Oxygen content, microstructure, and superconductivity of YBa2Cu3O7−x

1987 ◽  
Vol 2 (6) ◽  
pp. 743-749 ◽  
Author(s):  
M. P. A. Viegers ◽  
D. M. de Leeuw ◽  
C. A. H. A. Mutsaers ◽  
H. A. M. van Hal ◽  
H. C. A. Smoorenburg ◽  
...  

The influence of preparation conditions and microstructure on the superconductive properties of single-phase poly-crystalline YBa2Cu3O7−x was investigated by electron probe microanalysis, transmission electron microscopy (TEM), and x-ray powder diffraction as a function of temperature in various ambients supplemented by resistivity and susceptibility measurements. Leaching of Ba was observed when samples were brought in contact with water. The TEM imaging revealed that individual grains have an extremely defect-rich outer shell and an inner core with a domain structure with a and b axes interchanged. The transition temperature Tc was found to decrease with increasing quench temperature in the range 400–900°C. The Tc was observed to be linearly proportional to the difference in the orthorhombic cell parameters (b-a). Further implications are discussed.

1998 ◽  
Vol 13 (8) ◽  
pp. 2161-2169 ◽  
Author(s):  
Y. H. Li ◽  
K. A. Thomas ◽  
P. S. I. P. N. de Silva ◽  
L. F. Cohen ◽  
A. Goyal ◽  
...  

The structural changes and magnetoresistance (MR) properties of as-grown and post-annealed La0.7Ca0.3MnO3 films were investigated by transmission electron microscopy (TEM) and x-ray diffraction (XRD). The data for the films were compared to that for bulk La0.7Ca0.3MnO3 post-annealed under the same conditions. The main structure of the as-grown films was face-centered pseudo-cubic with a doubled perovskite unit cell, of size ∼2ap × ∼2ap × 2ap, where ap is the single perovskite parameter. The phase showed a cube-on-cube epitaxy with the underlying LaAlO3 substrate. Upon annealing to a saturation point, a minor primitive pseudo-tetragonal structure evolved, of cell parameters . A total of four possible orientations of the two structures was observed by TEM, comprised of one orientation of the ∼ 2ap × ∼ 2ap × ∼ 2ap cell, i.e., the cube-on-cube epitaxy, giving rise to (00l) peaks in x-ray, and three orientations of the cell, giving rise to a single (00l)/(hk0) peak in x-ray. The bulk La0.7Ca0.3MnO3 sample also contains the × structure. The difference between the bulk and the film and the effects of annealing on films can be ascribed to the influence of strain between the film and substate, induced by lattice mismatch.


Electrochemical hydrogenation, lithiation and sodiation of the phases GdFe2–xMx and GdMn2–xMx (M=Mn, Co, Ni, Zn, and Mg) and the influence of doping components on electrochemical characteristics of electrode materials on their basis were studied using X-ray powder diffraction method, scanning electron microscopy, energy dispersive X-ray analysis, X-ray fluorescent spectroscopy, cyclic voltammetry and electrochemical impedance spectroscopy. Phase analysis showed a simple correspondence between unit cell parameters of the phases and atomic radii of doping elements. Electrode materials based on GdFe2 and GdMn2 doped with 2 at.% of Co, Ni and Mg demonstrated better hydrogen sorption properties than those doped with Mn and Zn. Corrosion resistance of the doped electrodes was also better than of the binary analogues (e.g. corrosion potential of the GdFe2-based electrode was –0.162 V whereas that of GdFe1.96Ni0.04 was –0.695 V). The capacity parameters were increased in the following ranges: Zn<Mn<Mg<Co<Ni and Zn<Fe<Mg<Co<Ni for GdFe2–xMx and GdMn2–xMx, respectively. After fifty cycles of charge/discharge, we observed the changes in surface morphology and composition of the electrode samples. In the structure of studied Laves type phases with MgCu2-type structure, the most suitable sites for hydrogen atoms are tetrahedral voids 8a. During lithiation and sodiation of the phases, the atoms of the M-component of the structure are replaced by the atoms of lithium, and the atoms of gadolinium are replaced by the atoms of sodium. This difference in interaction is due to the difference in atomic sizes of the atoms. No insertion of lithium or sodium into the structural voids of the phases was observed.


