Xps Report

Electronic properties of material using
photoemission technique
Jagriti Ahuja, Indian Institute of Technology Mandi

Supervisor: Dr Bindu Radhamanay, Indian Institute of Technology Mandi
1. Aim of the experiment

• (i) To determine the fermi energy of Silver (Ag).
• (ii) To study the electronic properties of BaBiO3 using Photo-emission experiment.
2. Apparatus and tools required

1. XPS machine
2. BaBiO3 and Ag sample
3. Acetone (C3 H6 O)
3. Introduction
3.1. X-ray Photoelectron Spectroscopy (XPS)
The basic mechanism behind an XPS instrument is illustrated in figure 1. Photons of a specific energy are used to
excite the electronic states of atoms below the surface of the sample. Electrons ejected from the surface are energy
filtered via a hemispherical analyser (HSA) before the intensity for a defined energy is recorded by a detector.
Since core level electrons in solid-state atoms are quantized, the resulting energy spectra exhibit resonance peaks
characteristic of the electronic structure for atoms at the sample surface. While the x-rays may penetrate deep
into the sample, the escape depth of the ejected electrons is limited. That is, for energies around 1400 eV, ejected
electrons from depths greater than 10nm have a low probability of leaving the surface without undergoing an
energy loss event, and therefore contribute to the background signal rather than well defined primary photoelectric
peaks.
In principle, the energies of the photoelectric lines are well defined in terms of the binding energy of the electronic
states of atoms. XPS is a quantitative technique in the sense that the number of electrons recorded for a given
transition is proportional to the number of atoms at the surface.
Fig. 1. (a) Schematic view of the XPS instrument (b) XPS instrument used in laboratory
3.2. Principle of the Technique
Surface analysis by XPS is accomplished by irradiating a sample with mono energetic soft x-rays and analyzing
the energy of the detected electrons. Mg Ka (1253.6 eV) or Al K (1486.6 eV) x-rays are usually used. These
photons have limited penetrating power in a solid on the order of 1-10 micrometers. They interact with atoms
in the surface region, causing electrons to be emitted by the photoelectric effect. The emitted electrons have
measured kinetic energies given by:
KE = hv − BE − φ s (1)
where hv is the energy of the photon, BE is the binding energy of the atomic orbital from which the electron
originates, and φ is the spectrometer work function. The BE of a certain peak of an element in the spectrum can
then be compared to those of reference materials, or to tabulated values in databases, in order to determine the
”chemical state” of that element in the sample. The intensity of a certain elemental peak is, of course, proportional
to the concentration of that element in the sample. However, because the probabilities of ionizing different electron
states vary, the conversion of the measured counts under spectral peaks to concentrations values will require the
normalization of the counts by ”sensitivity factors” that corrects for these differing probabilities.
The XPS system can accommodate thin films, bulk samples up to 1cm thick, and powder samples. The sample
stage here is 60 mm by 60 mm and can hold as many samples as will fit into this area. Films can be inorganic or
organic/biological as long as they are dry.
4. Procedure
• Determine the analyzer work function by taking the narrow spectrum of silver(Ag).
• Determine the fermi energy from the silver spectrum.
• For a typical XPS investigation of BaBiO3 , obtain a broad scan survey spectrum to determine the elements
present in the compound.
• From the wide scan spectrum of BaBiO3 identify the peaks of different elements present in the given com-
pound.
5. Results
Figure 2 shows a narrow spectrum of Ag sample, fitted with Boltzmann distribution. Fig 3 shows the gaussian
distribution of the first derivative of intensity to determine the fermi edge of the silver atom. Fermi edge is the
energy level where binding energy of the electron is zero, which is used to determine the work function of some
other compound.
Fig. 2. Narrow spectrum of silver under XPS.

The value of the fermi-edge calculated from the graph is 1486.78 eV as shown in fig3. This fermi edge is use
to calcuate the work function vs intensity plot of BaBiO3 .
Fig. 3. Fermi edge calculation of silver metal under XPS.
Figure 4 shows the wide scan of BaBiO3 under x-ray photo-emission. The work function of the spectra is
determined by subtracting the binding energy of the cutoff from the photon energy.
Fig. 4. Wide scam of BaBiO3 under XPS.
Table 1 present the interpretation of the XPS spectrum accomplished by identifying the energy lines in the wide
scan.
Table 1. Peak identified in the spectrum of BaBiO3
Element Binding energy (eV) Transition level
Bismuth (Bi) 24 5d5/2
Bismuth (Bi) 157 4f7/2
Barium (Ba) 780.6 3d5/2
Barium (Ba) 796.0 3d3/2
Oxygen (O) 531.0 1s
6. Discussion
Detailed study of X-ray Photoelectron Spectroscopy (XPS) was done. also, analysis of chemical composition of
BaBiO3 and the peak identification in the spectrum of BaBiO3 was done using XPS technique.
7. Applications
XPS is a surface chemical analysis technique that is versatile in the range of samples it can be used to investigate:
• The technique provides quantification of chemical composition, chemical state and the occupied electronic
structure of the atoms within a material.
• XPS provides elemental the composition of the surface (within 1-10 nm usually), and can be used to deter-
mine the empirical formula of the surface compounds, the identity of elements that contaminate a surface,
the chemical or electronic state of each element in the surface, the uniformity of composition across top
surface and through the depth (by sequentially milling into the material and taking XPS data of the new
exposed surface).
• XPS is used to analyze a wide range of materials, for example metal alloys, other inorganic compounds such
as ceramics, polymers, semiconductors, catalysts, glasses, parts of plants biological materials such as cells,
bones and many others.
8. Precautions
1. All parts should be unscrewed carefully and wear gloves always in the labs.
2. Shoes must be worn in lab.
3. Handle the pump carefully so that oil must not come out.
4. Size of vacuum pump is large handle it carefully, unsure switch is off and wire is not in electric board.
5. Avoid any kind of dust in room,if dust particle enter ,system may Not work again.
6. Ensure working at starting before dismantle and after assemble.
9. References
1.https://www.jove.com/science-education/10474/x-ray-photoelectron-spectroscopy
2.https://en.wikipedia.org/wiki/Rotaryv ane p umpciten ote − 4

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Electronic properties of material using

Jagriti Ahuja, Indian Institute of Technology Mandi

1. Aim of the experiment

2. Apparatus and tools required

Fig. 2. Narrow spectrum of silver under XPS.

Fig. 3. Fermi edge calculation of silver metal under XPS.

Fig. 4. Wide scam of BaBiO3 under XPS.

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