X-ray diffraction (XRD) laboratory

GeniX High Flux Beam Delivery System

GeniX High Flux Beam Delivery System and INEL 120º PSD

Key facts

Technique: X-ray diffraction (XRD)

Used for: phase identification, quantification and crystal structure analysis

The X-ray diffraction facility comprises several state-of-the-art instruments used for phase identification, quantification and crystal structure analysis.

The laboratory can provide in-depth analysis expertise for a wide range of materials such as rocks, ores, sediments, meteorites, peats and soils, biominerals and nanomaterials. We can analyse single crystals and powders or materials on polished sections. Preparation labs are available for various pre-treatments of samples, including grinding powders and for clays, oriented mounts, glycol solvation, heating furnaces.

Enraf-Nonius Powder Diffraction Systems 120

The laboratory has three Enraf-Nonius Powder Diffraction Systems 120. Rapid data acquisition is achieved by using an INEL 120º curved position sensitive detector (PSD). The set up of each machine varies as follows

  • XRD-PSD2 – CuKa1 radiation – used for phase identification, phase quantification
  • XRD-PSD3 – CoKa1 radiation – used for phase identification, phase quantification, very well suited for iron bearing samples
  • GeniX High Flux Beam Delivery System – CuKa1/2 radiation – used with high-temperature stage (Anton Paar HTK10, 20-1600ºC) for monitoring phase transformations and reactions, very small samples possible (micro-to-milligrams, short data collection due to high-flux X-ray source)
Micro-XRD_Elphidium

Micro-XRD_Elphidium

Panalytical Scanning Diffractometer X’Pert Pro MPD Alpha1

  • Primary monochromator and para-focussing optics for high resolution measurements – Co or Cu radiation
  • Reflection and transmission geometry
  • Used for structural characterisation of powdered samples (Rietveld analysis): lattice parameters, crystallite size, microstrain analysis
Panalytical Scanning Diffractometer X’Pert Pro MPD Alpha1

Panalytical Scanning Diffractometer X’Pert Pro MPD Alpha1

Rigaku Rapid 2 Micro-XRD with curved 2D detector

  • Used for phase identification of very small objects (> 30 micrometer), flat polished sections and very small amounts of powder (micrograms)
  • Gandolfi-type movements can be programmed for samples with low numbers of crystallites to analyse a maximum of grain orientations.
Rapid2

Rapid2

Agilent X’Calibur Single Crystal Diffractometer with CCD area detector

  • Structural analysis of single crystals
  • Refinement of known crystal structures and solution of unknown (new) crystal structures
  • Well suited for small single crystals (>20 micrometer) and weakly scattering materials (including Li, B)
  • Cryo-heat system for phase transformation studies between 100 and 500 K.
X’Calibur

X’Calibur

PDF-4 database from ICDD

The most recent PDF-4 database from ICDD is available for phase identification. In difficult cases of phase assignments we can compare data with standards from our huge mineral collection in the Museum. Standard minerals from the Museum collection are used for quantification of multi-phase mixtures and particular experiences for clay-bearing samples can be offered.

Na-Smectite dehydration

Na-Smectite dehydration

Museum lead

Dr Jens Najorka

Equipment

  • Enraf-Nonius Powder Diffraction Systems 120
  • Panalytical Scanning Diffractometer X’Pert Pro MPD
  • Rigaku Rapid 2 Micro-XRD with curved 2D detector
  • Agilent X’Calibur Single Crystal Diffractometer with CCD area detector