Stoichiometry of alloy nanoparticles from laser ablation of PtIr in acetone and their electrophoretic deposition on PtIr electrodes

Charged Pt-Ir alloy nanoparticles are generated through femtosecond laser ablation of a Pt?Ir target in acetone without using chemical precursors or stabilizing agents. Preservation of the target's stoichiometry in the colloidal nanoparticles is confirmed by transmission electron microscopy (TEM)-energy-dispersive x-ray spectroscopy (EDX), high angle annular dark field (HAADF) scanning transmission electron microscopy (STEM)-EDX elemental maps, high resolution TEM and selected area electron diffraction (SAED) measurements. Results are discussed with reference to thermophysical properties and the phase diagram. The nanoparticles show a lognormal size distribution with a mean Feret particle size of 26 nm. The zeta potential of -45 mV indicates high stability of the colloid with a hydrodynamic diameter of 63 nm. The charge of the particles enables electrophoretic deposition of nanoparticles, creating nanoscale roughness on three-dimensional PtIr neural electrodes within a minute. In contrast to coating with Pt or Ir oxides, this method allows modification of the surface roughness without changing the chemical composition of PtIr.     

Study of Size Distribution in Nanostructured Se<Subscript>58</Subscript>Ge<Subscript>39</Subscript>Pb<Subscript>3</Subscript> Glass Using Various Characterization Methods

The present paper aims at the study of size distribution of particles in nanostructured Se₅₈Ge₃₉Pb₃ glass using X-ray diffraction (XRD), Transmission electron microscopy (TEM) and UV–visible spectrophotometer. The thin film sample has been prepared using melt quenching technique and inert gas consolidation method. The particle size distribution obtained from XRD and UV–Vis spectrophotometer shows more uncertainty than the results obtained from TEM measurements. The absorption spectra recorded on UV–Vis spectrophotometer is employed to get band gap values corresponding to different size distribution in sample. Further, it is concluded that TEM is the best measurement technique for size distribution as it has less uncertainty in the obtained results.     

Real time and in situ control of the gap size of nanoelectrodes for molecular devices

Molecular electronics is often limited by the lack of a simple method to fabricate nanoelectrodes with controlled gap size. This is partly attributed to the lack of a real time characterization in the fabrication. Here, we report a new method based on an electron induced deposition process operated in scanning electron microscopy that realizes in situ and real time characterization in the nanoelectrode fabrication; thus the gap size can be controlled easily and precisely. It is a clean and nondestructive process for carbon nanotube (CNT) electrodes. The mechanism is detailed. The nanoelectrodes have a pi-conjugated surface due to the deposition of sp(2)-rich amorphous carbon. As an application, DNA molecules are assembled between the CNT electrodes by pi-stacking interaction for current-voltage measurement. Our result provides a feasible route to prepare nanoelectrodes with controlled gap size, and it will be valuable for current efforts in molecular electronics and nanoelectronics.     

Quantum confinement effect of CdS nanoparticles dispersed within PVP/PVA nanocomposites

Nanocomposite films of CdS nanoparticles within PVP/PVA blend were prepared. The prepared films were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy, Ultraviolet–visible spectroscopy (UV–vis), transmission electron microscopy (TEM) and photoluminescence (PL) spectra. The amount of Cd⁺ used strongly influenced the size of the CdS nanoparticles, which was confirmed by XRD, UV–vis absorption spectra, PL emission spectra and TEM images. Smaller sized CdS nanoparticles were formed in higher content of cadmium. The results of XRD indicate that CdS nanoparticles were formed with hexagonal phase in the polymeric matrix. PL and UV–vis spectra reveal that nanocomposite films shows quantum confinement effect. Optical band gap and particle size were calculated and is in agreement with the results obtained from TEM data. The direct energy band gap was increased up to 2.86 eV.     

Structural, optical and electrical characterization of selenium sulphide nanostructured thin film

Thin film of selenium sulphide (Se₇₅S₂₅) has been prepared using inert-gas consolidation (IGC) method and micro-structural, optical and electrical measurements were carried out on the film. Scanning electron microscopy (SEM) studies show that the deposited film is well adherent and grains are uniformly distributed over the surface of the substrate. X-ray diffraction (XRD) analysis shows that the film is polycrystalline nature with single phase and crystallizes in the orthorhombic structure. The field emission transmission electron microscope (FETEM) revealed the uniform dispersion and an average particle size of 20 nm. Analysis of the optical absorption data indicates that the optical band gap E_opt of this film obeys Tauc's relation for the allowed non-direct transition with energy gap is 2.48 eV. Electrical conduction measurements also show the presence of two distinct phases of the materials and characteristic changes in transport properties due to the nanosize of the materials.     

