Dr. Abstract Octadecylamine-capped gold nanoparticles (ODA-Au-NPs) were prepared and characterized by using UV,Vis adsorption spectrum, transmission electron chromatography (TEM), SEM, and FT-IR. A simple but robust hydrophobic coating was easily developed by flushing a capillary with a solution of ODA-Au-NPs, because the positive charges were carried by the nanoparticles which strongly adsorb to the negatively charged inner surface of a fused-silica capillary via electrostatic and hydrophobic interactions. The chromatographic characteristics of the coated capillary was investigated by varying the experimental parameters such as buffer pH, buffer concentration, and percentage of organic modifier in the mobile phase. The results show that (i) resolution between thiourea and naphthalene is almost the same when comparing the electrochromatograms obtained using pH,7 buffer as mobile phase after and before the capillary column was operated using pH,11 and 3 mobile phase; (ii) no significant changes in retention time and deterioration in peak efficiency were found after 60,runs of test aromatic mixtures; and (iii) column efficiency up to 189,000 theoretical plates/meter for testosterone was obtained. All of the results indicated that the coating could act as a stable stationary phase for open tubular CEC as well as for bioanalysis. [source] Study on the enhancement of Ru(bpy)32+ electrochemiluminescence by nanogold and its application for pentoxyverine detectionELECTROPHORESIS, Issue 23 2005Yingju Liu Abstract In this work, CE separation with end-column Ru(bpy)32+ ECL detection for the quantitative determination of pentoxyverine was firstly performed. The experimental conditions, such as the applied potential, injection voltage, injection time, and the pH of separation buffer, were discussed in detail. Gold nanoparticles were found to enhance the ECL intensity at an appropriate volume ratio of nanogold with Ru(bpy)32+ but without changing their nanoproperties proved by transmission electron microscopy (TEM) and UV-vis spectra. The detection limits with or without nanogold were 6,nM and 0.6,,M, respectively. Successful separation of pentoxyverine, chlorpheniramine, and lidocaine was achieved. This method was also applied to monitor drug binding with HSA, and the binding constant for pentoxyverine was estimated as 1.8×103/M. [source] Separation and recovery of intact gold-virus complex by agarose electrophoresis and electroelution: Application to the purification of cowpea mosaic virus and colloidal gold complexELECTROPHORESIS, Issue 17 2004Carissa M. Soto Abstract Colloidal gold has been coupled to a mutant cowpea mosaic virus (CPMV), which contains 60 cysteine residues on the surface. A purification process was developed to separate the gold-containing viral nanoblocks (VNBs) from the free gold. Agarose electrophoresis was utilized to separate the mixture followed by electroelution of the desired sample to recover the intact virus. Mobility of Au-VNB and free colloidal gold was facilitated by the addition of thioctic acid (TA). 30% of the gold-containing virus was recovered after electroelution as determined by absorbance measurements. Histogram analysis of transmission electron microscopy (TEM) images demonstrated the efficient separation of gold-containing virus from free gold. TEM and scanning electron microscopy (SEM) images indicated that the virus was recovered intact. Monodisperse spherical particles of nominal size of 45 nm were observed under SEM. [source] Equine laminitis: Ultrastructural lesions detected in ponies following hyperinsulinaemiaEQUINE VETERINARY JOURNAL, Issue 7 2009A. R. NOURIAN Summary Reasons for performing study: Anatomical changes in the hoof lamellar tissue induced by prolonged hyperinsulinaemia have not been described previously. Analysis of the induced lesions may promote understanding of hyperinsulinaemic laminitis pathogenesis and produce clinical benefit. Objectives: To use light and transmission electron microscopy (TEM) to document hoof lamellar lesions in ponies clinically lame after prolonged hyperinsulinaemia. Methods: Nine clinically normal, mature ponies were allocated randomly to either a treatment group (n = 5) or control group (n = 4). The treatment group received insulin via a modified, prolonged euglycaemic hyperinsulinaemic clamp technique (EHCT) and were subjected to euthanasia when clinical signs of Obel grade II laminitis occurred. The control group was sham treated with an equivalent volume of 0.9% saline and killed at 72 h. Lamellar tissues of the right front feet were harvested and processed for TEM. Results: Lamellae from insulin treated ponies were attenuated and elongated with many epidermal basal cells (EBC) in mitosis. Unlike carbohydrate induced laminitis in horses there was no global separation at the lamellar dermal/epidermal interface among ponies. Sporadic EBC basement membrane (BM) separation was associated with the proximity of infiltrating leucocytes. In 2 ponies, the lamellar BM was thickened. The number of