X-Ray Crystallography Laboratory

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X-Ray Crystallography Laboratory

The scope of research works conducted by the laboratory comprises analyses of a solid body interior, including metallic substances, semiconductors, insulators and pulverulent and biological materials.

The laboratory also offers:

  • qualitative and quantitative phase analysis of solid, pulverulent and thin layer samples
  • determining of the crystalline structure of the tested substances in a wide range of temperature
  • following of phase transitions

Facing the customer demand and to confirm the quality of the services rendered, the Crystallography Laboratory works in the system compliant with the international standard PN-EN ISO/IEC 17025:2005.

  • The qualitative phase composition with the X-ray diffraction method for solid polycrystalline samples and in the pulverulent form with the possibility to determine the percentage share of the crystalline and amorphous phase in a sample.
  • The quantitative phase composition with the Rietveld’s method or internal pattern method within the range of 5 – 100%.
  • Determining of the crystalline texture with the X-ray diffraction method.
  • Phase identification and identity confirmation for samples of the pharmaceutical origin – active and auxiliary substances.
  • Measurements and determining of crystalline structures of monocrystalline samples within the temperature range of 80 – 500K.
  • Measurements of thin layers and epitaxial layers – reflection curves from symmetric and asymmetric planes, determining of the grid node maps reversed from the symmetric and asymmetric planes.
  • Grinding of rock, soil particles in a ball mill.

The accredited methods at the Crystallography Laboratory (AB 1661)

  • Products and construction materials – metals, composites: solid polycrystalline materials and powders (without the amorphous phase)
  • The qualitative phase composition. The X-ray diffraction method XRD on the basis of PN-EN 13925-1:2007 excluding points 7.4 – 7.11 and point 8
  • A grid parameter, crystallite dimensions. The X-ray diffraction method XRD – the Rietveld’s method on the basis of PN-EN 13925-1:2007 excluding points 7.6 – 7.11 and point 8
  • The quantitative phase composition, range: (5.0 – 100.0) %. The X-ray diffraction method XRD – the Rietveld’s method, the internal pattern method on the basis of PN-EN 13925-1:2007 excluding points 7.4 – 7.11 and point 8, PN-EN 13925 – 2:2004 excluding points 4.5, 6.3, 6.6

Products and construction materials: metals

  • The crystallographic texture The X-ray diffraction method XRD on the basis of PB-XRD-5 edition 2 of 24.07.2018.
  • The pharmaceutical products: drugs – active substances
  • The phase composition identification. The X-ray diffraction method XRD on the basis of Farmakopea Polska, edition X Vol. I, 2014 point 2.9.3

EQUIPMENT

X-ray diffractometer WAXS/SAXS – EMPYREAN, (PANalytical):

  • high voltage generator, power 4 kW, x-ray tubes Cu, Co and Ag
  • goniometer 240 mm in the vertical layout ensuring controlled lamp and detector movement with the resolution of 0.0001° and independent drive of angles θ and 2θ, range 2θ from – 110° to 168°
  • programmable primary optics with a set of apertures including a special aperture 1/32 Mo for low angle testing, Soller’s aperture 0.04, 0.02 and 0.01°, double-reflection hybrid monochromator 2xGe (220), converging lenses for testing tension textures and in-plane
  • Bragg-Brentano’s optics unit including programmable receiving apertures and fixed anti-dispersion apertures, triple axis module with the analysing crystal for high resolution testing, point scintillation deflector and semiconductor linear PIXcel3D mounted on a single double arm
  • high temperature attachment Anton Paar HTK1200N (od 25 do 1200 °C) and low temperature attachment Oxford Cryosystems PheniX (od -261 do 25 °C)
  • reference samples for testing SAXS, tensions, texture, reflectometry and epitaxial layers, patterns with NIST: LaB6, Al2O3, Si, ZnO, TiO2, Cr2O3, CeO2
  • the data base of powder diffraction patterns PDF-4+ and non-organic structures ICSD
  • ball mill, hydraulic press, laboratory sieves

Monocrystalline diffractometer – SuperNova (Dual Source), (Agilent Technologies):

  • four-wheel diffractometer provided with two inseparable micro focal X-ray lamps Mo and Cu
  • detector CCD Atlas with the diameter of 135 m

Katarzyna Pawlus – Skowron – Deputy Laboratory Manager

Jarosław Serafińczuk, Post-doctoral deg.  –  Senior Testing Engineer

Publishings of laboratory members:

  • Constructing anhydrous halide bridged manganese(II) clusters: synthesis, structures and magnetic properties, J. Utko, A. B. Canaj, C. J. Milios, D. Dobrzyńska, K. Pawlus, A. Mikołajczyk, T. Lis, Inorganica Chimica Acta, 409B, 2014, 458-464
  • Structural, vibrational and theoretical studies of anilinium trichloroacetate: new hydrogen bonded molecular crystal with nonlinear optical properties, H. Tanak, K. Pawlus, M. K. Marchewka, A. Pietraszko, Spectrochimica Acta Part A, 118, 2014, 82 – 93
  • Molecular structure, vibrational spectra and DFT computational studies of melaminium N-acetylglycinate dihydrate, H. Tanak, K. Pawlus, M. K. Marchewka, Journal of Molecular Structure, 1121, 2016, 142 – 155
  • R. Oliva, Sz. J. Zelewski , Ł. Janicki, K. .R Gwóźdź, J. Serafińczuk, M. Rudziński, E. Özbay, R. Kudrawiec, Determination of the band gap of indium-rich InGaN by means of photoacoustic spectroscopy, Semiconductor Science and Technology, 33, 2018, 035007
  • J. Serafinczuk, Determination of lateral block size and mosaic of crystals using in-plane X-ray diffraction, Crystal Research & Technology, 51, 2016, 276-281
  • Sz. Jasiecki, J. Serafińczuk, T. Gotszalk, and G. Schroeder, X-Ray Reflectometry Study of Self-Assembled Ionic Nanolayers, Journal of Nanomaterials, 2012, 2012
  • G. Zatryb, A. Podhorodecki, J. Serafińczuk, M. Motyka, M. Banski, J. Misiewicz, N.V. Gaponenko, Optical properties of Tb and Eu doped cubic YAlO3 phosphors synthesized by sol-gel method, Optical Materials, 35 (12), 2013, 2090-2094
  • Ł. Gelczuk, J. Serafińczuk, M. Dąbrowska-Szata, P. Dłużewski, Anisotropic misfit strain relaxation In lattice mismatched InGaAs/GaAs heterostructures grown by MOVPE, Journal of Crystal Growth, 310, 2008, 3014-3018
  • J. Serafinczuk, R. Kudrawiec, R. Kucharski, M. Zając, T. P. Gotszalk, Structural properties of bulk GaN substrates: impact of structural anisotropy on non-polar and semi-polar crystals, Crystal Research & Technology, 50, 2015, 903-908
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Posted by PORT - Polski Ośrodek Rozwoju Technologii, Posted on 08.10.2015
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