Determination of the size of water-soluble nanoparticles and quantum dots by field-flow fractionation

Field flow fractionation (FFF) technique is used to determine the size of water-soluble Au, ZnS, ZnS-Mn2+ nanoparticles, and CdSe, CdSe-DNA quantum dots (QDs). The results of the FFF measurements are compared with the particle size analysis using conventional techniques like scanning electron microscopy (SEM), transmission electron microscopy (TEM), and dynamic light scattering (DLS) studies. Water-soluble gold nanoparticles (AuNPs) stabilized by mercaptosuccinic acid (MSA) as the ligand when analyzed by the SEM and DLS showed evidence of extensive aggregation, preventing an accurate determination of the average particle size. The TEM analyses without staining offered a facile measurement of the nanoparticle core but average particle size determination required analysis of the TEM image using image analysis software. On the other hand the FFF is seemingly a convenient and easy method for the determination of the average particle size of the AuNPs. In case of the ZnS and ZnS-Mn2+ nanoparticles with mercaptopropionic acid (MPA) as the capping agent severe aggregation prevented accurate estimation of particle sizes even by the high resolution TEM (HRTEM), where as the size determination by the FFF was very facile. Analysis of the CdSe-DNA conjugate by the TEM was difficult as the sample got damaged upon exposure to the electron beam. The FFF cross-flow condition is apparently noninvasive and hence the technique was very effective in characterizing the CdSe-DNA QDs. Furthermore, using this simple technique it was possible to fractionate a sample of the AuNPs. The FFF measurement of water-soluble nanoparticles is an excellent complement to characterization of such particles by the conventional tools.     

Synthesis and characteristics of Ag/Pt bimetallic nanocomposites by arc-discharge solution plasma processing

Arc discharge in solution, generated by applying a high voltage of unipolar pulsed dc to electrodes of Ag and Pt, was used as a method to form Ag/Pt bimetallic nanocomposites via electrode erosion by the effects of the electric arc at the cathode (Ag rod) and the sputtering at the anode (Pt rod). Ag/Pt bimetallic nanocomposites were formed as colloidal particles dispersed in solution via the reduction of hydrogen radicals generated during discharge without the addition of chemical precursor or reducing agent. At a discharge time of 30?s, the fine bimetallic nanoparticles with a mean particle size of approximately 5?nm were observed by transmission electron microscopy (TEM). With increasing discharge time, the bimetallic nanoparticle size tended to increase by forming an agglomeration. The presence of the relatively small amount of Pt dispersed in the Ag matrix could be observed by the analytical mapping mode of energy-dispersive x-ray spectroscopy and high-resolution TEM. This demonstrated that the synthesized particle was in the form of a nanocomposite. No contamination of other chemical substances was detected by x-ray photoelectron spectroscopy. Hence, solution plasma could be a clean and simple process to effectively synthesize Ag/Pt bimetallic nanocomposites and it is expected to be widely applicable in the preparation of several types of nanoparticle.     

二氧化钛纳米晶的制备及其光致发光的研究

以Ti（SO4）2为前驱体,采用沉淀法制备了二氧化钛纳米晶,通过X射线衍射（XRD）、透射电子显微镜（TEM）和光致发光（PL）光谱对微晶进行表征。研究表明,制备的TiO2纳米晶呈类球形颗粒且分散性好,平均粒径最小约为4nm,热处理温度升高到750℃时,样品仍为单一的锐钛矿相;PL谱分析表明,室温下,用高于带隙的能量激发,在370～550nm范围内纳米TiO2粒子呈现出强而宽的发光带,分别对应于价带和导带间的电子跃迁以及表面态的发光;另外发现随焙烧温度升高,粒径增大的同时,发光峰的强度呈无规则变化,分析可能与表面态和晶粒内部缺陷的数量有关。     

Structural and electrochemical properties of Ag nano-dots combined amorphous Si electrodes for thin-film lithium rechargeable batteries

We have one-pot fabricated Si-based nanocomposite electrodes containing Ag nano-dots for thin-film Li rechargeable batteries by a co-sputtering method. The structural and electrochemical properties of the Si/Ag nanocomposite electrodes are investigated via transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), and cycler. The TEM and XRD results show that crystalline Ag nano-dots (approximately 5-9 in size) are well-dispersed within an amorpohous Si matrix. It is shown that the Si/Ag nanocomposite electrode shows much better structural stability than the Si only sample. It is also shown that the Si/Ag nanocomposite electrode shows superior capacity retention compared to the Si only electrode. The results indicate that the presence of the Ag nano-dots is important minimizing the formation of cracks in the electrode, so leading to the better life-time for thin-film Li rechargeable batteries.     

