Small-angle scattering, and its neutron expression small-angle neutron scattering (SANS), has developed into an invaluable tool for the investigation of microscopic and mesoscopic structures in ...recent decades ...
The KWS‐1 small‐angle neutron scattering (SANS) instrument operated by the Jülich Centre for Neutron Science (JCNS) at the research reactor FRM II of the Heinz Maier‐Leibnitz Zentrum in Garching near ...Munich has been recently upgraded. The KWS‐1 instrument was updated, from its active collimation apertures to the detector cabling. Most of the parts of the instrument were installed for the first time, including a broadband polarizer, a large‐cross‐section radio‐frequency spin flipper, a chopper and neutron lenses. A custom‐designed hexapod in the sample position allows heavy loads and precise sample positioning in the beam for conventional SANS experiments as well as for grazing‐incidence SANS under applied magnetic field. With the foreseen in situ polarization analysis the main scientific topic of the instrument tends towards magnetism. The performance of the polarizer and flipper was checked with a polarized 3He cell at the sample position. The results of these checks and a comparison of test measurements on a ferrofluid in a magnetic field with polarized and nonpolarized neutrons are presented.
Here we present an approach to measure dynamic membrane properties of phospholipid membranes close to an interface. As an example we show results of the membrane dynamics of a phospholipid membrane ...multilayer-stack on a solid substrate (silicon). On this sample we were able to measure local interaction and friction parameters using Grazing Incidence Neutron Spin Echo Spectroscopy (GINSES), where an evanescent neutron wave probes the fluctuations close to a rigid interface. With this method it is possible to access length scales in the nano to micrometer region as well as energies in the μeV range. Using a new neutron resonator structure we achieved the required intensity gain for this experiment. During our investigations we found an excitation mode of the phospholipid membrane that has not been reported previously and only became visible using the new methodology. We speculate that the energy transported by that undulation can also serve to distribute energy over a larger area of the membrane, stabilizing it. This new methodology has the capability to probe the viscoelastic effects of biological membranes, becoming a new tool for tribology on the nanoscale and has allowed the observation of the hitherto invisible property of phospholipid membranes using neutrons.
The reorientation of lamellae and the dependence of the lamellar spacing, D lam, on polymer volume fraction, ϕP, D lam ∝ ϕP –β, in diblock copolymer thin films during solvent vapor annealing (SVA) ...are examined by combining white light interferometry (WLI) and grazing-incidence small-angle X-ray scattering (GISAXS). A thin film of lamellae-forming poly(styrene-b-butadiene) prepared by spin-coating features lamellae of different orientations with the lamellar spacing depending on orientation. During annealing with ethyl acetate (EAC) vapor, it is found that perpendicular lamellae behave differently from parallel ones, which is due to the fact that their initial lamellar thicknesses differ strongly. Quantitatively, the swelling process is composed of three regimes and the drying process of two regimes. The first two regimes of swelling are associated with a significant structural rearrangement of the lamellae; i.e., the lamellae first become thicker, and then perpendicular and randomly oriented lamellae vanish, which results in a purely parallel orientation at the end of the swelling process. The rearrangement is attributed to the increase of mobility of the polymer chains imparted by the solvent and to a decrease of total free energy of the thin film. In the third regime of swelling, the scaling exponent is found to be β = −0.32. During drying, the deswelling is nonaffine which may be a consequence of the increase of nonfavorable segmental interactions as the solvent is removed.
Over the decades, small-angle neutron scattering has became a definitive method for structural investigation on the mesoscale between a few Angstrom up to a few 100 nm. This makes it an indispensable ...tool for non-destructive material investigations in fields ranging from chemistry and biology, over material sciences to solid state physics, especially taking into account the fundamental nature of neutrons, which makes it possible to probe different isotopes and, therefore, enhance contrast by choosing an appropriate isotope distribution or to probe the spin state of the investigated materials. This Special Issue is dedicated to elucidate the advances made with SANS over the last few years, which includes new instrumentation, sample environment and experimental control, as well as novel approaches and experimental techniques. The ideas and approaches collected here will serve both the experienced experimenter as well as the novice to appraise whether their specific experimental setup is feasible with new ideas.