2006 ◽  
Vol 15-17 ◽  
pp. 159-163 ◽  
Author(s):  
Kee Hyun Kim ◽  
Benny van Daele ◽  
Gustaaf Van Tendeloo ◽  
Yong Sug Chung ◽  
Jong Kyu Yoon

A hot dip aluminising process was carried out with a 1mm steel sheet dipped into the Al-10at.% Si melt in an automatic hot-dip simulator. When steel and liquid aluminium are in contact with each other, a thin intermetallic compound (IMC) is formed between the steel and the aluminium. The analysis and identification of the formation mechanism of the IMC is needed to manufacture the application products. Energy dispersive X-ray spectroscopy (EDX) and electron probe microanalysis (EPMA) are normally used to identify the phases of IMC. In the Al-Fe-Si system, numerous compounds with only slight differences in composition are formed. Consequently, EDX and EPMA are insufficient to confirm exactly the thin IMC with multiphases. In this study, transmission electron microscopy (TEM) analysis combined with EDX was used. The TEM sample was prepared with focused ion beam (FIB) sampling. The FIB lift-out technology is used to slice a very thin specimen with minimum contamination for TEM analysis. It is clearly shown that the IMC consists of Al-27 at. % Fe-10 at. % Si and is identified as Al8Fe2Si with a hexagonal unit cell (space group P63/mmc). The cell parameters are a= 1.2404nm and c= 2.6234nm.


2011 ◽  
Vol 412 ◽  
pp. 263-266
Author(s):  
Hong Wei Zhang ◽  
Li Li Zhang ◽  
Feng Rui Zhai ◽  
Jia Jin Tian ◽  
Can Bang Zhang

The higher mechanical strength of Al87Ce3Ni8.5Mn1.5 nanophase amorphous composites has been obtained with two methods. The first nanophase amorphous composites are directly produced by the single roller spin quenching technology. The method taken for the second nanophase amorphous composites is at first to obtain amorphous single-phase alloy, followed by annealed at different temperatures .The formative condition, the microstructure, the particle size, the volume fraction of α-Al phase and microhardness of nanophase amorphous composites etc have been investigated and compared by X-ray diffraction (XRD) and transmission electron microscopy (TEM) and differential scanning calorimetry (DSC). The microstructure of composites produced by the second method is higher than the former, the fabricated material structure of the system is more uniform and the process is easier to control.


1989 ◽  
Vol 169 ◽  
Author(s):  
Lauren E. H. McMills ◽  
Shu Li ◽  
Zhen Zhang ◽  
Martha Greenblatt

AbstractSingle-phase samples of T12Ba2CaCu2O8 and T12Ba2Ca2Cu3O10 have been prepared using a reliable and simple synthetic method. Samples were characterized by x-ray powder diffraction, magnetic susceptibility and four probe resistivity methods. The TcR=0 values for T12Ba2CaCu2O8 ranged from 100 to 105K, whereas those for T12Ba2Ca2Cu3O10 ranged from 96 to 107K. The relationship between the superconducting properties and the various preparation conditions are discussed.


2013 ◽  
Vol 802 ◽  
pp. 227-231
Author(s):  
Panida Pilasuta ◽  
Pennapa Muthitamongkol ◽  
Chanchana Thanachayanont ◽  
Tosawat Seetawan

Crystal structure of Zn0.96Al0.02Ga0.02O was analyzed by X-Ray diffraction (XRD) technique and the microstructure was observed by scanning electron microscopy (SEM), and transmission electron microscopy (TEM). The XRD results showed single phase and hexagonal structure a = b = 3.24982 Å, and c = 5.20661 Å. The SEM and TEM results showed the grain size of material arrangement changed after sintering and TEM diffraction pattern confirmed hexagonal crystal structure of Zn0.96Al0.02Ga0.02O after sintering.


