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The Gene and Linda Voiland School of Chemical Engineering and Bioengineering

In Situ Reactive Surface Analysis Center

This analytical center within the Gene and Linda Voiland School of Chemical Engineering and Bioengineering is one of the world’s foremost collection of chemical reactive surface analysis under <em>in situ</em> and operando conditions. The Center currently includes equipment for Raman spectroscopy, X-ray diffraction, and X-Ray photoelectron spectroscopy under active reaction conditions.

Raman Spectroscopy

Our LabRAM HR microscope system possesses dual path optics to allow fast, simple switching between Raman and FTIR mode at high spectroscopic resolutions. The spectrometer is coupled to a COHERENT Innova 90C FreD ion laser source (244nm / 488 nm) and a Ventus LP 532 laser (532 nm). The LabRAM HR has a true confocal pinhole with user controlled variable aperture, which fully matches the laser spot and provides high spatial resolution with maximum signal throughput. The high resolution mode is ideal for most applications where it is important for the precise characterization of position or shape of the Raman spectral features. It can also operate in a low/medium resolution for more routine analysis. To make this even more applicable to reactive surface chemistry analysis, we’ve installed the Linkam CCR1000 in situ cell enables real time Raman/FTIR monitoring under working conditions up to 1,000 C and 5 bar.

Contact: Dongmin Yun, dongmin.yun@wsu.edu

X-Ray Diffraction (XRD)

  • Rigaku Miniflex 600 – For routine powder diffraction with multi-sample changer/spinner and optical monochromator
  • Rigaku SmartLab – With multiple attachments allowing for all conventional high resolution XRD measurements as well as:
    • In situ measurement of samples under many variable conditions such as: temperatures, pressures, gas mixtures, active reactions, etc… from 0 to 10 bar and ambient temperature to 1200 C.
    • Cross beam optics: parallel beam or Bragg-Brentano measurements
    • Multiple high temperature reaction vessels with mass flow controlled reaction gas input
    • Grazing angle measurements (i.e. thin film)
    • Charge/discharge battery cells
    • Small Angle X-ray Scattering (SAXS)
    • High speed 1-D detector and traditional scintillation detectors
    • Monochromators and other optics

Contact: Billy Schmuck, bschmuck@wsu.edu

Rigaku Miniflex

Rigaku SmartLab

X-Ray Photoelectron Spectroscopy (XPS)

We are anticipating the imminent installation of an operando XPS custom built by Omnivac. It is configured on a radial design with several unique features; the highlights of which are operation under non-vacuum pressures and two high pressure reactors attached to the XPS analysis chamber allowing for fast sample transfer (from 600 C and 10 bar).

At 1 mbar ambient pressure, the XPS has an energy resolution of less than 3 meV (at 2 eV pass energy and 20 eV kinetic energy) for temperatures up to 600 C. Pass energies are 2, 5, 10, 20, 50, 100, and 200 eV with a kinetic energy range from 0.5 eV to 1,500 eV. Sensitivity tradeoffs can be made to operate at even higher reaction pressures. Under vacuum the XPS can operate from -196 C to 1,200 C.

Our XPS system includes a monochromatic focused aluminum X-ray source, a dual anode magnesium and aluminum source, and a high performance non-magnetic ultra violet source for photoelectron spectroscopy (UPS). With these sources and the multitude of instrument configurations, this instrument allows for one of a kind electron spectroscopy for chemical analysis (ESCA).

Contact: Billy Schmuck, bschmuck@wsu.edu