Presented by: MUHAMMAD FARAZ MM-04 Department of Materials Engineering NED University of Engineering & Technology

INTRODUCTION TO SEM
The scanning electron microscope (SEM) uses a focused beam of high-energy electrons to generate a variety of signals at the surface of solid specimens. Hi- magnification >100,000X and greater depth of field up to 100 times as compare to OM. Moreover, very high resolution than OM. The SEM is also capable of performing analysis of selected point locations on the sample; this approach is especially useful in qualitatively or semi-quantitatively determining chemical compositions (using EDS).

Essential Components
Essential components of SEM include the following:

Electron Source (W-filament or LaB6 in thermionic guns) Electron Lenses (electrostatic and electromagnetic) Sample Stage Detectors for all signals of interest (e.g. SE detector, BSE detector, EDS, etc.) Display / Data output devices SEM always have at least one detector (usually a secondary electron detector), and most have additional detectors depending upon requirements.

Diagramatic view of SEM

Electron / Sample Interaction

The signals that derive from electron sample interaction reveal information about the sample including external morphology (topography), chemical composition, and crystalline structure and orientation of materials making up the sample.

Characteristics of the signals generated

i) Secondary electrons (SE)

Produced by inelastic interactions. SE energy level is only 3 ~ 5 eV. Can be easily collected The maximum escape depth is about 5 nm in metal and 50 nm in insulators.
Backscattered electrons (BSE) Produced by elastic interactions. BSE energy level is about 60 ~80 % of incident one. Special detector is required to collect BSE.

ii)

iii)

X-rays

Large escape depth due to difficulty of x-ray absorption Energy and wavelength of x-ray can be used for chemical analysis, i.e.
i) Energy-Dispersive spectroscopy, EDS ii) Wavelength-Dispersive spectroscopy, WDS

ENERGY DISPERSIVE SPECTROSCOPY

EDX/EDS stands for Energy Dispersive X-ray spectroscopy. It is a technique used for identifying the elemental composition of the specimen It is basically a qualitative technique but could yield excellent quantitative data also with the use of modern efficient detectors. It detects the energy of the emitted x-rays to characterize the elemental composition of the analyzed volume. Features or phases 1 m or less can be analyzed. EDS measures the relative abundance of emitted x-rays (cps) vs. their energy Usually EDX or EDS are based on either Li-drifted Si or solid-state detectors.

Principle of Operation (EDS)

As the electron beam of the SEM is scanned across the sample surface, it generates both continuum and characteristic X-rays from the atoms in its path. The energy of each X-ray photon is characteristic of the element which produced it.
The EDS microanalysis system collects the characteristic X-rays, sorts and plots them by energy, and automatically identifies and labels the elements responsible for the peaks in this energy distribution. The EDS data are typically compared with either known or computer-generated standards to produce a full quantitative analysis showing the sample composition. When incident x-ray strikes the detector, it creates a pulse that is proportional to the energy of the x-ray. The charge pulse is converted to a voltage pulse by a chargesensitive preamplifier & signal is then sent to a multi channel analyzer where the pulses are sorted by voltage. Energy, as determined from the voltage measurement, for each incident x-ray is sent to a computer for display and further data evaluation.

X-Rays Emission During EDX

During EDX Analysis, the specimen is bombarded with an electron beam inside the scanning electron microscope. The bombarding electrons collide with the specimen atoms own electrons, knocking some of them off in the process.

A position vacated by an ejected inner shell electron is eventually occupied by a higher-energy electron from an outer shell. To be able to do so, however, the transferring outer electron must give up some of its energy by emitting an X-ray.

The amount of energy released by the transferring electron depends on which shell it is transferring from, as well as which shell it is transferring to.

Figure. - Elements in an EDX spectrum are identified based on the energy content of the X-rays emitted by their electrons as these electrons transfer from a higher-energy shell to a lower-energy one.

Example of EDX Spectrum

Detectors used in EDX System

There are two major types of detectors used for EDX: i. ii. Lithium drifted Silicon detector (SiLi) Silicon drifted detector (SDD) The SiLi must be operated at liquid nitrogen temperatures to reduce electronic noise. FET is cooled to liquid N2 temperature. Li is added to increase the resistivity of the Si SDD is capable of being used at relatively high temperatures. The SDD has several other advantages over the SiLi, including faster analytical capabilities and better resolution, as well as higher count rate. The larger count rates also have the added benefit of reducing the damage to the sample because smaller specimen currents can be used.

