X-ray powder diffractometer X-ray powder diffractometer
X-ray powder diffractometer radiation counter radiation counter
X-ray powder diffractometer
Powder diffractometer (see Jenkins & Snyder, chap. 7)
Bragg-Brentano geometry
X-ray powder diffractometer
To maintain the focusing geometry, when counter is rotated at rate of 2 /min, specimen is also rotated at rate of /min /min /min
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here, is main rotation axis - asymmetric broadening toward low 2 - negative 2 error up to 90° - positive 2 error beyond 90° Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here, is main rotation axis - asymmetric broadening toward low 2 - negative 2 error up to 90° - positive 2 error beyond 90°
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here, is main rotation axis Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here, is main rotation axis
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here is main rotation axis each section of Soller slit produces its own Debye ring from a specific region in the specimen divergence angle typically ±2.5° Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here is main rotation axis each section of Soller slit produces its own Debye ring from a specific region in the specimen divergence angle typically ±2.5°
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here is main rotation axis each section of Soller slit produces its own Debye ring from a specific region in the specimen divergence angle typically ±2.5° Bragg-Brentano instrument - errors (see Klug & Alexander) Axial divergence - axis, here is main rotation axis each section of Soller slit produces its own Debye ring from a specific region in the specimen divergence angle typically ±2.5°
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Flat specimen peak shifts to lower 2 & asymmetric broadening depends on beam divergence & 2 , plus specimen shape Bragg-Brentano instrument - errors (see Klug & Alexander) Flat specimen peak shifts to lower 2 & asymmetric broadening depends on beam divergence & 2 , plus specimen shape
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Specimen transparency Bragg-Brentano instrument - errors (see Klug & Alexander) Specimen transparency
Powder diffractometer Bragg-Brentano instrument - errors (see Klug & Alexander) Specimen displacement Usually largest error in expt'l data Neg. peak shift - ~0.01° 2 /15 displacement Asymmetric broadening toward lower 2 Bragg-Brentano instrument - errors (see Klug & Alexander) Specimen displacement Usually largest error in expt'l data Neg. peak shift - ~0.01° 2 /15 displacement Asymmetric broadening toward lower 2
Powder diffractometer Bragg-Brentano instrument Divergence slit choice Bragg-Brentano instrument Divergence slit choice
Powder diffractometer Bragg-Brentano instrument Divergence slit choice Or, theta-compensating slit - divergence slit opens as theta increases Bragg-Brentano instrument Divergence slit choice Or, theta-compensating slit - divergence slit opens as theta increases
Powder diffractometer Bragg-Brentano instrument Receiving slit choice Bragg-Brentano instrument Receiving slit choice
Powder diffractometer Bragg-Brentano instrument Receiving slit choice lowers intensity - little improvement in resolution poor resolution - little improvement in intensity Bragg-Brentano instrument Receiving slit choice lowers intensity - little improvement in resolution poor resolution - little improvement in intensity
Powder diffractometer Bragg-Brentano instrument Receiving slit choice correct slit size ~0.15° Bragg-Brentano instrument Receiving slit choice correct slit size ~0.15°
Powder diffractometer Alignment steps
Powder diffractometer Alignment steps Align to focal spot Set take-off angle Alignment steps Align to focal spot Set take-off angle
Powder diffractometer Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment
Powder diffractometer Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment
Powder diffractometer Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment Alignment steps Align to focal spot Set take-off angle Zero alignment 2:1 alignment
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard NIST 640c (Si) Alignment checks Run calibration pattern - use suitable standard NIST 640c (Si)
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard Alignment checks Run calibration pattern - use suitable standard
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard Watch for: Intensity loss Angle shifts Resolution loss Alignment checks Run calibration pattern - use suitable standard Watch for: Intensity loss Angle shifts Resolution loss
Powder diffractometer Alignment checks
Powder diffractometer Alignment check "Five fingers of quartz" Alignment check "Five fingers of quartz"
Powder diffractometer Alignment check "Five fingers of quartz" Measure: position & intensity of (203) 1 H 1 /H 2 Alignment check "Five fingers of quartz" Measure: position & intensity of (203) 1 H 1 /H 2
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard NIST 1976 (Al 2 O 3 ) Alignment checks Run calibration pattern - use suitable standard NIST 1976 (Al 2 O 3 )
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard Alignment checks Run calibration pattern - use suitable standard
Powder diffractometer Alignment checks Run calibration pattern - use suitable standard Alignment checks Run calibration pattern - use suitable standard