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A PRESENTATION ONElectron Spectroscopy for Chemical Analysis(ESCA)

[Session 2012-13] Presented by:- Usha sharma (Nanotechnology)contentsIntroductionphotoelectric effectPrinciple of ESCA(XPS)ComponentsElectron Energy AnalyzerX-ray MonochromatorAnalysis Capabilities ApplicationsAdvantage & disadvantages1. IntroductionElectron Spectroscopy for Chemical Analysis (ESCA), also known as X-ray Photoelectron Spectroscopy (XPS) is a widely used technique to investigate the chemical composition of surfaces.XPS which makes use of the photoelectric effect, was developed in the mid 1960s by Kai Siegbahn .ESCA is based on the photoelectric effect.

2. photoelectric effectIn the photoelectric effect,electronsare emitted from solids, liquids or gases when they absorb energy from light. Electrons emitted in this manner may be called photoelectrons.

ContdPhotoelectron spectroscopy uses monochromatic sources of radiation (i.e. photons of fixed energy). In XPS the photon is absorbed by an atom in a molecule or solid, leading to ionization and the emission of a core (inner shell) electron.

The kinetic energy distribution of the emitted photoelectrons (i.e. the number of emitted photoelectrons as a function of their kinetic energy) can be measured using any appropriate electron energy analyzer and a photoelectron spectrum can thus be recorded. ContdElectrons ejected from a solid via the photoelectric effect will be of two types: 1. Elastically scattered electrons which have ejected from the solid without suffering an energy loss. 2. Inelastically scattered electrons which have lost kinetic energy on their way out of the solid.

4. ComponentsSource of fixed-energy radiation (an x-ray source for XPS ).An electron energy analyzer (which can disperse the emitted electrons according to their kinetic energy, and thereby measure the flux of emitted electrons of a particular energy).High vacuum environment (to enable the emitted photoelectrons to be analyzed without interference from gas phase collisions).

Setup diagram of XPS system

Hemispherical electron energy analyzer

5. Electron Energy AnalyzerConcentric hemispherical analyzer (CHA)

FactorsAnalyzer radius Slit width Elements in the transfer lens Energy of the photoelectrons6. X-ray Monochromator

n = 2dsinFor Al K = 8.3 use (1010) planes of quartz crystald = 4.25 = 78.5Advantages of using X-ray mono chromator Narrow peak width Reduced background No satellite & Ghost peaks What information can we obtain from ESCA?Identification of elements near the surface and surface compositionLocal chemical environmentsOxidation states of transition metalsValence band electronic structureMorphology of thin films

7.Analysis capabilitiesElemental Analysis: atoms have valence and core electrons: Core-level Binding energies provide unique signature of elements.

Quantitative analysis: measure intensities, use standards or sensitivity factor8. ApplicationsSurface contaminationFailure analysisEffects of surface treatmentsCoating, filmsTri biological effectsDepth Profiling (Ar+ sputtering)

Advantages 1. surface sensitive (top few mono layers) 2. wide range of solids 3. relatively non-destructiveDisadvantages 1. expensive 2. slow, poor spatial resolution 3. requires high vacuum

9. Advantages & Disadvantages

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