Distortion in lattice-resolution scanned-probe microscope images

Author(s):  
L. Fei

Scanned probe microscopes (SPM) have been widely used for studying the structure of a variety material surfaces and thin films. Interpretation of SPM images, however, remains a debatable subject at best. Unlike electron microscopes (EMs) where diffraction patterns and images regularly provide data on lattice spacings and angles within 1-2% and ∽1° accuracy, our experience indicates that lattice distances and angles in raw SPM images can be off by as much as 10% and ∽6°, respectively. Because SPM images can be affected by processes like the coupling between fast and slow scan direction, hysteresis of piezoelectric scanner, thermal drift, anisotropic tip and sample interaction, etc., the causes for such a large discrepancy maybe complex even though manufacturers suggest that the correction can be done through only instrument calibration.We show here that scanning repulsive force microscope (SFM or AFM) images of freshly cleaved mica, a substrate material used for thin film studies as well as for SFM instrument calibration, are distorted compared with the lattice structure expected for mica.

Author(s):  
A. Zangvil ◽  
L.J. Gauckler ◽  
G. Schneider ◽  
M. Rühle

The use of high temperature special ceramics which are usually complex materials based on oxides, nitrides, carbides and borides of silicon and aluminum, is critically dependent on their thermomechanical and other physical properties. The investigations of the phase diagrams, crystal structures and microstructural features are essential for better understanding of the macro-properties. Phase diagrams and crystal structures have been studied mainly by X-ray diffraction (XRD). Transmission electron microscopy (TEM) has contributed to this field to a very limited extent; it has been used more extensively in the study of microstructure, phase transformations and lattice defects. Often only TEM can give solutions to numerous problems in the above fields, since the various phases exist in extremely fine grains and subgrain structures; single crystals of appreciable size are often not available. Examples with some of our experimental results from two multicomponent systems are presented here. The standard ion thinning technique was used for the preparation of thin foil samples, which were then investigated with JEOL 200A and Siemens ELMISKOP 102 (for the lattice resolution work) electron microscopes.


Author(s):  
Jan-Olov Bovin ◽  
Osamu Terasaki ◽  
Jan-Olle Malm ◽  
Sven Lidin ◽  
Sten Andersson

High resolution transmission electron microscopy (HRTEM) is playing an important role in identifying the new icosahedral phases. The selected area diffraction patterns of quasi crystals, recorded with an aperture of the radius of many thousands of Ångströms, consist of dense arrays of well defined sharp spots with five fold dilatation symmetry which makes the interpretation of the diffraction process and the resulting images different from those invoked for usual crystals. The atomic structure of the quasi crystals is not established even if several models are proposed. The correct structure model must of course explain the electron diffraction patterns with 5-, 3- and 2-fold symmetry for the phases but it is also important that the HRTEM images of the alloys match the computer simulated images from the model. We have studied quasi crystals of the alloy Al65Cu20Fe15. The electron microscopes used to obtain high resolution electro micrographs and electron diffraction patterns (EDP) were a (S)TEM JEM-2000FX equipped with EDS and PEELS showing a structural resolution of 2.7 Å and a IVEM JEM-4000EX with a UHP40 high resolution pole piece operated at 400 kV and with a structural resolution of 1.6 Å. This microscope is used with a Gatan 622 TV system with an image intensifier, coupled to a YAG screen. It was found that the crystals of the quasi crystalline materials here investigated were more sensitive to beam damage using 400 kV as electron accelerating voltage than when using 200 kV. Low dose techniques were therefore applied to avoid damage of the structure.


2020 ◽  
Author(s):  
Kiyofumi Takaba ◽  
Saori Maki-Yonekura ◽  
Koji Yonekura

AbstractA semi-automated protocol has been developed for rotational data collection of electron diffraction patterns by combined use of SerialEM and ParallEM, where SerialEM is used for positioning of sample crystals and ParallEM for rotational data collection. ParallEM calls standard camera control software through an AutoIt script, which adapts to software operational changes and to new GUI programs guiding other cameras. Development included periodic flashing and pausing of data collection during overnight or day-long recording with a cold field-emission beam. The protocol proved to be efficient and accurate in data collection of large-scale rotational series from two JEOL electron microscopes, a general-purpose JEM-2100 and a high-end CRYO ARM 300. Efficiency resulted from simpler steps and task specialization. It is possible to collect 12–20 rotational series from ∼ −68º to ∼ 68º at a rotation speed of 1º /s in one hour without human supervision.


