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BL02B2 Automatic In-situ Powder Diffractometer

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INS-0000001637

 The diffractometer with a multi modular system constructed by six MYTHEN detector is installed at the BL02B2 experimental hutch (Table 1 & Fig. 1). The time resolution is limited to 10 msec. The multi modular system usually takes powder diffraction data at different two 2θ positions because of interval between every detectors (two-step mode, Fig.2: left). In the case of observation of non-ambient experiment, it is useful to fix 2θ position of the multi modular system (single-step mode, Fig.2: right).

 A two-dimensional detector (XRD3025) is also installed. The detector can collect wide inverted space diffraction patterns in exceptionally short time periods. The detector is located on the lower side of the powder diffractometer (Fig.3), and it is possible to use the 1-dimensional micro-strip MYTHEN detectors and two-dimensional detectors for powder sample crystalline evaluation simultaneously. In addition, it is equipped with an electric XYZ stage, and the FPD can be moved according to the experimental conditions, in which a wide variety of non-ambient conditions can be used for powder diffraction experiments.

 The sample temperature can be controlled in a wide range of temperature (30 ∼ 1100 K). The high and low temperature nitrogen gas flow systems are installed for high-temperature (300 ∼ 1100 K) and low-temperature (90 ∼ 300 K) experiments (Fig.3). It is possible to carry out the automated data collection in dependence of temperature controlled by LabVIEWTM software. Under 90 K, temperature must be controlled by a helium gas flow temperature device. The combination of the MYTHEN detector system and the sample changer makes it possible to measure up to 50 samples automatically. The lowest (highest) measurement temperature is 5 K (1473 K) when using the low-temperature cryostat (furnace) option. The diffractometer also has an imaging plat detector (large Debye-Scherrer camera).

 By taking advantage of third-generation high-energy synchrotron radiation, the automatic in-situ powder diffractometer enables one a rapid and easy collection of high angular resolution powder data even for heavy materials. As a result, the beamline has flexibility for many levels of structural studies, for example, from measuring just lattice constants to obtaining accurate electron densities under extreme conditions.

    Table 1. Specifications of diffractometer.

    Automatic In-situ Powder Diffractometer
    MYTHEN 1 K detector Size (width × length × thickness): 64×8×1 mm3, 6 modules
      Camera radius: 477.46 mm
      2θcoverrage 1 - 75°, 0.006°/step (two-step mode)
        1 - 35°, 0.006°/step (single-step mode)
    Collimator size 0.1 (V) × 0.1 (H) mm2 ∼ 0.7 (V) × 3.0 (H) mm2

Fig1. Transmission-geometry powder diffractometer installed at the experimental hutch.

Fig1. Transmission-geometry powder diffractometer installed at the experimental hutch.

Fig 2. Measurement system for MYTHEN detector.

Fig 2. Measurement system for MYTHEN detector.

Fig 3. Temperature changing accessories.

Fig 3. Temperature changing accessories.

Last modified 2022-05-16 14:36
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