Graphene Quantum Dots-Supported Palladium Nanoparticles for Efficient Electrocatalytic Reduction of Oxygen in Alkaline Media

Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl2 in 1,2-propanediol at 80 °C in the presence of GQDs and then were subject to hydrothermal treatment at an elevated temperature within the range of 140 to 200 °C. Transmission electron mi...

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Published inACS sustainable chemistry & engineering Vol. 3; no. 12; pp. 3315 - 3323
Main Authors Deming, Christopher P, Mercado, Rene, Gadiraju, Vamsi, Sweeney, Samantha W, Khan, Mohammad, Chen, Shaowei
Format Journal Article
LanguageEnglish
Published American Chemical Society 07.12.2015
Subjects
graphene
hot water treatment
nanoparticles
oxygen
palladium
platinum
quantum dots
spectral analysis
temperature
transmission electron microscopy
X-radiation
X-ray photoelectron spectroscopy
Oxygen reduction
Defect
Palladium nanoparticle
Volcano plot
Hydrothermal
Graphene quantum dot
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Abstract Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl2 in 1,2-propanediol at 80 °C in the presence of GQDs and then were subject to hydrothermal treatment at an elevated temperature within the range of 140 to 200 °C. Transmission electron microscopic measurements showed a raspberry-like morphology for the samples before and after hydrothermal treatment at temperatures ≤160 °C, where nanoparticles of ca. 8 nm in diameter formed large aggregates in the range of 50 to 100 nm in diameter, and at higher hydrothermal temperatures (180 and 200 °C), chain-like nanostructures were formed instead. X-ray photoelectron and Raman spectroscopic measurements revealed that the GQD structural defects were readily removed by hydrothermal treatments, and the defect concentrations exhibited a clear diminishment with increasing hydrothermal temperature, as indicated by the loss of oxygenated carbons in XPS and a drop in the D to G band ratio in Raman measurements. Voltammetric studies showed apparent electrocatalytic activity toward oxygen reduction, with a volcano-shaped variation of the activity with GQD defect concentration, and the peak activity was observed for the sample prepared at 180 °C with a mass activity of 23.9 A/gPd and specific activity of 1.08 A/m2 at +0.9 V vs RHE. This peak activity is attributed to optimal interactions between Pd and GQD where the GQD defects promoted charge transfer from metal to GQDs and hence weakened interactions with oxygenated intermediates, leading to enhanced ORR activity. The corresponding defect concentration was higher than that identified with the platinum counterparts due to the stronger affinity of oxygen to palladium.
AbstractList Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl2 in 1,2-propanediol at 80 °C in the presence of GQDs and then were subject to hydrothermal treatment at an elevated temperature within the range of 140 to 200 °C. Transmission electron microscopic measurements showed a raspberry-like morphology for the samples before and after hydrothermal treatment at temperatures ≤160 °C, where nanoparticles of ca. 8 nm in diameter formed large aggregates in the range of 50 to 100 nm in diameter, and at higher hydrothermal temperatures (180 and 200 °C), chain-like nanostructures were formed instead. X-ray photoelectron and Raman spectroscopic measurements revealed that the GQD structural defects were readily removed by hydrothermal treatments, and the defect concentrations exhibited a clear diminishment with increasing hydrothermal temperature, as indicated by the loss of oxygenated carbons in XPS and a drop in the D to G band ratio in Raman measurements. Voltammetric studies showed apparent electrocatalytic activity toward oxygen reduction, with a volcano-shaped variation of the activity with GQD defect concentration, and the peak activity was observed for the sample prepared at 180 °C with a mass activity of 23.9 A/gPd and specific activity of 1.08 A/m2 at +0.9 V vs RHE. This peak activity is attributed to optimal interactions between Pd and GQD where the GQD defects promoted charge transfer from metal to GQDs and hence weakened interactions with oxygenated intermediates, leading to enhanced ORR activity. The corresponding defect concentration was higher than that identified with the platinum counterparts due to the stronger affinity of oxygen to palladium.
Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl₂ in 1,2-propanediol at 80 °C in the presence of GQDs and then were subject to hydrothermal treatment at an elevated temperature within the range of 140 to 200 °C. Transmission electron microscopic measurements showed a raspberry-like morphology for the samples before and after hydrothermal treatment at temperatures ≤160 °C, where nanoparticles of ca. 8 nm in diameter formed large aggregates in the range of 50 to 100 nm in diameter, and at higher hydrothermal temperatures (180 and 200 °C), chain-like nanostructures were formed instead. X-ray photoelectron and Raman spectroscopic measurements revealed that the GQD structural defects were readily removed by hydrothermal treatments, and the defect concentrations exhibited a clear diminishment with increasing hydrothermal temperature, as indicated by the loss of oxygenated carbons in XPS and a drop in the D to G band ratio in Raman measurements. Voltammetric studies showed apparent electrocatalytic activity toward oxygen reduction, with a volcano-shaped variation of the activity with GQD defect concentration, and the peak activity was observed for the sample prepared at 180 °C with a mass activity of 23.9 A/gPd and specific activity of 1.08 A/m² at +0.9 V vs RHE. This peak activity is attributed to optimal interactions between Pd and GQD where the GQD defects promoted charge transfer from metal to GQDs and hence weakened interactions with oxygenated intermediates, leading to enhanced ORR activity. The corresponding defect concentration was higher than that identified with the platinum counterparts due to the stronger affinity of oxygen to palladium.
Author Mercado, Rene
Deming, Christopher P
Gadiraju, Vamsi
Khan, Mohammad
Sweeney, Samantha W
Chen, Shaowei
AuthorAffiliation Department of Chemistry and Biochemistry
The Harker School
University of California
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  givenname: Vamsi
  surname: Gadiraju
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  givenname: Samantha W
  surname: Sweeney
  fullname: Sweeney, Samantha W
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  surname: Khan
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  givenname: Shaowei
  surname: Chen
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  email: Shaowei@ucsc.edu
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Graphene quantum dot
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Snippet Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl2 in 1,2-propanediol at 80 °C in the presence...
Graphene quantum dots (GQDs)-supported palladium nanoparticles were synthesized by thermolytic reduction of PdCl₂ in 1,2-propanediol at 80 °C in the presence...
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SubjectTerms graphene
hot water treatment
nanoparticles
oxygen
palladium
platinum
quantum dots
spectral analysis
temperature
transmission electron microscopy
X-radiation
X-ray photoelectron spectroscopy
Title Graphene Quantum Dots-Supported Palladium Nanoparticles for Efficient Electrocatalytic Reduction of Oxygen in Alkaline Media
URI http://dx.doi.org/10.1021/acssuschemeng.5b00927
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