noran system 7 - thermo fisher scientific
TRANSCRIPT
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NORAN System 7 Adding value to the Microprobe
Keith Thompson
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Introduction
• The microprobe is a world-class spectroscopic instrument
• Multiple WDS spectrometers for X-ray detection:
• Extreme energy resolution (~5 eV vs. ~130 eV for EDS)
• Excellent light element sensitivity
• Outstanding trace element sensitivity
• Accurate quantitative analysis w/ standards
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WDS separates Pb – S: Demonstrates the spectroscopic power of the WDS
S
Pb M-line @ 2346 eV
S k-line @ 2307 eV
39 eV separation
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Introduction
• The microprobe is a world-class spectroscopic instrument
• Multiple WDS spectrometers for X-ray detection:
• Extreme energy resolution (5 eV vs. 130 eV)
• Excellent low energy sensitivity
• Outstanding trace element sensitivity
• Accurate quantitative analysis w/ standards
• The NORAN System 7 brings additional value to microprobe analysis
• Rapid results with EDS
• Entire energy spectrum = Identification of elements without prior sample knowledge
• Quick survey mapping
• Spectral based Phase mapping with COMPASS
• Ability to run effectively in both imaging mode and analytical mode
• 5 kV, 0.5 nA vs. 30 kV, 100 nA
• Maximum analytical flexibility
• Best possible spatial resolution
• EDS and WDS nicely complement each other to provide the most complete analytical analysis.
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Example: Geological sample for analysis
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Quick overview with EDS reveals the major elements in the sample
10.5 nA, 20 kV
512 pixel
~ 0.6 microns/pixel
100 X-ray stores / pixel
300,000 stores/second
Time = 60 seconds
Estimated time for a
microprobe.
8 elements = 2 passes
with 4 spectrometers
Several hours @ 10 nA
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More than just EDS: Compass Phase mapping automatically identifies
the unique phases present, allowing us to quickly narrow our search region.
Region of interest
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Region of interest
Image acquired at 5 kV, 5 nA
Imaging mode – i.e. low kV, low nA – provides superior image detail.
However, these parameters are not suitable for microprobe analysis.
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Region of interest
Image acquired at 5 kV, 5 nA
Image acquired at 20 kV, 61 nA
Microprobe analysis parameters
Imaging mode – i.e. low kV, low nA – provides a superior image.
However, these parameters are not suitable for microprobe analysis.
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Quick EDS scan overview in the ROI reveals the major elements
61 nA, 20 kV
256 pixel
~ 0.25 microns/pixel
100 X-ray stores / pixel
Time = 10 seconds
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WDS maps of chosen elements identify two classes of chemistry in this regions: Sulfides and Oxides (silicates)
61 nA, 20 kV
256 pixel maps
~ 0.25 microns/pixel
Time = 30 minutes per
spectrometer per map
~ 1 hour for a 5 WDS
microprobe.
Adding another 2 lines
of interest increases
the time by 50%
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A look at the sulfide regions
Two sulfide types present: CuFeS and NiS
The WDS data, with collected standards and beam current, can provide a detailed quantitative
analysis of each of these regions.
Nickel Sulfide region
Copper Iron Sulfide regions
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A look at the oxide regions
Alumina-Silicate and Calcium Alumina-Silicate regions are identified
The WDS data, with collected standards and beam current, can provide a
detailed quantitative analysis of each of these regions.
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A potassium-rich, alumina silicate region
The EDS map clued me in to look for Potassium
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Adding the power of NORAN System 7
• The Microprobe data acquisition took a few hours, but the resulting
spectroscopy was very high quality.
• What does NORAN System 7 add?
• Phase Analysis
• Elemental Phase analysis combining the EDS data and the WDS data in a
single software platform
• True Spectrum based phase analysis to extract each unique phase with no
prior knowledge of the elements present.
• 5 kV analysis
• Sharper image quality but also improved spatial resolution
• Eliminates / Minimizes interaction volumes
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NORAN System 7 brings true Spectral Phase mapping with COMPASS
This phase mapping rapidly identifies the unique phases of interest.
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NORAN System 7 brings true Spectral Phase mapping with COMPASS
Looking at the interaction volumes, we thin phases running along the edge of
the primary phases: interaction zones
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NORAN System 7 brings true Spectral Phase mapping with COMPASS
Unfortunately, at 20 kV the X-ray interaction volume within the sample blurs the
phases, creating interaction zones
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0
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0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18
% A
t.
distance (microns)
5kV - Si 20 kV - Si
5 kV - S 20 kV - S
Quantifying the impact of interaction volume?
Line Scans across several regions @ 20 kV and @ 5 kV demonstrate a superior
spatial resolution when operating at 5 kV and < 5 nA beam current.
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Analysis at 5 kV brings a much sharper image resolution
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Analysis at 5 kV brings a much sharper image resolution
No interaction zones with 5 kV analysis
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Analysis at 5 kV brings a much sharper image resolution
5 kV analysis eliminates the interaction volumes
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WDS Phase mapping in NORAN System 7
WDS maps imported into NS7 to utilize the phase mapping capabilities
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Summary
• Microprobe advantage: Superior Spectroscopy
• Truly Excellent energy resolution – sharpest possible peaks for absolute accuracy in the energy spectrum.
• Better trace element sensitivity
• Superior light element sensitivity
• Better accuracy in Full Standards Quantitative analysis
• NORAN System 7 value
• EDS provides a rapid survey of the entire energy spectrum with no pre-knowledge of the elements present.
• ~ 50 - 100x faster acquisition than WDS
• COMPASS phase mapping rapidly identifies each unique phase of interest based entirely on the spectrum
acquired at each pixel.
• No pre-knowledge and very fast… Direct-to-Phase.
• Ability to acquire data on practical time scales at low kV, low nA for the sharpest electron images and the
best possible spatial resolution.
• Ability to integrate seamlessly and to share data with 3rd party software through the NSS-Portal
• The combined system provide unparalleled data acquisition and analysis capabilities.