X-Ray Diffusion and Diffraction (XRD)

X-ray diffraction gives information on the ordered solid at ambient temperature and during heat treatment. The geometric arrangement of the atoms and the distance between them constitute a unique identity card for each compound. X-ray diffusion at small angles studies the organisation of matter over a few nanometers.

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Leader

Josien Ludovic
Contacts : ludovic.josien@uha.fr ou laure.michelin@uha.fr

Description

Areas of activity :

The activities of the platform focus on the structural characterisation of all types of solid materials by X-ray diffraction or diffusion : identification of phases, study of crystallinity or organisation, reflectometry, grazing incidence, structural determination on powder, observation of phase transitions in temperature and controlled atmosphere. In addition, these characterisations can be supplemented by X-ray Fluorescence spectrometry analyses which make it possible to determine the chemical composition of a sample and thus facilitate structural identification.

Main equipment (strengths of the Institute) :

The platform has 3 diffractometers, one thermodiffractometer, one SAXS-WAXS and an X-ray fluorescence spectrometer :

  • 3 powder diffractometers : 2 in reflection geometry with autosampler (Bruker D8 ADVANCE and PANalytical, X’Pert PRO MPD) and 1 in transmission geometry (STOE Stadi-P and Bruker D8 ADVANCE)
  • 1 thermodiffractometer (PANalytical, X’Pert PRO MPD) equipped with a temperature chamber (Anton Paar HTK1200)
  • 1 x SAXS-WAXS small angle X-ray diffusion unit (Rigaku SMax 3000)
  • 1 Wavelength Dispersion X-Ray Fluorescence Spectrometer (PANalytical, Zetium)

Technical description

X-Ray Diffusion at Small Angles (SAXS / WAXS) Rigaku SMax 3000 Model with MicroMax-007HF

 

Location rue J. Starcky
Year of commissioning 2008
Rotating anode source size 70μm, copper (1.54Å)
Angular domain two possible domains
SAXS 0.085° to 2.25° 2θ (~1000Å à ~40Å)
WAXS 2.7° to 35° 2θ
Dimensions source – detector : 3.00m
sample – detector : 1.50m (SAXS), ~ 10.5cm (WAXS)
Optical OSMIC CMF (Confocal Max-FluxTM) and 3 pinholes (Ø400μm, 200μm, 650μm)
Detector two types of detectors
SAXS : 2D gas detector wire chamber type “Gabriel”, Ø12cm
WAXS : Fujifilm 15x15cm Flat Image (BAS-MS2325, 1500px)
Sample preparation constraint Powdered or solid samples (low absorbency), thin films, diluted solutions…
Usable accessories possibly capillaries
Self-service accessibility no

Contact : Jean-Marc Le Meins, Simon Gree

PANalytical X-ray Diffractometer, model X'Pert PRO MPD with feeder
Location rue A. Werner
Year of commissioning 2004
Anticathode copper (λ = 1.54Å)
Geometry reflection (Bragg-Brentano)
Goniometer vertical, system θ – θ
Angular domain of analysis 0.5 to 150° 2θ
Minimum angular pitch 0.002° 2θ
Type of detector X’Celerator
Monochromator carbon graphite (002) – rear position – removable
Passing capacity 45 samples
Sample preparation constraint powder samples or solid samples (diameter < 43mm, height < 6mm)
Self-service accessibility no – Samples are prepared by the users but the autosampler is programmed and checked by the Technical Authority

Contact : Laure Michelin, Ludovic Josien

PANalytical X-Ray Thermodiffractometer, X'Pert PRO MPD model

 

Location rue A. Werner
Year of commissioning 2003
Anticathode copper (λ = 1.54Å) or chromium (λ = 2.29Å)
Geometry reflection (Bragg-Brentano) or transmission (Debye-Scherrer)
Goniometer vertical, system θ – 2θ
Angular domain of analysis 0.5 to 130° 2θ
Minimum angular pitch 0.002° 2θ
Type of detector X’Celerator or proportional detector
Monochromator Germanium (111) – front position – removable
Specific configuration Anton Paar HTK1200 high temperature chamber under a specific atmosphere (neutral gas or oxygen, no reducing gas) and controlled heating up to 1200°C (manufacturer’s data)
Sample preparation constraint powdered samples. Possibility of solid samples for some configurations (height < 6mm)
Self-service accessibility partial
yes for analysis after training by the technical manager
no for configuration changes.

Contact : Laure Michelin, Ludovic Josien

Bruker D8 ADVANCE A25 X-ray diffractometer

 

Location rue J. Starcky
Year of commissioning 2016
Anticathode copper (λ = 1.54Å)
Geometry reflection (Bragg-Brentano), transmission
Goniometer vertical, scanning θ – θ
Angular domain of analysis Variable according to accessory and type of acquisition, typically 0.5 ° to 130° 2θ (reflection)
Minimum angular pitch 0.0001° 2θ
Autochanger capacity (autosampler) 15
Detector LynxEye XE-T with power discrimination (<380eV in high resolution mode)
Monochromator No
Sample preparation constraint Powder samples (400mg), fibres or solid samples with conditions.
Accessories Compact and motorized XYZ stage allows grazing incidence or reflectivity measurements to be taken.
Self-service accessibility No. The samples are prepared by the users but the Autochanger is programmed and verified by the person in charge of the machine.

Contact : Jean-Marc Le Meins, Simon Gree

STOE X-ray diffractometer, STADI-P model
Location rue A. Werner
Year of commissioning 1994
Anticathode copper (λ = 1.54Å)
Geometry transmission (capillary or flat plate)
Goniometer horizontal, scanning θ -2θ
Angular domain of analysis 3.0 to 110° 2θ
Minimum angular pitch 0.01° 2θ
Detector linear with spatial location (Position Sensitive Detector)
Monochromator in germanium (111), forward position – fixed
Sample preparation constraint powder samples only
Self-service accessibility yes – after training by the technical manager.

Contact : Laure Michelin, Ludovic Josien

PANalytical Wavelength Dispersion X-Ray fluorescence Spectrometer, Zetium model
Location rue A. Werner
Year of commissioning 2017
Anticathode Rhodium 4kW
Detector Scintillator, Gaseous and ED Flux (for Small Spot Mapping)
Domain of analysis Uranium Sodium Analysis + fluorine boron detection
Specific configuration Option to carry out an elementary mapping of the sample
Sample preparation constraint powdered samples or solid samples (diameter less than 40 mm)
Self-service accessibility no – Samples are prepared by the users but the autosampler is programmed and checked by the technical manager.

Contact : Laure Michelin, Ludovic Josien

IS2M

Bâtiment CNRS
15, rue Jean Starcky - BP 2488
68057 Mulhouse cedex

Bâtiment IRJBD
3 bis, rue Alfred Werner
68093 Mulhouse cedex

tel: (+33)3 89 60 87 00
fax: (+33)3 89 60 87 99

Réseaux sociaux

 

  

IS2M

Bâtiment CNRS
15, rue Jean Starcky - BP 2488
68057 Mulhouse cedex

Bâtiment IRJBD
3 bis, rue Alfred Werner
68093 Mulhouse cedex

tel: (+33)3 89 60 87 00
fax: (+33)3 89 60 87 99

Réseaux sociaux

 

  

IS2M

Bâtiment CNRS
15, rue Jean Starcky - BP 2488
68057 Mulhouse cedex

Bâtiment IRJBD
3 bis, rue Alfred Werner
68093 Mulhouse cedex

tel: (+33)3 89 60 87 00
fax: (+33)3 89 60 87 99

Réseaux sociaux