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X-Ray Diffraction

X-Ray Diffractometer (Rigaku SmartLab)

Contact: Dmitri Barbash

 

Important Features

       General Description

  • Designed for the structural analysis of bulk solids, powders, liquids, and thin films
  • Can analyze all crystalline forms, such as perfect, textured, polycrystalline, and also disordered and amorphous materials
  • Provides a complete range of structural X-ray measurements, including
    Powder X-ray diffraction – for phase ID and quantitative analysis
    High-resolution X-ray diffraction – for measurement of:
    thin films structure
    preferred orientation (texture analysis, pole figure, in-plane pole figure)
    crystal quality analysis (rocking curve/reciprocal space mapping)
    Grazing incidence X-ray diffraction – for thin films measurements
    X-ray reflectometry – for determination of thin films thickness
     
    SmartLab Guidance™ Software
    User friendly instrument control software selects optimal hardware configurations and provides fully automated optics alignment, sample alignment, slit and scan condition setting, and measurements.
    PDXL Comprehensive Analysis Package with ICDD database
    Automatic data reduction and peak list reporting
    Sonneveld-Visser and polynomial function background elimination.
    Rachinger method Kα2 elimination.
    Automatic and/or manual peak finding.
    • Phase ID and search and match capabilities.
    • Degree of crystallinity determination.
     
  •  X-ray generator:
    Cu anode X-ray tube: 3 kW, Long-Fine Focus; X-ray tube focal spot 0.4 mm x 12.0 mm
    Voltage: 20-60 kV, 1 kV step; Current: 2-60 mA, 1 mA step
    X-ray wavelength: Cu= 1.54 Å 
  • Incident Optics
    Cross Beam Shaping Optics (CBO) with Parabolic Mirror:
    User selectable Parallel Beam and Bragg-Brentano optical configurations for asymmetric and symmetric scanning geometries.
    Parallel Beam Optics
    Incident beam parabolic multilayer x-ray mirror compatible
    with all Parallel Beam optics including Ge channel-cut optics.
    Automated mirror control and alignment.
    CBO Selection Slit: Parallel Beam
    Variable Incident Slit: 0.05 – 7.0 mm, 0.01 mm step
    Height Limiting Slit: 2.0, 5.0, 10.0, and 15 mm
    Bragg-Brentano Optics
    CBO Selection Slit: Bragg-Brentano
    Variable Divergence Slit: 0.05 – 7.0 mm, 0.01 mm step
    Height Limiting Slit: 2.0, 5.0, 10.0 mm
    Soller Slits: 0.5° axial divergence
    Ge (220) 2-Bounce and 4-Bounce Incident Beam Monochromators
    High-resolution channel-cut incident beam monochromators for high-resolution parallel beam measurements
    of the crystal structure of highly perfect epitaxial materials.
  •  Goniometer System
    SmartLab High-Resolution Vertical θ/θ Goniometer
    High-resolution vertical theta-theta goniometer system with open architecture design for horizontal sample mounting and measurement.
    High-precision, vertical theta/theta geometry (horizontal sample)
    Optical encoder controlled
    Fully automated alignment
    Independently controlled theta (source) and theta (detector) axes
    Measuring range: -3 – 160° (2 theta)
    Scanning speed: 0.01°/min - 20°/min (theta)
    Scanning Method: theta(source)/theta (detector), independent or coupled
  • Sample Stages
    High Precision Motor driven Z-Stage for Horizontal Sample Measurement: Z = -10 ~ 1 mm / 0.0005 mm step
    100mm XY Sample Stage: mounts directly on the SmartLab high precision Z-stage with no alignment. XY mapping is possible over entire 100mm sample surface size.
    X,Y: ± 50 mm / 0.0005 mm step
    Sample Size: 200 mm φ (8” φ) diameter maximum
    XY Mapping: 100 mm φ (4” φ) diameter area
    Domed Hot Stage for high temperature analysis of thin samples
    Operating temperature: Room temperature to 1100 °C
    Temperature measurement: Pt−Pt10Rh (type S) thermocouple
    Atmospheres: Vacuum, air, inert gas
    Maximum operating pressure: 0.2 to 0.3 bar above atmospheric pressure
    Total transmission: Cu65% (primary and diffracted beam)
  • In-Plane Diffraction Attachment 
    The in-plane diffraction attachment provides an additional detector scanning axis orthogonal to the theta/2-theta diffraction plane. Allows measurement of in-plane structure factors from epitaxial films, in-plane reciprocal space maps from ultra thin (a few nm) films, and full pole figures
    Rx,Ry Direct Connect Tilt Stage: Two-axis tilt stage for in-plane alignment
    Rх Tilt Rotation: -5.0 – 5.0°, 0.002° step
    Ry Tilt Rotation: -5.0 – 5.0°, 0.002° step
    Phi Attachment for In-plane Sample Rotation
    In-plane sample rotation axis for in-plane alignment and in-plane texture analysis.
    Phi rotation: 360° free rotation, 0.002° step
    Step or continuous rotation of sample.
  • Diffracted Beam Optics
    Diffracted Beam Optics Assembly
    Modular beam path suitable for a wide range of diffracted beam optical configurations including parallel slit analyzers and Ge analyzer crystals, and dual receiving slits.
    Receiving Slit 1: Computer-Controlled, 0.05 mm - 20 mm, 0.01 mm step
    Parallel Slit Analyzer: 0.5° Angular Divergence
    Receiving Slit 2: Computer-Controlled, 0.05 mm - 20 mm, 0.01 mm step
    Kβ Filter: Nickel for Cu Radiation
    Attenuator: Computer-Controlled, Four attenuators included with different absorption rates
    Curved & Flat Diffracted Beam Monochromator
    Graphite crystal monochromator with unique design, allows use with either Bragg-Brentano or Parallel Beam optics. A simple 90° rotation of the crystal changes the surface from curved (Bragg-Brentano) to flat (Parallel Beam), or vice-versa, without realignment and without removing the monochromator from the system. This monochromator provides discrimination of CuKβ,W-L radiation, and fluorescent X-rays.
  • Detector
    High-efficiency scintillation counter and measuring electronics provide 700,000 cps or better linearity; Computer controlled pulse-height analyzer (PHA) and detector high-voltage settings; Computer-Controlled and Automated Dead time correction.
  
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