NORAN System 7 - Thermo Fisher Scientific

NORAN System 7 Adding value to the Microprobe

Keith Thompson

2 Proprietary & Confidential

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


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


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.


Example: Geological sample for analysis


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


More than just EDS: Compass Phase mapping automatically identifies

the unique phases present, allowing us to quickly narrow our search region.

Region of interest


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.


Region of interest



Microprobe analysis parameters

Imaging mode – i.e. low kV, low nA – provides a superior image.

However, these parameters are not suitable for microprobe analysis.


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


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%


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


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.


A potassium-rich, alumina silicate region

The EDS map clued me in to look for Potassium


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


NORAN System 7 brings true Spectral Phase mapping with COMPASS

This phase mapping rapidly identifies the unique phases of interest.



Looking at the interaction volumes, we thin phases running along the edge of

the primary phases: interaction zones



Unfortunately, at 20 kV the X-ray interaction volume within the sample blurs the

phases, creating interaction zones


0

5

10

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25

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45

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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.


Analysis at 5 kV brings a much sharper image resolution



No interaction zones with 5 kV analysis



5 kV analysis eliminates the interaction volumes


WDS Phase mapping in NORAN System 7

WDS maps imported into NS7 to utilize the phase mapping capabilities


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.

NORAN System 7 - Thermo Fisher Scientific

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