hemidesmosomes/,m of BM was decreased in all insulin treated ponies. Conclusions: Prolonged hyperinsulinaemia causes unique lamellar lesions normally characteristic of acute and chronic laminitis. Lamellar proliferation may be an insulin effect through its mitogenic pathway. Aberrant lamellar mitosis may lengthen and weaken the lamellar, distal phalanx attachment apparatus and contribute to the clinical signs that developed. Potential relevance: The study shows that insulin alone, in higher than normal circulating concentrations, induces profound, changes in lamellar anatomy. Medical control of insulin resistance and hyperinsulinaemia may ameliorate lesions and produce clinical benefit. [source] Equine laminitis: glucose deprivation and MMP activation induce dermo-epidermal separation in vitroEQUINE VETERINARY JOURNAL, Issue 3 2004K. R. French Summary Reasons for performing study: Acute laminitis is characterised by hoof lamellar dermal-epidermal separation at the basement membrane (BM) zone. Hoof lamellar explants cultured in vitro can also be made to separate at the basement membrane zone and investigating how this occurs may give insight into the poorly understood pathophysiology of laminitis. Objectives: To investigate why glucose deprivation and metalloproteinase (MMP) activation in cultured lamellar explants leads to dermo-epidermal separation. Methods: Explants, cultured without glucose or with the MMP activator p -amino-phenol-mercuric acetate (APMA), were subjected to tension and processed for transmission electron microscopy (TEM). Results: Without glucose, or with APMA, explants under tension separated at the dermo-epidermal junction. This in vitro separation occurred via 2 different ultrastructural processes. Lack of glucose reduced hemidesmosomes (HDs) numbers until they disappeared and the basal cell cytoskeleton collapsed. Anchoring filaments (AFs), connecting the basal cell plasmalemma to the BM, were unaffected although they failed under tension. APMA activation of constituent lamellar MMPs did not affect HDs but caused AFs to disappear, also leading to dermo-epidermal separation under tension. Conclusions: Natural laminitis may occur in situations where glucose uptake by lamellar basal cells is compromised (e.g. equine Cushing's disease, obesity, hyperlipaemia, ischaemia and septicaemia) or when lamellar MMPs are activated (alimentary carbohydrate overload). Potential relevance: Therapies designed to facilitate peripheral glucose uptake and inhibit lamellar MMP activation may prevent or ameliorate laminitis. [source] Treatment emergent mania responding to valproate in a Chinese female adolescent population with eating disorders: A case seriesEUROPEAN EATING DISORDERS REVIEW, Issue 6 2008Phern Chern Tor Abstract Eating disorders are commonly associated with depressive symptoms. In an adolescent and binge eating population fluoxetine is commonly used to treat co-morbid depression associated with eating disorders. In some patients this may precipitate treatment emergent mania (TEM). Risk factors in the adolescent population include being older, female, having a longer duration of illness, more previous mood episodes, a higher prevalence of subclinical hypothyroidism, early-onset anxiety and recent exposure to a mood-elevating agent. Diagnosis and management of these co-morbid conditions is challenging due to the overlapping symptomatology and the adverse effects of both conditions complicating pharmacological management. This is illustrated with three cases in a Chinese female adolescent population that experienced TEM while on fluoxetine and responded to valproate. Copyright © 2008 John Wiley & Sons, Ltd and Eating Disorders Association. [source] Highly Crystalline, Idiomorphic Na2Ti6O13 Whiskers Grown from a NaCl Flux at a Relatively Low TemperatureEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 19 2010Katsuya Teshima Abstract Well-developed, highly crystalline Na2Ti6O13 whiskers were successfully grown by cooling a NaCl flux at a relatively low temperature of 700 °C. The obtained Na2Ti6O13 whiskers were colorless and transparent. The whiskers grown at 700 °C were single phase and exhibit the lowest sizes of up to about 3.5 ,m,×,0.1 ,m. From the results of SEM, XRD, and TEM, it was confirmed that the Na2Ti6O13 whiskers have very good crystallinity and elongated in the [lang]010[rang] directions. Furthermore, the whiskers exhibited good photocatalytic activity under ultraviolet light irradiation. It is reasonable to suppose that NaCl can be adequately used to synthesize high quality and well-developed titanate whiskers in an environmentally friendly process of crystal growth. [source] Microporous Silica Hollow Microspheres and Hollow Worm-Like Materials: A Simple Method for Their Synthesis and Their Application in Controlled ReleaseEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 6 2010Mingwei Zhao Abstract Hollow silica microspheres and hollow worm-like materials were synthesized by using a simple method with the aid of 1-dodecyl-3-methylimidazolium bromide (C12mimBr). Hollow silica microspheres were initially produced by utilizing the combination of evaporation and an emulsion template. At a longer mixing time, the microspheres fused to form hollow worm-like silica materials due to the fusion of the emulsion templates. The resultant silica materials were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), and nitrogen adsorption/desorption. Both the hollow silica microspheres and the hollow worm-like materials are microporous. On the basis of experimental observations and the resulting products, a plausible formation mechanism is proposed. Preliminary tests demonstrate that the hollow silica microspheres and worm-like materials are capable of being loaded with Rhodamine B and releasing it, thus showing a great potential in controlled delivery applications. [source] Facile and Reproducible Synthesis of Nanostructured Colloidal ZnO Nanoparticles from Zinc Acetylacetonate: Effect of Experimental Parameters and Mechanistic InvestigationsEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 33 2009Alessia Famengo Abstract A facile and reproducible route to nanostructured colloidal ZnO nanoparticles was developed by controlled hydrolysis and condensation of zinc acetylacetonate in alkaline conditions. By reaction of an ethanolic solution of Zn(acac)2 with NaOH in a 1:2 molar ratio, after reflux, ZnO spherical nanoparticles were obtained that displayed a homogeneous size distribution; particle diameters ranged from 6 to 10 nm, as evidenced by transmission electron microscopy (TEM) analysis. The same reaction was carried out also in water, glycerol and 1,2-propanediol, to investigate the effect of the solvent viscosity and dielectric constant on the final features of the obtained material. Irrespective of the nature of the solvent, X-ray diffraction (XRD) analysis shows the formation ofhexagonal ZnO, whereas the presence of residual unreacted Zn(acac)2 could be ruled out. Indeed, different particle sizes and very different morphologies were obtained. Also the reflux step was shown to be a key factor in avoiding the fast precipitation of a floc and achieving a pure compound, which was isolated and thoroughly characterised. The composition of the obtained ZnO was determined by elemental analysis, X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA), showing the formation of pure ZnO. IR spectroscopy evidenced the presence of adsorbed organic ligands on the colloid surfaces. Diffuse reflectance infrared Fourier transform spectroscopy (DRIFT) revealed the presence of medium- to high-strength acidic sites on the ZnO surface. To gain a deeper insight into the formation mechanisms of these nanostructures, time-resolved UV/Vis and XAS studies were performed on the ethanol solution used for the synthesis of the oxide and also on the solid specimen, obtained after the refluxing step. No remarkable changes could be evidenced in the solution after the addition of an understoichiometric amount of NaOH, but the growth of the ZnO nanoparticles could be followed by UV/Vis spectra. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Controllable Synthesis of Shuttle-Shaped Ceria and Its Catalytic Properties for CO OxidationEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 26 2009Chunwen Sun Abstract Shuttle-shaped ceria was obtained in a high yield via a surfactant octadecylamine and urea assisted solvothermal process. The crystalline structure and morphology were characterized with powder X-ray diffraction (XRD), scanning electron microscope (SEM), and transmission electron microscope (TEM). Preliminary catalytic measurement shows that the shuttle-shaped CeO2 exhibits an enhanced activity for CO oxidation, which may be attributed to its higher porosity and more oxygen vacancies.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Ultrasound-Assisted Synthesis of CuO Nanorods in a Neat Room-Temperature Ionic LiquidEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 19 2009Tarek Alammar Abstract CuO nanorods were prepared via ultrasound-assisted synthesis in the room temperature ionic liquid (RTIL) 1-butyl-3-methylimidazoliumbis(trifluoromethylsulfonyl)imide [C4mim][Tf2N] as a reaction medium. The structure and morphology of CuO nanorods were characterized with X-ray powder diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), vibrational and UV/Vis absorption spectroscopy. The synthesized CuO nanocrystals are of rod like shape with lengths from 30 to 100 nm and diameters of about 10 nm. Quantum size effects were observed as the bandgap of the CuO nanorods was determined to 2.41 eV from UV/Vis absorption measurements, which is significantly larger than the bulk value. