Northwestern logo The Bedzyk Group Argonne National Lab logo

18 kW Rotating Four-Circle Diffractometer

The 18 kW is used for:

  • X-ray diffraction
  • Reciprocal space mapping
  • X-ray reflectivity
  • Scan in 3-D, angular and reciprocal space
  • Pole-figure scan
X-rays from point source on rotating anode go through Divergence Slit, are focused by Graphite (002) ParaFocusing and Sagital Focusing Monochromator, go though K-alpha-1 slit, diffract off sample, and then go through Guard Slit, Filter Box, and Detector Slit into Detector

Schematic of the 18 kW setup

Specifications:

  • 18 kW Ultrex Rigaku Rotating Anode (donated by Abbott Labs in 2006)
    • Cu Anode: Cu Kα1 λ = 1.5406 Å, Cu Kα2 λ = 1.54443 Å
    • Point Source: Normal Focus 0.5mm x 10 mm, 18 kW max power
      • The effective source size should be 0.5-mm high by 1-mm-wide due to 6° take-off angle. But we measure the width to be 0.5 mm wide (see figure).
    • Nominal operating power: 50 kV, 240 mA
    • Huber slits for controlling horizontal and vertical divergence (see figure).
    • Nominal setting: hsdgap = 0.7 mm wide by 14-mm-high
    • Graphite (002) Grade ZYA (< 0.5° mosaic) from Advanced Ceramics Corp.
      • Size: 25 x 25 x 2 mm
      • Para- focusing in the horizontal direction
      • Sagital-focusing in the vertical direction with Rs = 225 mm
      • 2d002 = 6.708 Å, Cu Kα1 qB = 13.28°
      • 1 to 1 focusing, F1 = F2 = F = RS/sin(q) = 980 mm. This is the distance from the source to the mono and from the mono to the sample.
    • Incident beam intensity monitor (NaI detector collecting scattered x-rays from Co coated Kapton foil) I0 = 8900 cps at hsdgap = 0.7mm and vsdgap = 14 mm.
    • Huber incident beam slits for passing Cu Kα1 and blocking Cu Kα2
      • Nominal setting ka2cen = 0,  ka2gap = 0.5 mm-wide by 1-mm high
  • Huber 4-circle diffractometer
    • Motorized Z-sample, zsamp=0 should put pin in COR (Center of Rotation)
    • Huber  1006 X-Y- c-f goniometer
    • Sample holder
    • 2-theta arm:  (Nominal settings)
      •  guard slit ( gshhcen=.64, gshgap=1.1,  gsvcen=1.4, gsvgap=8 )
      • XIA filter box, ( T = 0.24 x 0.01 for STB straight thru beam)
      • detector slit, ( dshhcen=.05, dshgap=1.0,  dsvcen=1.9, dsvgap=12 )
      • Cyberstar NaI X-ray detector ( 0 .3 m sec, 740V, Gain = 8, LL=2.5, UL=6.5)
  • Auxillary equipment:
    • Laser Level on Tripod
    • X-ray Eye
    • Goniometer pin
    • High-power zoom lens camera

The manual of this machine can be downloaded here

«Back to Equipment