X-ray diffraction

Powder X-Ray Diffraction Service is attached to the analysis and characterization platform for IRCELYON catalysis.
XRD is a basic technique for catalysis, fast and non-destructive.
Two fully programmable D8-Advance BRUKER diffractometers allow to work day and night without human intervention. One is equipped with an automated sample changer and the second with an Anton Paar XRK-900 reactor chamber.
Many information can be extracted from the analyses, such as the identification and quantification of phases, the crystallites size, the lattice parameters, the degree of crystallinity. For this, a large number of software (DIFFRAC EVA, HighScore Plus, TOPAS, FullProf …) and databases (PDF-4 + ICDD, COD, ICSD, CSD) are available to users.

Equipment

Two D8-Advance BRUKER with Bragg-Brentano Theta-Theta geometry and the advantage to keep the sample horizontal.

BRUKER D8-ADVANCE WITH AUTOCHANGER

Analytical capabilities Technical specifications
Allows to analyse samples in RT conditions with programs adapted to each of them with a fully motorized and programmable equipment. Cu anode X-Ray tube

LynxEye detector: 1 D fast detector

Ni filter

AUTOCHANGER automated sample changer: 6 towers of 15 positions

Programmable divergence (variable or fixed) and anti-scattering slits

Motorized anti-scatter screen according to 2-Theta

SAMPLE HOLDERS

Some commercial and many specially manufactured sample holders are available to fit the sample quantity.

SI low background sample holders
Airtight specimen holders for environmentally sensitive materials with kapton sheet or dome

Standard specimen holders in PMMA or PVC with different widths and depths
Universal sample cup for rotating sample stage

BRUKER D8-ADVANCE with Anton Paar XRK-900

Analytical capabilities Technical specifications
XRD in temperature under gas flow

Allows recordings in temperature and under gas flow (N2, H2, O2, air, He, gaseous mixture).

A rotating sample plate equipped with a sample cup completes the equipment when the chamber is removed.

 Cu anode X-Ray tube

LynxEye XE-T detector: 1D detector
Resolution in energy filtering white radiation, Kβ (Cu) and the fluorescence of most elements

Anton Paar XRK-900 reactor chamber with sample rotation:
– from 25°C to 800°C
– macor sample holder closed or open with sieve

Programmable divergence (variable or fixe) and anti-scattering slits

Results

Small angle diffraction of a mesoporous material (SBA-15)

XRD pattern of SBA-15 with time counting :
a) t=2s, b) and c) t=16s with a zoom (x7) in the case of c)

XRD in temperature under gas flow

In situ analyses : Structural evolution in temperature of Co3O4 (15weight%) supported on gamma Al2O3 by reduction under H2. Crystallite size: calculation by Rietveld Method
(FullProf1,Scherrer not possible)

  • Gamma Al2O3 support taken as background and refined
  • Co3O4 structure refined
  • Lattice parameters, crystallites size(5nm) calculated

1 http://www.ill.eu/sites/fullprof
C. Trevisanut, F. Bosselet, F. Cavani and J. M. M. Millet, Catal. Sci. Technol., 2015, 5, 1280–1289and https://hal.archives-ouvertes.fr/hal-01900864 C. Trevisanut, F. Cavani, J. M. M. Millet, Y. Aizac, F. Bosselet, Association Française de Cristallographie 2018, Jul 2018, Lyon, France. In situ experiments : X-ray diffraction patterns of magnetite used as cycling material during chemical looping process for H2 production from ethanol and water used as reducing and oxidizing species, recordings at 723K after successive pulsations of ethanol (in black) and water (in blue).

Keywords

  • Powder XRD
  • In situ XRD, XRD in temperature, XRD under gas flow
  • Crystallite size
  • Phases Analyses
  • Phases Quantification
  • Rietveld

Staff

  • Personnels techniques (en)

    • Yoann Aizac
    • Pierre Martinez-Ginouves

Publications

All recent publications