Energy-Dispersive X-Ray Spectroscopy

Energy-dispersive X-ray spectroscopy (EDX) is a surface analytical technique where

an electron beam hits the sample, exciting an electron in an inner shell, causing
its ejection and the formation of an electron hole in the electronic structure of the
element.

From: Nanofiber Composites for Biomedical Applications, 2017

Related terms:

High-Resolution Transmission Electron Microscopy, Aluminum Oxide, Titanium

Dioxide, Oxide, Nanowire, Energy-Dispersive Spectroscopy, Microstructure

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troscopy

Synthesis, characterization, and appli-

cations of nanobiomaterials for antimi-
crobial therapy
Chityal Ganesh Kumar, ... Sankalp Vinod Agarwal, in Nanobiomaterials in Antimi-
crobial Therapy, 2016

4.3.7 Energy Dispersive X-Ray Spectroscopy (EDS)

EDS analysis is used to discover the surface elemental composition and estimate
their proportion at different position, consequently giving an overall mapping of the
sample. In this technique, an electron beam strikes on the surface of the test sample.
The energy of the beam is typically in the range of 10–20 keV which causes X-rays to
be emitted from the sample. In general, the energy of the X-rays emitted depends
on the test sample. The electron beam moves across the sample and the images are
obtained for each element. The presence of Au, Ag, and Pd on the NP surface can be
easily identified; however, the low atomic number elements are difficult to detect
using EDS (Duran et al., 2005).

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From Zeolites to Porous MOF Materials

- The 40th Anniversary of International
Zeolite Conference
M. Grill, ... G. Djéga-Mariadassou, in Studies in Surface Science and Catalysis, 2007

3.1. Substrate study

EDS analysis on the stainless steel substrate after cleaning with acetone shows the
presence of Fe, Cr, Ni, O, Mo, Si and C. SEM study of the cleaned substrate reveals
that the stainless steel contains grains sized from 2 to 12 μm, with distinct grain
boundaries (Fig. 1a).

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.

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The Latest Analytical Electron Micro-
scope and its Application to Ceramics
Yoshiyasu Harada, Yuichi Ikuhara, in Handbook of Advanced Ceramics (Second
Edition), 2013

5.1 EDS Analysis

Figure 8 shows the principle of the EDS analysis. By using a semiconductor detector
(SSD: solid state detector) of a high-purity silicon single crystal doped with a trace
of lithium, it can make an elemental analysis by immediately converting all of the
energy of a characteristic X-ray generated from the specimen into a pulse voltage
according to the amplitude of the field-effect transistor (FET), and counting the pulse
number by a multichannel pulse-height analyzer. The spectrum is indicated where
X-ray energy is in horizontal axis and the number of photons is in the vertical axis.
In the EDS system, it is always necessary to cool SSD and FET to liquid nitrogen
temperature in order to suppress their thermal noise.

FIGURE 8. Constitution and block diagram of EDS system.

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.

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Failures of Rotorcraft and Fixed-Wing

Aircraft Aerospace Components
Victor K. Champagne, Marc S. Pepi, in Handbook of Materials Failure Analysis with
Case Studies from the Aerospace and Automotive Industries, 2016

2.1 Discussion of a Utility Helicopter Forward Longeron Failure

The crack initiation site contained an irreconcilable fracture morphology that was
covered with what appeared to be a discontinuous heavy oxide layer. EDS analysis
revealed the presence of a large oxygen concentration as compared to the remaining
fracture surface. The chemical composition of a polished section of the material
was also used for comparative purposes and contained a very small oxygen peak.
Therefore, it was reasonable to deduce that the layer in question was rich in oxygen.
In addition, the thickness of the oxide layer, as well as the physical shape of the
area encompassed by it, suggested that it formed by an alternative means other
than atmospheric corrosion or fretting. The remaining fracture surface contained
the effects of atmospheric corrosion in the form of dark oxide product which was
clearly distinguishable from the oxide contained at the crack origin. Fretting would
have produced minute, dark oxide particles, and which would have been caused by
some type of mechanical action, but this was not observed. The alleged oxide layer
and its morphology were consistent with that of a forming defect, such as a lap.
Further evidence substantiating this claim was the other laps found on the concave
surface of the part during stereoscopic examination (Figures 7.6 and 7.7). A series of
these cracks were located adjacent to the crack origin and extended parallel to the
fracture. Such a defect would have provided a suitable site for fatigue crack initiation
and propagation.

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Oxide-based Systems at the Crossroads

of Chemistry
Gianmario Martra, ... Leonardo Marchese, in Studies in Surface Science and Catal-
ysis, 2001

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.

