Incoming Electrons

backscattered electrons

X Rays Cathode Radiation

Aguer Electrons Secondary Electrons

0nelastic Scattering Elastically Scattered

Electrons Electrons

cattered electrons
 Incident
Backscatered Electron X-rays
Electrons Beam

Secondary
Auger Electrons
Electrons

Specimen

Elastically
Scattered Direct Inelastic ally
Electrons Beam Scattered
Electrons
 By Analyzing Emitted X-Ray
Energy Dispersive Spectroscopy (EDS) + SEM/ TEM Analytical
Electron
Wavelength Dispersive Spectroscopy (WDS) + SEM
Microscope
By Analyzing Inelastically Scattered Electrons (AEM)
Electron Energy Loss Spectroscopy (EELS) +TEM

By Analyzing Emitted Auger Electrons

Auger Electron Spectroscopy (AES)
Surface
When X-Ray Meets Material... Characterization
By Analyzing Emitted Photoelectrons
X-Ray Photoelectron Spectroscopy (XPS)
 Principles of EDS
Energy Dispersive (X-Ray) Spectroscopy (EDs)
" X-Ray counting is done by measuring the x-ray photon energies with a
Si(Ni)solid state detector
Usage
Add analytical capability on element concentration of SEM or TEM
Sample Requirements
Solids(polished), powders (compacted) or composites;
sample size: in SEM only limited by the stage size
in TEM 3mm diameter thin foil
Not destructive to sample

Limitation
" Lateral resolution: typically about 0.5um
as small as 1nm for thin samples in STEM
Sampling depth: 1um,can achieve 0.02 um depending on Zand
electron beam energy
Detection limits: 100-200ppm for isolated peaks in elements with Z> 10
1-2%wt. for Z<10 or overlapped peaks
Accuracy: with standards t4-5% deviation for concentrations >5%
 Principles of WDS
Wavelength Dispersive (X-Ray) Spectroscopy (WDS)
X-Ray counting is done by using a Bragg
reflector to wavelength-filter the x-rays on their
way to the detector

Bragg's Law
Nl=2dsin 0

With SEM
Advantages
" Superior spectral resolution (X10 times better than EDS)
Can detect lightelement Z4
Can detects 0.1%-several ppm
More accurate

Disadvantages
The equipment is more expensive
More Time consuming
More difficult to use

Usage
ldentification of spectrally overlapped elements such as Wor Ta in Si,
or N in Ti
Detect of low concentration species (down to 100 or even 10ppm)
such as P or S in metals
Analysis of Low atomic number elements such as oxidation in metals
 Comparison between EDS&WDS
EDS:
Normally detects Z>10(below
Na) thus typically can't be
detected 0, N, C. Sometimes if
using windowless or thin
window itcan detect Z> 4
Parallel technique
Can quickly scan for a wide
rang of possible elements
Good for use both with SEM or
TEM specimen
Time of a typical run take a few
minutes
WDS:
. Detects Z> 4
Serial technique
slow but can provide excellent
resolution
Requires very high x-ray
generation rates thus TEM
samples can't provide high
count (x-ray generation) rate
Time of a typical run take hours
 Principles of XPS
Sample Requirements
vacuum compatible materials, flat samples preferred
no destruction except to X-ray sensitive materials and during
depth profiling

Limitation
Range of elements: All except Hand He
Lateral resolution: 5mm-75pm
Sampling depth: 0.5-5nm
Detection limits: 0.01-0.3at.%
 Applications of XPS
O Routinely used in industry and research whenever elemental or
chemical state analysis is needed at surfaces and interfaces as well as
spatial resolution requirements are not demanding (typically greater
than 150 m).

OEg.'s:
examination for and identification of surface contaminations
Evaluation of materials processing steps (cleaning, plasma etching, thermal
oxidation, silicide thin-film formation etc.)
Evaluation of thin-film coating or lubricants
Failure analysis for adhesion between components(air oxidation, corrosion
etc.)
Tribological (or wear) activity
Effectiveness of surface treatrment of polymers or plastics
Surface composition differences for alloys