In any neutron scattering experiment the measurement of the position of the scattered neutrons and their respective velocities is necessary. In order to do so, a position sensitive detector as well ...as a way to determine the velocities is needed. Measuring the velocities can either be done by using only a single wavelength and therefore velocity or by creating pulses, where the start and end time of each pulse is known and registering the time of arrival at the detector, which is the case we want to consider here. This pulse shaping process in neutron scattering instruments is usually done by using a configuration of several choppers. This set of choppers is then used to define both the beginning and the end of the pulse. Additionally there is of course also a selection in phase space determining the final resolution that can be achieved by the instrument. Taking into account the special requirements of a specific instrument, here a small-angle neutron scattering instrument, creates an additional set of restrictions that have to be taken into account. In this manuscript a chopper configuration for two possible settings, namely a maximum flux and a high-resolution mode will be presented.
We investigate the cononsolvency effect of poly(N-isopropylacrylamide) (PNIPAM) in mixtures of water and methanol. Two systems are studied: micellar solutions of ...polystyrene-b-poly(N-isopropylacrylamide) (PS-b-PNIPAM) diblock copolymers and, as a reference, solutions of PNIPAM homopolymers, both at a concentration of 20 mg/mL in D2O. Using a stopped-flow instrument, fully deuterated methanol was rapidly added to these solutions at volume fractions between 10 and 20%. Time-resolved turbidimetry revealed aggregate formation within 10–100 s. The structural changes on mesoscopic length scales were followed by time-resolved small-angle neutron scattering (TR-SANS) with a time resolution of 0.1 s. In both systems, the pathway of the aggregation depends on the content of deuterated methanol; however, it is fundamentally different for homopolymer and diblock copolymer solutions: In the former, very large aggregates (>150 nm) are formed within the dead time of the setup, and a concentration gradient appears at their surface in the late stages. In contrast, the growth of the aggregates in the latter system features different regimes, and the final aggregate size is ∼50 nm, thus much smaller than for the homopolymer. For the diblock copolymer, the time dependence of the aggregate radius can be described by two models: In the initial stage, the diffusion-limited coalescence model describes the data well; however, the resulting coalescence time is unreasonably high. In the late stage, a logarithmic coalescence model based on an energy barrier which is proportional to the aggregate radius is successfully applied.
Lipid-based nanoparticles, also called vesicles or liposomes, can be used as carriers for drugs or many types of biological macromolecules, including DNA and proteins. Efficiency and speed of cargo ...delivery are especially high for carrier vesicles that fuse with the cellular plasma membrane. This occurs for lipid mixture containing equal amounts of the cationic lipid DOTAP and a neutral lipid with an additional few percents of an aromatic substance. The fusion ability of such particles depends on lipid composition with phosphoethanolamine (PE) lipids favoring fusion and phosphatidyl-choline (PC) lipids endocytosis. Here, we examined the effects of temperature, ionic strength, osmolality, and pH on fusion efficiency of cationic liposomes with Chinese hamster ovary (CHO) cells. The phase state of liposomes was analyzed by small angle neutron scattering (SANS). Our results showed that PC containing lipid membranes were organized in the lamellar phase. Here, fusion efficiency depended on buffer conditions and remained vanishingly small at physiological conditions. In contrast, SANS indicated the coexistence of very small (~50 nm) objects with larger, most likely lamellar structures for PE containing lipid particles. The fusion of such particles to cell membranes occurred with very high efficiency at all buffer conditions. We hypothesize that the altered phase state resulted in a highly reduced energetic barrier against fusion.
Small-K Advanced DIffractometer (SKADI is a Small-Angle Neutron Scattering (SANS) instrument to be constructed at the European Spallation Source (ESS). SANS instruments allow investigations of the ...structure of materials in the size regime between Angstroms up to micrometers. As very versatile instruments, they usually cater to the scientific needs of communities, such as chemists, biologists, and physicists, ranging from material and food sciences to archeology. They can offer analysis of the micro- and mesoscopic structure of the samples, as well as an analysis of the spin states in the samples, for example, for magnetic samples. SKADI, as a broad range instrument, thus offers features, such as an extremely flexible space for the sample environment, to accommodate a wide range of experiments, high-flux, and optimized detector-collimation system to allow for an excellent resolution of the sample structure, short measurement times to be able to record the internal kinetics during a transition in the sample, as well as polarized neutron scattering. In this manuscript, we describe the final design for the construction of SKADI. All of the features and capabilities presented here are projected to be included into the final instrument when going into operation phase.
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.
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