Single-Crystal Structural Study of La2Cu0.95Li0.05O4.

1987 ◽  
Vol 99 ◽  
Author(s):  
J. M. Delgado ◽  
J. S. Speck ◽  
R. K. McMullan ◽  
G. Diaz de Delgado ◽  
B. J. Wuensch

ABSTRACTA large crystal of flux-grown La2CuO4, examined through single-crystal neutron diffraction, was found to have an orthorhombic superstructure derived from the K2NiF4 structure type with a=5.359(1), b=5.363(1), c=13.127(2) Å. The pattern of systematically absent intensities indicated space group Pccn but meaningful refinement of thermal vibration parameters could not be obtained in this symmetry. Systematic examination of all possible orthorhombic subgroups of Fmmm yielded satisfactory refinement to R(F2)=2.57% only in space group Bmab. Incorporation in the crystal of Li derived from the flux results in an orthorhombic distortion smaller than found for pure La2CuO4. Refinement of the Cu site occupancy provided Cu0.95Li0.050(3), in excellent accord with a bulk chemical analysis. Reflections which violate the systematic absences of Bmab are attributed to a smaller volume fraction of domains in orientation twinned by 90° rotation about c. This interpretation is supported by transmission electron microscopy which revealed intergrown lamellae. Dark field imaging with a forbidden reflection illuminated only the twin lamellae.

2006 ◽  
Vol 6 (3) ◽  
pp. 698-703 ◽  
Author(s):  
T. Haber ◽  
M. Oehzelt ◽  
R. Resel ◽  
A. Andreev ◽  
A. Thierry ◽  
...  

This work focuses on studies of the single crystal nature of para-sexiphenyl structures grown on freshly cleaved KCl(100) surfaces. Two different kinds of morphologies, namely terrace like structures and needle like structures, are found by atomic force microscopy as well as by electron microscopy. Regardless of the morphology the individual crystallites show highly regular shapes. The crystalline alignment and the degree of order of the crystallites on the surface are determined by X-ray diffraction. Several epitaxial alignments of para-sexiphenyl on KCl(100) are observed and all of them are perfectly aligned on the surface. The rocking curve widths of the organic crystallites do not exceed 800″ which is approximately only the four fold of the substrates' ones. The single crystalline nature of para-sexiphenyl crystallites is proven by transmission electron microscopy, diffraction patterns, dark field imaging and high resolution techniques. Single crystalline terraced mounds reach diameters of several microns and heights of 50 nm. Single crystal needles show heights and breadths of more than 100 nm and lengths of several microns.


Author(s):  
Akira Tanaka ◽  
David F. Harling

In the previous paper, the author reported on a technique for preparing vapor-deposited single crystal films as high resolution standards for electron microscopy. The present paper is intended to describe the preparation of several high resolution standards for dark field microscopy and also to mention some results obtained from these studies. Three preparations were used initially: 1.) Graphitized carbon black, 2.) Epitaxially grown particles of different metals prepared by vapor deposition, and 3.) Particles grown epitaxially on the edge of micro-holes formed in a gold single crystal film.The authors successfully obtained dark field micrographs demonstrating the 3.4Å lattice spacing of graphitized carbon black and the Au single crystal (111) lattice of 2.35Å. The latter spacing is especially suitable for dark field imaging because of its preparation, as in 3.), above. After the deposited film of Au (001) orientation is prepared at 400°C the substrate temperature is raised, resulting in the formation of many square micro-holes caused by partial evaporation of the Au film.


Author(s):  
D. S. Pritchard

The effect of varying the strain rate loading conditions in compression on a copper single crystal dispersion-hardened with SiO2 particles has been examined. These particles appear as small spherical inclusions in the copper lattice and have a volume fraction of 0.6%. The structure of representative crystals was examined prior to any testing on a transmission electron microscope (TEM) to determine the nature of the dislocations initially present in the tested crystals. Only a few scattered edge and screw dislocations were viewed in those specimens.


Author(s):  
M. Awaji

It is necessary to improve the resolution, brightness and signal-to-noise ratio(s/n) for the detection and identification of point defects in crystals. In order to observe point defects, multi-beam dark-field imaging is one of the useful methods. Though this method can improve resolution and brightness compared with dark-field imaging by diffuse scattering, the problem of s/n still exists. In order to improve the exposure time due to the low intensity of the dark-field image and the low resolution, we discuss in this paper the bright-field high-resolution image and the corresponding subtracted image with reference to a changing noise level, and examine the possibility for in-situ observation, identification and detection of the movement of a point defect produced in the early stage of damage process by high energy electron bombardment.The high-resolution image contrast of a silicon single crystal in the [10] orientation containing a triple divacancy cluster is calculated using the Cowley-Moodie dynamical theory and for a changing gaussian noise level. This divacancy model was deduced from experimental results obtained by electron spin resonance. The calculation condition was for the lMeV Berkeley ARM operated at 800KeV.


Author(s):  
G. Lucadamo ◽  
K. Barmak ◽  
C. Michaelsen

The subject of reactive phase formation in multilayer thin films of varying periodicity has stimulated much research over the past few years. Recent studies have sought to understand the reactions that occur during the annealing of Ni/Al multilayers. Dark field imaging from transmission electron microscopy (TEM) studies in conjunction with in situ x-ray diffraction measurements, and calorimetry experiments (isothermal and constant heating rate), have yielded new insights into the sequence of phases that occur during annealing and the evolution of their microstructure.In this paper we report on reactive phase formation in sputter-deposited lNi:3Al multilayer thin films with a periodicity A (the combined thickness of an aluminum and nickel layer) from 2.5 to 320 nm. A cross-sectional TEM micrograph of an as-deposited film with a periodicity of 10 nm is shown in figure 1. This image shows diffraction contrast from the Ni grains and occasionally from the Al grains in their respective layers.


