Materials Chemistry - EH3

The materials chemistry hutch at ID15A (EH3) is dedicated to operando and time-resolved diffraction and imaging, total scattering, and diffraction computed tomography. The EH3 station is optimised for rapid alternation between the different techniques during a single operando experiment in order to collect complementary data on working systems. The high available energy (up to 120 keV) means that even highly absorbing systems may be studied. The combination of the beamline's optimised focusing optics and a photon-counting CdTe pixel detector allows for both unprecedented data quality at high energy and very rapid scanning or triggered experiments.

Key points

• Energy range 20 < E < 120 keV (monochromatic)
• Beam sizes from 0.3 µm to 1.8 mm

Techniques

• Angular dispersive diffraction
• Total scattering
• X-ray diffraction tomography
• X-ray absorption and phase-contrast imaging

Experimental hutch overview

EH3 contains four main elements mounted on highly stable granite platforms. From right to left, these are 1) secondary focusing using compound refractive lenses; 2) sample stage containing both high-resolution (HR) and heavy-duty (HD) sample towers; 3) detector stage with 2.5 m-long translations; and 4) an ancillary table offering the ability to mount a SAXS detector.

Typical experimental configurations

X-ray diffraction detectors

From 2025, EH3 is equipped with a Dectris Pilatus4 XE CdTe 4M, enabling a frame rate up to 4 kHz and a 100 ns readout time. Since 2016, ID15A has operated a Dectris Pilatus3 X CdTe 2M. Photon counting, CdTe-sensor detectors have brought unprecedented data quality at high energy, and have therefore replaced the flat panel Perkin Elmer 1621 as the EH3 detector for X-ray scattering and diffraction.

X-ray imaging detectors

A range of imaging cameras are available for experiments which require complimentary absorption tomography. These detectors are permanently mounted and can be used sequentially with the diffraction and/or SAXS detector and one another. The detectors system characteristics are listed below.

Complementary probes

Besides the equipment available on loan from the Sample Environment and Detector pools, several dedicated probes are available for simulataneous measure during scattering and/or imaging experiments. A dedicated Bruker Vertex 80 spectrometer, a Hiden QGA mass spectrometer are available for operando experiments combining DRIFTS, XRD/PDF and MS. Together with a remote-controlled rack of mass flow controllers and VICI electrovalves, these enable a wide array of heterogeneous catalysis experiments. The IR detector and Harrick operando reaction chamber are shown below mounted on the heavy-duty stage in EH3.

Fluorescence detectors can be used to perform simultaneous fluorescence mapping and XRD mapping or fluorescence CT and XRD-CT, or as a standalone probe in dedicated experiments (see Scientific Examples). A Mirion HPGe-CMOS and a Hitachi Vortex-EM with a 1 mm-thick Si crystal for high energies are available for simultaneous use. The detectors are coupled to with a FalconX and Mercury/XIA readout electronics allowing exposure times of a few milliseconds.

Sample environments

A number of sample environments are available to control the sample temperature in the range 80 - 1500 K. Lower temperatures are avaliable with cryostats from the sample environment pool.

Scientific Examples

The new beam line makes techniques like diffraction tomography, pair distribution function analysis, and ultra-fast hight energy diffraction routinely accessible to the full ESRF user community. Please see the Scientific Examples page for more information.