A novel submicron-gap electrode fabrication technology using thermal oxidation

A novel and reproducible method to fabricate submicron-gap electrodes using thermal oxidation has been presented. In this method, oxidation process determines the gap distance. The micron-level silicon electrode gaps with different shapes were first generated on the silicon wafer by conventional photolithography followed by deep reactive ion etching process. Then thermal oxidation was conducted to realize the transition from silicon to silicon dioxide, i.e. reduce the gap width. Finally, the planar electrodes with sub-micron spacing were formed by metallization and photolithography. Scanning electron microscopy (SEM) was used to examine the electrode configuration and the electrical properties of as-prepared electrode pairs were also characterized. The results showed that using the method investigated in this work, Au electrodes with a submicron-sized gap could be easily fabricated, with good uniformity and reproducibility.     

Carbon nanotube nanoelectronic devices compatible with transmission electron microscopy

We report on a novel method to fabricate carbon nanotube (CNT) nanoelectronic devices on silicon nitride membrane grids that are compatible with high resolution transmission electron microscopy (HRTEM). Resist-based electron beam lithography is used to fabricate electrodes on 50 nm thin silicon nitride membranes and focused-ion-beam milling is used to cut out a 200 nm gap across a gold electrode to produce the viewing window for HRTEM. Spin-coating and AC electrophoresis are used as methods to deposit small bundles of carbon nanotubes across the electrodes. We demonstrate the viability of this approach by performing both electrical measurements and HRTEM imaging of solution-processed CNTs in a device.     

纳米银导电墨水及其成膜性能研究

用化学还原法制备了纳米Ag粉,并通过X射线衍射(XRD)、激光粒度分析仪(LPSA)、透射电子显微镜(TEM)、扫描电子显微镜(SEM)等测试手段对样品进行性能表征。在所选择的实验条件下制备了类球形分布、分散性好的Ag纳米颗粒,其粒径主要分布在5～50nm范围,平均粒径为16nm,晶体结构为fcc结构。经涂布检测,Ag纳米墨水制备的墨膜均匀致密,150℃回火后,银粒子烧结明显,有微孔均匀分布。     

Impact of the Nanoscale Gap Morphology on the Plasmon Coupling in Asymmetric Nanoparticle Dimer Antennas

Coupling of plasmon resonances in metallic gap antennas is of interest for a wide range of applications due to the highly localized strong electric fields supported by these structures, and their high sensitivity to alterations of their structure, geometry, and environment. Morphological alterations of asymmetric nanoparticle dimer antennas with (sub)‐nanometer size gaps are assigned to changes of their optical response in correlative dark‐field spectroscopy and high‐resolution transmission electron microscopy (HR‐TEM) investigations. This multimodal approach to investigate individual dimer structures clearly demonstrates that the coupling of the plasmon modes, in addition to well‐known parameters such as the particle geometry and the gap size, is also affected by the relative alignment of both nanoparticles. The investigations corroborate that the alignment of the gap forming facets, and with that the gap area, is crucial for their scattering properties. The impact of a flat versus a rounded gap structure on the optical properties of equivalent dimers becomes stronger with decreasing gap size. These results hint at a higher confinement of the electric field in the gap and possibly a different onset of quantum transport effects for flat and rounded gap antennas in corresponding structures for very narrow gaps.     

Localized electron states near a metal/semiconductor nanocontact

The electronic structure of nanowires in contact with metallic electrodes of experimentally relevant sizes is calculated by incorporating the electrostatic image potential into the atomistic single particle Schr?dinger equation. We show that the presence of an electrode produces localized electron/hole states near the electrode. We found a strong nanowire size dependence of this localization effect. We calculate several electrode/nanowire geometries, with varying contact depths and nanowire radii. We demonstrate the change in the band gap of up to 0.5 eV in 3 nm diameter CdSe nanowires and calculate the magnitude of the applied electric field necessary to overcome the localization.     

Synthesis of cerium oxide nanoparticles by microwave technique using propylene glycol as a stabilizing agent

Cerium oxide nanoparticles have been synthesized by microwave method using cerium nitrate, propylene glycol and ammonia as a precursors. The material was characterized by XRD, SEM, TEM and UV–visible techniques. XRD analysis revealed all the relevant Bragg’s reflections for face centered cubic crystal structure of cerium oxide. The average particle size was obtained 9 nm from the extrapolation of the Williamson–Hall plot. The value of particle size determined from XRD was in good agreement with the SEM and TEM results. The direct optical band gap was found to be 3.12 eV.     

