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Title: Synthesis of Supported Pd0 Nanoparticles from a Single-Site Pd2+ Surface Complex by Alkene Reduction

Abstract

A surface metal-organic complex, (-AlOx)Pd(acac) (acac = acetylacetonate), is prepared by chemically grafting the precursor Pd(acac)(2) onto gamma-Al2O3 in toluene at 25 degrees C. The resulting surface complex is characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and dynamic nuclear polarization surface-enhanced solid-state nuclear magnetic resonance spectroscopy (DNP SENS). This surface complex is a precursor in the direct synthesis of size-controlled Pd nanoparticles under mild reductive conditions and in the absence of additional stabilizers or pretreatments. Indeed, upon exposure to gaseous ethylene or liquid 1-octene at 25 degrees C, the Pd2+ species is reduced to form Pd-0 nanoparticles with a mean diameter of 4.3 +/- 0.6 nm, as determined by scanning transmission electron microscopy (STEM). These nanoparticles are catalytically relevant using the aerobic 1-phenylethanol oxidation as a probe reaction, with rates comparable to a conventional Pd/Al2O3 catalyst but without an induction period. Diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and temperature-programmed reaction mass spectrometry (TPR-MS) reveal that the surface complex reduction with ethylene coproduces H-2, acetylene, and 1,3-butadiene. This process reasonably proceeds via an olefin activation/coordination/insertion pathway, followed by beta-hydride elimination to generate free Pd-0. The well-defined nature of the single-sitemore » supported Pd2+ precursor provides direct mechanistic insights into this unusual and likely general reductive process.« less

Authors:
 [1]; ORCiD logo [2];  [3];  [1];  [4]; ORCiD logo [4]; ORCiD logo [3]; ORCiD logo [1];  [5]; ORCiD logo [6]
  1. Northwestern Univ., Evanston, IL (United States). Department of Chemistry
  2. Northwestern Univ., Evanston, IL (United States). Department of Chemical & Biological Engineering
  3. Northwestern Univ., Evanston, IL (United States). Department of Materials Science & Engineering
  4. Ames Lab. and Iowa State Univ., Ames, IA (United States)
  5. Northwestern Univ., Evanston, IL (United States). Department of Chemistry; Argonne National Lab. (ANL), Argonne, IL (United States). Chemical Sciences & Engineering Division
  6. Northwestern Univ., Evanston, IL (United States). Department of Chemistry and Department of Chemical & Biological Engineering
Publication Date:
Research Org.:
Ames Lab., Ames, IA (United States); Argonne National Lab. (ANL), Argonne, IL (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES)
OSTI Identifier:
1427728
Alternate Identifier(s):
OSTI ID: 1461330
Report Number(s):
IS-J-9596
Journal ID: ISSN 0897-4756; TRN: US1802603
Grant/Contract Number:  
AC02-07CH11358; FG02-03ER154757; AC02-06CH11357; FG02-03ER15457
Resource Type:
Accepted Manuscript
Journal Name:
Chemistry of Materials
Additional Journal Information:
Journal Volume: 30; Journal Issue: 3; Journal ID: ISSN 0897-4756
Publisher:
American Chemical Society (ACS)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 36 MATERIALS SCIENCE

