Rajasekarakumar Vadapoo

Department
D of Physics,
University of Puerto Rico,PR-00931,USA.
More info: http://nanophysics.wordpress.com
ttp://nanophysics.wordpress.com

X-ray
ray Energy Dispersive Spectrometry (XEDS) and Electron Energy Loss
Spectrometry (EELS)
(EELS)- Report # 2.
Aim:

To confirm the atomic composition of the given sample by the spectroscopic method X-
ray Energy Dispersive Spectrometry
trometry (XEDS) and reconfirming by using Electron Energy Loss
Spectroscopy (EELS).

Experiment details:

The experiments were carried out in Carl zeiss 200 KeV TEM with the capability of
spectroscopic measurements of X
XEDS and EELS. The sample used was Fe3CoO4 nanoparticles.

Results and Discussions:

Image:

The fig.1 shows that the TEM image of Fe3CoO4 nanoparticles. As we see we have a distribution
of sizes of the nanoparticles ranging from 7.98 nm to as big as 22.7 nm. If we closely look at the
shapes of the nanoparticles, it shows the crystal facets. Fig.2. shows the TEM image of the
region where we have carried out the XEDS and EELS measurements of the given nanoparticles.
The black region in the left corners of the image is due to the selective area aperture corners.

Fig. 1 TEM image of Fe3CoO4 nanoparticles Fig.2. The area of XEDS &EELS taken.

X-ray Energy Dispersive Spectrometry (XEDS):

Fig. 3. The XEDS plot shows the presence of the elements present in the sample for the
corresponding peak.

1600

8.05
1400

1200

1000

800

600

400 0.51 4.51

0.74 6.41 8.92

200 0.93 6.93
4.97

0 1 2 3 4 5 6 7 8 9 10
Energy in keV

Fig. 4. The plot shows the measured XEDS energy of the peaks in keV.
 Experimental Reported Corresponding
(keV) (keV) lines
0.51 0.525 O Kα
0.74 0.776 Co Lα
0.93 0.93 Cu Lα
4.51 4.508 Ti Kα
4.97 4.931 Ti Kβ
6.41 6.398 Fe Kα
6.93 6.924 Co Kα
8.05 8.04 Cu Kα
8.92 8.904 Cu Kβ

Table. 1. Shows the experimentally observed XEDS peaks and the corresponding reported value
of X-Ray emission and absorption edge energies.

Fig. 3 & 4 shows the measured XEDS peaks corresponding possible elements and the
corresponding energies respectively. Table 1. Clearly shows that the experimentally observed
XEDS peaks exactly match with the corresponding reported lines of the element as shown in the
table as well as the corresponding elemental details shown in fig.3. From these details we can
confirm that the nanoparticles what we measured were containing the atomic elements Fe, Co &
O.

Energy Loss Spectrometry (EELS):

The measured EELS spectrum of the given sample is given below for the
corresponding elements present

Edge-type Reported edges (eV) Measured edges (eV)

Kα K(a,b) 1st Edge 2nd Edge 3rd Edge
C-K 277 282 ~ 277 ~ 292 ~ 318
O-k 525 531 ~532 ~ 538 ~ 565
Table. 2. Experimentally measured X-Ray energy emission and absorption edges along with the
reported edges of the element C & O.

Edge-type Reported edges (eV) Measured edges (eV)

Lα Lβ1 Lν1 LIII(ab) LII(ab) 1st Edge 2nd Edge
Co-L3 776 791 794 779 794 ~ 785 ~ 805
Fe-L3 705 718 721 709 720 ~ 715 ~ 725
Table.3. Experimentally measured X-Ray energy emission and absorption edges along with the
reported edges of the element Co & Fe.
 Digits Parallel EELS O - K

100.0

Intensity
50.0

0.0

530.0 550.0 570.0 590.0

Energy Loss eV

Digits Parallel EELS Co - L3 Digits Parallel EELS Fe - L3

40.0

40.0
30.0
Intensity

Intensity

20.0

20.0

10.0

0.0
0.0

-10.0
740.0 760.0 780.0 800.0 680.0 700.0 720
720.0 740.0
Energy Loss eV Energy Loss eV

Fig. 5. EELS spectrometry spectrums obtained in the experiment for the constituent elements of
the sample along with carbon.

The fig.5 & table.2, 3 show that the measured edges have little shift for most of the
constituent
tituent elements. It could be overcome by having the correction of exact Zero loss peak at
zero eV. Overall the measured edges match with the reported edges of the given constituent
elements which show that the particular elements are present in the given sample. The
broadening of peaks which cover the area of edges shows that it could have several edges
e merges
together and or contains some other fine structure details along with the edges.
edges

Conclusions:
We have carried out the Transmission Electron Microscopy imaging
maging of given Fe3CoO4
nanoparticles. The
he elemental characterization using XEDS & EELS show the existance of the
atomic elements Fe, Co and O in the measured region of the sample.