| Tomographic energy dispersive diffraction imaging to study the genesis of Ni nanoparticles in 3D within gamma-Al2O3 catalyst bodies. | |
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MedLine Citation:
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PMID: 19883079 Owner: NLM Status: PubMed-not-MEDLINE |
Abstract/OtherAbstract:
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Tomographic energy dispersive diffraction imaging (TEDDI) is a recently developed synchrotron-based characterization technique used to obtain spatially resolved X-ray diffraction and fluorescence information in a noninvasive manner. With the use of a synchrotron beam, three-dimensional (3D) information can be conveniently obtained on the elemental composition and related crystalline phases of the interior of a material. In this work, we show for the first time its application to characterize the structure of a heterogeneous catalyst body in situ during thermal treatment. Ni/gamma-Al(2)O(3) hydrogenation catalyst bodies have been chosen as the system of study. As a first example, the heat treatment in N(2) of a [Ni(en)(3)](NO(3))(2)/gamma-Al(2)O(3) catalyst body has been studied. In this case, the crystalline [Ni(en)(3)](NO(3))(2) precursor was detected in an egg-shell distribution, and its decomposition to form metallic Ni crystallites of around 5 nm was imaged. In the second example, the heat treatment in N(2) of a [Ni(en)(H(2)O)(4)]Cl(2)/gamma-Al(2)O(3) catalyst body was followed. The initial [Ni(en)(H(2)O)(4)]Cl(2) precursor was uniformly distributed within the catalyst body as an amorphous material and was decomposed to form metallic Ni crystallites of around 30 nm with a uniform distribution. TEDDI also revealed that the decomposition of [Ni(en)(H(2)O)(4)]Cl(2) takes place via two intermediate crystalline structures. The first one, which appears at around 180 degrees C, is related to the restructuring of the Ni precursor on the alumina surface; the second one, assigned to the formation of a limited amount of Ni(3)C, is observed at 290 degrees C. |
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Authors:
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Leticia Espinosa-Alonso; Matthew G O'Brien; Simon D M Jacques; Andrew M Beale; Krijn P de Jong; Paul Barnes; Bert M Weckhuysen |
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Publication Detail:
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Type: Journal Article |
Journal Detail:
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Title: Journal of the American Chemical Society Volume: 131 ISSN: 1520-5126 ISO Abbreviation: J. Am. Chem. Soc. Publication Date: 2009 Nov |
Date Detail:
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Created Date: 2009-11-20 Completed Date: 2010-02-09 Revised Date: - |
Medline Journal Info:
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Nlm Unique ID: 7503056 Medline TA: J Am Chem Soc Country: United States |
Other Details:
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Languages: eng Pagination: 16932-8 Citation Subset: - |
Affiliation:
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Inorganic Chemistry and Catalysis, Debye Institute for Nanomaterials Science, Utrecht University, Sorbonnelaan 16, 3584 CA Utrecht, The Netherlands. |
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