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Title: Chemical and Morphological Inhomogeneity of Aluminum Metal and Oxides from Soft X-ray Spectromicroscopy

Journal Article · · Inorganic Chemistry
 [1]; ORCiD logo [2];  [3]; ORCiD logo [1];  [3];  [3];  [4];  [3]; ORCiD logo [3];  [2];  [3];  [5]
  1. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division; Univ. of California, Berkeley, CA (United States). Dept. of Chemistry
  2. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Molecular Foundry
  3. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Chemical Sciences Division
  4. Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States)
  5. Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States). Advanced Light Source

Oxygen and aluminum K-edge X-ray absorption spectroscopy (XAS), imaging from a scanning transmission X-ray microscope (STXM), and first-principles calculations were used to probe the composition and morphology of bulk aluminum metal, α- and γ-Al 2 O 3 , and several types of aluminum nanoparticles. The imaging results agreed with earlier transmission electron microscopy studies that showed a 2 to 5 nm thick layer of Al 2 O 3 on all the Al surfaces. Spectral interpretations were guided by examination of the calculated transition energies, which agreed well with the spectroscopic measurements. The features we observed in the experimental O and Al K-edge XAS were used to determine the chemical structure and phase of the Al 2 O 3 on the aluminum surfaces. For unprotected 18 and 100 nm Al nanoparticles, this analysis revealed an oxide layer that was similar to γ-Al 2 O 3 and comprised of both tetrahedral and octahedral Al coordination sites. For oleic acid-protected Al nanoparticles, only tetrahedral Al oxide coordination sites were observed. Our results were correlated to trends in the reactivity of the different materials, which suggests that the structures of different Al 2 O 3 layers have an important role in the accessibility of the underlying Al metal toward further oxidation. Combined, the Al K-edge XAS and STXM results provided detailed chemical information that was not obtained from powder X-ray diffraction or imaging from a transmission electron microscope.

Research Organization:
Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
Sponsoring Organization:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
Grant/Contract Number:
AC02-05CH11231
OSTI ID:
1379849
Journal Information:
Inorganic Chemistry, Vol. 56, Issue 10; ISSN 0020-1669
Publisher:
American Chemical Society (ACS)Copyright Statement
Country of Publication:
United States
Language:
English
Citation Metrics:
Cited by: 10 works
Citation information provided by
Web of Science

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