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Our new Rigaku SmartLab XRD
Source
• Standard Copper anode sealed tube source
with Tungsten filament.
• Maximum power of 3 kW. Typically run at
1.76 kW (44 kV, 40 mA) to maximize life of
anode.
• Primary beam is 0.4 mm (vertical) x 12 mm
(horizontal)
Bragg-Brentano (BB) vs. Parallel Beam (PB)
selection slits
• BB simply allows the beam to diverge
• PB uses a multilayer mirror to produce a (vertically) parallel
beam. Still some slight divergence (~0.01°)
• Usually about 5° divergence horizontally (determined by soller
slits)
Soller and Length Limiting Slits
• Soller slits are boxes with many
metal sheets parallel to plane of
diffraction. They limit horizontal
beam divergence (typically 5°)
and the resulting low-θ
contribution to peaks.
• Length-limiting slits simply
reduce horizontal footprint of
beam on sample. Rule of
thumb: double length of slit to
get approx. beam width at
sample (with 5° divergence).
http://www.google.com/patents/EP0999555A1?cl=en
“PSA” and “PSC”
• = parallel slit analyzer (PSA) and parallel slit
collimator (PSC). C=incident side, A=receiving.
• Same construction as a soller slit, but foils are
oriented perpendicular to plane of diffraction.
• In contrast to soller slits, these actually
determine resolution of measurement. (Two
options are 0.5° and 0.114°)
• Finite width of foils reduces intensity.
Receiving and Incident Slits
• One incident slit and two receiving slits are computer controlled.
• The two receiving slits should be as narrow as possible (0.03 mm
min) to achieve maximum resolution.
• Very large reduction in intensity requires long counting times if
looking at Bragg reflections.
• Narrow slits ideal if measuring reflectivity or total external
reflection.
• In contrast to using PSA to limit resolution, slits can introduce a
peak shift if sample height is inaccurately determined.
http://www.stanford.edu/group/glam/xlab/MatSci162_172/LectureNotes/06_Geometry,%20Detectors.pdf
Monochromators/Filters
• A Ge monochromator (220 orientation, 2 bounce)
is optional on incident beam side. This selects
out only Kα1 radiation but at the expense of
intensity. Typically just used for single
crystals/thin films.
• Graphite monochromator optional on receiving
side. Will eliminate Kβ but not Kα2 radiation.
• Kβ filter is a simple Nickel plate on receiving side.
Nickel has a band edge between Kα and Kβ
energies. Reduces intensity ~ 30%.
Detector
• NaI scintillation point detector.
• Linear to about 500,000 cps. Automatic and
manual attenuation options.
From http://www4.nau.edu/microanalysis/Microprobe/WDS-Scintillation.html
Sample Alignment
• Software has preset and adjustable algorithms
for sample alignment.
• Typical alignment: Adjust height (Z) to achieve
direct beam half intensity, adjust
source/detector axis (ω) to maximize intensity
at optimal Z. Finally, adjust Z again when
measuring a small-angle reflection (~0.5°) to
achieve max intensity.
Sample Stages
• 3 stages available.
• Standard stage: Flat,
required to mount a
special slit used for aligning
optics. Also adequate for
basic powder diffraction.
• Euler Cradle: Allows
adjustment of χ and φ 
• Anton Paar: LN2
temperature control from
~85K to 450° C. No
adjustment of χ and φ
(Courtesy JIMgraphics)

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SmartLab.pdf

  • 1. Our new Rigaku SmartLab XRD
  • 2. Source • Standard Copper anode sealed tube source with Tungsten filament. • Maximum power of 3 kW. Typically run at 1.76 kW (44 kV, 40 mA) to maximize life of anode. • Primary beam is 0.4 mm (vertical) x 12 mm (horizontal)
  • 3. Bragg-Brentano (BB) vs. Parallel Beam (PB) selection slits • BB simply allows the beam to diverge • PB uses a multilayer mirror to produce a (vertically) parallel beam. Still some slight divergence (~0.01°) • Usually about 5° divergence horizontally (determined by soller slits)
  • 4. Soller and Length Limiting Slits • Soller slits are boxes with many metal sheets parallel to plane of diffraction. They limit horizontal beam divergence (typically 5°) and the resulting low-θ contribution to peaks. • Length-limiting slits simply reduce horizontal footprint of beam on sample. Rule of thumb: double length of slit to get approx. beam width at sample (with 5° divergence). http://www.google.com/patents/EP0999555A1?cl=en
  • 5. “PSA” and “PSC” • = parallel slit analyzer (PSA) and parallel slit collimator (PSC). C=incident side, A=receiving. • Same construction as a soller slit, but foils are oriented perpendicular to plane of diffraction. • In contrast to soller slits, these actually determine resolution of measurement. (Two options are 0.5° and 0.114°) • Finite width of foils reduces intensity.
  • 6. Receiving and Incident Slits • One incident slit and two receiving slits are computer controlled. • The two receiving slits should be as narrow as possible (0.03 mm min) to achieve maximum resolution. • Very large reduction in intensity requires long counting times if looking at Bragg reflections. • Narrow slits ideal if measuring reflectivity or total external reflection. • In contrast to using PSA to limit resolution, slits can introduce a peak shift if sample height is inaccurately determined. http://www.stanford.edu/group/glam/xlab/MatSci162_172/LectureNotes/06_Geometry,%20Detectors.pdf
  • 7. Monochromators/Filters • A Ge monochromator (220 orientation, 2 bounce) is optional on incident beam side. This selects out only Kα1 radiation but at the expense of intensity. Typically just used for single crystals/thin films. • Graphite monochromator optional on receiving side. Will eliminate Kβ but not Kα2 radiation. • Kβ filter is a simple Nickel plate on receiving side. Nickel has a band edge between Kα and Kβ energies. Reduces intensity ~ 30%.
  • 8. Detector • NaI scintillation point detector. • Linear to about 500,000 cps. Automatic and manual attenuation options. From http://www4.nau.edu/microanalysis/Microprobe/WDS-Scintillation.html
  • 9. Sample Alignment • Software has preset and adjustable algorithms for sample alignment. • Typical alignment: Adjust height (Z) to achieve direct beam half intensity, adjust source/detector axis (ω) to maximize intensity at optimal Z. Finally, adjust Z again when measuring a small-angle reflection (~0.5°) to achieve max intensity.
  • 10. Sample Stages • 3 stages available. • Standard stage: Flat, required to mount a special slit used for aligning optics. Also adequate for basic powder diffraction. • Euler Cradle: Allows adjustment of χ and φ  • Anton Paar: LN2 temperature control from ~85K to 450° C. No adjustment of χ and φ (Courtesy JIMgraphics)