Nanoscale characterization of gold colloid monolayers: a comparison of four techniques

Atomic force microscopy (AFM), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and near-field scanning optical microscopy (NSOM) have been used to characterize the nanostructure of Au colloid-based surfaces. Because these substrates are composed of particles whose dimensions are known prior to assembly, they are well-suited for a critical comparison of the capabilities and limitations of each nanoscale imaging technique. The three criteria for this comparison, which are relevant to the field of nanoparticle assemblies in general, are (i) accuracy in establishing particle size, particle coverage, and interparticle spacing; (ii) accuracy in delineating surface topography; and (iii) ease of sample preparation, data acquisition, and image analysis. For colloidal Au arrays, TEM gives the most reliable size and spacing information but exhibits the greatest constraints with regard to sample preparation; in contrast, AFM is widely applicable but yields data that are the least straightforward to interpret. For accurate information regarding nanometer-scale architecture of particle-based surfaces, a combination of at least one scanning probe method (AFM, NSOM) and one accelerated-electron method (TEM, FE-SEM) is required.     

Synthesis of aluminium nanoparticles by arc evaporation of an aluminium cathode surface

Aluminium nanoparticles (Al Nps) are synthesized using arc discharge method by applying direct current between aluminium electrodes in liquid environment without any use of vacuum equipment, heat exchangers, high temperatures furnaces and inert gases. After synthesis of Al Nps, in situ coating process on the nanoparticles was performed immediately. The effects of media on the yield and morphology of aluminium nanoparticles were investigated. Analysis result of the samples indicated that particle size was less than 30 nm, when 120 A/cm² arc current was used. In addition, coating agent can affect arc velocity, arc stability, morphology and composition of the nanoparticles. Resultant nanoparticles were identified using X-ray powder diffraction (XRD), also their surface morphology was studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM) and finally the accuracy of coating was assessed with infrared (IR) spectroscopy.     

Structural and optical properties of zinc sulphide-polyvinyl alcohol (ZnS-PVA) nanocomposite thin films: effect of Zn source concentration

ZnS-PVA nanocomposite thin films are grown by chemical bath deposition (CBD) method by varying the concentration of zinc source. Formation of nanocrystalline hexagonal ZnS is confirmed by X-ray diffraction. Hexagonal form is predominant at some lower concentration. The morphological properties of the films are determined by transmission electron microscope (TEM). The particle size as given by TEM indicates increase in particle size. Bandgap measured from UV-Visible transmission spectra shows a decreasing trend with decrease of Zn source concentration. Photoluminescence (PL) measurement showed blue emission centred at 417 nm and that the intensity decreases with decrease in Zn source concentration.     

Water sensor for a nonaqueous solvent with poly(1,5-diaminonapthalene) nanofibers

A water sensor for a nonaqueous solvent was fabricated using poly(1,5-diaminonapthalene (DAN) nanofibers, which were prepared through a catalytic chemical polymerization of the DAN monomer using Fe(III) salt as the catalyst. Poly(1,5-DAN) nanofibers were characterized by atomic force microscope (AFM), transmission electron microscope (TEM), scanning electron microscope (SEM), and UV-vis spectroscopy. The electrochemical properties of poly(1,5-DAN) nanofibers were investigated using cyclic voltammetry (CV). The electrochemical activity of poly(1,5-DAN) nanofibers was utilized for water sensing. The fabrication of water sensor was followed by placing one drop (about 2 microL) of 0.01% poly(1,5-DAN) nanofibers solution in the gap between two split gold electrodes (PBSA) and completely dried. The response of the water sensor in an acetonitrile solution was evaluated under optimized conditions. The linear dynamic range was from 0.05 to 20%, and the detection limit was determined to be 0.01%. The response of this sensor was shown to be comparable to that obtained with the Karl Fischer titration method.     

Synthesis and characterization of SnS nanosheets through simple chemical route

Tin Sulfide (SnS) nanosheets were synthesized by wet chemical route using ethylene glycol (EG) and without using any surfactant. Structural and phase purity were confirmed by powder X-ray diffraction pattern which shows the orthorhombic structure of SnS. The sheets like morphology and particle size of the synthesized product were identified by using analytical transmission electron microscope (TEM) and high resolution transmission electron microscope (HRTEM). Agglomeration of SnS nanoparticles was found to lead to the formation of nanosheets. UV-VIS-NIR absorption spectrum of SnS nanosheets shows the direct transition at 1.88 eV. Compared to bulk band gap a blue shift of 0.58 eV has been observed for direct transition. This is due to the quantum confinement effect. Room temperature photoluminescence spectrum of SnS nanosheets shows two emission bands at 1.75 and 1.57 eV respectively which are assigned to band gap and defect level transitions.