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Title: Fabrication of electrocatalytic Ta nanoparticles by reactive sputtering and ion soft landing

Abstract

About 40 years ago, it was shown that tungsten carbide exhibits similar catalytic behavior to Pt for certain commercially relevant reactions, thereby suggesting the possibility of cheaper and earth-abundant substitutes for costly and rare precious metal catalysts. In this work, reactive magnetron sputtering of Ta in the presence of three model hydrocarbons (2-butanol, heptane, and m-xylene) combined with gas aggregation and ion soft landing was employed to prepare organic-inorganic hybrid nanoparticles (NPs) on surfaces for evaluation of catalytic activity and durability. The electro-catalytic behavior of the NPs supported on glassy carbon was evaluated in acidic aqueous solution by cyclic voltammetry. The Ta-heptane and Ta-xylene NPs were revealed to be active and robust toward promotion of the oxygen reduction reaction, an important process occurring at the cathode in fuel cells. In comparison, pure Ta and Ta-butanol NPs were essentially unreactive. Characterization techniques including atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) were applied to probe how different sputtering conditions such as the flow rates of gases, sputtering current, and aggregation length affect the properties of the NPs. AFM images reveal the focused size of the NPs as well as their preferential binding along the step edgesmore » of graphite surfaces. In comparison, TEM images of the same NPs on carbon grids show that they bind randomly to the surface with some agglomeration but little coalescence. The TEM images also reveal morphologies with crystalline cores surrounded by amorphous regions for NPs formed in the presence of 2-butanol and heptane. In contrast, NPs formed in the presence of m-xylene are amorphous throughout. XPS spectra indicate that while the percentage of Ta, C, and O in the NPs varies depending on the sputtering conditions and hydrocarbon employed, the electron binding energies of the elements are similar for all of the NPs. Here, the difference in reactivity between the NPs is attributed to their Ta/C ratios. Collectively, the findings presented herein indicate that reactive magnetron sputtering and gas aggregation combined with ion soft landing offer a promising physical approach for the synthesis of organic-inorganic hybrid NPs that have potential as low-cost durable substitutes for precious metals in catalysis« less

Authors:
 [1];  [2];  [1];  [1];  [1]
  1. Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
  2. Michigan Technological Univ., Houghton, MI (United States)
Publication Date:
Research Org.:
Pacific Northwest National Lab. (PNNL), Richland, WA (United States)
Sponsoring Org.:
USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Chemical Sciences, Geosciences & Biosciences Division; USDOE Office of Science (SC), Biological and Environmental Research (BER) (SC-23); USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22)
OSTI Identifier:
1339839
Alternate Identifier(s):
OSTI ID: 1421077
Report Number(s):
PNNL-SA-122098
Journal ID: ISSN 0021-9606
Grant/Contract Number:  
AC05-76RL01830
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Chemical Physics
Additional Journal Information:
Journal Volume: 145; Journal Issue: 17; Journal ID: ISSN 0021-9606
Publisher:
American Institute of Physics (AIP)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; Ions and properties; Catalyst; Transmission electron microscopy; Transition metal carbides; Sputter deposition; Magnetron sputtering; Catalysis; Atomic force microscopy; X-ray photoelectron spectroscopy; Nanoparticles

Citation Formats

Johnson, Grant E., Moser, Trevor, Engelhard, Mark, Browning, Nigel D., and Laskin, Julia. Fabrication of electrocatalytic Ta nanoparticles by reactive sputtering and ion soft landing. United States: N. p., 2016. Web. doi:10.1063/1.4966199.
Johnson, Grant E., Moser, Trevor, Engelhard, Mark, Browning, Nigel D., & Laskin, Julia. Fabrication of electrocatalytic Ta nanoparticles by reactive sputtering and ion soft landing. United States. doi:10.1063/1.4966199.
Johnson, Grant E., Moser, Trevor, Engelhard, Mark, Browning, Nigel D., and Laskin, Julia. Tue . "Fabrication of electrocatalytic Ta nanoparticles by reactive sputtering and ion soft landing". United States. doi:10.1063/1.4966199. https://www.osti.gov/servlets/purl/1339839.
@article{osti_1339839,
title = {Fabrication of electrocatalytic Ta nanoparticles by reactive sputtering and ion soft landing},
author = {Johnson, Grant E. and Moser, Trevor and Engelhard, Mark and Browning, Nigel D. and Laskin, Julia},
abstractNote = {About 40 years ago, it was shown that tungsten carbide exhibits similar catalytic behavior to Pt for certain commercially relevant reactions, thereby suggesting the possibility of cheaper and earth-abundant substitutes for costly and rare precious metal catalysts. In this work, reactive magnetron sputtering of Ta in the presence of three model hydrocarbons (2-butanol, heptane, and m-xylene) combined with gas aggregation and ion soft landing was employed to prepare organic-inorganic hybrid nanoparticles (NPs) on surfaces for evaluation of catalytic activity and durability. The electro-catalytic behavior of the NPs supported on glassy carbon was evaluated in acidic aqueous solution by cyclic voltammetry. The Ta-heptane and Ta-xylene NPs were revealed to be active and robust toward promotion of the oxygen reduction reaction, an important process occurring at the cathode in fuel cells. In comparison, pure Ta and Ta-butanol NPs were essentially unreactive. Characterization techniques including atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) were applied to probe how different sputtering conditions such as the flow rates of gases, sputtering current, and aggregation length affect the properties of the NPs. AFM images reveal the focused size of the NPs as well as their preferential binding along the step edges of graphite surfaces. In comparison, TEM images of the same NPs on carbon grids show that they bind randomly to the surface with some agglomeration but little coalescence. The TEM images also reveal morphologies with crystalline cores surrounded by amorphous regions for NPs formed in the presence of 2-butanol and heptane. In contrast, NPs formed in the presence of m-xylene are amorphous throughout. XPS spectra indicate that while the percentage of Ta, C, and O in the NPs varies depending on the sputtering conditions and hydrocarbon employed, the electron binding energies of the elements are similar for all of the NPs. Here, the difference in reactivity between the NPs is attributed to their Ta/C ratios. Collectively, the findings presented herein indicate that reactive magnetron sputtering and gas aggregation combined with ion soft landing offer a promising physical approach for the synthesis of organic-inorganic hybrid NPs that have potential as low-cost durable substitutes for precious metals in catalysis},
doi = {10.1063/1.4966199},
journal = {Journal of Chemical Physics},
number = 17,
volume = 145,
place = {United States},
year = {2016},
month = {11}
}

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