Philips X'pert Modular Powder Diffractometer (XRD2)

  • Gary Harrison (Academic lead)

Facility/equipment: Equipment

    Equipments Details

    Description

    [XRD2] the modular powder diffractometer (MPD) from Philips (now [PANaytical]) is a stable robust XRD platform consistently operating 24 hours 7 days a week in both bulk and glancing incidence (GI) diffraction modes. A versatile machine that is used for phase identification, crystallite size and quantitative analysis for bulk and thin layer materials.

    Using a long fine focus copper anode x-ray source, it incorporates the options for Bragg Brentano operation (theta /2 theta) for large bulk samples covering up to a maximum size of 100 mm dia. x 100 mm height and weighing up to 1 kg and glancing incidence geometry for samples with thin coatings of just a few microns thickness. The theta:2theta mode has automatic slits on both the primary and secondary sides and a scan range of 0.75°- 143° 2θ.

    In glancing incidence mode long soller slits and a graphite monochromator are utilised mitigating x-ray fluorescence from samples Cr, Mn, Fe, Co, etc and to ensure the best possible resolution is achieved using this type of configuration.

    Combined with our in-house sample changer and control software this system can also be programmed to collect 6 samples in series in either bulk or GI modes.

    XRD2 - Philips X'pert MPD - exterior XRD2 - Philips X'pert MPD - interior
    Access

    This machine is open access to registered users via the sample submission queue or trained users via the XRD portal.
    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).
    Samples Size and Type

    Powder: A volume of 600 mm3 of powder (the physical amount by weight will clearly depend on the material under investigation) is required for the cartridge clip quick change holders.

    All other samples can be accommodated by the MPSS configuration and our in-house sample holders.
    Attachments

    2, 5, 10, and 20 mm mask
    Miniprop. small window point detector
    Proportional point detector
    MPSS - static sample mount
    Parallel plate collimator 0.27°
    Diffracted beam curved graphite monochromator (002)
    6 position sample auto changer carousel
    Silicon zero/low background holders
    Cartridge clip quick change static sample mount

    Example - Setups

    Bulk: Powder X-ray diffraction was undertaken using a Philips X’Pert – MPD theta-theta diffractometer (400 mm diameter) with a PW3011/10 (Miniprop. small window) point 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) incident beam Soller slit of 0.04 rad, incident beam mask 10 mm, programmable automated divergence slit giving a constant illuminated length of 10.0 mm, programmable anti-scatter slit observed length of 10.0 mm, receiving Soller slit of 0.04 rad and programmable receiving slit 0.20 mm. Data collections from 35 to 145° coupled 2theta/theta at 0.02° step 2 s/step was undertaken.

    Thin Film: Grazing Incidence powder X-ray diffraction was undertaken using a Philips X’Pert – MPD theta-theta diffractometer (400 mm diameter) with a PW1711 (Proportional) point 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). Incident beam Soller slit of 0.04 rad, incident beam mask 10 mm, programmable automated divergence slit giving a constant illuminated length of 10.0 mm, programmable anti-scatter slit observed length of 10.0 mm, receiving Soller slit of 0.04 rad, Parallel plate collimator 0.27° and diffracted beam curved graphite monochromator (002). Data collections from 10 to 85° 2theta scan with an incidence angle in Omega of 3° at 0.05° step size and 7 s/step was undertaken.

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