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
 


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: 785, 633, 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),
    see for example: Abstract online   ... ››

  • 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,
    see for example: Article online   ... ››

  • 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,
    see for example: Abstract online   ... ››

  • 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,
    see for example: Abstract online   ... ››
 


2-D photoluminescence spectroscopy of nano-structured MgO

(to see full size, click on the image)

Thermal analysis
  • Custom-designed setup for temperature-programmed reduction-oxidation reaction-oxidation experiments, chemisorption, and reactive frontal chromatography under flow conditions equipped with a TCD detector and a quadrupole mass spectrometer (Pfeiffer Vacuum): Abstract online   ... ››

  • 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: Abstract online   ... ››

  • 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 100bar.

  • Calve type in-situ calorimeter with plug-flow geometry Sensys Evo (Setaram) for studying the transformations of solid catalysts under conditions of catalytic reaction up to 800°C. The gas phase is simultaneously analyzed by the gas-chromatograph (Agilent) and custom-designed mass-spectrometer (Pfeiffer).
 
   
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   ... ››

    for application of temperature-programmed reaction and SSITKA experiments see for example:
    Article online   ... ››

  • Single and parallel reactors for hydrogenation reactions at high pressures,
    see for example: Abstract online   ... ››
 


Reaction network in selective oxidation of propane over vanadium oxide catalysts proposed based on temperature-programmed reaction and isotope exchange experiments

(to see full size, click on the image)

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Address: Fritz-Haber-Institut der Max-Planck-Gesellschaft, Faradayweg 4-6, 14195 Berlin, Germany    
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Tel: +49 30 8413 4404, Fax: +49 30 8413 4401, E-Mail: acsek@fhi-berlin.mpg.de