X-Ray Energy Dispersive Spectroscopy in the Environmental Scanning Electron Microscope

1998 ◽  
Vol 4 (S2) ◽  
pp. 182-183
Author(s):  
John F. Mansfield ◽  
Brett L. Pennington

The environmental scanning electron microscope (Environmental SEM) has proved to be a powerful tool in both materials science and the life sciences. Full characterization of materials in the environmental SEM often requires chemical analysis by X-ray energy dispersive spectroscopy (XEDS). However, the spatial resolution of the XEDS signal can be severely degraded by the gaseous environment in the sample chamber. At an operating pressure of 5Torr a significant fraction of the primary electron beam is scattered after it passes through the final pressure limiting aperture and before it strikes the sample. Bolon and Griffin have both published data that illustrates this effect very well. Bolon revealed that 45% of the primary electron beam was scattered by more than 25 μm in an Environmental SEM operating at an accelerating voltage of 30kV, with a water vapor pressure of 3Torr and a working distance of 15mm.

1997 ◽  
Vol 3 (S2) ◽  
pp. 1207-1208
Author(s):  
John Mansfield

Full characterization of materials in the environmental scanning electron microscope (Environmental SEM) often requires chemical analysis by X-ray energy dispersive spectroscopy (XEDS). However, a major problem arises because the spatial resolution of the XEDS signal is severely degraded by the gaseous environment in the sample chamber. The significant fraction of the primary electron beam is scattered after it passes through the final pressure limiting aperture and before it strikes the sample. Bolon and Griffin have both published data that illustrates this effect very well. Bolon revealed that 45% of the primary electron beam was scattered by more than 25μm in an Environmental SEM operating at an accelerating voltage of 30kV, with a water vapor pressure of 3Torr and a working distance of 15mm. Griffin’s work demonstrated that even at higher voltages (30 kV), shorter working distances (<10mm) and lower chamber pressures (2Torr), there is a significant fraction of the electron beam scattered out to over 400 μm away from the point where the primary beam strikes the sample.


Author(s):  
H. Soezima

There are few investigations discussed on resolution of the signals as spatial resolving power, at the scanning electron microscope analysis. There remains misunderstanding that better resolution is obtained only by making a primary electron beam diameter small. At the scanning electron microscope analysis, there are such signals as secondary electron, back scattered electron, absorbed electron, transmitted electron, auger electron, cathode luminescence and X-rays. The spatial resolutions of these signals are effected not only by primary electron diameter but also by accelerating voltage, sample density, electro conductivity of the sample, surface condition of the sample, relative position among the primary electron optics, sample and detection system, energy of the signals, potential and magnetic distribution, and current density distribution of primary electron beam.Some examples of the X-rays, that have the poorest resolving power in the signals, are shown below.


Author(s):  
W. Brünger

Reconstructive tomography is a new technique in diagnostic radiology for imaging cross-sectional planes of the human body /1/. A collimated beam of X-rays is scanned through a thin slice of the body and the transmitted intensity is recorded by a detector giving a linear shadow graph or projection (see fig. 1). Many of these projections at different angles are used to reconstruct the body-layer, usually with the aid of a computer. The picture element size of present tomographic scanners is approximately 1.1 mm2.Micro tomography can be realized using the very fine X-ray source generated by the focused electron beam of a scanning electron microscope (see fig. 2). The translation of the X-ray source is done by a line scan of the electron beam on a polished target surface /2/. Projections at different angles are produced by rotating the object.During the registration of a single scan the electron beam is deflected in one direction only, while both deflections are operating in the display tube.


2020 ◽  
Vol 16 (2) ◽  
pp. 12
Author(s):  
Solihudin Solihudin ◽  
Haryono Haryono ◽  
Atiek Rostika Noviyanti ◽  
Muhammad Rizky Ridwansyah

