D11 was conceived and designed by Konrad Ibel, Werner Schmatz and Tasso Springer and became operational in 1972 shortly after ILL’s first neutron beams became available. Soon after a high angle data bank (D11B) was added by Gernot Kostorz for studying diffuse scattering. The first few years were devoted to many pioneering experiments in the fields of polymers, materials, metallurgy as well as...
Following a period of strong development of the contrast variation method using H2O/D2O exchange on physical-chemical and readily available soluble protein samples,D11 hosted a number of challenging experiments in biology—in particular on protein-nucleic acid interactions. Important results were obtained on the inner structures of plant viruses, ribosomes and chromatin. A study of...
It was in September 1972 when Konrad Ibel and myself put a solution of sperm whale myoglobin into the sample chamber of D11. To our great surprise it was after a few seconds of irradiation by thermal neutrons – I think the A-selector was not yet in place – when a beautiful central peak of scattered neutron intensity emerged on the screen, the first picture of neutron small-angle scattering...
We will recap published and unpublished work initiated on D11, D17 and D1B with J.B. Hayter: what happens at low-q and high-q for common and uncommon ionic micelles made from self-assembled amphiphiles in a given solvent?
In the standard SAS range, the Hayter-Penfold decoupling procedure work well for all ionic micelles investigated as long as the chain length is not too short or too...
Wood is an abundant biological material with various technical applications ranging from sustainable building materials to advanced functional materials made of nanocelluloses. The structure of wood cell walls is hierarchical, consisting of well-oriented, elongated units from the molecular level to the macroscale. Our picture of the complex composite-like structure of wood cell walls and its...
Soon after the advent of High-Tc superconductors, it became clear that that important information could be obtained by observing the lattice of quantised flux lines in these and other unconventional and conventional superconductors. This meant that SANS scattering patterns contained Bragg peaks had to be analysed. I will compare the state of the art of early experiments with what is available...
The small-angle instruments at ILL have been instrumental for our soft matter research during the last 30 years. I will illustrate this with a number of research projects where SANS has been key in elucidating structural properties of various soft matter systems, covering diverse topics such as the formation of polymerlike micelles, the kinetics of the micelle-to-vesicle transition, gel...
Adding nanoparticles (NPs) to polymer solution or melt is an efficient strategy to improve the macroscopic polymer behavior (viscosity, mechanical reinforcement…) and design hybrid macromolecular materials with enhanced properties. Among the vast literature dealing with NPs and polymer, one fundamental question arises: do NPs modify the global and local polymer chain conformation? Such issue...
Small angle scattering is a really useful technique to understand the self-assembly of a range of N-functionalised dipeptides. These form micellar structures at high pH and gels at low pH. Gels with different properties can be formed by controlling the micellar species present prior to gelation, for example by changing the counter-ion, by the addition of salts or by a heat-cool cycle. To...
A magnetic field is one of the many tools that we can use to tune or adjust materials. In some cases, this is through the very direct coupling to atomic magnetic moments, giving rise to new structures. In other cases, the interaction is on the microscopic scale, for example, the rotation or growth of magnetic domains over a wide range of length scales. Some materials do not have direct...
The interface between rock matrix and pore space in sedimentary rocks is rough over seven orders of magnitude of the linear scale, from sub-nanometers (nearly molecular) to centimeters. Since the early 1980's, pore-matrix roughness has often been described using the framework of Mandelbrot's fractal geometry and the corresponding mathematical formalism for correlation functions; this...
Artefacts of interest in cultural heritage (CH) are often rare, precious, manifolds and complexes and their secrets are difficult to disclose.
The D11 instrument at Institut Laue Langevin (ILL) is a very unique instrument to investigate CH samples and their history. D11 uses: neutrons that are a no-destructive probe and the small angle neutron scattering (SANS) technique covering four decades...
To use the minimum q of a SANS instrument we require the longest collimation and detector distances combined with the longest wavelength. This combination maximizes how much gravity curves the neutron beam and how much the beam is spread due to the range of wavelengths. D11 is the only gravity limited SANS instrument in the world where at minimum q gravity prevents any transmission through the...
Self-assembled systems are generally highly dynamic structures characterized by molecular exchange, fluctuations and fusion/fission and morphological transitions. Examples include micelles formed by synthetic surfactants and block copolymers as well as lipid membranes. Despite their importance in technological and biomedical applications, the kinetic pathways associated with the formation and...
With regard to the increasing need for sustainable energy, developing strategies to exploit solar energy become more and more important. Inspired by natural systems it is highly promising to self-assemble building blocks into functional supramolecular units.
Electrostatic self-assembly leads to nanoscale shapes ranging from spheres and cylinders over vesicles to networks. Key to a targeted...
Dendrimers are synthetic macromolecules having a defined architecture. Starting from a trifunctional monomer (generation 0), subsequent generations are connected to this initial core from which in a treelike structure results. Small-angle neutron scattering (SANS) has been extremely useful for the characterization of these molecules since it allows us to change the contrast through mixtures of...
