Rigaku SmartLab 3 kW

  • Gary Harrison (Technical Specialist)

Facility/equipment: Equipment

    Equipments Details

    Description

    This is one of the newest machine within the x-ray diffraction facility and hosts a range of specialist attachments, detector and capabilities. The Rigaku SmartLab has a theta:theta geometry the same as the Bruker D8 Advance and PANalytical X’Pert Pro [XRD5]. As with the Bruker, the x-ray source is a copper sealed tube target producing Cu kα and kβ emission lines from a generator in this case operating at 40 kV and 30 mA (1.2 kW).

    The SmartLab is a state of the art powder diffractometer capable of undertaking many different kinds of experiments. It has a series of primary optics allowing it to operate like the Bruker D8 Advance with a parallel beam or like the PANalytical X’Pert Pro [XRD5] and utilising a nickel foil to remove the Cu kβ radiation. It is unique in the XRD suite as it also has a Ge(220) double bounce monochromator (primary optic) which is able to strip Cu kα2 emission lines producing just a Cu kα1 x-ray source. This is currently finding significant use in the study of deformation density and line profile analysis.

    The system also hosts three state of the art detectors allowing for data collections to be completed at significantly greater speeds and therefore shorter times than either the Bruker D8 or the theta:2theta systems. One of these detectors the Hypix-3000 is a 2D hybrid semiconductor detector. This allows for the collection of part of the diffraction cone produced during the powder experiment. It is useful as it allows access to diffraction which could be missed with the other systems. Both the Hypix-3000 and D/teX Ultra 250 detectors have XRF suppression by high and low energy discrimination allowing the collection of samples containing fluorescent elements such as Cr, Mn, Fe, Co, etc when using copper radiation.

    Wavelengths
    This machine operates using a Copper Line Focus X-ray tube with Nickel kβ absorber (0.02 mm; Kβ = 1.392250 Å) producing Kα radiation (Kα1 = 1.540598 Å, Kα2 = 1.544426 Å, Kα ratio 0.5, Kαav = 1.541874 Å).

    It also has provision for a Molybdenum Line Focus X-ray tube with Zirconium kβ absorber (0.02 mm; Kβ = 0.63229 Å) producing Kα radiation (Kα1 = 0.70930 Å, Kα2 = 0.71359 Å, Kα ratio 0.5, Kαav = 0.71073 Å).

    Sample Size and Type
    Due to the motorised x,y-stage and the unique Rigaku sample holder technology this machine can accommodate a range of sample shapes and sizes. The limiting factor is weight which should not exceed 2 kg. In order to measure the entirety of the sample surface automatically the sample should not exceed 20 mm2.
    Attachments
    CBO [BB and PB modes] Ge(220)x2 Monochromator
    CBO-f
    0.5, 5, 10, 15, 20 mm ISL/mask
    0.3, 0.2, 0.1 and 0.05 mm collimator sizes
    (0.05 mm collimator can no longer be aligned at the present time is therefore not available)
    Motorised incident slit
    Motorised 20:20-xy mapping sample stage
    Motorised Rx-Ry tilt sample stage
    SCP - point detector
    D/trek Ultra 250 1D-detector [19.4 mm, pixel size = 75 μm] - broken
    Hypix-3000 2D-detector [38.5 mm x 77.5 mm, 385 x 775 pixels, pixel size = 100 μm x 100 μm]
    In-plane arm
    Silicon zero/low background holders
    Powder sample holder 0.2, 0.5 mm deep
    Transmission holder
    Alignment laser
    High resolution alignment video microscope

    Example - Setups

    Please note that if you are not certain which detector was used for your measurement - all data collected in 2019 was on the Hypix since the D\teX developed a significant fault in 2018.

    {Delete/amend appropriately}

    Bulk Sample BB: Powder X-ray diffraction was undertaken using a Rigaku SmartLab 3K diffractometer (300 mm diameter) and Hypix-3000(H) (38.5 mm active length) 2D-detector operating in 1D mode in Bragg-Brentano geometry employing a Copper Line Focus X-ray tube with Ni kβ absorber (0.02 mm; Kβ = 1.392250 Å) Kα radiation from a Rigaku Cross Beam Optic (CBO) (Kα1=1.540598 Å, Kα2=1.544426 Å, Kα ratio 0.5, Kαav=1.541874 Å). An incident beam Soller slit of {5.0°}, incident beam mask of {10 mm} and programmable incidence slit {1.0 mm} and receiving Soller slit of {5.0°} were used.

    Data collection from 35 to 145° coupled theta/2theta at 0.01° step and 1 deg/minute was undertaken.

    Bulk Sample PB:
    Powder X-ray diffraction was undertaken using a Rigaku SmartLab 3K diffractometer (300 mm diameter) and Hypix-3000(H) (38.5 mm active length) 2D-detector operating in 1D mode in theta-omega geometry employing a Copper Line Focus X-ray tube with parallel beam selection from the Rigaku Cross Beam Optic (CBO) giving Kα radiation (Kα1=1.540598 Å, Kα2=1.544426 Å, Kα ratio 0.5, Kαav=1.541874 Å). An incident beam Soller slit of {5.0°}, incident beam mask of {10 mm} and programmable incidence slit {1.0 mm} and receiving Soller slit of {5.0°} were used.

    Data collection from 35 to 145° coupled theta/2theta at 0.01° step and 1 deg/minute was undertaken.

    Deformation Density - CMWP Profile: Powder X-ray diffraction was undertaken using a Rigaku SmartLab 3K diffractometer (300 mm diameter) and Hypix-3000(H) (38.5 mm active length) 2D-detector operating in 1D mode in theta-omega geometry employing a Copper Line Focus X-ray tube with parallel beam selection from the Rigaku Cross Beam Optic (CBO) to the Rigaku Ge(220)x2 optic producing monochromatic Kα1 radiation (Kα1=1.540598 Å). A custom incident double slit holder (GHM) matched to the incident beam mask of {10 mm} and programmable incidence slit {1.0 mm} and receiving Soller slit of {5.0°} were used.

    A minimum of 10 data collections were undertaken over an angular range from 35 to 145° coupled theta/2theta at 0.01° step and 1 deg/minute were undertaken and merged for final data analysis.

    2D - Mesurements: Powder X-ray diffraction was undertaken using a Rigaku SmartLab 3K diffractometer ({300} mm diameter) and Hypix-3000(H) ( mm active area) 2D-detector operating in 1D mode in Bragg-Brentano geometry employing a Copper Line Focus X-ray tube with parallel beam selection from the Rigaku Cross Beam Optic (CBO) to the Focussed Rigaku Cross Beam Optic (CBO-f) producing a point focus beam shape with Kα radiation (Kα1=1.540598 Å, Kα2=1.544426 Å, Kα ratio 0.5, Kαav=1.541874 Å). The beam was collimated using an incident beam collimator {0.1 mm} in diameter.

    Data collection from 15 to 105° coupled theta/2theta at 0.04° step and 15 deg/minute was undertaken with simultaneous oscillation in Phi+/-45° and Chi+/-5°.

    Details

    NameRigaku SmartLab 3 kW
    Acquisition date1/03/15
    ManufacturersRigaku

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