APPES at ALS

Ambient pressure photoemission spectroscopy (APPES) with synchrotron light at Advanced Light Source (ALS)

1st Generation Instrument (Currently used at the ALS beamline 9.3.2.):

M. Salmeron, D. F. Ogletree, H. Bluhm, F.G. Requejo

2nd Generation Instrument (Currently at ALS beamline 11.0.2 and BESSY beamline U49/2-PGM1)
This is an upgraded version of the original instrument, designed and built by a collaboration between the Lawrence Berkeley National Laboratory, Berkeley, CA, USA, and the Fritz-Haber-Institut der Max-Planck-Gesellschaft, Berlin, Germany  (add link to FHI and BESSY)

Why ambient pressure photoemission spectroscopy?
The use of the original for UHV restricted surface sensitive technique
opens a wide field of new applications like e.g.:

-Study of surface chemistry under thermodynamic equilibrium with various gases  (including water vapor!)

-Study of catalytic reactions in realistic conditions of pressure and temperature

-Study of free liquids

-Study of biological surfaces in humid environments

Problem that have to be solved for HPPES:

-Electrons are scattered by gas molecules

-Analyzer needs UHV

-X-ray source needs UHV

Solutions:
-Capture of electrons in analyzer arm before collision with gas molecules =>gap between sample and analyzer of less than 1 mm

-Modification of electrostatic lens system of analyzer to implement 3 differential pumping sections (Pressure drop between hemisphere and high pressure chamber around 10E8)
=>Electron beam has to be focused through 2 apertures in lens arm

-Light from X-ray source passes window for protection of source (e.g. Al e.g. Al, Si, Be)

The Endstation System at the ALS / LBNL:

The endstation consists of two UHV-chambers for sample preparation/characterization and the actual high pressure measurements.

*Preparation Chamber:
- Heating, LN2 Cooling, Sputtering with Plasma Source, Option for Evaporator with Quartz micro balance
-AES, LEED, Mass spectrometer

*High Pressure Chamber:
-Heating, LN2 Cooling
-XPS or NEXAFS in pressures up to 10 torr (later probably up to 100 torr)
-Surface reaction products detection with Mass spectrometer in lens arm

*Sample holder and Transfer system:
-Thermionic’s STLC System with transferable thermocouple
-Load lock for sample introduction

Sample – Beam – Analyzer – Geometry:

Beam – sample geometry for solids or liquids:

Analyzer angles:

Angle in xy-plane: 45º,  Elevation angle: 35º = (111) direction
=> Magic angle for either horizontal or vertical polarization!

Analyzer modifications:

Commercial Phoibos 150 Analyzer from Specs: 2/3 of lens section replaced
Images show general concept, slight modifications were performed on final lens system.
Analyzer- and lens drawings by Klaus Ihmann from Fritz-Haber-Institut in Berlin

 

High Pressure Photoemission Spectroscopy (HPPES) at ALS

High Pressure Photoemission Spectroscopy at ALS

Guido

Water droplet at the sample stage

 

 

Contact information

Materials Sciences Division
Mail Stop 66R0200 (Office: 66-208)
Lawrence Berkeley National Laboratory
1 Cyclotron Road, Berkeley
California 94720 USA
Phone: +1-510-486-6704
FAX: +1-510-486-7768
Email: mbsalmeron*lbl.gov (replace * by @)
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