scholarly journals High Resolution Powder Electron Diffraction in Scanning Electron Microscopy

Materials ◽  
2021 ◽  
Vol 14 (24) ◽  
pp. 7550
Author(s):  
Miroslav Slouf ◽  
Radim Skoupy ◽  
Ewa Pavlova ◽  
Vladislav Krzyzanek

A modern scanning electron microscope equipped with a pixelated detector of transmitted electrons can record a four-dimensional (4D) dataset containing a two-dimensional (2D) array of 2D nanobeam electron diffraction patterns; this is known as a four-dimensional scanning transmission electron microscopy (4D-STEM). In this work, we introduce a new version of our method called 4D-STEM/PNBD (powder nanobeam diffraction), which yields high-resolution powder diffractograms, whose quality is fully comparable to standard TEM/SAED (selected-area electron diffraction) patterns. Our method converts a complex 4D-STEM dataset measured on a nanocrystalline material to a single 2D powder electron diffractogram, which is easy to process with standard software. The original version of 4D-STEM/PNBD method, which suffered from low resolution, was improved in three important areas: (i) an optimized data collection protocol enables the experimental determination of the point spread function (PSF) of the primary electron beam, (ii) an improved data processing combines an entropy-based filtering of the whole dataset with a PSF-deconvolution of the individual 2D diffractograms and (iii) completely re-written software automates all calculations and requires just a minimal user input. The new method was applied to Au, TbF3 and TiO2 nanocrystals and the resolution of the 4D-STEM/PNBD diffractograms was even slightly better than that of TEM/SAED.

Nanomaterials ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 962
Author(s):  
Miroslav Slouf ◽  
Radim Skoupy ◽  
Ewa Pavlova ◽  
Vladislav Krzyzanek

We introduce a novel scanning electron microscopy (SEM) method which yields powder electron diffraction patterns. The only requirement is that the SEM microscope must be equipped with a pixelated detector of transmitted electrons. The pixelated detectors for SEM have been commercialized recently. They can be used routinely to collect a high number of electron diffraction patterns from individual nanocrystals and/or locations (this is called four-dimensional scanning transmission electron microscopy (4D-STEM), as we obtain two-dimensional (2D) information for each pixel of the 2D scanning array). Nevertheless, the individual 4D-STEM diffractograms are difficult to analyze due to the random orientation of nanocrystalline material. In our method, all individual diffractograms (showing randomly oriented diffraction spots from a few nanocrystals) are combined into one composite diffraction pattern (showing diffraction rings typical of polycrystalline/powder materials). The final powder diffraction pattern can be analyzed by means of standard programs for TEM/SAED (Selected-Area Electron Diffraction). We called our new method 4D-STEM/PNBD (Powder NanoBeam Diffraction) and applied it to three different systems: Au nano-islands (well diffracting nanocrystals with size ~20 nm), small TbF3 nanocrystals (size < 5 nm), and large NaYF4 nanocrystals (size > 100 nm). In all three cases, the STEM/PNBD results were comparable to those obtained from TEM/SAED. Therefore, the 4D-STEM/PNBD method enables fast and simple analysis of nanocrystalline materials, which opens quite new possibilities in the field of SEM.


2011 ◽  
Vol 189-193 ◽  
pp. 1036-1039
Author(s):  
Jing Ling Ma ◽  
Jiu Ba Wen ◽  
Yan Fu Yan

The precipitates of Al-5Zn-0.02In-1Mg-0.05Ti-0.5Ce (wt %) anode alloy were studied by scanning electron microscopy, X-ray microanalysis, high resolution transmission electron microscopy and selected area electron diffraction analyses in the present work. The results show that the alloy mainly contains hexagonal structure MgZn2 and tetragonal structure Al2CeZn2 precipitates. From high resolution transmission electron microscopy and selected area electron diffraction, aluminium, Al2CeZn2 and MgZn2 phases have [0 1 -1]Al|| [1 -10]Al2CeZn2|| [-1 1 0 1]MgZn2orientation relation, and Al2CeZn2 and MgZn2 phases have the [0 2 -1]Al2CeZn2|| [0 1 -10]MgZn2orientation relation.


Minerals ◽  
2019 ◽  
Vol 9 (4) ◽  
pp. 206 ◽  
Author(s):  
James Hower ◽  
Dali Qian ◽  
Nicolas Briot ◽  
Eduardo Santillan-Jimenez ◽  
Madison Hood ◽  
...  

Fly ash from the combustion of eastern Kentucky Fire Clay coal in a southeastern United States pulverized-coal power plant was studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). TEM combined with elemental analysis via energy dispersive X-ray spectroscopy (EDS) showed that rare earth elements (REE; specifically, La, Ce, Nd, Pr, and Sm) were distributed within glassy particles. In certain cases, the REE were accompanied by phosphorous, suggesting a monazite or similar mineral form. However, the electron diffraction patterns of apparent phosphate minerals were not definitive, and P-lean regions of the glass consisted of amorphous phases. Therefore, the distribution of the REE in the fly ash seemed to be in the form of TEM-visible nano-scale crystalline minerals, with additional distributions corresponding to overlapping ultra-fine minerals and even true atomic dispersion within the fly ash glass.


