Instrumentation of Department of Electrochemistry at Nano-Scale

A: Major Equipment for Standard and Advanced Electrochemical Techniques

1) Potentiostats/galvanostats: several EG&G PAR 273A (USA), two EG&G PAR 263A (Princeton Applied Research, USA), AUTOLAB PGSTAT12, three PGSTAT30, Metrohm AUTOLAB 302N (FRA, ECD, ADC10M, SCAN250), two PGSTAT101 and one PGSTAT204 (Metrohm, Switzerland), bipotentiostat/galvanostat WD 20 and AFP2 (Pine Research Instrumentation, USA), several Eco-Tribo polarographs (Polarosensors), several polarographic analyzers PA3 and PA4 (Laboratorní přístroje, Czech Republic), several home-made potentiostats

2) Impedance spectrum analyzers: two-channel network signal analyzer system SR780 (Stanford Research Systems, USA), two FRA modules for EIS measurements (Metrohm, Switzerland), three lock-in amplifiers SR830 (Stanford Research Systems, USA), several single channel lock-in amplifiers

3) Electrode units: two 663VA stand (Metrohm, Switzerland), three rotating disk electrodes (Metrohm, Switzerland and Pine Research Instrumentation, USA), several Static Mercury Drop Electrode systems (SMDE, Laboratorní přístroje, Czech Republic), several rotating disk electrodes (RDE, Laboratorní přístroje, Czech Republic), home-made ultramicro-electrodes and insulated STM tips, single crystal gold mircoelectrodes, home-made amalgam electrode systems.

4) Electrochemical Scanning Probe Microscope: Agilent SPM 5500 (Keysight Technologies, UK), both AFM and STM options, MAC III mode, variable temperature (-5 to 150°C) and controlled-environment option, electric force and Kelvin force microscopy.

5) Scanning Tunneling Microscopy Break Junction System: home-made setup for single molecule conductance measurements and Mechanically-Controllable Break Junction System: home-made setup for single molecule conductance measurements
Home-made instrumentation and "black box" for ECL (Electrochemically generated luminescence)equipped with photomultipliers Carl Zeiss, Jena and HAMAMATSU.

    B: Spectrometers for in-situ combination with electrochemistry

    1) UV-VIS absorption spectrometers: diode array Agilent 8453, Shimadzu UV-1800 and a miniature spectrometer STS-UV (Ocean Optics) with equipment (cells, electrodes, quartz-fibers) for in-situ spectroelectrochemistry

    2) FTIR spectrometer Nicolet iS50 NIR-FTIR with ATR option (Thermo Scientific) with equipment (cells, electrodes) for in-situ spectroelectrochemistry

    3) EPR spectrometer: Varian E4 with equipment (cells, electrodes) for in-situ spectroelectrochemistry

    4) Ultrasound generator Bandelin Sono+ (20kHz, 100 Watt) and High-frequency ultrasound generator BTL-4000 (1 and 3 MHz) with the half-inch ultrasound horn and with equipment (cells, electrodes) for in-situ sonoelectrochemistry.

    5) Fluorescence spectrometer LS50B (Perkin Elmer)

    C: Available Methods

    1) Electrochemical Methods:

    All standard and advanced methods for fundamental research, electrosynthesis and electroanalysis in aqueous as well as in dry, aprotic (organic) media or in liquid SO2 are commonly used, including dc-polarography, linear sweep and cyclic voltammetry, differential pulse polarography and voltammetry, square-wave polarography and voltammetry, bulk electrolysis, coulometry, chronoamperometry, chronocoulometry, chronopotentiometry, AC polarography and voltammetry, electrochemical impedance spectroscopy, fast scan rate voltammetry using ultramicroelectrodes.
    For all measurements electrodes of various shape and material are available: mercury, mercury amalgams, platinum, gold, single crystal gold, silver, glassy carbon, graphite, BDDE (Boron-Doped Diamond Electrodes), optically transparent Indium-Tin Oxide (ITO) electrodes, platinum and gold ultramicroelectrodes as well as insulated SPM ultramicroelectrodes for electrochemical scanning probe microscopy.
    Studies of electron transfer mechanisms and kinetics, electrochemical transformation of the organic compounds, investigation of intramolecular electron interaction between two or more redox centers, studies of the relationship between structure - redox properties - activity (bio-, photo-, catalytic-, pharmacology-, ...), adsorption studies.
    Voltammetric analysis in batch and flow systems - analytical application in electroanalytical sensors, biosensors and flow-through detection.

    2) Spectroelectrochemical Methods:
    In-situ combination of electrochemistry with UV-VIS-NIR, FTIR and EPR spectroscopy in mechanistic studies of the systems undergoing redox transformation in aqueous as well as organic solvents, interception and identification of (radical) intermediates, characterization of products, evaluation of kinetics and stability.
    In-situ sono(electro)chemistry - studies of cavitation in bulk as well as at the electrode surface, generation and investigation of nanobubbles.

    3) Methods for self-assembly characterization at the electrode-electrolyte interface include differential capacitance measurements, STM and AFM imaging under potential control, force measurements and conductance measurements, QCM measurements etc. for electrode modification, mechanistic studies on modified electrodes, sensor development.

    4) Methods for charge transport studies in self-assembled monolayers and single molecule junctions include temperature dependent I-V measurements, scanning tunneling spectroscopy, STMBJ and MCBJ for single molecule conductance studies. Applications in electrode modification, mechanistic studies on modified electrodes, single molecule response, molecular electronics.

    5) Electrochemically generated chemiluminescence (ECL) as a method for detection of very shortly living radical intermediates in mechanistic studies or as a method for alternative generation of singlet and triplet states and evaluation of their energies.

    6) Quantum chemical calculations of HOMO-LUMO energies, electron distribution, optimized geometry, transmission functions, molecular conductance and junction geometries

    7) Theoretical modeling of voltammetric curves, UV-vis and EPR spectra, as well as of physicochemical data using program PHREEQC.

    D: Additional equipment

    1) Water purification system: Integral5, Milli-Q (Merck, Germany)

    2) Quartz crystal microbalance: QCM200 (Stanford Research Systems, USA)

    3) Dry box: Labstar 50 (MBraun, Germany)

    4) Grinder/Polisher: Metaserv 2000, Buehler (Germany)

    5) Inverted Metallurgical microscope: MTM Intraco Micro

    6) Rotating vacuum evaporator: Heidolph and Büchi (Germany)

    7) Amalgam mixer: Dentomat compact DEGUSSA-HÜLS (Brasil)

    8) pH-ORP meter HI3220 (Hanna Instruments)

    9) Conductivity Meter 4010 (Jenway)

    10) Thermostats

    11) UV-lamp (Krüss, Optronics), laser source

    12) Melting-point meter (Kofler)

    13) Equipment for flash-chromatography

    15) Optical microscopes

    Department of Electrochemistry at the Nanoscale