The beamline ID31 is dedicated to studies of interface and materials processing using high energy X-rays. It offers a portfolio of hard X-rays characterization techniques including reflectivity (XRR), wide and small angle diffraction (WAXS and SAXS), both in transmission and in grazing incidence geometries, but also combined with auxiliary techniques like imaging. The beamline optical design allows rapid change of the beam properties, like the photon energy, the bandwidth and the focus. It allows to install complicated and heavy experimental setups. The state-of-the-art Pilatus CdTe 2M from DECTRIS is installed in the large volume experimental hutch, so that it can be positioned to adapt the reciprocal space resolution with ease. Two detectors at the end of the hutch - a flat panel CMOS and an imaging detector - allow combining SAXS and X-Ray imaging with WAXS. This particular combination is one of the unique beamline capabilities, making it attractive for scientists worldwide studying energy materials and materials in general.  

The beamline development focused improving the capabilities towards multi-modal simultaneous operando experiments and housing additive manufacturing systems for operando studies. For this, the SAXS capabilities were improved, the safety conditions for laser related studies were installed in the experimental hutch and the throughput of diffraction tomography experiments was enhanced. Two gas distribution systems for both, low and high pressures, were designed and are available for the beamline users. 

In the beamline we have developed an in-house research program in the domain of electrocatalysis and battery research, as well as various unique sample environments, like grazing incidence electrochemical cells, fuel cells, electrolyser cell, microfluidic cell, hydrogen storage reactor and various battery cells. In this sense, the program focuses on exploring the materials for energy applications. We take advantage of the beamline multi-modal capabilities to study materials for energy conversion and storage devices during its functioning conditions, from both, fundamental and applied perspectives. This approach allows to do a correlative analysis leading to more holistic understanding of such devices. This is a critical step in the optimization of this kind of technologies, as the materials need to function in synchronization in order to achieve the necessary performance. Furthermore, we are developing new reflectivity based techniques to characterize quantum devices and exploiting new class of 2D materials for electrocatalysis. 

The complexity of heterogeneous devices such as fuel cells, organic solar cells, rechargeable batteries, catalytic materials, etc., can only be studied adequately by a combination of experimental methods, in order to reveal the interplay between the microscopic material properties and the macroscopic device performances. As the need for combining techniques has been instrumental in the development of electron microscopy it is seen as equally important for the evolution of hard x-ray synchrotron methods applied in-situ for studying both real devices under operating conditions and idealized model systems under precisely controlled environments. In summary and as pointed out before, ID31 enables a portfolio of hard x-ray characterization techniques including reflectivity, wide angle diffraction both in transmission and grazing incidence geometry, small angle x-ray scattering, and imaging methods coupled with a great versatility in choosing beam sizes, energy bandwidth and detectors optimized for high energy x-rays. The design  enables many different studies with remarkable potential.

 

Selected publications:

Laetitia Dubau et al., ACS Catalysis, 6(2016), pp 4673–4684