Fritz-Haber-Institut der Max-Planck-Gesellschaft  

Inorganic Chemistry – Reactivity Group
  

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Reactivity Group:
Annette Trunschke
 
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Methods:
 
The sophisticated formulation and complexity of heterogeneous catalysts requires the application of controlled synthesis conditions and well-defined chemicals for their reproducible preparation. The work of the group is targeted on a deeper understanding of catalyst synthesis ranging from the assembly of molecular building blocks in solution to phase transformations during thermal pretreatment procedures. New synthetic concepts are developed using automated laboratory reactor systems for precipitation and hydrothermal synthesis equipped with probes for measuring pH, conductivity, turbidity, viscosity, pressure, temperature, Raman, and UV-vis spectra. The thermal treatments are performed in rotating furnaces under controlled atmosphere.

In collaboration with other groups of the Department of Inorganic Chemistry morphology, bulk, and electronic structure of precursors and catalysts are investigated ex-situ and in-situ by electron microscopy, X-ray diffraction, photoelectron spectroscopy, and conductivity measurements. Molecular spectroscopy is used to understand catalyst synthesis, and to analyze bulk and surface properties of the catalysts. The nature and number of the active sites at the catalyst surface and the reaction mechanisms are addressed by adsorption of reactants and probe molecules in static or flow operation at 77-873 K, in-situ spectroscopic experiments including the confirmation of catalyst operation by product analysis, and microreactor studies.
 
Examples of the technical equipment:


Synthesis
  • Automated laboratory reactor system (Mettler-Toledo Labmax®)

  • Analytic autoclaves (Premex Reactor AG),
    see for example: Abstract online   ... ››

  • MULTWAVE PRO 50Hz (Anton Paar Germany GmbH) for microwave-assisted synthesis

  • Malvern Zetasizer Nano System for determination of particle size distributions and zeta potentials of suspensions

  • Rotating furnaces for thermal treatment under controlled flow of variable gas mixtures, for detailed description of a rotating oven, see for example: Thesis Thomas Cotter, 2011  ... ››
 


Analytical autoclave HPM-PT-040 (Premex Reactor AG) coupled with a
Raman Spectrometer RXN1 (Kaiser Optics)

(to see full size, click on the image)

Molecular spectroscopy
  • Raman spectrometer TriVista TR557 (S&I Spectroscopy & Imaging GmbH) equipped with a confocal Raman microscope, lasers sources: 532, 488, 457, 442, 355, 325, 266 nm, Linkam CCR-1000 reactor stage for in-situ studies coupled with a micro GC (Agilent) and a mass spectrometer OmniStar (Pfeiffer Vacuum)

  • FITR spectrometers (Cary 680 (Agilent), Varian-670 FTIR spectrometer, Spectrum 100 (Perkin Elmer)) equipped with MCT detectors and in-situ cells for measurements in transmission, diffuse reflectance and ATR

  • UV-vis-NIR spectrometer Cary 5000 (Agilent) and Lambda 650 UV-vis spectrometer (Perkin Elmer) equipped with Harrick DR accessories (HVC-VUV-4) for in-situ studies

  • Photoluminescence spectrometer LS-55 (Perkin Elmer) equipped with a red-sensitive photomultiplier R928 from Hamamatsu Photonics that allows the detection of emissions in the range between 200 and 900 nm and a sample pretreatment and gas dosing system
 


2-D photoluminescence spectroscopy of nano-structured MgO

(to see full size, click on the image)

Thermal analysis
  • Temperature-programmed reduction-reaction-oxidation instrument TPDRO-1100 (CE Instruments), see for example: Abstract online   ... ››

  • Home-made setup for temperature-programmed reduction-reaction-oxidation-desorption experiments, chemisorption, and reactive frontal chromatography equipped with a TCD detector and a quadrupol mass spectrometer (Pfeiffer Vacuum)

  • STA449 Jupiter thermoanalyser (Netzsch) for simultaneous thermal analysis up to 1600°C, equipped with the pulse box for PulseTA® . The setup is coupled with a quadrupole mass spectrometer QMS200 Omnistar (Pfeiffer Vacuum) for monitoring the evolution of the gas phase

  • High pressure thermobalance (Rubotherm) coupled with GAM 200 mass-spectrometer for in-situ thermoanalysis up to 1000°C and 40bar,
    see for example: Abstract online   ... ›› and: Abstract online   ... ››

  • The Differential scanning calorimeter HP DSC827e (METTLER) allows precise measurements of the phase transitions in different atmospheres up to 600°C and 10MPa
 
   
Test reactors
  • Single-tube, cascade, and parallel (ILS) fixed-bed reactors for gas phase oxidation equipped with GC-MS, GC (Agilent), on-line gas analyzer (X-Stream, Emerson/Rosemount), and MS OmniStar™ (Pfeiffer Vacuum),
    for application of a parallel reactor see for example:
    Abstract online   ... ››

  • Single and parallel reactors for hydrogenation reactions at high pressures,
    see for example: Abstract online   ... ››
 
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   Webmaster: Olaf Trunschke
Address: Fritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, 14195 Berlin, Germany    
Abteilung Anorganische Chemie - Direktor Prof. Dr. Robert Schlögl    
Tel: +49 30 8413 4404, Fax: +49 30 8413 4401, E-Mail: acsek@fhi-berlin.mpg.de