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Synthesis and Characterization of Single-Crystalline Lanthanum Fluoride with a Ring-Like NanostructureEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 16 2009Yang Tian Abstract LaF3 ring-like nanostructures with a diameter of less than 2 ,m have been fabricated by a facile, effective, and environmentally friendly molten salt synthesis route in which NaNO3 and KNO3 (2:1 molar ratio) act as reaction media and the rare-earth nitrate and NaF as precursor. X-ray diffraction, TEM, HR-TEM, energy dispersive X-ray spectroscopy, and photoluminescence spectroscopy are all used to characterize the as-prepared samples. Experiments peformed with different reaction times indicate that a central-etching of the plates from the inner part towards the edge during nanocrystal growth plays a key role in the formation of LaF3 nanorings since no other templates/surfactants are present in our system. Additionally, the luminescence properties of LaF3 nanorings doped with Eu3+ cation have been investigated andcompared with those of bulk materials and nanoparticles with a size of approximately 50 nm. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] Sonoelectrochemical Synthesis of Metallic Aluminum NanoparticlesEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 14 2009Chinnathambi Mahendiran Abstract In this paper, we report for the first time on the room-temperature preparation of metallic aluminum nanoparticles by the pulsed sonoelectrochemical method. The prepared nanoparticles were characterized by X-ray diffraction (XRD), high-resolution scanning electron microscopy, transmission electron microscopy (TEM), and high-resolution transmission electron microscopy. TEM analysis shows that the prepared aluminum nanoparticles range from 10 to 20 nm in size. The XRD pattern confirms the formation of metallic aluminum nanoparticles. The results show that the sonoelectrochemical technique is a promising method for the fabrication of air-sensitive metallic nanoparticles that have a high, negative reduction potential.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2009) [source] InN@SiO2 Nanomaterials as New Blue Light EmittersEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 23 2008Prabhakaran Munusamy Abstract In this article we report blue photoluminescence (, 450 nm) from InN@SiO2 nanomaterials. The InN@SiO2 nanomaterials were prepared by a simple precipitation reaction followed by a solid-state reaction. Various control experiments demonstrate that the interface between the InN and SiO2 seems to play a crucial role in the origin of the blue emission from the InN@SiO2 nanomaterial. The InN@SiO2 nanomaterial was characterized by using analytical methods such as TEM, XRD, Raman, XPS, and photoluminescence spectroscopy, which confirmed the existence of InN on SiO2 with a small excess of nitrogen relative to indium.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] Controlled Synthesis of Cobalt Flowerlike Architectures by a Facile Hydrothermal RouteEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 17 2008Ya-jing Zhang Abstract Cobalt flowerlike architectures composed of hexagonal nanoplatelets have been synthesized by a simple hydrothermal reduction method. The architectures are fabricated by the reaction of CoCl2 with NaOH at 140,180 °C in the presence of sodium dodecyl benzenesulfonate (SDBS), with NaH2PO2·H2O as reducing agent. The diameters of the flowers range from 8 to 10 ,m, and the average thickness of the hexagonal sheets is about 100 nm. Higher reaction temperatures and the proper concentration of sodium hydroxide (NaOH) are key requirements for the fabrication of the flowerlike architectures. A growth mechanism for these architectures is proposed on the basis of the characterization by X-ray diffraction, scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The magnetic hysteresis loops at 5 K and 295 K of the cobalt flowerlike architectures show ferromagnetic characteristics with coercivities of 371 Oe and 197 Oe, respectively. Our work may shed light on the designed fabrication of complex 3D architectures of other materials.(© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] Microwave-Assisted Hydrothermal Synthesis of Structurally and Morphologically Controlled Sodium Niobates by Using Niobic Acid as a PrecursorEUROPEAN JOURNAL OF INORGANIC CHEMISTRY, Issue 8 2008Amauri J. Paula Abstract There are many advantages to using a microwave as a source of heat in hydrothermal reactions. Because it is a quick and homogeneous way to crystallize ceramic powders, it was used in this work for the production of antiferroelectric sodium niobate (NaNbO3) in a cubic-like form and its intermediary phase, disodium diniobate hydrate (Na2Nb2O6.H2O), with a fiber morphology. The syntheses were carried out by treating niobic acid (Nb2O5·nH2O) with NaOH. By changing the reaction time and the concentration of the reactants, particles with different structures and different morphologies could be obtained. The structural evolution of the products of this reaction was elucidated on the basis of the arrangement of the NbO6 octahedral units. Conclusive results were obtained with morphological and structural characterizations through XRD, TEM, MEV, and NMR and Raman spectroscopy. (© Wiley-VCH Verlag GmbH & Co. KGaA, 69451 Weinheim, Germany, 2008) [source] | ||||||||||||||||||||||||||||||||||||||||