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CHEM02200704003 Nilamadhab Pandhy - Homi Bhabha National ...

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Chapter 3<br />

repeated over three different places on the surface, and the data presented is a representative of the<br />

whole surface. The pressure inside the chamber during measurement was around 10 -7 Pa.<br />

3.1.4.3 X-ray Photoelectron Spectroscopy<br />

X-ray Photoelectron Spectroscopy (XPS) or Electron Spectroscopy for Chemical Analysis<br />

(ESCA) is a surface analysis technique that is unique in providing the information regarding the<br />

bonding in different chemical states of elements. Its application is wide spread involving oxidation<br />

state determination of elements, identification of the chemical state of the metal oxide films,<br />

surface analysis of semi-conducting and insulating materials, and elemental depth profiling etc<br />

[85-87]. XPS in combination with traditional electrochemical techniques has long been used for<br />

understanding and solution of different types of corrosion problems. It is invaluable in the field of<br />

corrosion science, and the areas of corrosion research which are finding major applications are (a)<br />

for understanding the phenomenon of passivity, (b) compositional analysis at interface, (c)<br />

selective oxidation phenomenon, (d) assessment of mass transport process, and (e) the interaction<br />

of materials in different electrochemical environment [88-90]. However, the inability to detect<br />

hydrogen is one of the limitations in understanding greater details of overlapping mechanism of<br />

various corrosion phenomena [91].<br />

XPS involves irradiating a sample with X-rays of a characteristic energy and measuring the<br />

energy of flux of electrons leaving the surface [92]. The energy spectrum for the ejected electrons<br />

is a combination of an overall trend due to energy loss processes within the sample, transmission<br />

characteristics of the spectrometer, and resonance structures that derive from electronic states of<br />

the material under analysis. In principle it consists of (a) X-ray source, (b) electronic focusing<br />

system, (c) electron energy analyzer, and (d) detector. The schematic of X-ray photoelectron<br />

spectroscopy is shown in Fig. 3.7 [92].

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