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Xray Presentation

This document is an outline for a presentation on x-ray generation and analysis. It introduces x-ray analysis as a technique for elemental analysis or chemical characterization of a sample based on interaction between an x-ray source and the sample. It describes the different types of x-rays generated including continuous x-rays and characteristic x-rays, and explains how characteristic x-rays can be used for elemental identification and quantitative analysis since their energy is unique to each element. The document also provides an overview of the components of an EDS setup including the beam source, x-ray detector, pulse processor, and analyzer.

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51 views24 pages

Xray Presentation

This document is an outline for a presentation on x-ray generation and analysis. It introduces x-ray analysis as a technique for elemental analysis or chemical characterization of a sample based on interaction between an x-ray source and the sample. It describes the different types of x-rays generated including continuous x-rays and characteristic x-rays, and explains how characteristic x-rays can be used for elemental identification and quantitative analysis since their energy is unique to each element. The document also provides an overview of the components of an EDS setup including the beam source, x-ray detector, pulse processor, and analyzer.

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Saeedeh Ghaffari

Nanofabrication
Fall 2011

•Aug 21, 2021 •1


Outline
Introduction
X-Ray Generation
Analysis
Detection
Reference

•Aug 21, 2021 •2


Introduction

•Aug 21, 2021 •3


Introduction

•Aug 21, 2021 •4


Introduction
An analytical technique used for the
elemental analysis or chemical
characterization of a sample
Relies on the investigation of an interaction of
some source of X-ray excitation and a sample
 Determines characteristic of an atom due to
the a unique atomic structure

•Aug 21, 2021 •5


Types of X-ray
Continuous x-rays
 background radiation
 must be subtracted

for quantitative analysis

Characteristic x-rays
 elemental identification
 quantitative analysis

Example of Eds spectrum

•Aug 21, 2021 •6


Continuous(Bremsstrahlung)
 The energy emitted as an
x-ray when the electron
incident on a specimen is
bent on its trajectory
 Decelerated by the
electrostatic field of a
nucleus
 This x-ray does not have
a value unique to an
element
 This background is
excluded for quantitative
analysis

•Aug 21, 2021 •7


Characteristic
 An incoming high-energy
electron dislodges an inner-shell
electron in the target, leaving a
vacancy in the shell
 An outer shell electron then
“jumps” to fill the vacancy
 A characteristic x-ray
(equivalent to the energy
change in the “jump”) is
generated

•Aug 21, 2021 •8


Characteristic
•The difference
in energy
between two
orbits has a
unique value
for each
element, the
energy of the
emitted x-ray is
also unique to A typical spectrum obtained on mineral particles of up
the element to 2μm diameter. The peaks are labeled with the EDX
line of the corresponding element

•Aug 21, 2021 •9


Pure Ge Silica glass
Several examples
of EDS spectra
Characteristic
Al film on Si
Graphite

Pure Al Organic

•Aug 21, 2021 •10


Electron Transition
•A variety of
characteristic energy X-
rays is generated as
the various displaced
inner-shell electrons
are replaced by the
various outer-shell
electrons

•Aug 21, 2021 •11


Electron Transition

•Aug 21, 2021 •12


Characteristic

Typical characteristic x-ray and their names

•Aug 21, 2021 •13


X-Ray Energies
 X ray Energies are a function of Z (atomic number)
 K lines: lighter elements
 L lines: heavier elements
 M, N .. lines: the heaviest elements
 Kα:
 Be (Z = 4) 110 eV
 Fe (Z = 26) 6.4 keV
 Au (Z = 79) 68.8 keV
 Lα:
 Fe 0.70 keV
 Au 9.71 keV
 A threshold energy to eject electron increases with atomic number

 Note: The EDX detectors work well only in the range 1-20 kev

•Aug 21, 2021 •14


X-Ray Analysis
 Qualitative Analysis:
 Peak energy gives
qualitative information
about the constituent
elements

 Quantitative Analysis:
 Peak intensity gives
information about the
element composition to
find the changes in
concentration of elements

• Note: The minimum detection limits vary from approximately 0.1 to


a few atom percent, depending on the element and the sample matrix.

•Aug 21, 2021 •15


EDS Setup
• Four primary
components of the
EDS setup:

• Beam source

• X-ray detector

• Pulse processor

• Analyzer

•Aug 21, 2021 •16


EDX Detector
• Crystal detects X-
rays
• Liquid nitrogen cools
crystal to reduce noise
and also pumps dewar
• Window separates
detector from column
vacuum
• Collimator eliminates
stray x-rays

•Aug 21, 2021 •17


EDX Detector
•X-rays pass through :
• collimator
• electron trap
• window
• gold layer
• dead layer into Li-drifted Si
crystal (SiLi)

•Aug 21, 2021 •18


Solid State Detector in EDX

EDX

•Aug 21, 2021 •19


Si(Li) Crystal
Anti-reflective Ice
Gold electrode
Al coating 30 nm Gold
Silicon inactive layer (p-type) ~100 nm electrode
20 nm

X-ray

Holes Electrons

(–) (+)
Window
Be, BN, Active silicon
diamond,
(intrinsic)
polymer
0.1 m — 7 m 3 mm
–1000 V bias
Aug 21, 2021 20
X-Ray Detection
 Electron - hole pairs created.
 Each electron-hole pair requires a mean energy of 3.8 eV
 Bias voltage sweeps charge carriers to either side
 Charge proportional to Xray energy

 Note: Charge is small! Noise is a potential problem.


 Note: High energy X-rays may not be dissipated in the
active region of the crystal! Incomplete charge collection.
 (EDX spectrometers work best in the region 1-20 Kev)

•Aug 21, 2021 •21


X-Ray Processing

1. X-ray comes in, creates an e h pair


2. Charge pulse enters FET, converted to voltage pulse
3. Voltage pulse amplified several thousand times
4. Analog-to to-digital converter used to assign pulse to specific energy
5. Computer assigns x-ray as a ‘count’ in a multi-channel analyzer

•Aug 21, 2021 •22


References
 Robert Edward Lee, Scanning
electron microscopy and X-ray
microanalysis, Prentice-Hall
(1993)
 Goldstein book
 Wikipedia: energy dispersive X-
ray spectroscopic
 Let’s familiarize ourselves with
the SEM booklet
 Microanalyst.net

•Aug 21, 2021 •23


Thanks for your Concentration

•Aug 21, 2021 •24

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