Motivated by the patented idea of using scCO2-microemulsions as a starting material for the production of polymer nanofoams [1], we developed a new high-pressure cell together with Ralf Schweins and Peter Lindner in 2006. We were able to demonstrate its functionality in a first test SANS experiment at D11 in March 2007. In this and a series follow-up experiments we could show that...
Linking polysaccharides and polypeptides together leads to fully biocompatible copolymers with unique properties for healthcare applications: not only they are fully biodegradable, but also they offer specific recognition and docking properties to membrane receptors of biological cells. Moreover, the two blocks can respond to external stimuli, such as pH, temperature, or the presence of...
Protein solutions can exhibit rather complex behavior, in particular at high concentrations, i.e. "crowding" conditions.
For a comprehensive understanding of the structures,
from the molecular level to oligomers to larger-scale structures arising, e.g., in phase separating systems,
small-angle scattering plays a crucial role. This is also the basis for the interpretation of the associated...
Deep eutectic solvents (DES) are promising novel solvents obtained through the complexation of a halide salt such as choline chloride with a hydrogen bond donor such as urea or glycerol, enabling them to be tuned for particular properties, including low toxicity and sustainability. They are of increasing interest to replace organic solvents in applications from synthesis to pharmaceutical...
Surfactant self-assembly is an important phenomenon in a wide range of processes and applications. SANS has played a central and key role in developing our understanding of surfactant self-assembly. From the early 1980’s D11 has been the leading and pioneering SANS instrument for such studies. Three key issues from some the early studies on D11, associated with micelle models, the...
Nanosuspensions are sub-micron-sized colloidal dispersions of nano-sized drug particles stabilised by surfactant and/or polymer. Nanosuspensions are of considerable interest as a means of solving the problems of poor water solubility and low bioavailability exhibited by many drugs, and which pose significant challenges for the preparation of a medicine for patient use. Despite the fact that...
I will try to tell you a story about our hour after hour life – with mixture of stress and pleasure to be by the side of this beautiful leading machine, building a special relationship as D11 co-users, with different colleagues along my career. It actually started here!
This should cover different science cases, where D11 was useful in different ways: polymer gels, stretched...
The striking difference in the scattering length density of H and D offers a chance to vary or tune the neutron scattering contrast of selected components in complex systems while retaining the chemistry of the systems. Such contrast variation in turn provides unique opportunities for structural analysis in the field of Soft Matter not accessible to other scattering techniques like for...
Quasicrystals are a peculiar state of order, which is fundamentally different from classical ordered crystalline states. Discovered in 1982 for MnAl-alloys, it has since then been found for more than 100 different metal alloys.
In a 2009 D11 summer nightshift we discovered a micellar phase showing an unusual SANS-pattern with 12-fold rotational symmetry. When published in 2011, it was the...
Being among the first users of D11, I will give during my talk an outlook of the topics I investigated with this SANS camera. My first use of D11 dates back to Mai 1975 for studying the chain conformation in a crystalline polymer, namely isotactic polystyrene (iPS). Unlike polyethylene, that was studied simultaneously by other group of scientists, iPS did not display any isotopic segregation...
Polyelectrolytes are a class of material that have appealed to researchers in many different areas owing to their versatility and potential applications. The existing studies mostly deal with their behaviour in aqueous solutions due to their lack of solubility in other media. Here we have utilized carboxymethyl cellulose (CMC), which is widely available as a sodium salt, NaCMC. The solubility...
The active substance resolution in oral application of badly soluble drugs of the BCS classes 2 and 4 depends on the drug interaction with micelles and liposomes formed from bile and pharmaceutical formulation in the duodenum part of the small intestine. During the passage of the second duodenum half, i.e. after bile influx, the native and drug lipid nanoparticles depict a sequence of...
Modular targeting materials bearing a specific ligand head can supply a cell or tumor receptor recognition to radiotherapy enhancers, hydrophobic drugs (BCS classes 2, 4) or mRNA, entrapped in nanoscaled drug carriers, e.g. liposomes, micelles and polymer particles. This drug / co-drug complex concept requires the synthesis of special modular targeting materials.
We synthesized targeting...
Indirect radiation therapy IRT of cancer uses heavy metals as specific absorbers and local converters of external radiation into cell toxic secondary products, e.g. free radicals. The IRT principle can be applied with neutron and hard X-ray/ gamma photon radiation. Both can be focused by tomographic irradiation methods. The local radiotherapy effect can be enforced, if the heavy element can be...
Cyclodextrins (CD) are cyclic oligosaccharides formed by α-(1-4)-D-glucopyranoses linked units. Their unique shape and the presence of a cavity provide particular physicochemical properties, including the ability to form host-guest complexes [1]. Cyclodextrin-surfactants host-guest complexes are a flourishing research field due to the availability and diversity of surfactants and the tendency...
Prohibitins (PHB) are highly conserved heterodimeric proteins composed of two subunits PHB1 and PHB2 arranged to make a multimeric ring at the inner mitochondrial membrane [1]. They play a crucial role in premature cellular ageing, tumour suppression, cell cycle regulation, apoptosis, and mitochondrial homeostasis via their function in the intermembrane space (IMS) of mitochondria (between the...
