Proto AXRD

  • Gary Harrison (Academic lead)

Facility/equipment: Equipment

    Equipments Details

    Description

    The Proto AXRD is the newest addition to the Department of Materials XRD Laboratory. Although the priority usage for this 600 W tiny bench top diffractometer is teaching, specifically undergraduate and MSc practical classes, it packs a mighty punch with a small footprint allowing it to be used to collect high, Rietveld, quality diffraction patterns.

    The diffractometer can undertake three different scan types:

    Coupled Scan: Bragg-Brentano θ/2θ Scans (Rotating Sample, Rotating Detector)
    Decoupled Scan: Glancing Incidence Diffraction (GID) (Fixed sample, Rotating Detector)
    Decoupled Scan: Rocking curves and Stress Analysis (Rotating sample, Fixed Detector)

    Wavelengths
    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).

    Samples Size and TypeFor powder: A volume of 66 or 266 mm3 of powder (the physical amount by weight will clearly depend on the material under investigation) can be loaded into the double-sided sample holders. Glass slides, quartz or silicon zero/reduce background holders are also available for supporting smaller quantities of powder - these may require the use of an adhesive such as Vaseline grease.

    For monolith: Maximum size equals 40 mm diameter by ideally 15 mm deep (35 by 10 mm when using the aluminium holder). Samples can be any shape that can be centred and fits within this footprint - flat surfaces will give better results.

    Attachments
    Dectris Mythen 1K (1280 channels) 0.1, 0.2, 0.5, 1.0, 2.0 mm source slits
    4 x double-sided sample holders (13 and 26 mm diameter cavity; 0.5 mm depth)
    2 x deep sample cups (35 mm diameter; 10.25 mm depth)
    1 x Quartz low background holder
    LaB6 powder disc - reference and calibration6 x position sample changer

    Parameters
    Radius: 142 mm
    Angular Range: -4 to 150 ° 2θ
    Detector: Dectris Mythen 1K

    Example - Setups
    Bulk Sample: Powder X-ray diffraction was undertaken using a Proto AXRD θ-2θ diffractometer (284 mm diameter) with sample spinner and Dectris Mythen 1K (3.22° active length*) 1D-detector 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 (Kα1=1.540598 Å, Kα2=1.544426 Å, Kα ratio 0.5, Kαav=1.541874 Å). An incident beam Soller slit of 0.4 mm, 0.5* mm fixed divergence slit, and receiving Soller slit of 0.6 mm were used.

    A data collection from 15 to 145° coupled θ/2θ at 0.019935° step with 1* x multiplier at 2 s/step with a fixed detector mode of 320 active channels (0.81° 2θ) was undertaken.

    *Please note these values may change depending upon your experiment. For example the active length of the detector can be set to be static or dynamic based on the collection mode. In dynamic mode the detector active length can change throughout the experiment increasing with 2θ angle. The step multiplier can be changed between 1 and 10.

    Details

    NameProto AXRD
    Acquisition date31/07/18
    ManufacturersProto Manufacturing

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