One of the main goals in catalysis is the characterization of solid/gas interfaces in a reaction environment. The electronic structure and chemical composition of surfaces become heavily influenced by the surrounding environment. However, the lack of surface sensitive techniques that are able to monitor these modifications under high pressure conditions hinders the understanding of such processes. This limitation is known throughout the community as the “pressure gap.” We have developed a novel experimental setup that provides chemical information on a molecular level under atmospheric pressure and in presence of reactive gases and at elevated temperatures. This approach is based on separating the vacuum environment from the high-pressure environment by a silicon nitride grid—that contains an array of micrometer-sized holes—coated with a bilayer of graphene. Using this configuration, we have investigated the local electronic structure of catalysts by means of photoelectron spectroscopy and in presence of gases at 1 atm. The reaction products were monitored online by mass spectrometry and gas chromatography. The successful operation of this setup was demonstrated with three different examples: the oxidation/reduction reaction of iridium (noble metal) and copper (transition metal) nanoparticles and with the hydrogenation of propyne on Pd black catalyst (powder).
Skip Nav Destination
Article navigation
Research Article|
May 25 2016
Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap
J. J. Velasco-Vélez;
J. J. Velasco-Vélez
a)
1Department of Heterogeneous Reactions,
Max Planck Institute for Chemical Energy Conversion
, Mülheim an der Ruhr 45470, Germany
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
V. Pfeifer;
V. Pfeifer
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
M. Hävecker;
M. Hävecker
a)
1Department of Heterogeneous Reactions,
Max Planck Institute for Chemical Energy Conversion
, Mülheim an der Ruhr 45470, Germany
Search for other works by this author on:
R. Wang;
R. Wang
3Engineering Department,
University of Cambridge
, Cambridge CB3 0FA, United Kingdom
Search for other works by this author on:
A. Centeno;
A. Centeno
4
Graphenea
, San Sebastian 20018, Spain
Search for other works by this author on:
A. Zurutuza;
A. Zurutuza
4
Graphenea
, San Sebastian 20018, Spain
Search for other works by this author on:
G. Algara-Siller;
G. Algara-Siller
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
E. Stotz;
E. Stotz
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
K. Skorupska;
K. Skorupska
1Department of Heterogeneous Reactions,
Max Planck Institute for Chemical Energy Conversion
, Mülheim an der Ruhr 45470, Germany
Search for other works by this author on:
D. Teschner;
D. Teschner
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
P. Kube;
P. Kube
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
P. Braeuninger-Weimer;
P. Braeuninger-Weimer
3Engineering Department,
University of Cambridge
, Cambridge CB3 0FA, United Kingdom
Search for other works by this author on:
S. Hofmann;
S. Hofmann
3Engineering Department,
University of Cambridge
, Cambridge CB3 0FA, United Kingdom
Search for other works by this author on:
R. Schlögl;
R. Schlögl
1Department of Heterogeneous Reactions,
Max Planck Institute for Chemical Energy Conversion
, Mülheim an der Ruhr 45470, Germany
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
A. Knop-Gericke
A. Knop-Gericke
2Department of Inorganic Chemistry,
Fritz-Haber-Institut der Max-Planck-Gesellschaft
, Berlin 14195, Germany
Search for other works by this author on:
a)
Authors to whom correspondence should be addressed. Electronic addresses: velasco@fhi-berlin.mpg.de and mh@fhi-berlin.mpg.de
Rev. Sci. Instrum. 87, 053121 (2016)
Article history
Received:
February 01 2016
Accepted:
May 09 2016
Citation
J. J. Velasco-Vélez, V. Pfeifer, M. Hävecker, R. Wang, A. Centeno, A. Zurutuza, G. Algara-Siller, E. Stotz, K. Skorupska, D. Teschner, P. Kube, P. Braeuninger-Weimer, S. Hofmann, R. Schlögl, A. Knop-Gericke; Atmospheric pressure X-ray photoelectron spectroscopy apparatus: Bridging the pressure gap. Rev. Sci. Instrum. 1 May 2016; 87 (5): 053121. https://doi.org/10.1063/1.4951724
Download citation file:
Sign in
Don't already have an account? Register
Sign In
You could not be signed in. Please check your credentials and make sure you have an active account and try again.
Sign in via your Institution
Sign in via your InstitutionPay-Per-View Access
$40.00