Enhanced Solubility of Cu in Ag Nanoparticles Synthesized by Inert Gas Condensation

2004 ◽  
Vol 854 ◽  
Author(s):  
Abdullah Ceylan ◽  
C. Ni ◽  
S. Ismat Shah

ABSTRACTAg-Cu alloy nanoparticles were prepared by rapid condensation of metal flux obtained by the simultaneous evaporation of high purity Cu and Ag wires on a tungsten boat in the presence of circulating He gas. Structural properties of the samples prepared at different conditions were investigated by using X-ray diffraction (XRD), transmission electron microscopy (TEM) and selected area diffraction (SAD) patterns. X-ray diffraction patterns showed that particles were phase separated. The particle size obtained either from Scherer's formula or the TEM images show no systematic change on the size of either Cu or Ag particles in the evaporation temperature range between 800 and 1400 °C. By using lattice constant values and Vegard's law, the composition of the particles was calculated to be 6.6 vol% Cu in Ag. Electron diffraction images revealed that particles were softly agglomerated; these electron diffraction results were also consistent with XRD results regarding phase separation. Individual diffraction rings of the Cu and Ag were observed in the SAD patterns.

2014 ◽  
Vol 70 (a1) ◽  
pp. C1080-C1080
Author(s):  
Yifeng Yun ◽  
Wei Wan ◽  
Faiz Rabbani ◽  
Jie Su ◽  
Sven Hovmöller ◽  
...  

Electron Crystallography is an important technique for studying micro- and nano-sized crystals[1]. Crystals considered as powder by X-ray diffraction behave as single crystals by electron diffraction. Recently we developed a new method, Rotation Electron Diffraction (RED) for three-dimensional diffraction data collection by combining electron beam tilt with goniometer tilt on a transmission electron microscope (TEM)[2]. Here we apply the RED method on an unknown oxide sample in a Ni-Se-Cl-O system, which may show special physical properties, for example magnetic properties. The crystals in the sample were less than a few micrometers in sizes. Powder X-ray diffraction patterns of the sample could not be indexed by existing known phases. The sample was thus studied by TEM. Five 3D RED datasets were collected from five crystals with different morphologies using the software package RED. The data processing was also performed using the software RED-processing. The unit cell and space groups of all the five phases were obtained using RED and the structures of four of five phases were solved. Nearly all peaks in the powder X-ray diffraction pattern could be indexed using these five phases. To conclude, five phases from a powder sample have been identified using RED. RED is a powerful method for phase identification of multiphasic samples with nano-sized crystals.


2014 ◽  
Vol 47 (3) ◽  
pp. 879-886 ◽  
Author(s):  
He Zheng ◽  
Jianbo Wang ◽  
Zhongling Xu ◽  
Jianian Gui

A previous transmission electron microscopy (TEM) analysis revealed the existence of monoclinic Li2MnO3in the lithium-rich and oxygen-deficient Li1.07Mn1.93O4−δpowder. Interestingly, the monoclinic phase exhibits different nanoscale lamellar variants involving a rotation of the stacking direction by 120 or 240° along the pseudo-threefold axis,i.e.the [103]M//[111]C(M and C denote the monoclinic and cubic phases, respectively) zone axis. Here, a theoretical X-ray diffraction (XRD) study of Li2MnO3employing theDIFFaXprogram is presented. It is found that, with the occurrence of different stacking configurations, the characteristic superstructure reflections with 2θ between 20 and 35° (Cu Kα) in the XRD pattern become more and more broadened with the increasing degree of stacking disorder, indicating that XRD may fall short in detecting the presence of the monoclinic Li2MnO3phase. Moreover, selective peak asymmetry appears when the stacking sequence becomes extremely disordered. Further selected-area electron diffraction and theoretical neutron diffraction investigation may clarify the similar ambiguity concerning the crystal phases of other structurally related compound cathode materials for lithium-ion batteries (e.g.LiNi1/2Mn1/2O2, LiNi1/3Co1/3Mn1/3O2).