I will try to tell you a story about our hour after hour life – with mixture of stress and pleasure to be by the side of this beautiful leading machine, building a special relationship as D11 co-users, with different colleagues along my career. It actually started here!
This should cover different science cases, where D11 was useful in different ways: polymer gels, stretched...
Whoever tried to prepare homemade mayonnaise, knows how much energy input the formation of water/oil emulsions require. In addition to that, in order to provide stability to the emulsion, the presence of components which stabilize the system are required. This role is played by some of proteins and the lecithin contained in the egg yolk, for the case of mayonnaise. In most of other
emulsions,...
M-type barium hexaferrites (BaM) has attract a lot of attention due to their multiferroic and other functional properties [1, 2]. We have investigated the doped M-Type Barium hexafer-rite, BaFe12-xTxO19, where T = Sc with x = 2.5. The structural and magnetic properties were characterized using XRD, VSM and Neutron diffraction measurements. XRD analysis reveals that the samples are in single...
We outline a modeling scheme for calculating the scattering profiles from complex biological samples, such as multi-domain membrane proteins with intrinsically disordered regions and embedded in phospholipid nanodiscs. The scheme bases itself on a hybrid of classical form factor based modeling and the well known spherical harmonics-based formulation of small-angle scattering amplitudes.
We...
Biological, polymer and medical samples may depict a wide particle size spectrum from nm to µm scale. The particle structure in solution can be studied without radiation damage by SANS up to 1 µm size (ILL-D11, 30m distance, 15Å), and at high intensity by SAXS. The particle size distribution is available by dynamic light scattering DLS, while this requires with concentrated original samples of...
50 YEARS OF D11
Poster Abstract
Introduction
The newly developed Polyion complex (PIC) micelles have unparalleled significance in the
construction of functionalized and ordered mesoporous materials. MesoPIC micelles are
fabricated through the electrostatic complexation between a charged double hydrophilic block
copolymer (DHBC) and an oppositely charged polyelectrolyte. The...
Activated carbons are among the most widely employed materials in catalysis, either as supports or as catalysts on their own. The reasons of their success are mainly their low cost and their elevated specific surface area (SSA), which is enlarged by the activation process (i.e., the treatment of a char precursor at high temperature in the presence of either a chemical agent, e.g. phosphoric...
Protein solutions can exhibit rather complex behavior, in particular at
high concentrations, i.e. "crowding" conditions. For a comprehesive understanding of the structures,from the molecular level to oligomers to larger-scale structures arising, e.g., in phase separating systems,small-angle scattering plays a crucial role. This is also the basis for the interpretation of the associated...
Soft colloids are ubiquitous in synthetic and biological material as e.g. vesicles, dendrimers, microgels, polymer-grafted nanoparticles, micelles, star polymers and certain proteins. They display a dual character between a polymer and the archetypical hard sphere colloid. Due to this hybrid nature, soft colloids macroscopically show interesting structural [1] and dynamical [2] properties...
Pharmaceutical nanocarriers are complexes composed of frame materials, e.g. lipids or polymers, and medically active materials, such as bio-chemical drugs or biological agents, e.g. proteins or mRNA. The structure is the key to the medical application and safety. The formulation depends on the application pathway, which may be oral (tablets, capsules), pulmonary (inhalation), intramuscular...
Bio-energy converting membrane proteins couple the transport of material across a membrane, e.g. protons, with the reversible formation or cleavage of an energy rich chemical bond (ATP). Thus local energy is stored and available in the cell lumen or tissue, by temporal energized protein state.
The most common energy transfer protein ATP-Synthase (M = 500 000) and its catalytic head F1ATPase...
Nanoparticles circulating in the human blood depict a protein corona [Tenzer et al.]. This principle can be used for site specific drug targeting by receptor recognition after attachment of an artificial specific protein corona to drug loaded nanoparticles, lipoplexes, liposomes and polymers, which contain a protein-binding anchor component, and the therapeutic drug or mRNA.
We have studied...
Mixtures of simple molecules may lead to complex systems with unforeseen properties of particular interest such as reactivity or solubility. This is the case of aqueous solutions of alcohol and oil, typically found in all kind of liquors, cosmetics or solvents for liquid-liquid extraction.
The archetypal case of this family is the ternary mixture of water, ethanol and octanol. Its phase...
The understanding of protein crystallization is of great interest for many areas of biological research. Examples include drug delivery of crystalline substrates and structural biology, which relies on diffraction-quality crystals. Some crystallization pathways are characterized by a one-step process and can be described by classical nucleation theory (CNT). However, for different systems,...
Elastin-like peptides (ELPs) mimic the hydrophobic repeat units of elastin, a protein rendering biological tissues such as lung, ligaments and blood vessels elastic. ELPs collapse hydrophobically upon crossing a lower critical solution temperature (LCST). Due to their stimulus-responsive properties, ELPs are of interest for many application areas including biomaterials, protein purification...
In quantum materials, interactions between unpaired electrons can lead to the formation of complex magnetization textures, that themselves generate novel quantum effects ripe for exploitation in applications. When the periodicity of these textures are incommensurate with the host crystal lattice, SANS can play the key role in both their observation, and the efficient characterization of their...