<p>Komposit forsterit-karbon merupakan salah satu material modifikasi dari forsterit yang berpotensi memiliki sifat isolator panas baik. Karbon dalam komposit dapat mengisi cacat titik pada kristal forsterit. Arang sekam padi (residu gasifikasi) mengandung SiO2 amorf dan karbon yang tinggi. Penelitian ini bertujuan menentukan pengaruh suhu kalsinasi dalam medium gas inert (dengan pengaliran gas argon) terhadap karakteristik komposit forsterit-karbon dari arang sekam padi dan magnesium karbonat. Metode penelitian meliputi preparasi arang sekam padi hasil gasifikasi, dan sintesis forsterit-karbon. Proses sintesis komposit forsterit karbon dilakukan dengan cara mencampurkan arang sekam padi dengan kalium karbonat pada rasio mol magmesium terhadap silikon sebesar 2 : 1 kemudian dikalsinasi dengan suhu divariasikan (700, 800, 900, dan 1000 oC). Selanjutnya sampel hasil sintesis dikarakterisasi dengan Fourier-transform infrared (FTIR), X-ray diffraction (XRD), dan scanning electron microscope-energy dispersive spectroscopy (SEM-EDS). Hasil karakterisasi dengan FTIR dan XRD diperoleh kesimpulan bahwa forsterit mulai terbentuk pada suhu kalisiasi 800 oC dan sempurna pada suhu 1000 oC, karenanya komposit yang terbentuk pada 1000 oC dimungkinkan sebagai forsterit-karbon, di mana unsur-unsur yang terkandung ditunjukkan oleh SEM-EDS.</p><p> </p><p><strong>The Effect of Calcination Temperature on the Characteristics of Forsterite-Carbon Composites Synthesized in Argon Gas Medium</strong>. Forsterite-carbon composite is one of the material modifications of forsterite, which potentially has a good heat insulation property. Carbon in composites can fill point defects in forsterite crystals. Rice husk charcoal, as gasification residues, contains high amorphous SiO2 and carbon. This study aims to determine the effect of temperature on the calcination of a mixture of rice husk charcoal and magnesium carbonate under an inert gas (argon gas) on the characteristics of the forsterite-carbon composite produced. The experimental research performed includes the preparation of gasified rice husk charcoal and the synthesis of the carbon-forsterite composite. The synthesis process of the carbon-forsterite composites was carried out by mixing rice husk charcoal with potassium carbonate at a mole ratio of magnesium to silicon of 2 : 1. The mixture was then calcined with varying temperatures (700, 800, 900, and 1000 °C). Furthermore, the synthesized sample was characterized by Fourier-transform infrared (FTIR), X-ray diffraction (XRD), and scanning electron microscope-energy dispersive spectroscopy (SEM-EDS). The FTIR and XRD analysis show that the forsterites began to form at a calcination temperature of 800 °C and perfectly formed at a temperature of 1000 °C; therefore, the composite formed at 1000 °C is possible as forsterite-carbon, in which the contained elements were indicated by SEM-EDS.</p>


1997 ◽  
Vol 3 (S2) ◽  
pp. 385-386 ◽  
Author(s):  
Brendan J. Griffin

The environmental SEM is an extremely adaptive instrument, allowing a range of materials to be examined under a wide variety of conditions. The limitations of the instrument lie mainly with the restrictions imposed by the need to maintain a moderate vacuum around the electron gun. The primary effect of this has been, in a practical sense, the limited low magnification available. Recently this has been overcome by modifications to the final pressure limiting aperture and secondary electron detector (Fig.l). The modifications are simple and users should be brave in this regard.A variety of electron detectors now exist including various secondary, backscattered and cathodoluminescence systems (Figs 2-5). These provide an excellent range of options; the ESEM must be regarded as a conventional SEM in that a range of imaging options should be installed. In some cases, e.g. cathodoluminescence, the lack of coating provides an advantage unique to the low vacuum SEMs.


1998 ◽  
Vol 510 ◽  
Author(s):  
S.A. McHugo ◽  
A.C. Thompson ◽  
H. Padmore

AbstractWe present x-ray fluorescence (XRF) results from studies of metal impurities in silicon. A synchrotron-based XRF microprobe, with μm spatial resolution, was used to detect and map the impurities. The sensitivity of the XRF microprobe was determined for copper and iron in silicon using well-characterized standard samples. We have concluded the system can detect one iron or copper precipitate in silicon with a radius of ≈14nm. This sensitivity pertains to other relevant impurities in silicon, such as, chromium, manganese, cobalt, nickel and gold. Furthermore, we have detected and spatially mapped metal impurity precipitates in silicon, which are undetectable by Energy Dispersive Spectroscopy in a Scanning Electron Microscope. These results exhibit the extraordinary sensitivity of the XRF microprobe for metal impurities in semiconductors.


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