NORAN System 7 Adding value to the Microprobe Keith Thompson
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 2 Proprietary & Confidential
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 3 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) 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. 4 Proprietary & Confidential
Example: Geological sample for analysis 5 Proprietary & Confidential
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 6 Proprietary & Confidential
More than just EDS: Compass Phase mapping automatically identifies the unique phases present, allowing us to quickly narrow our search region. Region of interest 7 Proprietary & Confidential
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. 8 Proprietary & Confidential
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. 9 Proprietary & Confidential
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 10 Proprietary & Confidential
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% 11 Proprietary & Confidential
A look at the sulfide regions Copper Iron Sulfide regions Two sulfide types present: CuFeS and NiS Nickel Sulfide region The WDS data, with collected standards and beam current, can provide a detailed quantitative analysis of each of these regions. 12 Proprietary & Confidential
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. 13 Proprietary & Confidential
A potassium-rich, alumina silicate region The EDS map clued me in to look for Potassium 14 Proprietary & Confidential
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 15 Proprietary & Confidential
NORAN System 7 brings true Spectral Phase mapping with COMPASS This phase mapping rapidly identifies the unique phases of interest. 16 Proprietary & Confidential
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 17 Proprietary & Confidential
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 18 Proprietary & Confidential
% At. Quantifying the impact of interaction volume? 50 45 40 5kV - Si 20 kv - Si 5 kv - S 20 kv - S 35 30 25 20 15 10 5 0 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 distance (microns) 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. 19 Proprietary & Confidential
Analysis at 5 kv brings a much sharper image resolution 20 Proprietary & Confidential
Analysis at 5 kv brings a much sharper image resolution No interaction zones with 5 kv analysis 21 Proprietary & Confidential
Analysis at 5 kv brings a much sharper image resolution 5 kv analysis eliminates the interaction volumes 22 Proprietary & Confidential
WDS Phase mapping in NORAN System 7 WDS maps imported into NS7 to utilize the phase mapping capabilities 23 Proprietary & Confidential
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 3 rd party software through the NSS-Portal The combined system provide unparalleled data acquisition and analysis capabilities. 24 Proprietary & Confidential