Combined Use of Structure Imaging and Microanalysis in Structure-Composition Analysis By A 400-KV High-Resolution Analytical Electron Microscope

Author(s):  
Yoshio Bando ◽  
Yoshizo Kitami ◽  
Mamoru Mitcmo

One of the limitations in the use of the conventional analytical electron microscope (AEM) with lower voltages of 100 to 200 kV is based on its poor image resolution compared to normal transmission electron microscope. Because of this, it is difficult to carry out structure determination by directly observing individual atom arrangements in crystals. However, a new AEM with an intermediate voltage of 400 kV (JEM-4000EX, TEMSCAN) is fully capable of high resolution observation under equipment of an energy dispersive x-ray spectrometer (EDS) and an electron energy loss spectrometer (EELS). The present paper shows crystal structure images of sialon polytypes and corresponding EDS and EELS spectra, and describes the usefullness of combined techniques of structure imaging and microanalysis in structure-composition determination.

Author(s):  
Y. Bando ◽  
Y. Matsui ◽  
Y. Kitami ◽  
Y. Inomata ◽  
T. Oikawa ◽  
...  

There are some fundamental limitations in the use of the conventional analytical electron microscope (AEM), which restricts notably observation capabilities of high resolution imaging and microanalysis, mainly due to its poor image resolution and low peak to background ratio in EDS and EELS spectra, because operating voltages are lower in the range of 100 to 200 kV. It can be expected that such observation capabilities are very much improved with the increase of the accelerating voltage. From the point of view, a new JEM-4000EX AEM with an intermediate voltage of 400 kV is much prefered. The present paper describes some advantages of the 400 kV high resolution AEM in the use of both high resolution observation and microanalysis in EDS and EELS.Fig.1 shows a phase contrast transfer function (CTF) curve, obtained for the JEM-4000EX with full analytical systems, in which a side entry specimen holder of beryllium stage with tilting angles of 30° in X-Y double axes is used. The EDS detector with a high angle location of 68, an energy analyzer (ASEA40) and a scanning image device (ASID40) are attached to the column.


1998 ◽  
Vol 4 (S2) ◽  
pp. 184-185
Author(s):  
J. A. Small ◽  
J. A. Armstrong ◽  
D. S. Bright ◽  
B. B. Thorne

The addition of the Si-Li detector to the electron probe, the scanning electron microscope, and more recently the transmission electron microscope (resulting in the analytical electron microscope) has made it possible to obtain elemental analysis on individual “particles” with dimensions less than 1 nm using EDS. Although some initial particle studies on micrometer-sized particles were done on the electron probe using wavelength dispersive spectrometers, WDS, the variability and complexity of many particle compositions coupled with the high currents necessary for WDS made elemental analysis of particles by WDS difficult at best. In addition, the use of multiple spectrometers, each with a different view of the particle and therefore different particle geometry as shown in Fig. 1, limited the quantitative capabilities of the technique. With the introduction of the Si-Li detector, there was only one spectrometer with a single geometry resulting in the development of various procedures for obtaining quantitative elemental analysis of the individual particles.


Author(s):  
Kurio Fukushima ◽  
Yoshihiro Arai ◽  
Masahiro Kawasaki ◽  
Yasushi Kokubo

Intended for atomic-level observation and analysis in the material science field, a 300 kV ultrahigh resolution analytical electron microscope (UHRAEM) has been newly developed on the basis of the JEM-2010, a 200 kV UHRAEM. There are two versions: the UHR version, intended for ultrahigh resolution observation with a point resolution of 0.17 nm and the multi-purpose HT version, featuring specimen tilt angles as large as± 40° , and heating and cooling holders. The external view of the instrument is shown in Fig.1. Some characteristic features of the 300 kV UHRAEM are shown as follows.Electron Gun: An extremely stable and compact 300 kV election gun is constructed with 10-stage accelerating tube. SF6 gas is used for electric insulation.


1984 ◽  
Vol 41 ◽  
Author(s):  
J. Bentley ◽  
E. A. Kenik ◽  
P. Angelini ◽  
A. T. Fisher ◽  
P. S. Sklad ◽  
...  

AbstractPreliminary results on the performance of an analytical electron microscope (AEM) operating at 300 kV have been obtained and compared with the performance at 100 kV. Some features of the anticipated improvements for transmission electron microscopy (TEM) imaging, convergent beam electron diffraction (CBED), energy dispersive X-ray spectroscopy (EDS), and electron energy loss spectroscopy (EELS) have been studied from the aspect of materials science applications. The electron microscope used was a Philips EM430T operated with a LaB6 cathode and equipped with EDAX 9100/70 EDS and Gatan 607 EELS systems.


1998 ◽  
Vol 4 (S2) ◽  
pp. 212-213
Author(s):  
R.D. Leapman ◽  
C.R. Swyt-Thomas ◽  
D. v. Agoston ◽  
N. Pivovarova ◽  
S.B. Andrews

In high-resolution biological energy-dispersive x-ray (EDX) microanalysis it is often necessary to measure very low elemental concentrations. As an example, calcium, a physiologically important element, typically occurs in subcellular compartments at concentrations of 10-100 atomic parts per million (corresponding to 1-10 millimole/kg dry weight of sample) and it is ultimately desirable to measure the concentration of this element with a standard error of ±1 atomic ppm (or ± 0.1 millimole/kg). Detection of calcium in biological specimens is further complicated by the presence of relatively high levels of potassium (around 0.5 atomic % or 500 millimole/kg), which gives rise to overlap of the K Kβ and Ca Kα peaks in the EDX spectrum. Counting statistics are frequently the limiting factor for detectability, but this is not necessarily the case because in the analytical electron microscope it is possible to collect spectra for long periods using a high probe current.


1998 ◽  
Vol 4 (S2) ◽  
pp. 186-187
Author(s):  
J. R. Michael

Energy-dispersive x-ray spectrometry (EDS) with a SiLi detector has become a standard technique in the analytical electron microscope (AEM). There have been many difficulties to overcome involving both the interfacing of the spectrometer to the microscope and in developing robust techniques for quantitative analysis of thin specimens. The AEM is a difficult environment for EDS due to the high accelerating voltages (100-400 kV) typically used and due to constraints on detector placement relative to the specimen as a result of the confined space within the specimen region of the AEM. The first published account of the installation of SiLi EDS on a transmission electron microscope (TEM) occurred in 1969. In this paper and subsequent publications, these authors described many of the difficulties that still haunt EDS in the AEM.The initial attempts at interfacing EDS to a TEM column demonstrated that the. specimen stage of a TEM was not ideal for this purpose.


Author(s):  
J. Bentley ◽  
A. T. Fisher ◽  
E. A. Kenik ◽  
Z. L. Wang

The introduction by several manufacturers of 200kV transmission electron microscopes (TEM) equipped with field emission guns affords the opportunity to assess their potential impact on materials science by examining applications of similar 100-120kV instruments that have been in use for more than a decade. This summary is based on results from a Philips EM400T/FEG configured as an analytical electron microscope (AEM) with a 6585 scanning transmission (STEM) unit, ED AX 9100/70 or 9900 energy dispersive X-ray spectroscopy (EDS) systems, and Gatan 607 serial- or 666 parallel-detection electron energy-loss spectrometers (EELS). Examples in four areas that illustrate applications that are impossible or so difficult as to be impracticable with conventional thermionic electron guns are described below.


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