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Title: Quantitative X-ray microanalysis for the study of nanometer-scale phases in the AEM

Technical Report ·
DOI:https://doi.org/10.2172/28201· OSTI ID:28201
 [1];  [1];  [2]
  1. Oak Ridge National Lab., TN (United States). Metals and Ceramics Div.
  2. Univ. of Minnesota, Minneapolis, MN (United States). Dept. of Chemical Engineering and Materials Science

Secondary excitation can be a large source of inaccuracy in quantitative X-ray microanalysis of inhomogeneous specimens in the AEM. The size of the secondary excitation component in the measured X-ray spectrum is sensitive to the geometry of the thin foil specimen. Secondary excitation has been examined in a self-supporting disc specimen of composition NiO-20 wt.% TiO{sub 2} which has been partially masked by a gold slot washer. The ratio of the intensities of the characteristic K{sub a} peaks of Ti and Ni in X-ray spectra from a periclase-structured phase, of nominal composition NiO, has been measured to be N{sub Ti}/N{sub Ni} {approx} 0.005. There is no apparent Ti L{sub 2,3} signal in the corresponding electron energy-loss spectrum. The secondary excitation contribution to the characteristic Ti K{sub a}-peak from all sources can therefore be no larger than 0.5%. It should be possible to reduce this modest level of secondary excitation still further with a better masking arrangement.

Research Organization:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Organization:
USDOE, Washington, DC (United States)
DOE Contract Number:
AC05-84OR21400
OSTI ID:
28201
Report Number(s):
CONF-931108-112; ON: DE95006623; TRN: AHC29510%%6
Resource Relation:
Conference: Fall meeting of the Materials Research Society (MRS), Boston, MA (United States), 29 Nov - 3 Dec 1993; Other Information: PBD: [1993]
Country of Publication:
United States
Language:
English