Rethinking EDS Keith Thompson Jan 21, 2014 Outline Background on - - PowerPoint PPT Presentation

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Rethinking EDS Keith Thompson Jan 21, 2014 Outline Background on - - PowerPoint PPT Presentation

Rethinking EDS Keith Thompson Jan 21, 2014 Outline Background on EDS detector technology Discussion of modern EDS detectors Finding the right detector for your application Proprietary & Confidential 2 EDS & WDS: 1950s


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Rethinking EDS

Keith Thompson Jan 21, 2014

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Outline

  • Background on EDS detector technology
  • Discussion of modern EDS detectors
  • Finding the right detector for your application
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EDS & WDS: 1950s

  • The first “EDS-styled” analytical technique was actually WDS
  • Based on Bragg diffraction
  • First EPMA built in 1949 by Raymond Castaing
  • The spectrometer looked at 1 element at a time
  • The spectrometer was manually adjusted
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1960s: EDS becomes mainstream with Si(Li) detectors

Whole spectrum at once type of analysis Computing power to run the system and process the data Acceptance of EDS in the SEM community

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Drawbacks to the first Si(Li) EDS detectors

  • X-ray loss in Be window
  • Window required to protect Si(Li) module
  • No spectrum < 1 keV with Be windows
  • Poor energy resolution and count rates
  • ~ 145 eV at < 2,000 X-ray stores per second
  • ~ 200 eV at up to 20,000 X-ray stores per second
  • Inherent limitations to active area
  • The constant requirement for Liquid Nitrogen!

Despite these drawbacks, LN-cooled detectors would dominate EDS for 40 + years

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1988: First no-LN cooled detector

  • Mechanical cooling with Peltier devices were used to replace Liquid

Nitrogen cooled detectors.

  • No LN ever again!
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SuperDry at high count rates: 54,000 cps

  • Resolution at count rate remained a challenge
  • Window transmission challenges remained
  • Potential reliability concerns with mechanical vibration (shaking of the

electron image) and water recirculation (water leaks)

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Modern EDS for the new Millennium

  • Novel light element windows allowed transmission to Be
  • PC-based acquisition and data storage
  • Element mapping evolves into Spectral Imaging
  • SDD – based EDS detectors commercially available
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The SDD revolution

SDD vs. LN circa 2002 Same sensitivity in one third the time! (Spectra taken at same beam current)

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SDD Benefit versus Si(Li) at High Throughput

  • At high count rates, conventional Si(Li) experiences significant peak shift

and loss of sensitivity for light elements

  • The UltraDry SDD maintains resolution at high count rates

Si(Li) Spectrum SDD Spectrum

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2nd generation SDD: Improved Light element

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3rd Generation Silicon Drift Detector

Si(Li)

Larger detectors for faster throughput: 10, 30, 60, 100 Improved energy resolution Improved light element

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Outstanding low energy resolution

Clear peak separation Excellent peak – background

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SDD Gen 3 vs. SDD Gen 2

60 mm2 10 mm2

10 mm2

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Large Area detectors: What does it mean to me?

256 pixel x 192 pixel resolution 20 second acquisition

CuFeS Quartz NiFeS FeS Epoxy

10 mm2 detector 15 counts/pixel 100 mm2 detector 120 counts/pixel1 Larger area detectors collect more X-rays under identical circumstances

  • 1. Collection rate saturated at 300,000 stored counts per second
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Steady resolution with count rate

60 mm2 SDD detector at: 10,000 cps 100,000 cps 300,000 cps

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Light Element Detection – Li mapping

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A retrospective

  • Before 2000
  • LN dominated
  • Slow count rates
  • Poor energy resolution
  • Be windows….. Poor light element
  • No spectral imaging…. Pick your element and hit “Go”
  • Modern detectors
  • Large area detectors
  • Very high count rates
  • Outstanding energy resolution across the spectrum
  • Light element detection to Li
  • How does my detector stack up against my application?
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Spectral resolution Active area … SIZE Fast mapping Large mosaics Complex mapping at low energy Many elements over a large area Careful Quant of trace elements TEM & nanoscale Microprobe Point & shoot applications Failure analysis Quality control Defect review Light element analysis

… Lithium detection … B in glass

w/ EBSD

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Introducing: ThermoScientific UltraDry Compact EDS system

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Thermo Scientific UltraDry Compact EDS system

  • What it is:
  • A stream-lined, smaller and cost-effective EDS

detector

  • Fixed length, standardized design that bolts easily

to the WDS port

  • Who needs it?
  • Those who want to perform high-quality, chemical

analysis in an electron microscope but don’t have the budget to pay for a high-end spectroscopic instrument.

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UltraDry Compact EDS

Spectral resolution Active area … SIZE Fast mapping Large mosaics Complex mapping at low energy Many elements over a large area Careful Quant of trace elements TEM & nanoscale Microprobe Point & shoot applications Failure analysis Quality control Defect review Light element analysis

… Lithium detection … B in glass

w/ EBSD

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More than adequate Spectral Performance

The overall spectral performance we expected from 2nd generation SDDs …. We still get that and more.

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Ideal for Point & Shoot analysis

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Element mapping when you need it

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Spectral Imaging: example extracted linescan

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Spectral Imaging: example area extraction

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The ThermoScientific Compact EDS System

Everything you’ve come to expect from EDS detector technology