Approach

We use potentiostats to control and measure electrocatalytic performance.

• Bio-Logic SP-150e - potentiostat with two potentiostat/galvanostat channels with electrochemical impedance spectroscopy (EIS). It is capable of performing cyclic voltammetry, linear sweep voltammetry, chronoamperometry, chronopotentiometry, and electrochemical impedance spectroscopy. It has a ± 10 µA to ± 1 A current range with a resolution of 0.004% of the selected range, ± 10 V adjustable range between -20 to 20 V with a 76 µV resolution, 20 µs acquisition time, and 1 MHz to 10 µHz EIS capability.
• Bio-Logic SP-300 - potentiostat with two potentiostat/galvanostat channels with electrochemical impedance spectroscopy (EIS). It is capable of performing cyclic voltammetry, linear sweep voltammetry, chronoamperometry, chronopotentiometry, and electrochemical impedance spectroscopy. It has a ± 10 nA to ± 1 A current range with a resolution of 0.004% of the selected range, ± 12 V range with a 76 µV resolution, 20 µs acquisition time, and 7 MHz to 10 µHz EIS capability.

We design custom electrochemical cells to enable in situ techniques. Some cells are 3D printed and others are machined using PEEK.

• ATR–SEIRAS  - electrochemical cell with optional lid for use with Pike VeeMax III ATR attachment
  • Corson, E. R., Kas, R., Kostecki, R., Urban, J. J., Smith, W. A., McCloskey, B. D., Kortlever, R. In-situ ATR–SIERAS of Carbon Dioxide Reduction at a Plasmonic Silver Cathode. Journal of the American Chemical Society, 2020, 142 (27), 11750–11762.
• GC - Front-illuminated photoelectrochemical cell with temperature control for precise gaseous product quantification
  • Corson, E. R., Creel, E. B., Kim, Y., Urban, J. J., Kostecki, R., McCloskey, B. D.  A Temperature-Controlled Photoelectrochemical Cell for Quantitative Product Analysis. Review of Scientific Instruments, 2018, 89, 055112.
• MakerBot Method X 3D Printer - a shared instrument at the KU Nanofabrication facility. Prints objects using a variety of materials via fused deposition modeling. Soluble support material maintains the integrity of complex shapes during the printing process. Objects up to 7.5" x 7.5" x 7.75"  (19 x 19 x 19.6 cm) in size can be printed. Layer resolution is 20–400 microns, depending on material. Nozzle diameter is 0.4 mm.

We fabricate nanostructured electrodes through various methods including chemical deposition, electrochemical deposition, electrochemical roughening, electron-beam evaporation, sputtering, dip-coating, and lithography. 

We use in situ vibrational spectroscopy to understand the mechanisms of (photo)electrocatalysis.

• ThermoFisher Scientific Nicolet iS50 - FTIR spectrometer with a KBr beamsplitter, liquid-nitrogen-cooled MCT detector, and rapid series data collection. It has a measurement speed of 65 scans per second at 16 cm−1 resolution, remote triggering capabilities to start in tandem with the potentiostat, a signal to noise ratio of 55,000:1, spectral resolution down to 0.09 cm−1 , and a wavenumber range from 600 to 7,800 cm−1 . A Pike VeeMAX III attachment is used with a custom-designed electrochemical cell to perform in situ ATR– SEIRAS.
• Renisha Virsa Raman Analyser - Raman analyzer with a 532 nm laser. It is equipped with 5x, 20x, and 50x objective lenses. The 50 mW laser intensity can be controlled from 0–100% with 0.1 mW precision. The fiber optic probe is 5 m long and has an XYZ positioning mount with a 100 nm step size. A custom-designed electrochemical cell is used to perform in situ SERS.

We perform ex situ product analysis to quantify the selectivity of the electrochemical reactions.

• Shimadzu GC 2030 - analysis of permanent gases and hydrogen. It is equipped with three detetectors: a TCD with argon carrier gas for hydrogen detection down to 50 ppm, a TCD with hydrogen carrier gas for nitrogen detection down to 50 ppm, and a methanizer FID for detection of carbon dioxide, carbon monoxide, methane, ethane, and ethylene down to 0.1 ppm. Three gas-sampling valves allow in-line operation during electrochemical experiments using a custom electrochemical cell and gas manifold.
• NMR - liquid product analysis. KU Nuclear Magnetic Resonance (NMR) core laboratory consists of nine instruments. The lab occupies more than 3000 sq. ft. in four different buildings on the KU-Lawrence campus: Malott Hall, the Shankel Structural Biology Center (SBC), the Multidisciplinary Research Building (MRB), and McCollum Laboratories.

We perform in situ experiments at synchrotrons to characterize the electrode–electrolyte interface.

• X-ray Reflectivity (XRR) and Resonant Anomalous X-ray Reflectivity (RAXR) - measure the structure of the electric double layer (EDL) with sub-angstrom resolution.
  • Proposal No. S-XV-ST-5984 - Structure of the Electric Double Layer during Nitrate Reduction, Stanford Synchrotron Radiation Lightsource (SSRL)