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Electron Spectrometer: XPS/AES (Kratos multitechnique)

Quick Specs

  • Capable of XPS, AES, SIMS, and ion scattering spectroscopy analysis
  • DC heating and LN2 cooling
  • Ion sputtering with Ar or He
  • SEM imaging

The Kratos multitechnique surface analysis system is based on the Kratos Axis 165 Electron Spectrometer and is designed to investigate surface composition and surface chemistry, such as oxidation. The system may be applied to a broad range of research areas, including material sciences (electronic thin films, nanosized inorganic materials), catalysis, and corrosion.

The instrument contains electron imaging, electron spectroscopy, and primary and secondary ion scattering capabilities that allow a wide variety of chemical and elemental analyses to be performed. Among the important features of the electron spectrometer portion of this instrument is the self-compensated charge neutralization system, which allows excellent high-resolution data to be collected on polymers and other insulating surfaces, including a wide variety of natural mineral samples.

Connecting the instrument to one or more elements of the EMSL portable experimental stations can facilitate a wide variety of unique experiments. For example, a specimen can be cleaned and analyzed in the multitechnique system, transported to the electrochemical portable test station under ultrahigh vacuum conditions, exposed to solution and electrochemical testing, and then returned to the analysis system. This type of approach can be used to study corrosion, erosion, adsorption, and solution coating phenomena. Thin film deposition, plasma processing, and optical portable experimental stations expand the range of possible experiments; the instrument serves as an especially powerful analytical link to these portable systems.

Performance Specifications

This multitechnique research instrument is built around a hemispherical analyzer included in the Kratos Axis 165 system. This analyzer allows Auger electron spectroscopy (AES), ion scattering spectroscopy, and X-ray photoelectron spectroscopy (XPS) to be performed using electrons, monochromatic and non-monochromatic X-rays, and ions as source or primary particles. An ABB Extrell quadrupole ion detector has been incorporated to allow detection of sputtered ions for secondary ion mass spectroscopy (SIMS).

X-ray Sources Dual anode (magnesium and aluminum) and monochromatic
XPS Data for Ag 3d – Non-monochromatic magnesium anode 15 kV 30 mA
  PASS ENERGY (EV) KILOCOUNTS/S FULL WIDTH HALF MAX (FWHM)
ENERGY RESOLUTION (EV)
Aperture: Slot 5 1,030 0.80
20 6,500 0.838
40 12,500 1.00
80 24,000 1.36
Aperture: 120 μm 5 200 0.79
20 1,160 0.842
40 2,100 0.975
80 3,780 1.37
Aperture: 60 μm 5 48 0.76
20 217 0.84
40 384 0.977
80 616 1.319
Aperture: 30 μm 5 7.2 0.77
20 25.8 0.8
40 50.1 0.9
80 73.5 1.24
XPS Data for Ag 3d - Monochromatic aluminum anode 15 kV 30mA
  PASS ENERGY (EV) KILOCOUNTS/S FWHM ENERGY
RESOLUTION (EV)
Aperture: Slot 5 65 (5 mA-15 mA) 0.45
20 550 (5 mA-15 mA) 0.48
40 1,560 (5 mA-15 mA) 0.56
80 3,145 (5 mA-15 mA) 0.74
Aperture: 120 μm 5 26.1 (15 mA) 0.45
20 58.2 (15 mA) 0.47
40 132 (15 mA) 0.545
80 198 (15 mA) 0.757
Aperture: 60 μm 5 4.35 (30 mA) 0.43
20 8.7 (30 mA) 0.44
40 17.7 (30 mA) 0.54
80 26.7 (30 mA) 0.68
Aperture: 30 μm 5 0.900 (30 mA) 0.43
20 1.75 (30 mA) 0.44
40 3.1 (30 mA) 0.46
80 4.5 (30 mA) 0.64
Electron Beam 100 nm at 12 kV
AES (Cu LMM 10kV 10 nA) Sensitivity 585,000 cps
S/N 500
Ion Sputtering Argon or Helium  
SIMS Positive and Negative Static SIMS and Residual Gas Analyzers  

Additional features and capabilities of the instrument include:

The laboratory is equipped with a variety of ways to cut, polish, and clean specimens prior to analysis or experiment. All work performed with this instrument and in the associated laboratory must be performed in compliance with EMSL practices and permits.

Sample Preparation and Handling

The instrument is equipped for using both the standard Kratos specimen handling and EMSL specimen platens. Kratos offers a standard specimen stub of 1 cm in diameter. Specimens up to 2.5 cm are common. A bar allowing the capacity for three or more stubs is available. A modified bar is used to hold the EMSL platen. Almost any vacuum-compatible specimen that fits within the x-y dimensions of the holder and is less than 0.3-inch thick can be analyzed.

The EMSL sample platen can hold specimens up to 1 inch in diameter, although smaller specimens are preferred. This holder allows interconnection with other parts of the EMSL transfer system. This overall capability allows samples to be prepared and altered in several unique ways that include electrochemical and liquid exposure, plasma treatment, coating deposition, optical exposure, and processing by heating and cooling.

Specimen handling for surface analysis and vacuum work involves several considerations. Users not familiar with these needs and requirements should contact the equipment custodians listed on this page or refer to American Society for Testing and Materials E-1078, Standard Guide for Specimen Preparation and Mounting in Surface Analysis.

Individuals may use this instrument independently following training related to the specific technique and system. However, users are encouraged to work with EMSL staff to develop experimental procedures.

  1. Investigation of the hygroscopic growth of self-assembled layers of N-alkyl-N-methylpyrrolidinium bromides at the interface between air and organic salt .
  2. Radionuclide Sensors for Environmental Monitoring: From Flow Injection Solid-Phase Absorptiometry to Equilibration-Based Preconcentrating Minicolumn Sensors with Radiometric Detection.
  3. Hydrogen-Bond Acidic Polymers for Chemical Vapor Sensing.
  4. Characterization Challenges for Nanomaterials.
  5. NOx uptake on alkaline earth oxides (BaO, MgO, CaO and SrO) supported on ?-Al2O3.
Kim, Do Heui | , 509-371-6489