Energy-Dispersive X-Ray Spectros
Energy-Dispersive X-Ray Spectros
Energy-Dispersive X-Ray Spectros
Related terms:
Fig. 1. SEM images of the substrate after (a) acetone cleaning, (b) etching and (c)
calcination
Etching of the substrate with hydrochloric acid modified drastically the substrate
surface (Fig. 1.b). This treatment leads to a selective attack of the surface similar to
pitting corrosion, creating small cavities in the surface. However, no chlorine could
be detected on the surface by EDS, which could be explained by the careful rinsing
of the plate after treatment.
Calcination of the stainless steel plates at 700 °C for 8 h resulted in the formation
of an oxide layer, confirmed by EDS. The oxide completely covers the substrate,
although the grain boundaries can still be distinguished. The layer has a porous
structure, as seen in Fig. 1c.
There are two kinds of EDS detectors which are used with AEM. One is a normal
detector (Be-window type) which detects an X-ray through Be-window of about 7-μm
thickness and the other is UTW (ultrathin window)-type detector which detects an
X-ray through the window where a thin plastic film is coated with about 0.1-μm-thick
aluminum. The elements that are heavier than Na (Z = 11) are detectable in case
of Be-window type, because Be film absorbs X-ray, while with the UTW type, the
detectable elements are the ones that are heavier than C (Z = 6). In other words,
with the UTW type, the analysis capability of light elements such as C, N, O, etc. is
the biggest feature. The feature of Be-window type is the high detection efficiency
because it can make an effective area of the detector large.
EDS can provide not only a qualitative analysis but also a quantitative analysis and
it has the feature that elemental analysis can be done easily. However, the utmost
disadvantage is that the energy resolution is as low as about 150 eV. Therefore,
spectrum overlapping occurs and attention will be needed in interpretation.
There are principally two methods in EDS analysis. One is the point analysis method
in which the electron probe is stopped at one point on the specimen by using
TEM/STEM, and an X-ray spectrum is acquired. The other is the elemental mapping
method, which scans two-dimensionally the electron probe on the specimen by
using STEM, modulates the brightness corresponding to the intensity of a certain
characteristic X-ray, synchronizes with a scanning signal, and displays the two-di-
mensional image of the characteristic X-ray intensity on the liquid crystal monitor.
The most advanced AEM with FEG along with a Cs-corrector can focus the minimum
electron probe diameter on the specimen to be 0.1 nm or so. Therefore, the atomic
level point analysis and two-dimension elemental mapping are possible and is widely
used for research in the material science field.
2.2 Methods
X-ray diffraction spectra of the samples were recorded with a PW 1050 Philips
spectrometer with Co K incident radiation. Transmission electron micrographs and
electron dispersion spectroscopy (EDS) analysis were obtained with a Philips CM 12
instrument equipped with Philips 9100 attachment.
UV-vis diffuse reflectance (DR UV-vis) and FTIR spectroscopic measurements were
carried out on the samples put in suitably designed cells permanently attached to
conventional vacuum lines (residual pressure: 1 × 10− 6 Torr; 1 Torr = 133.33 Pa)
allowing all thermal and adsorption-desorption experiments to be carried out in
situ. For DR UV-vis measurements the powder sample was put in an optical quartz
cell. The spectra were recorded by using a Perkin-Elmer Lambda 19 spectropho-
tometer equipped with an integrating sphere and using BaSO4 as reference. For
FTIR measurements, the samples, in form of self-supporting pellets, were placed
in a quartz cell with KBr windows. The spectra were collected with a Bruker IFS 88
instrument (resolution: 4 cm− 1), and were reported in absorbance, having subtracted
the spectrum of the samples before the adsorption. Their intensity was normalized
with respect to the “density” (mg · cm− 2) of the pellets.
Photo-oxidation tests were carried out as described in the literature [14]. Before the
photoreaction, the samples were heated in air up to 673 K, and then evacuated.
Subsequently the samples were treated in oxygen (100 Torr) at 673 K for 1 h, followed
by evacuation at 673 K for 1 h. The photo-oxidation of propene was carried out for
2 h in a closed quartz reaction vessel (123.6 cm3). The temperature of the catalyst
bed was elevated up to 313-323 K by photoirradiation. The reactants were propene
(100 μmol, 15 Torr) and oxygen (200 μmol, 30 Torr). The catalyst (200 mg) was spread
on the flat bottom (12.6 cm2) of the vessel. A 200 W Xe lamp was used as a light
source. Products in gas phase and products desorbed by photoirradiation for 10 min
were analyzed separately by gas chromatography, followed by analysis of desorbed
products by heating at 573 K.
Figure 5.15. HRTEM image and EDS spectra of ball-milled LiAlH4 doped with TiCl3
for 24 h.
RO Membrane Characterization
Ahmad Fauzi Ismail, ... Takeshi Matsuura, in Reverse Osmosis, 2019
Source: Reprinted with permission from Webster et al. [110]. Copyright 2009 Amer-
ican Cancer Society.
Webster et al. [110] used both scanning electron microscopy and EDS in combina-
tion to identify the presence of deca-BDE associated with plastic flakes present in
dust particles. These results indicated that deca-BDE was released to the environ-
ment by physical abrasion or weathering of the original BFR-containing plastic.