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X-ray Diffraction

X-ray laboratory

CNMS offers an array of X-ray diffraction and small-angle scattering techniques to determine crystal structure and morphology.  These techniques can be used collaboratively with neutron scattering.

High Resolution X-Ray Powder Diffractometer (PANalytical X'Pert Pro MPD)

The PANalytical X'Pert MPD Pro is a conventional 1.8kW sealed X-ray tube source, using a Cu target, and a vertical circle goniometer. The default configuration of this instrument is in Bragg-Brentano geometry with a high-speed high-resolution X'Celerator position sensitive detector. This combination usually gives excellent quality X-ray powder diffraction data over relatively short data collection times. Unlike previous generations of linear position sensitive detectors, the X'Celerator has high resolution, with a minimum step size <0.001deg, and a high dynamic range.

In-situ, ex-situ, ambient and non-ambient X-ray powder diffraction measurements are performed to identify crystal phase and phase transition using Rietveld Refinement.

Applications

  • In-situ temperature-dependent X-ray diffraction measurement
  • In-situ X-ray diffraction measurement during chemical reaction
  • X-ray diffraction measurement for powders and bulk films, and phase identification

Specifications

  • Nonambient sample stages: XRK-900 (25 °C ~ 900 °C), TTK-450 (-190 °C ~ 450 °C) and Phenix Cryostage (12 K ~ 300 K)
  • Sample spinner with automatic sample changer (15 samples).
  • Various gas environments: Inert gases, CO2, N2 and vacuum.
  • Parallel beam optics are also available for irregular samples or asymmetric measurements
  • ICDD (International Centre for Diffraction Data) is provided for phase identification

 

High Resolution X-Ray Thin Film Diffractometer (PANalytical X'Pert PRO MRD)

The PANalytical X'Pert MRD Pro is a conventional 1.8 kW sealed X-ray tube source, using a Cu target, a horizontal circle goniometer and Open Eularian Cradle (OEC) sample stage. The default configuration of this instrument is in Bragg-Brentano geometry with a hybrid mirror for monochromatic incident beam, parallel plate collimator (or triple axis monochromator) and a sealed Xe proportional counter with a minimum step size 0.0001°.

X-ray diffraction measurements for thin films, both single crystals and polycrystalline (X-ray diffraction and reflectivity) from RT to 900°C, also used to measure powders.

Applications

Types of capable measurements are crystal orientation, degree of crystallinity, stresses/strain of single crystal thin film, reciprocal space mapping of sample surfaces, density and film thickness determination (x-ray reflectivity), Pole figure and low angle measurement as low as 0.1°.

Specifications

  • Nonambient sample stages: DHS-900 (25 °C ~ 900 °C)
  • Various gas environments: Inert gases, CO2, N2 and vacuum.

 

Small-angle X-ray scattering (Anton Paar SAXSess mc²)

SAXSess mc² allows time- and temperature-dependent, and static small-angle X-ray scattering (SAXS) experiments to be performed fully automatically. It is used to investigate structures from 1 nm to 200 nm present in many different kinds of liquid and solid (samples. Grazing-incidence scattering (GI-SAXS) studies of nanostructured surfaces are also possible.

The SAXSess mc² employs a conventional 2.0 kW sealed X-ray tube (line and/or point collimation) microsource, using a copper target with a CCD and imaging plate detector for 2D data acquisition. The X-ray optics uses focusing graded multilayer optics for advanced line and point collimator in conjunction with Kratky camera.

Applications

Study structures ranging from a few to tens of nanometers scale including colloids, proteins, surfactants, catalysts, microemulsions, polymers, liquid crystals, fibers, nanocomposites

Specifications

The SAXSess mc² is equipped with autosamplers, TCS temperature-controlled stages (-150~°C … 300 °C with ± 0.1 °C resolution), VarioStage for GISAXS. Software SAXSquant™ data acquisition & analysis software is available for advanced data interpretation.

 

Recent Publications

Jordan A. Hachtel, Jingsong Huang, Ilja Popovs, Santa Jansone-Popova, Jong K. Keum, Jacek Jakowski, Tracy C. Lovejoy, Niklas Dellby, Ondrej L. Krivanek, and Juan Carlos Idrobo, Science 363 (6426), 525-528 (2019)

Bin Yang, Wenmei Ming, Mao‐Hua Du, Jong K Keum, Alexander A Puretzky, Christopher M Rouleau, Jinsong Huang, David B Geohegan, Xiaoping Wang, Kai Xiao. Advanced Materials 30 (22), 1705801 (2018).

Bin Yang, Ondrej Dyck, Jonathan Poplawsky, Jong K Keum, Sanjib Das, Alexander Puretzky, Tolga Aytug, Pooran C Joshi, Christopher M Rouleau, Gerd Duscher, David B Geohegan, Kai Xiao. Angewandte Chemie International Edition 54, 14862 (2015)

Yin, Panchao; Wu, Bin; Mamontov, Eugene; Daemen, Luke L; Cheng, Yongqiang; Li, Tao; Seifert, Soenke; Hong, Kunlun; Bonnesen, Peter V; Keum, Jong Kahk; Journal of the American Chemical Society 138 (15), 2638-2643 (2016).

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