The X-ray center houses numerous instruments for material characterization by X-ray diffraction methods of a wide variety of samples. We also provide space and utensils to prepare samples yourself.

Below is an overview of some of the equipment at the X-ray Center as well as the sample preparation room.

Our devices:

Scientist sitting next to single-crystal diffractometer and evaluates data on the computer.

© Klaus Ranger

Scientist places sample in single crystal diffractometer

© Klaus Ranger

Characteristics

  • Geometry: ¼ Euler cradle
  • Anode: Cu and Mo microfocus X-ray sources
  • Monochromatization: multilayer mirrors
  • Beam sizes: ∅ 0.2 mm (Cu); 0.2 mm (Mo).
  • Distance sample-detector (SD): 40-140 mm.
  • Sample movement: ¼ Euler cradle
  • Sample adjustment: video adjustment system
  • Detector: Dectris Eiger CdTe 1M

Non-ambient

  •     Oxford Cryostream 800 (90 - 400 K)
  •     Stoe Heatstream (400 - 1000 K)

Applications

  •     Structure elucidation of weakly scattering crystals
  •     Structure elucidation of complex structures (modulated, twinned)
  •     Diffuse scattering

Material diffractometer GADDS from Bruker Interior view

© Klaus Ranger

Scientists in front of X-ray diffraction device.

© Klaus Ranger

Characteristics

  •     Geometry: Θ/Θ- diffractometer; parallel beam
  •     Anode: Cu microfocus X-ray source
  •     Monochromatization: Montel mirror
  •     Beam sizes: 2x2 mm², ∅1, 0.5, 0.3, 0.08 mm
  •     distance anode-sample (AS): 100 - 300 mm
  •     Distance sample-detector (SD): 100 - 300 mm
  •     Sample movement: ¼ Euler cradle; xyz stage (load capacity 2 kg).
  •     Sample adjustment: video adjustment system with laser
  •     Detector: Vantec 2000 (angular range 2θ= 32°, ψ= 63° with SD= 220 mm)

Non-ambient

  •  Load frame (planned)

Applications

  • Qualitative/quantitative phase analyses (e.g. corrosion products, residual austenite analyses)
  • Stress analysis (bulk and thin film samples)
  • Texture analysis (bulk and thin film samples)
  • Microdiffraction (up to beam sizes > 80 μm)
  • "Reciprocal space mapping" thin films

Exterior view: Powder diffractometer from the front

© Klaus Ranger

Interior view of powder diffractometer: X-ray tube on the left, sample holder in the center and detector on the right.

© Klaus Ranger

Characteristics

  •     Geometry: Θ/Θ - diffractometer; Bragg-Brentano
  •     Anode: Cu - X-ray source
  •     Monochromatization: a) Ni filter; b) secondary monochromator graphite
  •     Beam sizes: variable beam apertures (primary/secondary automatic)
  •     distance anode-sample (AS): 240 mm
  •     distance sample-detector (SD): 240 mm
  •     Sample movement: spinner without sample environment
  •     Sample changer for 15 samples
  •     Detector: a) X'Celerator semiconductor detector (2.1°); b) alternatively proportional counter (0D) with graphite monochromator

no option for non-ambient measurements

Applications

  •     Qualitative/quantitative phase analyses under ambient conditions (e.g. routine measurements for synthesis control)
  •     Reflectance measurements/transmittance measurements

Exterior view: Powder diffractometer from the front

© Klaus Ranger

Interior view of powder diffractometer, X-ray tube on the left, sample holder in the center, and detector on the right.

© Klaus Ranger

Characteristics

  •     Geometry: Θ/Θ- diffractometer; Bragg-Brentano
  •     Anode: Cu -X-ray source
  •     Monochromatization: a) Ni filter; b) secondary monochromator graphite
  •     Beam sizes: variable beam apertures (primary/secondary automatic)
  •     distance anode-sample (AS): 240 mm
  •     distance sample-detector (SD): 240 mm
  •     Sample movement: spinner without sample environment; fixed for sample environment
  •     Detector: a) X' Celerator semiconductor detector (2.1°); b) Scintillation detector (0D)

Non-ambient

  •     Closed-cycle cryostat (11K > T < 310 K)
  •     Anton Paar HTK 1200 N (T < 1200°C); air, nitrogen atmosphere
  •     Anton Paar XRK 900 reaction chamber (P < 10bar; T < 900°C); gas atmospheres (Ar, H2, CO, CO2, mixtures)
  •     Anton Paar TTK450 chamber (100K > T < 470K)

Applications

  •     Qualitative/quantitative phase analysis of crystalline fractions
  •     Amorphous phase fractions
  •     Crystallite sizes
  •     Residual austenite analysis

under non-ambient conditions:

  •     Reflection measurements/transmission measurements
  •     Capillary measurements

Exterior view of material diffractometer from the front.

© Klaus Ranger

Interior view of material diffractometer: Fixation of the sample in the diffractometer, the sample are 2 fingers of a statue.