Schematic Diagram of EDS

Typical EDS Detector

Analytical Information
a) Qualitative Analysis: Sample x-ray energy values from the EDS spectrum are compared with known characteristic x-ray energy values to determine the presence of an element in the sample. Elements from Be to U can be detected. Quantitative Analysis: Quantitative results can be obtained from the relative x-ray counts at the characteristic energy levels for the sample constituents. The accuracy of standard less analysis depends on the sample composition. Greater accuracy is obtained using known standards with similar structure and composition to that of the unknown sample. Elemental Mapping: Characteristic x-ray intensity is measured relative to lateral position on the sample. Variations in x-ray intensity at any characteristic energy value indicate the relative conc. for the applicable element across the surface.

b)

c)

d)

Line Profile Analysis: SEM beam is scanned along a pre-selected line across the sample while x-rays are detected for discrete positions along the line. Analysis of the x-ray energy spectrum at each position provides plots of the relative elemental concentration for each element versus position along the line.

Advantages of EDX
Complete compositional information within few seconds Low cost as compared to WDX Simple and easy to operate the system Convenient to identify elements Good for elements with higher Atomic Numbers (Z) Low Background

Limitation of EDX/EDS
There are energy peak overlaps among different elements, particularly those corresponding to x-rays generated by emission from different energylevel shells (K, L and M) in different elements.

EDS cannot detect the lightest elements, typically below the atomic number of Na for detectors equipped with a Be window.
Necessary requirement of Liquid Nitrogen.

Typical Applications (EDS)

Biggest advantage is chemical composition on micro-level. Foreign material analysis Corrosion evaluation coating composition analysis. Rapid material alloy identification. Small component material analysis Phase identification and distribution Morphology and chemical composition of the samples can be indentified. The chemical and structural behavior of atmospheric particles can be characterized Specimens of different size, shape and geometry can be investigated.

WAVELENGTH DISPERSIVE SPECTROSCOPY

WDX/WDS stands for Wavelength Dispersive X-ray Spectroscopy. WDX analysis works in pretty much the same way as EDX analysis, except that its detector classifies and counts the impinging X-rays in terms of its characteristic wavelengths. WDX identifies the elemental composition of materials imaged in the SEM with an order of magnitude better spectral resolution, sensitivity and ability to determine concentrations of light elements than is achievable with EDS.

Gas detectors are used for WDX analysis. A WDS detector is known as a gas-filled or gas proportional counter.
Another commonly used detector is Scintillation detector.

Detectors used in WDX System

For WDX system the detection may essentially be carried out by any of the following detectors: Gas Ionization Detectors Gas Flow Proportional Counters A WDS detector is known as a gas-filled or gas proportional counter. One variation on this type of detector consists of a gas-filled cylinder containing a tungsten wire running down the middle and a thin window through which electrons can enter the detector.

Principle of Operation (WDS)

WDX can be used for quantitative analysis by using standards for all elements present in the sample. The X-rays emitted by the sample being analyzed are collimated by parallel copper blades (called collimator or Soller slits), and irradiate a known single crystal at a precise angle. The single crystal diffracts the photons (Bragg's law) which are collected by a detector, usually a scintillation counter or a proportional counter. The single crystal, the specimen, and the detector are mounted precisely on a Goniometer with the distance from the source of x-rays (the specimen) and the crystal equal to the distance from the crystal to the detector. Usually operated under vacuum to reduce the absorption of soft radiation (low-energy photons) by the air and thus increase the sensitivity for the detection and quantification of light elements (between Boron and Oxygen).

Schematic Diagram of WDS

Typical Applications (WDS)

Applications include:
Identification of spectrally overlapped elements, such as S in the presence of Pb or Mo W or Ta in Si, or N in Ti Detection of low concentration species (down to 100 or even 10 ppm) P or S in metals Contaminants in precious metal catalysts Analysis of low atomic number elements Composition of advanced ceramics and composites Oxidation and corrosion of metals

Advantages of EDS over WDS

EDS has shorter time consumption as compared to WDS. Consists of Non destructive method X-Ray source for sample. In EDS sample preparation is easy. EDS has high accuracy and sensitivity. In EDS sample damage and chamber contamination chances are less.

WDS crystal and optics are expensive and have more failure modes.
In a WDS system, about 30% of the X-rays entering the detector are actually counted whereas in an EDS system, almost 100% are counted.

Advantages of WDS over EDS

A much better energy resolution, preventing many peak overlap errors frequently encounters in EDS analysis. WDS has lower background noise. WDX has a much finer spectral resolution than EDX. Ability to determine concentration of lighter elements. WDS has more accurate quantitative analysis.