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X-ray laboratory


X-ray Diffraction (XRD)

X-Ray Laboratory of the NanoBioMedical Centre has two modern and stand-alone X-ray diffractometers, EMPYREAN and X'Pert PRO MRD (PANalytical).
The availability of state-of-the-art research equipment and qualified staff ensure the highest level of scientific research. Professional research equipment allows for carrying out the didactic activities and ensures its high level.

EMPYREAN X-ray diffractometer (PANalytical) with equipment



This powder diffractometer is working in Bragg-Brentano geometry and has standard equipment of Cu tube working at linear/dot source, reflection-transmission spinner (plus automatic sample changer), and a fast PIXcel 3D linear detector, working in four modes.
Additionally, EMPYREAN has accessories: Co and Ag tubes, solid sample stage, temperature stage TTK 450, computed tomography stage, capillary spinner, scintillation detector and two self-contained cooling systems: i) OxfordCryosystems (Cryostream 700 Series, Plus), ii) Anton Paar (TCU 110), working in the range from -193 °C to + 227 °C and from -193 °C to + 450 °C, respectively.
 
The wide range of configuration combined with ‘PreFIX’ system (pre-aligned fast interchangeable X-ray modules) allow us to perform various types of measurements, such as:
- quantitative and qualitative phase analysis (based on the latest ICDD PDF4+ database),
- phase analysis in wide range of temperature (solid/liquid - using capillaries),
- analysis of the distribution of distance between pairs of particles contained in a given volume - PDF (Pair Distribution Function),
- measurement of average size and distribution of pore size/grains using SAXS method (Small Angle X-ray Scattering),
- computed tomography (CT);

X'Pert PRO MRD X-ray diffractometer (PANalytical) with equipment:



X'Pert PRO MRD with goniometer of five degrees of freedom: X-Y-Z-Phi-Chi is dedicated mainly for thin layer analysis. Standard equipment includes Cu tube, working at linear/dot source, magnetic stage, two proportional detectors Xe, crossed slits (controlling the beam height and width between 0 mm and 10 mm).
Additionally X'Pert PRO MRD has following accessories: parabolic mirror MRD, programmable beam attenuator Ni 0.125 mm, 4-crystal symmetrical monochromator Cu Ge(200), parallel plate collimator, programmable receiving slit with FASS, triple axis (Monochromator 3xGe200 Cu Sym. double, Rocking curve optics double).
 
Area of research:
- reflectivity measurement,
- rocking curve measurement,
- reciprocal space mapping,
- phase analysis at low incident angle,
- pole figure measurement,
- stress analysis.

Sample results



Spectral X-ray powder diffraction pattern for pharmacologically active substance from the L-type vasodilatation antagonists group nifedipine with structural identification based on the ICDD PDF4 +


SAXS diffractogram for ink-bottle silicone pores; Confirmation of crystalline structure type F4132

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