© Klaus Ranger

Characteristics

  •     Geometry: Θ/Θ - diffractometer; Bragg-Brentano (focusing mirror; Cu(Kα1,2)), parallel beam geometry (mirror; Cu(Kα1,2)), channel-cut monochromator (CuKα1), GID; capillary/reflectance and transmission geometry
  •     Anode: Cu/Mo/Ag - X-ray source
  •     Monochromatization: a) filter (Cu, Mo, Ag); b) mirror (parallel geometry; focusing for Cu anode)
  •     Beam sizes: variable beam apertures (primary/secondary automatic)
  •     distance anode-sample (AS): 240 mm
  •     Distance sample-detector (SD): 240 mm
  •     Sample movement: spinner without sample environment; fixed for sample environment
  •     Tilting stage for stress and texture measurements
  •     Setup for GID measurements on thin films
  •     Reflectometer attachment
  •     Detector: a) PIXCel 3D semiconductor detector; b) scintillation detector (0D) for Ag radiation

Non-ambient

  • Currently not foreseen

Applications

  •     Qualitative/quantitative phase analysis of crystalline components
  •     Amorphous phase fractions, crystallite sizes, etc.
  •     Stress/texture measurements
  •     Reflectometry measurements
  •     GID measurements on thin films
  •     Measurements for PD analysis

under ambient conditions:

  • Capillary/reflection and transmission geometry

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APEX II single crystal diffractometer interior view

© Klaus Ranger

Evaluation of diffractometer data on screen

© Klaus Ranger

Characteristics

  •     Geometry: 4-circle with kappa geometry
  •     Anode: Mo X-ray source
  •     Monochromatization: graphite
  •     beam size: variable collimators, 0.4-0.8 mm
  •     distance sample-detector (SD): 36-180 mm
  •     2D CCD detector

Non-ambient

  •     Cooling up to 90 K and heating up to 450 K in dry nitrogen atmosphere

Applications

  •     Structure elucidation (organics, organometallics and inorganics).
  •     Determination of absolute configuration (elements ≥ S)
  •     Structure function relationships (e.g., nonlinear optical materials)
  •     Crystallographically challenging problems: stacking fault orders, twins, modulation
  •     Phase transitions (e.g., magnetic or ferroelectric transitions)

X-ray fluorescence spectrometer from the front

© Klaus Ranger

Close-up view of inserting a sample into the spectrometer.

© Klaus Ranger

Characteristics

X-ray tube SST-mAX

  • Anode: Rh standard

Goniometer

  • Type: θ/2θ decoupled with Direct Optical Position Sensing (DOPS)
  • Angular accuracy: 0.0025° θ and 2θ

Optical path

  • Primary collimators: 3 max.: 100, 150, 300, 550, 700 or 4000 μm
    Primary beamfilters 4 max.: One may be used as beam stop
    Crystals: 8 max.: LiF420, LiF220, LiF200, Ge111 (flat/curved), PE002 (flat/curved), InSb (flat/curved),TlAP coated, PX1, PX4, PX5, PX6, PX7, PX10
  • Detectors: Flow, scintillation, sealed Xe in tandem with flow counter as duplex counter (optional), Hi-Per Scint (optional)

Counting electronics

  • Type: Dual multi channel analyser with digital signal processor

Sample handling

  • Types: Solid, fused beads, filters, pressed/loose powders and liquids
  • Handling: All samples are fitted in sample holders during measurement. Liquids and loose powders in disposable (P2) liquid cells, which are fitted in liquid sample holders
  • Dimensions: 51.5 mm Ø x 40 mm height, maximum
  • Weight: Max. 400 g including sample holder
  • Sample changer: X-Y changer with priority position for 1 sample (detected) and 2 empty holders with capacity for 8 trays for 8 sample holders and 1 tray for 4 sample holders.
    Optional: High-capacity changer up to 209 uncupped samples of 32 mm or 140 uncupped samples of 40 mm diameter
  • Changer trays: for: 8 sample holders, 8 flex positions, 8 steel rings (Ø 51.5 mm), 21 samples (Ø 25 mm), 12 samples (Ø 32 mm), 10 samples (Ø 41 mm), or 4 sample holders (SPC/monitor tray)
  • Loading: Air lock with programmable pumping time, one or two position turret mechanism, sample-surface down, direct loading of unmounted samples in holder in loading position
  • Spinner: 0.5 rev/s

Applications

Wavelength dispersive X-ray fluorescence spectrometer for quantitative elemental analysis except Hydrogen, Lithium and Beryllium in solid state materials.

Sample preparation:

Scientist prepares powder sample.

© Klaus Ranger

Scientist prepares powder sample.

© Klaus Ranger

Scientist prepares powder sample.

© Klaus Ranger

Scientist prepares powder sample.

© Klaus Ranger

Three prepared powder samples in sample holders.

© Klaus Ranger

Storage cabinet for dosimeters.

© Klaus Ranger

Storage box for utensils and chemicals on table.

© Klaus Ranger

Clock with mathematical symbols or formulas instead of numbers.

© Klaus Ranger