From single-site tantalum complexes to nanoparticles of TaxNy and TaOxNy supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy

Mohandas, Janet C.; Abou-Hamad, Edy; Callens, Emmanuel; Samantaray, Manoja K.; Gajan, David; Gurinov, Andrei; Ma, Tao; Ould-Chikh, Samy; Hoffman, Adam S.; Gates, Bruce C.; Basset, Jean-Marie

doi:10.1039/c7sc01365e

Title: From single-site tantalum complexes to nanoparticles of Ta_xN_y and TaO_xN_y supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy

Journal Article · Thu Jun 08 00:00:00 EDT 2017 · Chemical Science

DOI:https://doi.org/10.1039/c7sc01365e· OSTI ID:1624951

^[1]; Abou-Hamad, Edy ^[1];

^[1];

^[1]; Gajan, David ^[2];

^[1];

^[3];

^[1]; Hoffman, Adam S. ^[3];

^[3];

^[1]

King Abdullah Univ. of Science and Technology, Thuwal (Saudi Arabia)
Univ. of Lyon (France)
Univ. of California, Davis, CA (United States)

Air-stable catalysts consisting of tantalum nitride nanoparticles represented as a mixture of Ta_xN_y and TaO_xN_y with diameters in the range of 0.5 to 3 nm supported on highly dehydroxylated silica were synthesized from TaMe₅ (Me = methyl) and dimeric Ta₂(OMe)₁₀ with guidance by the principles of surface organometallic chemistry (SOMC). Characterization of the supported precursors and the supported nanoparticles formed from them was carried out by IR, NMR, UV-Vis, extended X-ray absorption fine structure, and X-ray photoelectron spectroscopies complemented with XRD and high-resolution TEM, with dynamic nuclear polarization surface enhanced NMR spectroscopy being especially helpful by providing enhanced intensities of the signals of ¹H, ¹³C, ²⁹Si, and ¹⁵N at their natural abundances. The characterization data provide details of the synthesis chemistry, including evidence of (a) O₂ insertion into Ta–CH₃ species on the support and (b) a binuclear to mononuclear transformation of species formed from Ta₂(OMe)₁₀ on the support. A catalytic test reaction, cyclooctene epoxidation, was used to probe the supported nanoparticles, with 30% H₂O₂ serving as the oxidant. The catalysts gave selectivities up to 98% for the epoxide at conversions as high as 99% with a 3.4 wt% loading of Ta present as Ta_xN_y/TaO_xN_y.

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Research Organization:: SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States)

Sponsoring Organization:: USDOE Office of Science (SC)

Grant/Contract Number:: AC02-76SF00515

OSTI ID:: 1624951

Journal Information:: Chemical Science, Vol. 8, Issue 8; ISSN 2041-6520

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 12 works

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Title: From single-site tantalum complexes to nanoparticles of Ta_xN_y and TaO_xN_y supported on silica: elucidation of synthesis chemistry by dynamic nuclear polarization surface enhanced NMR spectroscopy and X-ray absorption spectroscopy