HOME > Equipment > BL08W-XAFS

BL08W-XAFS

INFORMATION

Any unauthorized reproduction, copying, or alteration of information on this website is prohibited.
Latest news and schedules for beamline upgrades are available on this page. Please also check it for updates.

Experimental Techniques

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

*Supports both step scan and quick scan, and measurement with high-temperature cell.

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.

Beam Characteristics

  • Energy 2.1-13[keV]
  • Flux 1.8-21x1010[photons/s] (the below figure)
  • Beam size Approx. 100 μm (estimated value)
  • Exposure time 50 seconds or less

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 Equipment

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

Vaccum chamber

Vaccum chamber

  • Measurement method: Partial Fluorescence Yield(PFY) and Total Electron Yield(TEY)
  • Measurement ambience: high vaccum(Approx. 10-6[Pa])
  • Required time for vaccuming: Approx. between 20 and 60 minutes

Plate for setting sample

Plate for setting sample

Transfer vessel(ICF70)

Transfer vessel(ICF70)

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

Ionization chambers and 4-Elements Silicon Drift Detector

Ionization chambers and 4-Elements Silicon Drift Detector

  • Measurement method: Transmission Method(TM) and PFY
  • Measurement ambience: atmosphere
  • Ionization gas: N2, N2+Ar

Conversion Electron Yield(CEY) detector

Conversion Electron Yield(CEY) detector

  • Measurement method: CEY and PFY
  • Measurement ambience: He
  • Measurement sample must be electrically conductive.

High-temperature cell

High-temperature cell

  • Measurement method: TM and PFY
  • Measurement ambience: atmosphere and several gas
  • Maximum Size of sample: 10[mm] diameter and 1[mm] thickness
  • Measument temperature: under 600[degC]
  • Required time for cooling: Approx. 1 hour (600 to 40[degC])

Detector

  • 4-elements silicon drift detector (Techno AP Co., Ltd. XSDD50-04GR).
  • Ionization chambers (Applied Photon Technology Co., Ltd. S-1194B1, S-1196B1)
  • CEY detector (Uses He gas)
    ※Obtaining He cylinders has become difficult in recent years. If the He cylinder becomes empty, this method may no longer be available.

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