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 »
- Authors:
-
[2];
[4];
[3];
[1];
[6]
- Northwestern Univ., Evanston, IL (United States). Department of Chemistry
- Northwestern Univ., Evanston, IL (United States). Department of Chemical & Biological Engineering
- Northwestern Univ., Evanston, IL (United States). Department of Materials Science & Engineering
- Ames Lab. and Iowa State Univ., Ames, IA (United States)
- Northwestern Univ., Evanston, IL (United States). Department of Chemistry; Argonne National Lab. (ANL), Argonne, IL (United States). Chemical Sciences & Engineering Division
- Northwestern Univ., Evanston, IL (United States). Department of Chemistry and Department of Chemical & Biological Engineering
- Publication Date:
- Research Org.:
- Ames Laboratory (AMES), Ames, IA (United States); Argonne National Laboratory (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. doi: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 = {Fri Feb 02 00:00:00 EST 2018},
month = {Fri Feb 02 00:00:00 EST 2018}
}
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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 »
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Works referencing / citing this record:
Pd Single‐Atom Catalysts on Nitrogen‐Doped Graphene for the Highly Selective Photothermal Hydrogenation of Acetylene to Ethylene
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Figures/Tables have been extracted from DOE-funded journal article accepted manuscripts.