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Hydrogen Storage Materials

Yoshitsugu Kojima, ... Takayuki Ichikawa, in New and Future Developments in
Catalysis, 2013

5.4.2.5.5 Al-Based Nano-Composite Materials

Figure 5.15 shows a HRTEM image of the LiAlH4 doped with TiCl3 ball-milled for
24 h [135]. The ball-milled specimen that appears in the HRTEM image exhibits
many dark portions, which are several tens of nm. EDS analysis is specific to
the region marked by the square. The EDS results show that the dark portions
of the transmission electron micrograph are attributed to Ti and Al as shown in
Figure 5.15. Since Cl is not observed in the dark portions, the ball-milled LiAlH4
doped with TiCl3 forms a nano-composite material of LiAlH4 and Al–Ti, while Cl
and Al are detected in the light colored portions. The catalytic activity defined by
the H2 desorption capacity by a mechanochemical reaction decreases in the series
TiCl3 > ZrCl4 > VCl3 > NiCl2 > ZnCl2. Transition metal trialuminides Al3X (X = Ti,
Zr, V, Ni) are prepared by the mechanochemical reaction of LiAlH4 and the metal
chlorides, while the reaction of LiAlH4 and ZnCl2 yields Zn. The high catalytic activity
is attributed to the lower percentage d-character and the electronegativity of those
transition metals [135].

Figure 5.15. HRTEM image and EDS spectra of ball-milled LiAlH4 doped with TiCl3
for 24 h.

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Scientific Bases for the Preparation of
Heterogeneous Catalysts
W. Walerczyk, ... J. Okal, in Studies in Surface Science and Catalysis, 2010

2.2 Experimental methods

All samples were studied using X-ray powder diffraction (XRD) to phase identification
and average grain size calculation; XRD patterns, including Small Angel X-Ray
Scattering (SAXS), were detected using X'Pert-Pro PANalytical instrument. Elemen-
tal analysis and the impurity identification were done by using energy dispersive
X-ray (EDS) analysis, EDAX9800. High resolution transmission electron microscopy
(HRTEM) images and selected area electron diffraction (SAED) patterns were done
with Philips CM20 SuperTwin microscope to study morphology and microstructure
of the samples. Nitrogen adsorption-desorption isotherms at -196 °C were collected
using an Autosorb-1 Quantachrome to examine samples textural properties. Metal
dispersion in catalysts was found from H2 chemisorption measurements performed
on home-made volumetric glass apparatus equipped with a high vacuum system.
Catalytic activity tests were performed in a fixed-bed flow reactor, at atmospheric
pressure with volume ratio isobutane/air=1:500; reaction products were analyzed by
gas chromatography.

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RO Membrane Characterization
Ahmad Fauzi Ismail, ... Takeshi Matsuura, in Reverse Osmosis, 2019

3.3.4 Energy Dispersive X-Ray Spectroscopy

Energy-dispersive X-ray spectroscopy (EDS, EDX, or XEDS), sometimes called energy
dispersive X-ray analysis (EDXA) or energy dispersive X-ray microanalysis (EDXMA),
is an analytical technique used for the elemental analysis or chemical character-
ization of a sample. The EDS analysis can be used to determine the elemental
composition of individual points or to map out the lateral distribution of elements
from the imaged area. It can also be used to obtain compositional information
on quasi-bulk specimens (low SEM magnification, high accelerating voltage) or on
specific particles, morphologies, or isolated areas on filters or within deposits. The
EDS has an analytical capability that can be coupled with several applications includ-
ing SEM, TEM, and scanning transmission electron microscopy (STEM). Beverly et
al. [42] demonstrated that EDS, combined with XPS, FTIR, and SEM, is a valuable
diagnostic tool for the analysis of polymeric RO membrane failure and provides
valuable information to aid the manufacturers in designing better membranes for
RO.

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Atmospheric Fate and Behavior of POPs

Walter J. Shields, ... Laurel Royer, in Environmental Forensics for Persistent Organic
Pollutants, 2014

6.4.5.1 Case Study 1: Microscopy and Elemental Mapping of

Particles
Forensic microscopy involves the use of stereoscopic microscopy combined with
micro XRF spectrometry (XRFS) or X-ray energy dispersive spectrometry (EDS)
[112,148]. Stereoscopic microscopy allows determination of the origin of the dust
particle (e.g., hairs, pollen, plant fibers, skin, soil, plastic fragments, and textile fibers)
by visual observation. XRFS or EDS analysis allows mapping of the bromine content
within the dust particles. Chemical analytical analysis by gas chromatography with
mass spectrometry can also be conducted on the dust particle to determine the
specific BFRs producing the bromine signature determined by XRFS [112]. Figure
6.13 presents a closeup composite image of a dust particle showing the presence of
bromine, calcium, and/or iron.
 Figure 6.13. A closeup composite image of a dust particle created using secondary
electrons (shown in red) and backscatter electrons (shown in green). EDS showed
that the green patches contain bromine, calcium, and/or iron.

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.

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