Extending ζ-factor microanalysis to boron-rich ceramics : Quantification of bulk stoichiometry and grain boundary composition

Copyright © 2019 Elsevier B.V. All rights reserved..

Accurate quantification of light elements which produce only soft X-ray lines via X-ray energy dispersive spectrometry (XEDS) has been traditionally difficult due to poor X-ray emission and detector efficiencies at low energies and significant X-ray absorption effects. The ζ-factor microanalysis method enables one to correct for these shortcomings; however, ζ-factor microanalysis has not yet been thoroughly applied to inorganic materials which are entirely or mostly composed of light elements such as boron carbide, boron nitride, or boron suboxide. This work successfully extended ζ-factor microanalysis to boron-rich ceramics and accurately determined stoichiometries of multiple boron carbides and measured grain boundary compositions of a boron carbide mixed with additives consisting of rare-earth ions. Various strategies were employed to experimentally determine a full range of ζ-factors and measurements were validated using materials of known composition including silicon hexaboride and silicon carbide. Overall, this work has shown that XEDS is a viable technique for light element quantification in (scanning) transmission electron microscopy, in terms of both the accuracy and precision, which is comparable or superior to the complementary electron energy loss spectrometry.

Medienart:

E-Artikel

Erscheinungsjahr:

2019

Erschienen:

2019

Enthalten in:

Zur Gesamtaufnahme - volume:202

Enthalten in:

Ultramicroscopy - 202(2019) vom: 01. Juli, Seite 163-172

Sprache:

Englisch

Beteiligte Personen:

Marvel, C J [VerfasserIn]
Behler, K D [VerfasserIn]
LaSalvia, J C [VerfasserIn]
Domnich, V [VerfasserIn]
Haber, R A [VerfasserIn]
Watanabe, M [VerfasserIn]
Harmer, M P [VerfasserIn]

Links:

Volltext

Themen:

ζ-factor quantitative microanalysis
Analytical electron microscopy
Boron-rich armor ceramics
Grain boundary excess quantification
Journal Article
X-ray energy dispersive spectrometry

Anmerkungen:

Date Revised 20.11.2019

published: Print-Electronic

Citation Status PubMed-not-MEDLINE

doi:

10.1016/j.ultramic.2019.04.008

funding:

Förderinstitution / Projekttitel:

PPN (Katalog-ID):

NLM296980641