Introduction and Applications of Auger Electron Microscopy AEM

Introduction
The Auger effect was discovered by Pierre
Auger in 1925 while working with X rays and using a Wilson cloud chamber. Tracks corresponding to ejected electrons were
observed along a beam of X rays. The aim of Auger electron imaging is to obtain quantitative surface elemental distribution maps at high spatial resolution

Working Principle -1
When an atom is struck by a high energy electron (typically in the range 1 to 25 keV) there is some probability of a core level electron being ejected.

The atom is then in an energetic ionic state with an electron missing from a core level.
One mechanism by which the atom can relax into a lower energy state is for another electron one electron falls from a higher level to fill an initial core hole in the K-shell and the energy liberated in this process is simultaneously transferred to a second electron ; a fraction of this energy is required to overcome the binding energy of this second electron, the remainder is retained by this emitted Auger electron as kinetic energy.

Working Principle -2

Working Principle -3
Two-step process, generates Auger electron
differs from XPS 1) generate excited ion as before: A + hn A+* + eor using an electron beam A + ei- A+* + ei- + eAwhere: ei- is the beam electron after interaction with A and loss of kinetic energy. eA- is ejected from A inner orbital 2) excited ion may relax by emitting an Auger electron (eA-) with kinetic energy (Ek) A+* A++ + eAor by fluorescence (X-ray fluorescence) A+* A+ + hnf Kinetic energy of emitted electron (Ek) is independent of the energy of photon or electron that

Kinetic energy (EK) of the Auger electron is: EK = (Eb Eb) Eb = Eb 2Eb where: (Eb-Eb) energy released in relaxation of the excited ion Eb energy required to remove the second electron from its orbit

Working Principle -4
The Auger electron has a characteristic energy which depends upon a number of factors: The chemical element involved The energy level within which the initial hole was formed The energy level of the electron which eventually fills the hole The initial energy level of the electron which eventually becomes the the Auger electron

Auger emissions are described in terms of the type of orbital transitions involved in the production of an electron KLL: 1. removes a K electron 2. transition of an L electron to the K orbital 3. ejection of a second L electron

 Two competing
processes: X-ray fluorescence

AEM: Efficiency of Auger Electron Production

Auger electron emission

Auger electrons

number of K photons produced number of K shell vacancies created

predominate at lower atomtomic number (Z)

Auger 1 K

AES: Instrumentation
AES instruments are designed like an
SEM often they are integrated with an SEM/EDXA system

Unlike an SEM, AES instruments are

designed to reach higher vacuum (10-8 torr)

Helps keep surfaces clean and free from adsorbed gases, etc

Basic components:
Electron source/gun Electron energy analyzer Electron detector Control system/computer Ion gun (for depth profiling)

Primary Electron Sources

Three kinds of primary electron sources are in common use in Auger electron spectrometers A tungsten cathode source consists of a wire filament bent in the shape of a hairpin. Lanthanum hexaboride (LaB6) cathodes provide higher current densities Field Emission electron sources consist of very sharp tungsten points at which electrical fields can be >10E7 V/cm.

Auger instruments have primary electron beam columns similar to electron microscopes. The columns may include both electrostatic and magnetic lenses for beam focusing

Electron Energy Analyzers

Electron energy analyzers measure the number of ejected electrons as a function of the electron energies. The analyzers must be located in a high vacuum chamber and isolated from stray magnetic fields (including the earths) that deflect electrons The schematic shows a cross section of a cylindrical mirror analyzer in red.

 The primary electron beam hits the sample surface at the source point of the analyzer. Auger electrons move outward in all directions and some pass through the grid covered aperture in the inner cylinder.

A variable negative potential on the outer cylinder bends the Auger electrons back through a second aperture on the inner cylinder and then through an exit aperture on the analyzer axis.

Electron Detector
Electron Multipliers Discrete dynode detector
An electron multiplier consists of a series of electrodes called dynodes
each connected along a resistor string. The signal output end of the resistor string attaches to positive high voltage. The other end of the string goes to the electron multiplier case and ground. When a particle electron strikes the first dynode it produces secondary electrons. The secondary electrons are accelerated into the next dynode where each electron produces more secondary electrons. A cascade of secondary electrons ensues. The dynode acceleration potential controls the electron gain.

Ultra High Vacuum environment

The surface analysis necessitates the use of a UHV

environment

Contamination of the specimen surface is critical for highly reactive surface materials, where the sticking coefficient for most residual gases is very high (near unity).

the background pressure is reduced to the low 1010torr range in order to minimize the influence of residual gases in surface analysis measurements

AEM: Image Surface Analysis

ANALYTICAL INFORMATION
Spatial resolution is approximately 0.3 microns. Depth resolution is dependent upon sample and sputtering parameters (less than 100 resolution is not unusual). Typical sputtering rate is ca. 30 /min. SAMPLE REQUIREMENTS Maximum of "x" (18 mm x 12 mm). Height should not exceed " (12 mm). must be conductive or area of interest must be grounded properly. Insulating samples including thick insulating films (ca. 3000 ) cannot be analyzed SUPPLEMENTAL INFORMATION:

Minimum area of analysis - 0.3 microns 10% relative error (i.e. estimated error in repeated analyses), 20% absolute error (i.e. error between analysis and known standard). hr per sample .Depth profiles may take longer depending on the total depth being sputtered.

AEM VS SEM

For true surface analysis, AES is better than SEM/X-ray emission (electron microprobe) because it is much more surface sensitive

AEM can be easily made quantitative using standards.

The major advantages of AeM over SEM are greater lateral and depth analytic resolution and ease of light-element detection. The Spatial resolution of AEM is 0.030 pm The Spatial resolution of SEM is 1 - 3 pm

Advantages of Auger Electron Microscopy Sensitivity to atoms of low atomic number Minimal matrix effects

High spatial resolution

Detailed examination of solid surfaces

Electron beam more tightly focused than X-ray beam

Almost any solid can be analyzed.

Sample can be analyzed as it is.

Estimated time to obtain the survey spectrum from a sample varies from 1 to 5 min.

Disadvantages of Auger Electron Microscopy

not used to provide structural and oxidative state information (XPS)

quantitative analysis is difficult

It does not provide for nondestructive depth profiles
It requires that samples be small and compatible with high vacuum

Analyzes conducting and semiconducting samples. Special procedures are required for nonconducting samples. Only solid specimens can be analyzed. Samples that decompose under electron beam irradiation cannot be studied.

General Uses
Identification of elements on surfaces of materials Quantitative determination of elements on surfaces Depth profiling by inert gas sputtering Phenomena such as adsorption, desorption, and surface segregation from the bulk Determination of chemical states of elements In situ analysis to determine the chemical reactivity at a surface

Auger electron elemental map of the system

Common Applications

Qualitative analysis through fingerprinting spectral analysis Identification of different chemical states of elements Determination of atomic concentration of elements Depth profiling Adsorption and chemisorption of gases on metal surfaces Interface analysis of materials deposited in situ on surfaces

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