All facilities and equipment necessary for conducting BEES research are currently available for use at CWRU, the participating universities, and BNL. These include equipment/instrumentation for spectroscopic, surface/chemical, and electrochemical analysis and high-speed computations. Several of the KRs have joint appointments with Oak Ridge National Laboratory and have access to specialized facilities to support their research. The techniques, instrumentation, and facilities of the KRs are all available to the EFRC.
BEES researchers (MD, and DH) have state-of-the-art facilities available to them at Oak Ridge National Laboratory (ORNL, Oak Ridge, TN), National Institute of Standards Center for Neutron Research (NIST-NCNR, Gaithersburg, MD), and the Advanced Photon Source (APS) Argonne National Laboratory (ANL, Lemont, IL) to characterize electrolyte solutions for both Thrusts 1 and 2 (i.e., DESs, microemulsions and NOHMs) in terms of structure, dynamics and transport properties. SAXS and Ultra SAXS (USAXS) has been used routinely to determine structure of microemulsions and NOHMs using the Rigaku SAXS instrument at ORNL and beamlines at ANL-APS, respectively. SANS and USANS are available to us at ORNL (Bio-SANS, GP-SANS, EQ-SANS and USANS beam lines) and NIST (NG7 and NGB 30m SANS). Through selective deuteration and neutron contrast matching techniques, SANS provides more definitive structural information than SAXS as well as interactions between nanodispersions. The SANS instruments possess unique sample environments to allow us to probe structural changes with temperature control and in the presence of electrical current cycles and shear stress. Both ORNL and NIST possess NR instrumentation that allow us to probe the interactions of the nanostructured electrolyte solutions at the interface with electrode surfaces at atomic resolution, the latter of which can be modified chemically by us. Similar to SANS, we are able to control temperature and incorporate electrical currents into the sample environment. In fact, we are working with NIST scientists to develop a new reflectometry cell that will allow us to monitor the structure of soft electrolytes near a surface in the presence of an electric field. To probe the dynamics of electrolyte solutions, neutron spin-echo and quasielastic neutron scattering (NSE and QENS, respectively) are available at both NIST and ORNL, with QENS providing a smaller length and time scale. For instance, NSE can be used to measure the thermal motions of microemulsions’ surfactant monolayers while QENS can probe the internal and lateral motions of individual surfactant molecules.
At BNL, in the lab of BEES key researcher MV, there are special in situ electrochemical imaging and spectroscopic equipment. To gain a deeper understanding of electrodeposition and dissolution of metals in DESs, specifically the initial electro-nucleation stages, local and in-situ techniques like electrochemical scanning tunneling microscopy (ECSTM) and IR are necessary. ECSTM is a very powerful tool for local investigation of the electrode surface and processes taking place at the electrode-solution interface. A great advantage of this technique is that it allows performing time imaging within a widely variable resolution range. Thus, surface changes caused by reactions (electrodeposition, DES decomposition) can be monitored in time at fixed or variable electrochemical conditions (potential for example). Infrared spectroscopy techniques facilitate studying electrode/electrolyte interfaces at a molecular level, providing information on adsorption/desorption, surface bonding, orientation, and coordination of the adsorbed species. With well calibrated system, quantitative or semi-quantitative analysis is possible. At BNL, there are two Molecular Imaging ECSTMs for in situ surface structural studies and a fast-scan Nicolet iS50 FTIR spectrometer equipped with liquid nitrogen cooled MCT-A detector for in situ IRRAS and SEIRAS infrared studies (IRRAS= Infrared Reflectance Absorption Spectroscopy, ATR-SEIRAS=Attenuated Total Reflectance Infrared Absorption Spectroscopy). We also have a customized electrochemical cell and lens configuration that is capable of in situ electrochemical IRRAS measurement and ATR-SEIRAS measurement. The electrochemical cell is capable of atmosphere and temperature control.
Located at Hunter College, key researcher SG has unique NMR equipment in his lab used in this project, including:
- A Stelar Spinmaster 1T fast Field Cycling Nuclear Magnetic Resonance Relaxometer
- Broadband relaxation data in local fields ranging from ~0.002 – 1 T for investigation of molecular diffusive and rotational motions, and the possible coupling between them.
- A High pressure NMR probe
- Hydrostatic pressure as a thermodynamic variable allows the computation of molecular activation volumes. Range: atmospheric to 250 MPa
Standard 300, 400, and 500 MHz NMR instruments are also available as well as a 900 MHz shared facility at the NY Structural Biology Center.