Flexible Sample Environment for the Investigation of Soft Matter at the European Spallation Source: Part II—The GISANS Setup

Abstract

The FlexiProb project is a joint effort of three soft matter groups at the Universities of Bielefeld, Darmstadt, and Munich with scientific support from the European Spallation Source (ESS), the small-K advanced diffractometer (SKADI) beamline development group of the Jülich Centre for Neutron Science (JCNS), and the Heinz Maier-Leibnitz Zentrum (MLZ). Within this framework, a flexible and quickly interchangeable sample carrier system for small-angle neutron scattering (SANS) at the ESS was developed. In the present contribution, the development of a sample environment for the investigation of soft matter thin films with grazing-incidence small-angle neutron scattering (GISANS) is introduced. Therefore, components were assembled on an optical breadboard for the measurement of thin film samples under controlled ambient conditions, with adjustable temperature and humidity, as well as the optional in situ recording of the film thickness via spectral reflectance. Samples were placed in a 3D-printed spherical humidity metal chamber, which enabled the accurate control of experimental conditions via water-heated channels within its walls. A separately heated gas flow stream supplied an adjustable flow of dry or saturated solvent vapor. First test experiments proved the concept of the setup and respective component functionality.

Solvation Behavior of Poly(sulfobetaine)-Based Diblock Copolymer Thin Films in Mixed Water/Methanol Vapors

“…This chamber was connected to a custom-made gas-flow system, which enabled a precise control of the vapor composition while ensuring a stable ambient temperature. Details of the working principle of the gas-flow system are provided in the SI and in our previous publications. ,,, Kinetic ToF-NR data were recorded during water swelling and during methanol exchange, each for 2 h with a time resolution of 5.5 s. The obtained data were binned. Static measurements of the dry, swollen (in water vapor), and contracted (in water/methanol vapor) thin-film states between the dynamic processes took 45 min.…”

Technical Specification of the Small-Angle Neutron Scattering Instrument SKADI at the European Spallation Source

“…A kinematic mounting system will be installed in order to allow for an effective and speedy setup of the different experiments to be performed at SKADI. This kinematic mounting system will allow an off-instrument preparation of the experimental setup and several user groups have already developed corresponding sample environments [4][5][6]. This setup is designed to take up a load of up to 990 kg on the area of a EUR-pallet.…”

“…In addition, further practical requirements for performing experiments, such as sample area and environment, will be considered. Here, we want to highlight the extensive collaboration with user groups in order to develop state-of-the art sample environments [4][5][6].…”

Foam aging under free drainage analysed using associated operando techniques

“…A first cell was manufactured in the early 2000s and consisted of a Plexiglas cell with a quartz window allowing the study of foam at a single given height 50 . Since then, interest in this technique has continued to grow with new cells recently developed 51 . The technique has been employed to probe stimuli responsive foams 43,44 , foams stabilized by polymeric surfactants 45 , proteins 46 , or, more recently, nano-ions 48 .…”