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Instrumentation and Methods

Experimental Systems:

The group operates cutting-edge instruments and develops new experimental solutions that bridge between ideal ultraclean environments and true operation conditions (high-pressure, solid/liquid, electrochemical, photoelectrochemical environments).

A unique molecular beam / spectroscopy / reactor experiments been designed and set up, which allows us to perform most complex kinetic experiments in a quantitative, reproducible and fully remote-controlled fashion. Among other facilities, the system includes:

The image shows MOBY II at the laboratory.

MOBY-II (image: FAU)

  • Pulsed / chopped supersonic molecular beam source
  • Four modulated effusive beam sources
  • Vacuum-FT-IR-spectrometer for time resolved surface IR spectroscopy (TR-IRAS)
  • In-situ UV photochemistry in UHV
  • Fast ion-counting quadrupole mass spectrometer (QMS) w. multichannel scaling
  • Fast TR-IRAS-compatible pressure gap reactor
  • High-pressure cell for polarization-dependent TR-IRAS
  • Various preparation and characterization techniques for model surfaces (TPD, LEED, AES, etc.)
  • Vacuum sample transfer system

A new operando spectroscopy system brings together approaches to the preparation of catalytically active materials from different projects within the Excellence Cluster Engineering of Advanced Materials, including single-crystal based model catalysts, porous materials and films, powders, ionic liquid films, heterogenized homogeneous catalysts and others.

Libuda's laboratory with CIRCAT

CIRCAT (image: FAU)

The key features of the system include:

  • IRAS (IR Reflection Absorption Spectroscopy)
  • TR-IRAS (Time Resolved IR Spectroscopy, including Step Scan FTIR and Rapid Scan FTIR)
  • PM-IRAS (Polarization Modulation IRAS)
  • TIRS (Transmission IR Spectroscopy)
  • DRIFTS (Diffuse Reflection IR FT Spectroscopy)
  • Transient and Stationary Experiments (Pulse Gas Dosing and Laser Heating)
  • Real-Time Mass Spectrometry
  • Online High Sensitivity Gas Chromatography
  • Vacuum Transfer of UHV-Prepared Model Catalysts

A new high-end UHV-IRAS facility allows time-resolved in-situ studies of surface reactions, deposition, growth processes and nanomaterial synthesis.
SMURF at Libuda's laboratory

SMURF (image: FAU)

The key features include:

  • Vacuum-FT-IR-spectrometer for time resolved surface IR spectroscopy (TR-IRAS)
  • Combined IR spectroscopy in the FIR and MIR region (automatic beamsplitter changer)
  • Two remote-controlled gas dosers for adsorption studies
  • Two metal evaporator sources in IR measurement position
  • Two IL/organic evaporator sources in IR measurement position
  • TPD in IR measurement position
  • Four modulated effusive beam sources
  • Various preparation and characterization techniques for model surfaces (TPD, LEED, AES, etc.)
  • Vacuum sample transfer system

The IR spectro-electrochemistry system allow in-situ studies on electrified interfaces, both on real materials and on ideal model surface. The system allows electrochemical characterization and sample transfer under controlled conditions, including in-situ and time resolved photoelectrochemical studies.
ELISA I at Libuda's lab

ELISA I (image: FAU)

The key features include:

  • High-end vacuum-FT-IR-spectrometer
  • IR optics for fixed and variable angle
  • Time resolved interfacial IR spectroscopy (rapid scan and step scan)
  • Home-built electrochemical cells for IR spectroscopy in external reflection and in ATR
  • Spectroelectrochemistry in internal and external reflection (EC-IRRAS, SNIFTIRS, LPSIRS, SEIRAS)
  • Gas supply system for electrocatalytic studies (e.g. fuel cell, electrolysers, electrosynthesis)
  • Electrochemical characterization methods (cyclic voltammetry, electrochemical impedance spectroscopy)
  • Single crystal electrochemistry and characterization

The new ELISA II system allows in-situ preparation of complex model catalysts in UHV and direct sample transfer to the (spectro)electrochemical cell.
ELISA II at Libuda's lab

ELISA II (image: FAU)

The key features include:

  • UHV system with sample preparation (e.g. PVD) and characterization facilities (LEED, AES, TPD, etc.)
  • Sample transfer system (vacuum/protective gas)
  • Electrochemical characterization techniques: cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS)
  • Direct transfer to electrochemical IR spectroscopy (EC-IRRAS), differential electrochemical mass spectrometry (DEMS), electrochemical atomic force microscopy (EC-AFM), electrochemical scanning tunneling microscopy (EC-STM)

The new EMMA system is designed for electrochemical mass spectrometry at thin film samples, nanostructured electrodes and complex model electrodes prepared in UHV (direct sample transfer).
EMMA at Libuda's lab

EMMA (image: FAU)

The key features include:

  • Double differentially pumped UHV system with QMS
  • Differential electrochemical mass spectrometry (DEMS) in thin-film configuration
  • Online electrochemical mass spectrometry (OLEMS) with microprobe for planar model electrodes

The new ELSA system combines electrochemical scanning tunneling microscopy (EC-STM) and atomic force microscopy (EC-AFM) in controlled atmosphere with the preparation and transfer of complex model electrodes prepared in UHV (direct sample transfer).
ELSA at Libuda's lab

ELSA (image: FAU)

The key features include:

  • Electrochemical atomic force microscopy (EC-AFM)
  • Electrochemical scanning tunneling microscopy (EC-STM)
  • Sample transfer environment from UHV
  • Controlled gas environment and supply system
  • EC-STM tip preparation