Author(s):  
Xianghong Tong ◽  
Oliver Pohland ◽  
J. Murray Gibson

The nucleation and initial stage of Pd2Si crystals on Si(111) surface is studied in situ using an Ultra-High Vacuum (UHV) Transmission Electron Microscope (TEM). A modified JEOL 200CX TEM is used for the study. The Si(111) sample is prepared by chemical thinning and is cleaned inside the UHV chamber with base pressure of 1x10−9 τ. A Pd film of 20 Å thick is deposited on to the Si(111) sample in situ using a built-in mini evaporator. This room temperature deposited Pd film is thermally annealed subsequently to form Pd2Si crystals. Surface sensitive dark field imaging is used for the study to reveal the effect of surface and interface steps.The initial growth of the Pd2Si has three stages: nucleation, growth of the nuclei and coalescence of the nuclei. Our experiments shows that the nucleation of the Pd2Si crystal occurs randomly and almost instantaneously on the terraces upon thermal annealing or electron irradiation.


1999 ◽  
Vol 5 (S2) ◽  
pp. 670-671 ◽  
Author(s):  
O.L. Krivanek ◽  
N. Dellby ◽  
A.R. Lupini

Even though two generations of electron microscopists have come to accept that the resolution of their instruments is limited by spherical aberration, three different aberration correctors showing that the aberration can be overcome have recently been built [1-3]. One of these correctors was developed by us specifically for forming small electron probes in a dedicated scanning transmission electron microscope (STEM) [3, 4]. It promises to revolutionize the way STEM instruments are built and the types of problems that they are applied to.As was the case with the Berlin Wall, when a barrier that was once thought immovable finally crumbles, many of the consequences can be quite unexpected. For STEM, the removal of spherical aberration (Cs) as the main resolution limit is likely to lead to a new paradigm in which:1) The resolution at a given operating voltage will improve by about 3x relative to today's best. When Cs can be adjusted arbitrarily in a STEM being used for microanalysis or dark field imaging, defocus and Cs are set to values that optimally oppose the effect of the 5th-order spherical aberration C5.


2020 ◽  
Vol 155 ◽  
pp. 01005
Author(s):  
Weiwei Liu ◽  
Yuanyuan Guo ◽  
Mai Zhang ◽  
Jian Zhang

A Re-containing single-crystal superalloy was used to research the high temperature low stress creep behavior. Transmission electron microscope, scanning electron microscope and some other research methods are employed. The results and analysis are summarized below: Two mechanisms for the steady creep are found in this experiment. The volume fraction of pores after creep test at 1100°C increased more than 2 times compared with that before test, but the increasing at 1000°C is relatively small, which reveals that temperature has an great influence on the formation of pore during creep; There are two types of pores associated with fracture during the creep process. One is the casting shrinkage located between the interdentritic, which is formed in the solidification of the alloy. Another type of pore is nucleated and growing during the creep deformation.


2007 ◽  
Vol 62 (8) ◽  
pp. 1059-1070 ◽  
Author(s):  
Marco Wendorff ◽  
Caroline Röhr

In the ternary system Ba-Al-Ge new intermetallic compounds which are lying on or close to the binary section BaAl2 -BaGe2 were synthesized from the elements and characterized on the basis of X-ray single crystal data. The Al-content x in the compounds BaAlxGe2−x forming the AlB2 structure type ranges from x = 1.4 [BaAl1.4Ge0.6 space group P6/mmm, a = 443.5(1), c = 512.4(1) pm, Z = 1, R1 = 0.0222] to the stoichiometric ordered compound BaAlGe [space group P6̅m2, a = 434.9(1), c = 513.6 pm, Z = 1, R1 = 0.0252]. In the two new Ge-rich barium intermetallics Ba5Al2Ge7 [space group C2/m, a = 859.8(4), b = 1031.5(4), c = 1847.8(6) pm, β = 103.23(3)°, Z = 4, R1 = 0.0553] and Ba7Al4Ge9 [space group Fmm2, a = 1032.7(5), b = 2559(2), c = 862.1(4) pm, Z = 4, R1 = 0.1197] complex Al/Ge polyanions are present, which consist of (1) Al/Ge-ribbons of condensed planar sixmembered rings comparable to the anions in Ba3Al2Ge2, and (2) [Ge/Al]5 clusters comparable to the anions in the tetrelides Ba3M5. The building units (1) and (2) are connected via Al-Ge bonds to form complex ribbons in the case of Ba5Al2Ge7 and sheets in the case of Ba7Al4Ge9. The electron count in the two compounds supports an interpretation of the structures according to the Zintl concept and the Wades rules. The small formal electron excess, caused by the incomplete transfer of charge from Ba towards the Al/Ge polyanions, decreases with the Ge content of the compound.


2009 ◽  
Vol 15 (S2) ◽  
pp. 1082-1083
Author(s):  
D Masiel ◽  
B Reed ◽  
T LaGrange ◽  
ND Browning

Extended abstract of a paper presented at Microscopy and Microanalysis 2009 in Richmond, Virginia, USA, July 26 – July 30, 2009


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