2003 ◽  
Vol 802 ◽  
Author(s):  
K. T. Moore ◽  
M. A. Wall ◽  
A. J. Schwartz ◽  
B. W. Chung ◽  
J. G. Tobin ◽  
...  

ABSTRACTHere, we demonstrate the power of electron energy-loss spectroscopy (EELS) in a transmission electron microscope (TEM) to investigate the electronic structure plutonium. Using EELS, TEM, and synchrotron-radiation-based X-ray absorption spectroscopy (XAS), we provide the first experimental evidence that Russell-Saunders (LS) coupling fails for the 5f states of Pu. These results support the assumption that only the use of jj or intermediate coupling is appropriate for the 5f states of Pu. EELS experiments were performed in a TEM and are coupled with image and diffraction data, therefore, the measurements are completely phase specific. It is shown that EELS in a TEM may be used to circumvent the difficulty of producing single-phase or single-crystal samples due to its high spatial resolution.


2009 ◽  
Vol 1228 ◽  
Author(s):  
Masataka Hakamada ◽  
Yasumasa Chino ◽  
Mamoru Mabuchi

AbstractMetallic nanoporous architecture can be spontaneously attained by dealloying of a binary alloy. The nanoporous architecture can be often fabricated in noble metals such as Au and Pt. In this study, nanoporous Ni, Ni-Cu are fabricated by dealloying rolled Ni-Mn and Cu-Ni-Mn alloys, respectively. Unlike conventional Raney nickel composed of brittle Ni-Al or Cu-Al intermetallic compounds, the initial alloys had good workability probably because of their fcc crystal structures. After the electrolysis of the alloys in (NH4)2SO4 aqueous solution, nanoporous architectures of Ni and Ni-Cu with pore and ligament sizes of 10–20 nm were confirmed by scanning electron microscopy and transmission electron microscopy. X-ray diffraction analyses suggested that Ni and Cu atoms form a homogeneous solid solution in the Ni-Cu nanoporous architecture. The ligament sizes of nanoporous Ni and Ni-Cu were smaller than that of nanoporous Cu, reflecting the difference between diffusivities of Ni and Cu at solid/electrolyte interface. Ni can reduce the pore and ligament sizes of resulting nanoporous architecture when added to initial Cu-Mn alloys.


2006 ◽  
Vol 16 (01n02) ◽  
pp. 127-136
Author(s):  
P. MALAR ◽  
TAPASH RANJAN RAUTRAY ◽  
V. VIJAYAN ◽  
S. KASIVISWANATHAN

Polycrystalline ingots of CuInSe 2 and CuIn 3 Se 5 were synthesized by melt-quench technique starting from the stoichiometric mixture of constituent elements. X-ray Diffraction (XRD) studies confirmed the single-phase nature of the materials. Compositional analysis by Particle Induced X-ray Emission (PIXE) showed that the compounds are near stoichiometric. Thin films of CuInSe 2 and CuIn 3 Se 5 were grown from pre-synthesized CuInSe 2 and CuIn 3 Se 5 powders. The films were polycrystalline, single-phase and near stoichiometric in nature, as indicated by Transmission Electron Microscopy (TEM) and PIXE studies.


2004 ◽  
Vol 19 (12) ◽  
pp. 3665-3670 ◽  
Author(s):  
D.Z. Guo ◽  
K. Yu-Zhang ◽  
A. Gloter ◽  
G.M. Zhang ◽  
Z.Q. Xue

Single crystalline nanorods (15–200 nm in diameter and hundreds nanometers in length) have been formed on the carbon-covered W wires by simple electric heating under a vacuum of 5 × 10−4 Pa. The chemical composition and crystalline structure of the nanorods were carefully investigated by various characterization techniques such as scanning electron microscopy, transmission electron microscopy, Raman spectroscopy, energy dispersive x-ray spectroscopy and electron energy loss spectroscopy. After ruling out any possible existence of carbon nanotubes (CNTs), tungsten carbide, W–Fe alloying, and formation of other types of tungsten oxides, monoclinic W18O49 phase has been well identified. The mechanism of nanorod formation of sub-tungsten oxide (∼WO2.7 compared to WO3) will be discussed in relation to the sample preparation conditions.


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