Nano-probe x-ray analysis and high-resolution imaging on planar defects in high-pressure synthesized infinite-layer superconductor

Author(s):  
Y. Y. Wang ◽  
H. Zhang ◽  
V. P. Dravid ◽  
H. Zhang ◽  
L. D. Marks ◽  
...  

Azuma et al. observed planar defects in a high pressure synthesized infinitelayer compound (i.e. ACuO2 (A=cation)), which exhibits superconductivity at ~110 K. It was proposed that the defects are cation deficient and that the superconductivity in this material is related to the planar defects. In this report, we present quantitative analysis of the planar defects utilizing nanometer probe xray microanalysis, high resolution electron microscopy, and image simulation to determine the chemical composition and atomic structure of the planar defects. We propose an atomic structure model for the planar defects.Infinite-layer samples with the nominal chemical formula, (Sr1-xCax)yCuO2 (x=0.3; y=0.9,1.0,1.1), were prepared using solid state synthesized low pressure forms of (Sr1-xCax)CuO2 with additions of CuO or (Sr1-xCax)2CuO3, followed by a high pressure treatment.Quantitative x-ray microanalysis, with a 1 nm probe, was performed using a cold field emission gun TEM (Hitachi HF-2000) equipped with an Oxford Pentafet thin-window x-ray detector. The probe was positioned on the planar defects, which has a 0.74 nm width, and x-ray emission spectra from the defects were compared with those obtained from vicinity regions.

Author(s):  
Robert A. Grant ◽  
Laura L. Degn ◽  
Wah Chiu ◽  
John Robinson

Proteolytic digestion of the immunoglobulin IgG with papain cleaves the molecule into an antigen binding fragment, Fab, and a compliment binding fragment, Fc. Structures of intact immunoglobulin, Fab and Fc from various sources have been solved by X-ray crystallography. Rabbit Fc can be crystallized as thin platelets suitable for high resolution electron microscopy. The structure of rabbit Fc can be expected to be similar to the known structure of human Fc, making it an ideal specimen for comparing the X-ray and electron crystallographic techniques and for the application of the molecular replacement technique to electron crystallography. Thin protein crystals embedded in ice diffract to high resolution. A low resolution image of a frozen, hydrated crystal can be expected to have a better contrast than a glucose embedded crystal due to the larger density difference between protein and ice compared to protein and glucose. For these reasons we are using an ice embedding technique to prepare the rabbit Fc crystals for molecular structure analysis by electron microscopy.


Author(s):  
J.M. Cowley

By extrapolation of past experience, it would seem that the future of ultra-high resolution electron microscopy rests with the advances of electron optical engineering that are improving the instrumental stability of high voltage microscopes to achieve the theoretical resolutions of 1Å or better at 1MeV or higher energies. While these high voltage instruments will undoubtedly produce valuable results on chosen specimens, their general applicability has been questioned on the basis of the excessive radiation damage effects which may significantly modify the detailed structures of crystal defects within even the most radiation resistant materials in a period of a few seconds. Other considerations such as those of cost and convenience of use add to the inducement to consider seriously the possibilities for alternative approaches to the achievement of comparable resolutions.


Author(s):  
J.L. Batstone ◽  
J.M. Gibson ◽  
Alice.E. White ◽  
K.T. Short

High resolution electron microscopy (HREM) is a powerful tool for the determination of interface atomic structure. With the previous generation of HREM's of point-to-point resolution (rpp) >2.5Å, imaging of semiconductors in only <110> directions was possible. Useful imaging of other important zone axes became available with the advent of high voltage, high resolution microscopes with rpp <1.8Å, leading to a study of the NiSi2 interface. More recently, it was shown that images in <100>, <111> and <112> directions are easily obtainable from Si in the new medium voltage electron microscopes. We report here the examination of the important Si/Si02 interface with the use of a JEOL 4000EX HREM with rpp <1.8Å, in a <100> orientation. This represents a true structural image of this interface.


Author(s):  
W. Coene ◽  
F. Hakkens ◽  
T.H. Jacobs ◽  
K.H.J. Buschow

Intermetallic compounds of the type RE2Fe17Cx (RE= rare earth element) are promising candidates for permanent magnets. In case of Y2Fe17Cx, the Curie temperature increases from 325 K for x =0 to 550 K for x = 1.6 . X ray and electron diffraction reveal a carbon - induced structural transformation in Y2Fe17Cx from the hexagonal Th2Ni17 - type (x < 0.6 ) to the rhombohedral Th2Zn17 - type ( x ≥ 0.6). Planar crystal defects introduce local sheets of different magnetic anisotropy as compared with the ordered structure, and therefore may have an important impact on the coercivivity mechanism .High resolution electron microscopy ( HREM ) on a Philips CM30 / Super Twin has been used to characterize planar crystal defects in rhombohedral Y2Fe17Cx ( x ≥ 0.6 ). The basal plane stacking sequences are imaged in the [100] - orientation, showing an ABC or ACB sequence of Y - atoms and Fe2 - dumbbells, for both coaxial twin variants, respectively . Compounds resulting from a 3 - week annealing treatment at high temperature ( Ta = 1000 - 1100°C ) contain a high density of planar defects.


1986 ◽  
Vol 77 ◽  
Author(s):  
Mary Beth Stearns ◽  
Amanda K. Petford-Long ◽  
C.-H. Chang ◽  
D. G. Stearns ◽  
N. M. Ceglio ◽  
...  

ABSTRACTThe technique of high resolution electron microscopy has been used to examine the structure of several multilayer systems (MLS) on an atomic scale. Mo/Si multilayers, in use in a number of x-ray optical element applications, and Mo/Si multilayers, of interest because of their magnetic properties, have been imaged in cross-section. Layer thicknesses, flatness and smoothness have been analysed: the layer width can vary by up to 0.6nm from the average value, and the layer flatness depends on the quality of the substrate surface for amorphous MLS, and on the details of the crystalline growth for the crystalline materials. The degree of crystallinity and the crystal orientation within the layers have also been investigated. In both cases, the high-Z layers are predominantly crystalline and the Si layers appear amorphous. Amorphous interfacial regions are visible between the Mo and Si layers, and crystalline cobalt suicide interfacial regions between the Co and Si layers. Using the structural measurements obtained from the HREM results, theoretical x-ray reflectivity behaviour has been calculated. It fits the experimental data very well.


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