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BL08W-XAFS

INFORMATION

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Experimental Techniques

  • Tender X-ray XAFS
  • Hard X-ray XAFS

*Supports both step scan and quick scan

Overview

This beamline utilizes a double-crystal monochromator to perform XAFS measurements in the tender to hard X-ray energy range. For hard X-ray measurements, in-situ measurements are possible using a sample environment.

Usable gases are limited to harmless gases such as N2 and CO2.
Additionally, please be aware that advanced measurements may require time for instrument setup and alignment, which is included in the user's allocated beamtime.

Beam Characteristics

  • Energy 2.1-13keV
  • Flux 5.6-49x1011 cps (calculated value)
  • Beam size Approx. 100 μm (estimated value)

Hutch size

Approx. 12.5 m (optical axis direction) x 4 m (width) x 4 m (height)

Light Source and Optics

This beamline utilizes a 5-pole multipole wiggler as its light source and employs a liquid nitrogen-cooled silicon double-crystal monochromator, providing monochromatic X-rays in the tender-to-hard X-ray energy range.
Focusing is achieved with a bent cylindrical mirror, and a double-mirror system for higher harmonic rejection is also installed within the experimental hutch.

Experimental Station

Experimental Equipment

"Tender X-ray XAFS Measurement System" (For use below approximately 4 keV)

  • Total Electron Yield (TEY) and Partial Fluorescence Yield (PFY) can be measured simultaneously (TEY requires the sample to be conductive. Please consider techniques such as metal deposition).
  • Measurements are performed under vacuum (He gas not allowed).

"Hard X-ray XAFS Measurement System" (For use above approximately 4 keV)

  • Measurements are performed in air.
  • Samples are typically mounted on slide mounts, but the sample geometry is not restricted.

Detector

  • For tender X-ray fluorescence measurements: 4-element silicon drift detector (Techno AP Co., Ltd. XSDD50-04GR).
  • Various ion chambers for hard X-rays (Applied Photon Technology Co., Ltd.)
  • For hard X-ray fluorescence measurements: 4-element silicon drift detector (Techno AP Co., Ltd. XSDD50-04GR)
  • Conversion Electron Yield (CEY) detector (Uses He gas; we have one He cylinder for this fiscal year. Obtaining He cylinders has become difficult in recent years. If the He cylinder becomes empty, this method may no longer be available. Additionally, the conversion electron yield method requires the sample to be conductive. Please consider techniques such as metal deposition for insulator materials.)

Layout

BL08W-XAFS Layout

XAFS Measurement using transmission method

ZnO EXAFS

Figure: Zn EXAFS spectrum measured by transmission method

  • Measurement sampleZnO pellet
  • Measurement elementZn K-edge
  • Measurement methodtransmission method
  • Measurement ambienceatmosphere
  • Exposure time0.1sec
  • Measurement range~k15
  • Measurement timeabout 710sec
Cu foil EXAFS

Figure: Cu EXAFS spectrum measured by transmission method(quick scanning)

  • Measurement sampleCopper foil
  • Measurement elementCu K-edge
  • Measurement methodtransmission method(Quick Scanning)
  • Measurement ambienceatmosphere
  • Exposure time0.012sec
  • Measurement range~k15
  • Measurement timeabout 75sec
MnO2 EXAFS

Figure: MnO2 EXAFS spectrum measured by transmission method

  • Measurement sampleMnO2 pellet
  • Measurement elementMn K-edge
  • Measurement methodtransmission method
  • Measurement ambienceatmosphere
  • Exposure time0.1sec
  • Measurement range~k16
  • Measurement timeabout 950sec
TiO2 EXAFS

Figure: TiO2 EXAFS spectrum measured by transmission method

  • Measurement sampleTiO2 pellet
  • Measurement elementTi K-edge
  • Measurement methodtransmission method
  • Measurement ambienceatmosphere
  • Exposure time0.1sec
  • Measurement range~k16
  • Measurement timeabout 950sec

XAFS Measurement using Partial Fluorescence Yield(PFY) method

Ag XANES

Figure: Ag XANES spectrum measured by PFY method

  • Measurement sampleAgO powder
  • Measurement elementAg L3-edge
  • Measurement methodPFY method
  • Measurement ambiencevaccum
  • Exposure time1sec
  • Measurement range~k6
  • Measurement timeabout 850sec
S XANES

Figure: S XANES spectrum measured by PFY method

  • Measurement sampleK2SO4 powder
  • Measurement elementS K-edge
  • Measurement methodPFY method
  • Measurement ambiencevaccum
  • Exposure time1sec
  • Measurement range~k6
  • Measurement timeabout 850sec
P XANES

Figure: P XANES spectrum measured by PFY method

  • Measurement sampleFePO4 powder
  • Measurement elementP K-edge
  • Measurement methodPFY method
  • Measurement ambiencevaccum
  • Exposure time1sec
  • Measurement range~k6
  • Measurement timeabout 850sec

XAFS Measurement using Conversion Electron Yield (CEY)

Mn steel XANES

Figure: Mn XANES spectrum in steel measured by CEY method

  • Measurement samplesteel
  • Measurement elementMn K-edge
  • Measurement methodCEY method
  • Measurement ambienceherium
  • Exposure time1sec
  • Measurement range~k6
  • Measurement timeabout 680sec
Cu foil XANES

Figure: Cu XANES spectrum of copper foil measured by CEY method

  • Measurement samplecopper foil
  • Measurement elementCu K-edge
  • Measurement methodCEY method
  • Measurement ambienceherium
  • Exposure time1sec
  • Measurement range~k6
  • Measurement timeabout 680sec

Amount of measurement time

Measurement time calculation formula

(number of pre-edge steps + XANES steps + EXAFS steps(steps*(k-number after XANES)))
* (exposure time + diffraction crystal moving time(over 1sec, defind by X-ray energy))

Measurement time calculation example

  • exposure time : 0.1 sec
  • diffraction crystal moving time : 1.0 sec
  • wave number : K16
  • XANES(~K4) steps : 250
  • other steps : 30

Measurement time = ( 30 + 250 + 30 * ( K16 - K4 )) * ( 0.1 + 1.0) ⇒ about 704 sec

Sample Preparation Example

Powder

Fig: Powder

For transmission, PFY, TEY, CEY method

Pellet

Fig: Pellet

For transmission method

Liquid

Fig: Liquid

For transmission, PFY method

Large sample

Fig: Large sample

For PFY, TEY, CEY method