Department of
Inorganic Chemistry


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Axel Knop-Gericke
 
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BESSY laboratory
 
BESSY laboratory:
 
ISISS, BElChem, and CAT@EMIL facilities

The ultimate surface and element sensitivity on the one hand and the possibility to vary the information depth on the other hand adds an extra quality to XPS when operated with a tuneable X-ray source like a synchrotron. In addition, X-ray absorption spectra (XAS) can be taken at a synchrotron. The HZB (Helmholtz-Zentrum Berlin) and the FHI/MPI-CEC operate three laboratories dedicated to synchrotron based ambient pressure XP spectroscopy at the 3rd generation X-ray source BESSY located in the south east of Berlin. These facilities are: ISISS (Innovative Station for In Situ Spectroscopy), CAT@EMIL (Energy Materials In Situ Laboratory Berlin), and the currently under construction BElChem laboratory (Berlin Joint Lab for ElectroChemical Interfaces). A scheme of the design approach of these facilities is shown as Fig. 1. These laboratories combine in a unique matter a state of the art soft X-ray beamline, a ambient pressure XPS endstation (AP-XPS), and a proper, permanent infrastructure on site for experiments with a chemical background.


Synchrotron X-ray spot in front of the entrance aperture of the AP-XPS spectrometer visible on a fluorescence screen.
Fig. 1: Scheme of approach
The beamlines are designed following the principle of a plane grating monochromator (PGM) working in collimated light (Fig. 2). A refocussing optics allows creating small enough X-ray spots with an optimized match to the size of the entrance aperture of the AP-XPS electron spectrometer. This allows a flexible operation adapted to the different needs of the users. For example the monochromator can be operated in different modes i.e. high flux, high spectral resolution, or higher order suppression (thereby increasing the spectral purity of delivered X-ray beam). The beamlines exploit the synchrotron radiation of either a bending magnet (ISISS) or an APPLE II type undulator (CAT@EMIL and BElChem) with the option of variable polarized light.
Fig. 2: The optical layout of the ISISS beamline at BESSY exemplifying the typical layout of a PGM based beamline with vertically collimating mirror M1 and refocussing optics M4.
 
The beamlines offer a high photon flux up to 1*1012 photons/ sec/ 0.1A ring current and a broad energy range 90eV - 2000eV with a high photon flux. The monochromatic photon flux of the ISISS, CAT@EMIL and BElChem beamlines is compared in Fug. 3 for exit slit settings that result in a similar spectral resolution of all three beamlines. In phase 2 of the EMIL project (scheduled to be finished in 2020) the available energy range at CAT will be increased to the tender X-ray range of 2keV – 10keV by exploiting the radiation of an additionally installed cryogenic in-vacuum undulator (U17) and implementing a nitrogen cooled double crystal monochromator (DCM) in the beamline. This will establish a unique beamline at BESSY II that covers a very wide and continuous photon energy range from the soft energy region up to the tender X-ray region combined in one focus. The MPG operates a high kinetic energy AP-XPS spectrometer inside the CAT lab. This spectrometer is capable to cover a kinetic energy range of photoelectrons up to 7000eV nicely matching the available photon energy range for excitation at the CAT beamline.
Fig. 3: Photon flux after passing a Si3N4 X-ray membrane of the three beamlines ISISS, CAT@EMIL (UE48 CAT), and BElChem (UE56/2-PGM1) at similar spectral resolution. Exit slit sizes as indicated.
 
The photon beam is re-focused after the exit slit to ensure a high brilliant X-ray spot at the sample position. The spot size is typically 150µm x 80µm (h x v) as exemplified for ISISS in Fig. 4.

More information about the high pressure XPS apparatus can be found here.

The AP-XPS spectrometers are operated inside dedicated laboratories. Fig. 5a and 5b show the ISISS lab. The installation of an elaborated ventilation and safety system makes it feasible to use hazardous substances (e.g. flammable, explosive, or poisonous) as feed gas. At ISISS you can find a preparation lab on site, too (Fig. 5c). This allows basic sample pre-treatments like washing, drying and pelletising.


Fig. 4: Typical X-ray focus size at ISISS
   
Fig. 5a: ISISS hutch at BESSY Fig. 5b: HP-XPS inside hutch Fig. 5c: Preparation lab
While the ISISS and BElChem facilities are located inside the BESSY experiment hall, the CAT laboratory is part of a newly constructed laboratory and office building outside of but directly connected to the experiment hall of BESSY (Fig. 6). CAT offers about 150m2 of lab space and a sophisticated infrastructure that is required for in situ experiments with a chemical background like for instance gas supply and management, lab and local ventilation systems, exhaust lines, gas sensors, safety cabinets, and a glove box for air sensitive materials.


Figure 6: The EMIL building is an annex to the BESSY II experiment hall.
The BElChem beamline is under friendly user operation but not inside a hutch. It is planned to establish a dedicated BElChem laboratory similar to ISISS and CAT@EMIL during the summer shut-down at BESSY in 2020. The optical layout of the existing beamline will be upgraded to give an even better match to the planned scientific projects in a 2nd phase. A sketch of the planned lab can be found as Fig. 7. An additional tender X-ray beamline will be constructed within the framework of the BElChem project by HZB/MPG.
 
Figure 7: Sketch of the planned BElChem laboratory adding an additional DCM tender X-ray beamline to the project. The by that time modified ISISS lab is shown as well.
The CAT@EMIL beamline has started friendly user operation at the end of 2019. As example, some results are presented as Fig. 8.
Figure 8: In situ spectra of a Co3O4 catalyst for the 2-propanol oxidation reaction (sample courtesy of the CRC/TRR 247 project in collaboration with the University Duisburg/Essen). (a) Co 2p, (b) O 1s and (c) C 1s regions acquired in a 1:1 mixture of 2-propanol and O2 (0.5 hPa) at room temperature, showing an additional C 1s component just below 287 eV from adsorbed 2-propanol species.
For more information please contact Dr. Axel Knop-Gericke or Dr. Michael Hävecker.
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