PANaytical X’Pert Pro (XRD5)

  • Gary Harrison (Senior Technical Specialist)

Facility/equipment: Equipment

    Equipments Details

    Description

    The PANalytical X’Pert Pro ([XRD5]) has a theta:theta geometry the same as our [Bruker D8 Discover]. As with the Bruker, the x-ray source is a copper sealed tube target producing Cu kα and kβ emission lines from a generator operating at 40 kV and 40 mA. Unlike the Bruker there is no primary optic and the detector does not utilise a graphite monochromator for normal use (one is available for fluorescent samples Cr, Mn, Fe, Co, etc). A nickel foil is used to crucially remove the Cu kβ radiation. The state of the art X’Celerator detector system of the X’Pert Pro allows for data collections to be completed at significantly greater speeds/shorter times.
    This is a versatile machine that is used for phase identification, crystallite size and quantitative analysis for bulk materials. Scan range of 0.75°- 143°. A beam knife is available for low angle work.

    XRD5 - PANaytical X’Pert Pro - exterior XRD5 - PANaytical X’Pert Pro - 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

    For back loading powder: A volume of 482 mm3 of powder (the physical amount by weight will clearly depend on the material under investigation).

    For monolith: Maximum size equals 44 mm diameter by ideally 5 mm deep [no greater than 6 mm] (samples can be any shape that can be centred and fits within this footprint - flat surfaces will give better results).
    Attachments

    5, 10, and 20 mm mask
    Beam knife
    Diffracted beam monochromator
    Sample spinner
    3x15 sample auto changer carousel
    Silicon zero/low background holders
    Static sample mount

    Example - Setups

    Bulk Sample: Powder X-ray diffraction was undertaken using a Philips X’Pert – PRO theta-theta PW3050/60 diffractometer (480 mm diameter) with PW3064 sample spinner and X’Celerator (2.122° 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 0.04 rad, 2° fixed anti scatter slit, incident beam mask of 10 mm and programmable automated divergence slit giving a constant illuminated length of 10.0 mm and receiving Soller slit of 0.04 rad were used.

    Data collections from 35 to 145° coupled 2theta/theta at 0.02° step 2 s/step was undertaken.

    With diffracted beam monochromator: Powder X-ray diffraction was undertaken using a Philips X’Pert – PRO theta-theta PW3050/60 diffractometer (480 mm diameter) with PW3064 sample spinner and diffracted beam graphite monochromator (symmetric (002)) with a X’Celerator (2.122° 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 0.04 rad, 2° fixed anti scatter slit, incident beam mask of 5 mm and programmable automated divergence slit giving a constant illuminated length of 5.0 mm were used.

    Data collections from 35 to 146° coupled 2theta/theta at 0.033° step 530 s/step was undertaken.

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