Simultaneous SAXS/SANS Method at D22 of ILL: Instrument Upgrade

Abstract

A customized portable SAXS instrument has recently been constructed, installed, and tested at the D22 SANS instrument at ILL. Technical characteristics of this newly established plug-and-play SAXS system have recently been reported (J. Appl. Cryst. 2020, 53, 722). An optimized lead shielding arrangement on the SAXS system and a double energy threshold X-ray detector have been further implemented to substantially suppress the unavoidable high-energy gamma radiation background on the X-ray detector. The performance of the upgraded SAXS instrument has been examined systematically by determining background suppression factors (SFs) at various experimental conditions, including different neutron beam collimation lengths and X-ray sample-to-detector distances (SDDX-ray). Improved signal-to-noise ratio SAXS data enables combined SAXS and SANS measurements for all possible experimental conditions at the D22 instrument. Both SAXS and SANS data from the same sample volume can be fitted simultaneously using a common structural model, allowing unambiguous interpretation of the scattering data. Importantly, advanced in situ/real time investigations are possible, where both the SAXS and the SANS data can reveal time-resolved complementary nanoscale structural information.

Investigating Growth of Gold Nanorods by Simultaneous Small‐Angle X‐Ray and Neutron Scattering

“…This effect has been negated in a recent upgrade. [ 36 ] For this sample, a progressive increase of a characteristic SAXS 1D signal at Q > 0.04 Å −1 is observed (Figure 2a), which arises from the growing AuNRs. In the early time regime (<30 min) directly after the mixing step, no characteristic SAXS signal from already present Au seeds or nascent AuNR in the solution could be detected due to the small total volume of the particles (2 to 5 nm in radius) in the dispersion.…”

Neutron and muon characterisation techniques for battery materials

“…This includes the most difficult components to study such as the interfaces, as well as any operating system which is so complex due to the many chemical and physical reactions that take place over multiple length and time scales. Complementary techniques used simultaneously are the best way to capture multiple aspects of these systems, and as X-ray sources can be relatively small there are some examples of simultaneous neutron and X-ray capabilities; SAXS and SANS at D22 of ILL, 148 neutron and X-ray Tomography (NeXT) system at the NIST thermal neutron imaging facility, 149 and X-ray and neutron imaging on the NEUTRA (thermal neutrons) and ICON (cold neutrons) beamlines at SINQ, PSI. 150 Meanwhile, the opportunity to combine operando data sets of neutron and muon experiments represents an exciting challenge; a detailed correlation between site occupancy diffusion characteristics can be used to well understand the fundamental structure–property relationships of materials during cycling.…”

Spatiotemporal Studies of Soluble Inorganic Nanostructures with X‐rays and Neutrons

“…X-rays are mainly scattered by electrons, whereas neutrons are scattered by nuclei. [34] This means the obtained scattering length density (SLD) from Xrays and neutrons are different representatives of the same structure, providing complementary and comprehensive information. [35] One must consider the composition of studied solutions; specifically absorption edges of the component elements.…”

“…X‐rays and neutrons share basic scattering principles, while their main differences originate from how they interact with atoms. X‐rays are mainly scattered by electrons, whereas neutrons are scattered by nuclei [34] . This means the obtained scattering length density (SLD) from X‐rays and neutrons are different representatives of the same structure, providing complementary and comprehensive information [35] .…”