Scattering and diffraction methods

Wide angle x-ray scattering (WAXS)

Analyte

  • Native and man-made polymers, composites, basic material, inorganic matters
    • Sample quantity: polymers: 0.5 cm3 - 1 cm3, inorganic matters: mg-range

 

Equipment

  • X-ray diffraction instrument: two-circle diffractometer (D5000, Bruker-AXS)
    • Monochromator: Ge(111) primary monochromator
    • Wave length: Cu-Kα1; λ = 0.15406 nm
    • Detector: scintillation counter
    • Operation (standard): symmetrical transmission geometry
    • Accessories: equipment for the investigation of liquids
  • X-ray diffraction instrument: texture goniometer equipped with an closed Eulerian cradle (four-circle diffractometer, D5000, Bruker-AXS)
    • Monochromator: Ni-filter
    • Wave length: Cu-Kα; λ = 0.1542 nm
    • Detector: scintillation counter
    • Operation: transmission or reflection geometry
  • X-ray diffraction instrument: flat-film camera
    • Monochromator: Ni-filter
    • Wave length: Cu-Kα; λ = 0.1542 nm
    • Detector: X-ray film
    • Operation (standard): transmission geometry
    • Accessories: heater, small angle camera

 

Evaluation methods and targets

  • Characterization of the supermolecular structure of native and man-made polymers
    • Determination of the crystallinity and the crystallite sizes (adapted Ruland-Vonk-Verfahren, Fraunhofer IAP software WAXS VII)
  • Characterization of the preferred orientation of polymers
    • Recording of complete pole figures
    • Determination of texture types from pole figures (transmission, reflection)
    • Determination of quantitative orientational parameters
    • Quantitative determination of fiber orientation (Herman´s orientation factor, Fraunhofer IAP-software)
    • Qualitative characterization of the crystalline orientation from flat-film diagrams
  • Qualitative and quantitative phase analysis
    • Qualitative phase analysis using peak fitting; line profile analysis (Topas-P, Bruker-AXS)
    • Quantitative phase analysis (line profile analysis by whole powder pattern fitting, Fraunhofer IAP-software)
    • Quantitative Rietveld analysis (Topas-R, Bruker-AXS)
    • Qualitative and quantitative phase analysis using X-ray flat-film diagrams

 

Applications

  • Determination of the crystallinity and the crystallite sizes of pulps and starch
  • Characterization of the orientation of cellulosic fibers, foils and casings
  • Quantitative determination of the content of different modifications of a substance (e.g. phase analysis of cellulose I / II: fiber-reinforced sausage casings )
  • Quantitative phase analysis of composites materials (e.g. quantitative analysis of the fiber content in fiber-reinforced composites)
  • Quantitative Rietveld analysis of cement

 

Comparative and additional methods

  • Small angle X-ray scattering (SAXS)
  • Nuclear magnetic resonance spectroscopy (NMR)
  • Scanning electron microscopy (SEM)
  • Transmission electron microscopy (TEM)
  • Optical microscopy (OM)