2014 ◽  
Vol 68 (8) ◽  
Author(s):  
Selvakumar Dhanasingh ◽  
Dharmaraj Nallasamy ◽  
Saravanan Padmanapan ◽  
Vinod Padaki

AbstractThe influence of cetyltrimethylammonium bromide and ethylene glycol on the size and dispersion of indium oxide nanoparticles prepared under hydrothermal conditions was investigated. The precursor compound, indium hydroxide, obtained by the hydrothermal method in the absence as well as the presence of cetyltrimethylammonium bromide, was converted to indium oxide by sintering at 400°C. The formation of nanoscale indium oxide upon sintering was ascertained by the characteristic infrared adsorption bands and X-ray diffraction patterns of indium oxide. Transmission electron microscopy and band gap values confirmed that the cetyltrimethylammonium bromide facilitated the formation of indium oxide nanoparticles smaller in size and narrower in distribution than those prepared without the assistance of cetyltrimethylammonium bromide.


2015 ◽  
Vol 68 (8) ◽  
pp. 1293 ◽  
Author(s):  
Pakvipar Chaopanich ◽  
Punnama Siriphannon

Hydroxyapatite (HAp) nanoparticles were successfully synthesized from an aqueous mixture of Ca(NO3)2·4H2O and (NH4)2HPO4 by a facile single-step refluxing method using polystyrene sulfonate (PSS) as a template. The effects of reaction times, pH, and PSS concentration on the HAp formation were investigated. It was found that the crystalline HAp was obtained under all conditions after refluxing the precursors for 3 and 6 h. The longer refluxing time, the greater the crystallinity and the larger the crystallite size of the HAp nanoparticles. The HAp with poor crystallinity was obtained at pH 8.5; however, the well-crystallized HAp was obtained when reaction pH was increased to 9.5 and 10.5. In addition, the X-ray diffraction patterns revealed that the presence of PSS template caused the reduction of HAp crystallite size along the (002) plane from 52.6 nm of non-template HAp to 43.4 nm and 41.4 nm of HAp with 0.05 and 0.2 wt-% PSS template, respectively. Transmission electron microscopy images of the synthesized HAp revealed the rod-shaped crystals of all samples. The synthesized HAp nanoparticles were modified by l-aspartic acid (Asp) and l-arginine (Arg), having negative and positive charges, respectively. It was found that the zeta potential of HAp was significantly changed from +5.46 to –24.70 mV after modification with Asp, whereas it was +4.72 mV in the Arg-modified HAp. These results suggested that the negatively charged amino acid was preferentially adsorbed onto the synthesized HAp surface.


2007 ◽  
Vol 7 (2) ◽  
pp. 525-529 ◽  
Author(s):  
Bo Zhou ◽  
Jun-Jie Zhu

A chemical co-reduction route in aqueous solution was developed to synthesize Bi100−xSbx alloys at room temperature. The hydrolyses of Bi(III) and Sb(III) were effectively avoided by selecting proper raw materials and coordinator. X-ray diffraction analysis indicated that the as-prepared Bi100−xSbx alloys were homogeneous and phase-pure, and the Bi/Sb ratios in the alloys were very close to those in the aqueous solutions. The transmission electron microscope observation showed that the as-prepared Bi100−xSbx (x = 0∼100) alloys were particles with a size of tens of nanometers. The selected area electron diffraction patterns confirmed the high crystallinity, the homogeneousness, and the composition controllability of as-prepared alloys. All these characters and the nanometer-scaled size of the alloys are believed to be beneficial to the thermoelectric property of the Bi100−xSbx alloys.


2007 ◽  
Vol 7 (2) ◽  
pp. 634-640 ◽  
Author(s):  
M. Siliani ◽  
M. A. López-Manchado ◽  
J. L. Valentín ◽  
M. Arroyo ◽  
A. Marcos ◽  
...  

Novel millable polyurethane (PU)/organoclay nanocomposites have been successfully prepared by conventional transformation techniques. One natural (C6A) and two organically modified (C15A and C30B) montmorillonites have been used as clays for preparing PU nanocomposites. The optimum dispersion of nanofiller at a nanometer scale in PU matrix was confirmed by X-ray diffraction patterns and transmission electron microscopy. A substantial improvement of the PU properties by addition of only a small amount of organoclay was observed. It is worthy to note that the organoclays show a different interfacial interaction with the PU matrix, which was reflected in different macroscopic properties. Thus, C30B organoclay seems to react with PU chains to form covalent bonds, while C15Aonly interacts physically with PU chains. Mechanical and barrier properties are analyzed.


