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Structural Characterization of Platinum Alloy Nanoparticle Synthesis using 195-Pt NMR

Undergraduate #34
Discipline: Chemistry and Chemical Sciences
Subcategory: Chemistry (not Biochemistry)

Rickey Terrell - University of Cincinnati


To decrease costs of fuel cell fabrication, it is necessary to minimize precious metal loadings. A novel solution is dispersing platinum catalysts in nanoparticle form. The synthesis approach used to make these nanoparticles is directly related to their morphology and, as a consequence, their catalytic activity. Therefore, it is imperative to have characterization methods to observe the dynamic evolution of the chemical structures produced during the synthesis process. Previous structural data was acquired using EXAFS and Mössbauer Spectroscopy; however, a more robust method is nuclear magnetic resonance spectroscopy (NMR). In addition to being more readily accessible, NMR provides a greater flexibility of testing parameters and analysis tools. To confirm its utility in this field, experimental 195-Pt NMR data was collected and compared to data acquired using alternative characterization methods. Nanoparticle precursor solutions were synthesized containing three previously confirmed complexes: [Pt(SnCl3)]5-, [PtCl2(SnCl3)2]2-, and [PtCl3(SnCl3)]2-. All NMR data was collected using a Bruker 500 MHz spectrometer. The identity of the complexes in the solution were confirmed using both literature chemical shift values and theoretical NMR parameter calculations. Both experimental and theoretical 195-Pt chemical shift data aligns with past studies of platinum complexes in precursor nanoparticle solutions. With this new characterization method, NMR will provide a better understanding of nanoparticle synthesis mechanisms leading to the development of more catalytically active nanoparticles for fuel cell applications. Short term future work will include investigation of different platinum alloy nanoparticle synthesis to identify the relationship between alloy metal identity and nanoparticle properties. This research was funded by the National Science Foundation.

Funder Acknowledgement(s): National Science Foundation

Faculty Advisor: Dr. Anastasios Angelopoulos, angeloas@ucmail.uc.edu

Role: I completely developed and tested this new structural characterization method. I synthesized all samples, collected and analyzed all experimental NMR data, and completed all theoretical DFT calculations.

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This material is based upon work supported by the National Science Foundation (NSF) under Grant No. DUE-1930047. Any opinions, findings, interpretations, conclusions or recommendations expressed in this material are those of its authors and do not represent the views of the AAAS Board of Directors, the Council of AAAS, AAAS’ membership or the National Science Foundation.

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