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Phase Identification of Nanomaterials with SEM

One of Bruker’s QUANTAX EDS/EBSD system most appreciated feature is its advanced integration of the EBSD and EDS techniques. The excellent integration is available also for electron transparent samples and is especially powerful when combining the eFlash FS and the unique XFlash® FlatQUAD EDS detector. This combination provides unrivaled data quality, spatial resolution and high throughput. Especially when combined with the patented TKD sample holder and the newly released X-ray mask. In this application example, oxide dispersion-strengthened ferritic alloy demonstrates the need for simulatenous TKD and EDS measurement with the XFlash® FlatQUAD to perform phase identification as well as distinction of crystallographically similar phases.

Bright Field ARGUS image of the measured area. The sample is a TEM foil of ferritic ODS steel, oxides particles are detected. The combined TKD/EDS measurement was done at 20 kV and 6 nA.
EDS result from the simultaneous TKD/EDS measurement with eFlash FS and XFlash FlatQUAD. Identification and distribution of Titanium oxides particles are revealed. Output count rate is ~1 Million counts per second, i.e. >3000 counts per spectrum. right: X-rella mask for TKD sample holder. it blocks stray X-rays, allowing to collect EDS signal from the TKD sample only.
EDS result from the simultaneous TKD/EDS measurement with eFlash FS and XFlash FlatQUAD. Identification and distribution of Yttrium oxides particles are revealed. Output count rate is ~1 Million counts per second, i.e. >3000 counts per spectrum. right: X-rella mask for TKD sample holder. it blocks stray X-rays, allowing to collect EDS signal from the TKD sample only.
EBSD orientation distribution result (IPF Z map) with indexing hit rate of 87% . The oxide phases identification is performed offline to optimize the time spent at the SEM, using the detected bands and quantified spectra.
EBSD Phase maps with Ferrite in red, cubic titania in green and trigonal yttria in blue. EBSD phase map based on Kikuchi bands indexing only: some misindexing between the cubic phases.
Reanalyzed EBSD Phase map without misindexing thanks to the EDS quantification assistance.