2015 ◽  
Vol 2015 ◽  
pp. 1-6 ◽  
Author(s):  
Wei-Lin Wang ◽  
Chia-Ti Wang ◽  
Wei-Chun Chen ◽  
Kuo-Tzu Peng ◽  
Ming-Hsin Yeh ◽  
...  

Ta/TaN bilayers have been deposited by a commercial self-ionized plasma (SIP) system. The microstructures of Ta/TaN bilayers have been systematically characterized by X-ray diffraction patterns and cross-sectional transmission electron microscopy. TaN films deposited by SIP system are amorphous. The crystalline behavior of Ta film can be controlled by the N concentration of underlying TaN film. On amorphous TaN film with low N concentration, overdeposited Ta film is the mixture ofα- andβ-phases with amorphous-like structure. Increasing the N concentration of amorphous TaN underlayer successfully leads upper Ta film to form pureα-phase. For the practical application, the electrical property and reliability of Cu interconnection structure have been investigated by utilizing various types of Ta/TaN diffusion barrier. The diffusion barrier fabricated by the combination of crystallizedα-Ta and TaN with high N concentration efficiently reduces the KRc and improves the EM resistance of Cu interconnection structure.


1994 ◽  
Vol 346 ◽  
Author(s):  
Carol S. Houk ◽  
Gary A. Burgoine ◽  
Catherine J. Page

ABSTRACTWe have investigated the homogeneity of sol‐gel derived YBa2Cu307‐s from the solution phase to the final product using transmission electron microscopy (TEM), x‐ray diffraction (XRD), and Energy Dispersive X‐ray (EDX) lateral mapping techniques. The starting solutions contain stoichiometric amounts of the metal 2‐(2‐methoxyethoxy)ethoxide components in 2‐(2‐methoxyethoxy)ethanol and appear to be homogeneous by TEM with a uniform distribution of particles having an average size of less than 40 â. Through elemental mapping we see elemental segregation in the high temperature (950 °C) products, which are orthorhombic by XRD. In elemental maps of gel samples fired to 700 °C, which are tetragonal by XRD, we also see elemental inhomogeneity within particles and phase zoning in maps of products from finely ground gels. A comparison of elemental maps and x‐ray diffraction patterns of the products from gel processing and conventional solid state processing is made.


Clay Minerals ◽  
1977 ◽  
Vol 12 (1) ◽  
pp. 59-66 ◽  
Author(s):  
M. J. Wilson ◽  
J. M. Tait

AbstractX-ray diffraction and electron microscopy show that halloysite occurs widely in soils derived from a variety of parent rocks (granite, gabbro, schist and slate) in north-east Scotland. Both tubular and non-tubular forms are observed, the latter being characterized by electron diffraction patterns with 001 reflection either absent or very weak and diffuse. Clay fractions from a poorly drained profile separated without prior drying of the soil samples contain essentially dehydrated halloysite at the surface, this becoming progressively more hydrated with depth. Since halloysite occurs extensively in soils of widely varying drainage class the mineral is probably not the result of recent soilforming processes but may have originated during Tertiary or interglacial weathering.


2008 ◽  
Vol 8 (3) ◽  
pp. 1481-1488 ◽  
Author(s):  
Marguerite Germain ◽  
Philip Fraundorf ◽  
Sam Lin ◽  
Elena A. Guliants ◽  
Christopher E. Bunker ◽  
...  

We describe the synthesis and characterization of srilankite (Ti2ZrO6) nanowires. The nanowires are produced via hydrothermal synthesis with a TiO2/ZrO2 mixture under alkaline conditions. The zirconium titanate nanowires have median diameters of 60 nm and median lengths of 800 nm with the 〈022〉 axis along the length of the nanowire. Electron microscopy, energy dispersive X-ray spectroscopy, powder X-ray diffraction, and electron diffraction are used to characterize the phases and compare nanowires produced with varying molar ratios of Ti and Zr. Electron diffraction patterns produced from single nanowires show highly crystalline nanowires displaying a compositional-ordering superlattice structure with Zr concentrated in bands within the crystal structure. This is in contrast to naturally occurring bulk srilankite where Zr and Ti are randomly substituted within the crystal lattice. Streaking is observed in the electron diffraction patterns suggesting short-range ordering within the superlattice structure.


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