Citation Formats

Mouat, Aidan R., Whitford, Cassandra L., Chen, Bor-Rong, Liu, Shengsi, Perras, Frédéric A., Pruski, Marek, Bedzyk, Michael J., Delferro, Massimiliano, Stair, Peter C., and Marks, Tobin J. Synthesis of Supported Pd0 Nanoparticles from a Single-Site Pd2+ Surface Complex by Alkene Reduction. United States: N. p., 2018. Web. https://doi.org/10.1021/acs.chemmater.7b04909.
Mouat, Aidan R., Whitford, Cassandra L., Chen, Bor-Rong, Liu, Shengsi, Perras, Frédéric A., Pruski, Marek, Bedzyk, Michael J., Delferro, Massimiliano, Stair, Peter C., & Marks, Tobin J. Synthesis of Supported Pd0 Nanoparticles from a Single-Site Pd2+ Surface Complex by Alkene Reduction. United States. https://doi.org/10.1021/acs.chemmater.7b04909
Mouat, Aidan R., Whitford, Cassandra L., Chen, Bor-Rong, Liu, Shengsi, Perras, Frédéric A., Pruski, Marek, Bedzyk, Michael J., Delferro, Massimiliano, Stair, Peter C., and Marks, Tobin J. Fri . "Synthesis of Supported Pd0 Nanoparticles from a Single-Site Pd2+ Surface Complex by Alkene Reduction". United States. https://doi.org/10.1021/acs.chemmater.7b04909. https://www.osti.gov/servlets/purl/1427728.
@article{osti_1427728,
title = {Synthesis of Supported Pd0 Nanoparticles from a Single-Site Pd2+ Surface Complex by Alkene Reduction},
author = {Mouat, Aidan R. and Whitford, Cassandra L. and Chen, Bor-Rong and Liu, Shengsi and Perras, Frédéric A. and Pruski, Marek and Bedzyk, Michael J. and Delferro, Massimiliano and Stair, Peter C. and Marks, Tobin J.},
abstractNote = {A surface metal-organic complex, (-AlOx)Pd(acac) (acac = acetylacetonate), is prepared by chemically grafting the precursor Pd(acac)(2) onto gamma-Al2O3 in toluene at 25 degrees C. The resulting surface complex is characterized by inductively coupled plasma atomic emission spectroscopy (ICP-AES), X-ray photoelectron spectroscopy (XPS), X-ray absorption spectroscopy (XAS), and dynamic nuclear polarization surface-enhanced solid-state nuclear magnetic resonance spectroscopy (DNP SENS). This surface complex is a precursor in the direct synthesis of size-controlled Pd nanoparticles under mild reductive conditions and in the absence of additional stabilizers or pretreatments. Indeed, upon exposure to gaseous ethylene or liquid 1-octene at 25 degrees C, the Pd2+ species is reduced to form Pd-0 nanoparticles with a mean diameter of 4.3 +/- 0.6 nm, as determined by scanning transmission electron microscopy (STEM). These nanoparticles are catalytically relevant using the aerobic 1-phenylethanol oxidation as a probe reaction, with rates comparable to a conventional Pd/Al2O3 catalyst but without an induction period. Diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and temperature-programmed reaction mass spectrometry (TPR-MS) reveal that the surface complex reduction with ethylene coproduces H-2, acetylene, and 1,3-butadiene. This process reasonably proceeds via an olefin activation/coordination/insertion pathway, followed by beta-hydride elimination to generate free Pd-0. The well-defined nature of the single-site supported Pd2+ precursor provides direct mechanistic insights into this unusual and likely general reductive process.},
doi = {10.1021/acs.chemmater.7b04909},
journal = {Chemistry of Materials},
number = 3,
volume = 30,
place = {United States},
year = {2018},
month = {2}
}

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Figures / Tables:

Figure 1 Figure 1: (A) Pd(3d5/2) XPS spectra of (-AlOx)Pd(acac) (purple), PdO/Al2O3 (green), and Pd(acac)2 (black). (B) DNP SENS 1H-13C CPMAS NMR of (i) (-AlOx)Pd(acac), (ii) (- AlOx)Pd(acac) after 96 h in 1-octene at 25 °C, and (iii) after 120 h in 1-octene at 25 °C. Red dots denote signals attributable tomore » the (-AlOx)Pd(acac) complex. Orange dots denote signals attributable to free acetylacetone on the alumina surface. Green dots represent an unidentified surface species, possibly surface acetate. Blue dots represent carbonate.« less

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  • Choi, Kwang-Min; Akita, Tomoki; Mizugaki, Tomoo
  • New Journal of Chemistry, Vol. 27, Issue 2
  • DOI: 10.1039/b207098g

Hydroxyapatite-Supported Palladium Nanoclusters:  A Highly Active Heterogeneous Catalyst for Selective Oxidation of Alcohols by Use of Molecular Oxygen
journal, September 2004

  • Mori, Kohsuke; Hara, Takayoshi; Mizugaki, Tomoo
  • Journal of the American Chemical Society, Vol. 126, Issue 34
  • DOI: 10.1021/ja0488683

Selective oxidation with air on metal catalysts
journal, September 1997


Effect of Catalysis on the Stability of Metallic Nanoparticles:  Suzuki Reaction Catalyzed by PVP-Palladium Nanoparticles
journal, July 2003

  • Narayanan, Radha; El-Sayed, Mostafa A.
  • Journal of the American Chemical Society, Vol. 125, Issue 27
  • DOI: 10.1021/ja035044x

ATHENA , ARTEMIS , HEPHAESTUS : data analysis for X-ray absorption spectroscopy using IFEFFIT
journal, June 2005


    Works referencing / citing this record:

    Pd Single‐Atom Catalysts on Nitrogen‐Doped Graphene for the Highly Selective Photothermal Hydrogenation of Acetylene to Ethylene
    journal, February 2019


    Palladium single atoms supported by interwoven carbon nanotube and manganese oxide nanowire networks for enhanced electrocatalysis
    journal, January 2018

    • Xiang, Weikai; Zhao, Yonghui; Jiang, Zheng
    • Journal of Materials Chemistry A, Vol. 6, Issue 46
    • DOI: 10.1039/c8ta09034c