Analysis of catalytic gas products using electron energy-loss spectroscopy and residual gas analysis for operando transmission electron microscopy

Benjamin K. Miller, Peter Crozier

Research output: Contribution to journalArticle

19 Scopus citations

Abstract

Operando transmission electron microscopy (TEM) of catalytic reactions requires that the gas composition inside the TEM be known during the in situ reaction. Two techniques for measuring gas composition inside the environmental TEM are described and compared here. First, electron energy-loss spectroscopy, both in the low-loss and core-loss regions of the spectrum was utilized. The data were quantified using a linear combination of reference spectra from individual gasses to fit a mixture spectrum. Mass spectrometry using a residual gas analyzer was also used to quantify the gas inside the environmental cell. Both electron energy-loss spectroscopy and residual gas analysis were applied simultaneously to a known 50/50 mixture of CO and CO2, so the results from the two techniques could be compared and evaluated. An operando TEM experiment was performed using a Ru catalyst supported on silica spheres and loaded into the TEM on a specially developed porous pellet TEM sample. Both techniques were used to monitor the conversion of CO to CO2 over the catalyst, while simultaneous atomic resolution imaging of the catalyst was performed.

Original languageEnglish (US)
Pages (from-to)815-824
Number of pages10
JournalMicroscopy and Microanalysis
Volume20
Issue number3
DOIs
StatePublished - Jun 2014

Keywords

  • EELS
  • catalyst
  • environmental TEM (ETEM)
  • in situ TEM
  • mass spectrometry
  • operando

ASJC Scopus subject areas

  • Instrumentation

Fingerprint Dive into the research topics of 'Analysis of catalytic gas products using electron energy-loss spectroscopy and residual gas analysis for operando transmission electron microscopy'. Together they form a unique fingerprint.

  • Cite this