1997 ◽  
Vol 3 (S2) ◽  
pp. 1017-1018
Author(s):  
L. E. Thomas ◽  
R. C. Hugo ◽  
J. T. Stanley

Electron diffraction patterns taken in transmission electron microscopes are widely used for phase identification and orientation determination of crystallites as small as hundreds or even tens of nanometers in size. The analyses typically require rather tedious measurement of the patterns, and matching of calculated d-spacings and angles with those of known phases. Recently, the analysis of these patterns has been facilitated by powerful desktop computer programs that use digitally captured images for on-line measurement and simulation matching of" the diffraction spot and Kikuchi line patterns. This presentation will illustrate an application of computer-aided pattern simulation and matching for precise determination of crystal orientations.Two experimental TV camera arrangements were used to record diffraction patterns in a TEM. These included a cooled-CCD camera located on the electron optical axis below the microscope viewing chamber, and a simple TV-rate CCD that recorded directly from the inclined fluorescent viewing screen of the microscope.


1993 ◽  
Vol 294 (3) ◽  
pp. A670
Author(s):  
DavidJ. Keller ◽  
FransiskaS. Franke

2001 ◽  
Vol 16 (12) ◽  
pp. 3361-3365 ◽  
Author(s):  
Yuan-fang Liu ◽  
Jing-hui Zeng ◽  
Wei-xin Zhang ◽  
Wei-chao Yu ◽  
Yi-tai Qian ◽  
...  

Nanorods Bi3Se4 were synthesized directly through the reaction between BiCl3 and elemental selenium in an autoclave with hydrazine hydrate as solvent at 165 °C for 10 h. X-ray powder diffraction patterns, x-ray photoelectron spectra, and transmission electron microscope images show that the products are well-crystallized hexagonal Bi3Se4 nanorods. The solvent hydrazine hydrate played an important role in formation and growth of Bi3Se4 nanorods. The possible reaction mechanism was proposed.


1992 ◽  
Vol 281 ◽  
Author(s):  
X. W. Wang ◽  
D. J. Finnigan ◽  
R. Noble ◽  
P. Mattocks

ABSTRACTThere are two phases of CdS, wurtzite (hexagonal) and zincblende (cubic). To the best of our knowledge there is no report on the growth of large single crystal cubic CdS. Although there have been reports on the vapor deposition of cubic dominated CdS thin films, physical measurements were limited. Substrate material has been considered as the primary factor in attaining the cubic dominated CdS thin films. We report new results on CW Nd:YAG laser deposition of CdS thin films at various temperatures. X-ray diffraction patterns show that the films deposited at 200°C have a dominant cubic phase, those at 400°C being hexagonal. Optical transmission measurements reveal room temperature absorption edges of 515nm and 500nm for films deposited at 200°C and 400°C, respectively. Transmission electron microscopy further reveals differences in crystal structure of the two films. Raman spectra of the cubic film is similar to that of the hexagonal film.


A type IaB diamond specimen containing partially decomposed platelets, dislocation loops and voidites has been investigated by transmission electron microscopy. The dislocation loops were found to be prismatic and interstitial in nature, some with Burgers vector ½ a <110> previously reported, but most with Burgers vector a <001>. Burgers vector analysis of the bounding dislocation of partially decomposed platelets shows that the a <001> loops are formed by transformation of the platelets, by nucleation and climb of a <00(1— f )> dislocation, combining with the a <00 f > dislocation bounding the platelet. The climb mechanism is driven by the need to generate vacancies for the decomposition of the platelets and to accommodate the nitrogen either in small clusters in solution in the lattice or in voidites. Glide dislocations interacting with the platelets are likely to act as nucleating centres for the climb process. The ½ a <110> dislocation loops are considered to be formed by dissociation of the a <001> loops, promoted by interaction with glide dislocations and involving prismatic slip and conservative climb. Voidites are assumed to originate as bubbles of fluid nitrogen formed at high pressure and temperature as a result of decomposition of the platelets; at room temperature they may be liquid or solid depending on the pressure, which cannot be estimated accurately. Electron diffraction patterns and microscope images of voidites prove that many consist of a solid phase at 300 K. It is suggested that the diamond has been subjected to a drop in pressure at high temperature, causing platelet decomposition and the generation of voidites, that may occur during ejection of the diamond to the earth’s surface.


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