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Characterization of the Solid-Electrolyte Interface on Sn Film Electrodes by Electrochemical Quartz Crystal Microbalance

Bennett, Raffeal A
http://rave.ohiolink.edu/etdc/view?acc_num=osu1399048324

Abstract Details

2014, Master of Science, Ohio State University, Chemistry.
Lithium-ion batteries (LIBs) have been very successful as a source of rechargeable energy storage. These LIBs typically use graphite as an anode, which has high cyclability (> 200 cycles)(1) but a low charge capacity (372 mAh/g) compared to several pure metal anodes. Conversely, Sn is a promising low-cost, high charge capacity material (959 mAh/g) but suffers from low cyclability (20 useable cycles or less)(2, 3) due to irreversible capacity loss. This irreversible loss can be attributed to initial reduction of Sn-oxide (SnO/SnO2), formation/destruction of the (solid-electrolyte interface) SEI layer, and “pulverization” of electroactive Sn material (due to volumetric strain). In this study all three processes were electrochemically analyzed using galvanostatically electrodeposited Sn thin films. These Sn thin films were optimized for surface uniformity and reproducibility by screening films plated at 2 current densities (1 and 10 mA/cm 2), at 3 plating times (80, 240 and 600 s), and with 2 solution compositions (500 mM H2SO4 +10 mM SnSO4 with and without 5 mM hydroquinone) by profilometry, scanning electron microscopy, and optical microscopy. The optimal plating parameters were determined to be 1 mA/cm2 with hydroquinone at 80 s (~37 nm) and 240 s (~200 nm). Cyclic voltammetry and galvanostatic cycling with potential limitation (GCPL) was used to analyze 200 nm Sn films. Three peak couples were resolved using cyclic voltammetry at 4 scan rates (0.1, 1, 5 and 20 mV/s). These peaks were most resolved at 0.1 mV/s and appeared at potentials that correlated with literature. GCPL displayed a trend of capacity loss in almost every cycle and a cumulative capacity loss of ~ 90% on the 50th cycle. Electrochemical quartz crystal microbalance was performed on 37 nm Sn thin films with cyclic voltammetry between 0.4-2.0 V vs. Li/Li+ at 1 mV/s. The mass density change per cycle observed was 5.01 μg/cm 2 for the 1st cycle, 1.30 μg/cm 2 for the 2nd cycle, 0.43 μg/cm 2 for the 3rd cycle, 1.15 μg/cm 2 for the 4th cycle, and 0.40 μg/cm 2 for the 5th cycle. Also, mass/charge ratios observed around peak potentials ranged from 9.4 g/mol e- to 24 g/mol e-. The (mass change per mole of electrons) mpe values obtained from the first cycle were the highest. Continuous, irreversible mass deposition was observed each cycle in addition to the lithiation and delithiation processes (7 g/mol e-). These results can be accounted for by the possible formation of a Li2AuSn2 alloy and the use of a bottom potential limit that is 300 mV higher than in the other studies. Qualitatively this study does agree with the findings in literature about the gravimetric response of Sn electrode while cycled within a LIB test cell.
Anne Co (Advisor)
Susan Olesik (Committee Member)
92 p.
Chemistry
Electrochemistry QCMB SEI Sn tin

Recommended Citations

Citations

  • Bennett, R. A. (2014). Characterization of the Solid-Electrolyte Interface on Sn Film Electrodes by Electrochemical Quartz Crystal Microbalance [Master's thesis, Ohio State University]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=osu1399048324

    APA Style (7th edition)

  • Bennett, Raffeal. Characterization of the Solid-Electrolyte Interface on Sn Film Electrodes by Electrochemical Quartz Crystal Microbalance. 2014. Ohio State University, Master's thesis. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=osu1399048324.

    MLA Style (8th edition)

  • Bennett, Raffeal. "Characterization of the Solid-Electrolyte Interface on Sn Film Electrodes by Electrochemical Quartz Crystal Microbalance." Master's thesis, Ohio State University, 2014. http://rave.ohiolink.edu/etdc/view?acc_num=osu1399048324

    Chicago Manual of Style (17th edition)

osu1399048324
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This open access ETD is published by The Ohio State University and OhioLINK.