1993 ◽  
Vol 8 (7) ◽  
pp. 1473-1476 ◽  
Author(s):  
B. Grushko

The decagonal phase was studied by transmission and scanning electron microscopy in an Al62Cu24Co14 alloy annealed at 550–850 °C. The electron diffraction patterns of the decagonal phase exhibited weak quasiperiodic odd-n reflections in the [1-2100] zone axis corresponding to the equilibrated structure. The relative intensities of these reflections were significantly lower in the Al62Cu24Co14 than in the Al68Cu11Co21 decagonal phase. Diffuse scattering observed previously at the same positions can be related to a nonequilibrium state of the decagonal phase.


2001 ◽  
Vol 16 (1) ◽  
pp. 101-107 ◽  
Author(s):  
Takeo Oku ◽  
Jan-Olov Bovin ◽  
Iwami Higashi ◽  
Takaho Tanaka ◽  
Yoshio Ishizawa

Atomic positions for Y atoms were determined by using high-resolution electron microscopy and electron diffraction. A slow-scan charge-coupled device camera which had high linearity and electron sensitivity was used to record high-resolution images and electron diffraction patterns digitally. Crystallographic image processing was applied for image analysis, which provided more accurate, averaged Y atom positions. In addition, atomic disordering positions in YB56 were detected from the differential images between observed and simulated images based on x-ray data, which were B24 clusters around the Y-holes. The present work indicates that the structure analysis combined with digital high-resolution electron microscopy, electron diffraction, and differential images is useful for the evaluation of atomic positions and disordering in the boron-based crystals.


2013 ◽  
Vol 456 ◽  
pp. 533-536
Author(s):  
Yan Zhi Lou

In this paper, high resolution electron microscopy (HREM) was used to observe nanosized Fe2M precipitates in M50NiL steel, and crystal structure of which was also investigated by selected area electron diffraction (SAED). At the same time, the orientation relationship between the Fe2M and the martensite matrix was also studied. The results suggested that crystal structure of Fe2M is close-packed hexagonal, and lattice parameters about a=b=0.473nm, c=0.772nm, α=β=90°, γ=120°. The orientation relationship between the nanoprecipitates Fe2M and martensite is and .


Author(s):  
T. Nagatani

Although the main development of scanning electron microscopy (SEM) has been accomplished mostly by the Cambridge group and it has not been changed so much for about two decades, it should be noted that there have been two important developments to pursuing high resolution of better than 1nm.Most notably, use of a field emission gun developed by Crewe et al for the scanning transmission electron microscope (STEM) to form a fine electron beam has been most effective in SEMs due to its high brightness and low energy spread. Thus, several models of field emission (FE) SEMs have been developed in the early ’70s and commercialized with a resolution of 2∼3nm at around 30kV.The second development is to use a highly excited objective lens. The specimen has to be set inside the pole-pieces (so-called “in-lens” type).


Author(s):  
Kenneth H. Downing ◽  
Robert M. Glaeser

The contrast observed in images of beam-sensitive, crystalline specimens is found to be significantly less than one would predict based on observations of electron diffraction patterns of the specimens. Factors such as finite coherence, inelastic scattering, and the limited MTF of the photographic emulsion account for some decrease in contrast. It appears, however, that most of the loss in signal is caused by motion of the specimen during exposure to the electron beam. The introduction of point and other defects in the crystal, resulting from radiation damage, causes bending and lateral motion, which degrade the contrast in the image. We have therefore sought to determine whether the beam-induced specimen motion can be reduced by reducing the area of the specimen which is illuminated at any one time.


Materials containing planar boundaries are of general interest and complete understanding of their structures is important. When direct imaging of the boundaries by, for instance, high-resolution electron microscopy, is impracticable, details of their structure and arrangement may be obtained from electron diffraction patterns. Such patterns are discussed in terms of those from intergrowth tungsten bronzes as specific examples. Fourier-transform calculations for proposed structures have been made to establish, in conjunction with optical-diffraction analogues, the features of the far-field diffraction patterns. These results have been compared with diffraction patterns obtained experimentally by transmission electron microscopy. The aim of the study, to show that the arrangement of the boundaries in these complicated phases can be deduced from their diffraction patterns without the need for high-resolution imaging, has been achieved. The steps to be taken to make these deductions are set out.


2009 ◽  
Vol 42 (2) ◽  
pp. 242-252 ◽  
Author(s):  
Cyril Cayron ◽  
Martien Den Hertog ◽  
Laurence Latu-Romain ◽  
Céline Mouchet ◽  
Christopher Secouard ◽  
...  

Odd electron diffraction patterns (EDPs) have been obtained by transmission electron microscopy (TEM) on silicon nanowires grownviathe vapour–liquid–solid method and on silicon thin films deposited by electron beam evaporation. Many explanations have been given in the past, without consensus among the scientific community: size artifacts, twinning artifacts or, more widely accepted, the existence of new hexagonal Si phases. In order to resolve this issue, the microstructures of Si nanowires and Si thin films have been characterized by TEM, high-resolution transmission electron microscopy (HRTEM) and high-resolution scanning transmission electron microscopy. Despite the differences in the geometries and elaboration processes, the EDPs of the materials show great similarities. The different hypotheses reported in the literature have been investigated. It was found that the positions of the diffraction spots in the EDPs could be reproduced by simulating a hexagonal structure withc/a= 12(2/3)1/2, but the intensities in many EDPs remained unexplained. Finally, it was established that all the experimental data,i.e.EDPs and HRTEM images, agree with a classical cubic silicon structure containing two microstructural defects: (i) overlapping Σ3 microtwins which induce extra spots by double diffraction, and (ii) nanotwins which induce extra spots as a result of streaking effects. It is concluded that there is no hexagonal phase in the Si nanowires and the Si thin films presented in this work.


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