A small angle neutron scattering (SANS) experiment using very cold neutrons (VCN)

This paper describes the results of SANS measurements of small samples using the very cold neutron (VCN) beam of the PF2 instrument at the Institut Laue Langevin (ILL), France. In addition to a classical SANS pinhole collimation, the experiment used a polarizing supermirror as a monochromator and a magnetic sextupole lens to focus the neutron beam in order to gain intensity and avoid any material in the neutron beam besides the sample.     

Nano-meter-sized domain formation in lipid membranes observed by small angle neutron scattering

Using a contrast matching technique of small angle neutron scattering (SANS), we have investigated a phase separation to liquid-disordered and liquid-ordered phases on ternary small unilamellar vesicles (SUVs) composed of deuterated-saturated, hydrogenated-unsaturated phosphatidylcholine lipids and cholesterol, where the equilibrium size of these domains is constrained to less than 10nm by the system size. Below a miscibility temperature, we observed characteristic scattering profiles with a maximum, indicating the formation of nano-meter-sized domains on the SUVs. The observed profiles can be described by a multi-domain model rather than a mono-domain model. The nano-meter-sized domain is agitated by thermal fluctuations and eventually ruptured, which may result in the multi-domain state. The kinetically trapped nano-meter-sized domains grow to a mono-domain state by decreasing temperature. Furthermore, between the miscibility and disorder-order transition temperature of saturated lipid, the integrated SANS intensity increased slightly, indicating the formation of nano-meter-sized heterogeneity prior to the domain nucleation.     

Coarsening of antiferromagnetic domains in multilayers: the key role of magnetocrystalline anisotropy

The domain structure of an antiferromagnetic superlattice is studied. Synchrotron M?ssbauer and polarized neutron reflectometric maps show micrometer-size primary domain formation as the external field decreases from saturation to remanence. A secondary domain state consisting mainly of at least 1 order of magnitude larger domains is created when a small field along the layer magnetizations induces a bulk-spin-flop transition. The domain-size distribution is reproducibly dependent on the magnetic prehistory. The condition for domain coarsening is shown to be the equilibrium of the external field energy with the anisotropy energy.     

Small angle neutron scattering observation of chain retraction after a large step deformation

The process of retraction in entangled linear chains after a fast nonlinear stretch was detected from time-resolved but quenched small angle neutron scattering (SANS) experiments on long, well-entangled polyisoprene chains. The statically obtained SANS data cover the relevant time regime for retraction, and they provide a direct, microscopic verification of this nonlinear process as predicted by the tube model. Clear, quantitative agreement is found with recent theories of contour length fluctuations and convective constraint release, using parameters obtained mainly from linear rheology. The theory captures the full range of scattering vectors once the crossover to fluctuations on length scales below the tube diameter is accounted for.     

Detection of submicron-sized raft-like domains in membranes by small-angle neutron scattering

Using coarse grained models of heterogeneous vesicles we demonstrate the potential for small-angle neutron scattering (SANS) to detect and distinguish between two different categories of lateral segregation: 1) unilamellar vesicles (ULV) containing a single domain and 2) the formation of several small domains or “clusters” (~10 nm in radius) on a ULV. Exploiting the unique sensitivity of neutron scattering to differences between hydrogen and deuterium, we show that the liquid ordered (lo) DPPC-rich phase can be selectively labeled using chain deuterated dipalymitoyl phosphatidylcholine (dDPPC), which greatly facilitates the use of SANS to detect membrane domains. SANS experiments are then performed in order to detect and characterize, on nanometer length scales, lateral heterogeneities, or so-called “rafts”, in ~30 nm radius low polydispersity ULV made up of ternary mixtures of phospholipids and cholesterol. For 1:1:1 DOPC:DPPC:cholesterol (DDC) ULV we find evidence for the formation of lateral heterogeneities on cooling below 30 °C. These heterogeneities do not appear when DOPC is replaced by SOPC. Fits to the experimental data using coarse grained models show that, at room temperature, DDC ULV each exhibit approximately 30 domains with average radii of ~10 nm.     

Small angle neutron scattering at very high time resolution: Principle and simulations of ‘TISANE’

The time resolution of SANS experiments is generally limited by frame overlap to some ms. We report on a new time-resolved stroboscopic SANS method, called TISANE, offering μs time resolution without a major sacrifice in intensity by making use of very large frame overlap. We may explore a new field in neutron scattering and complement the emerging field of time resolved small angle X-ray scattering. Here we discuss the principle of TISANE, its mathematical treatment and its limitations.     

Shear-induced ordering of lamellar and gyroid structures observed in a nonionic surfactant/water system

The shear-induced ordering of lamellar and gyroid structures of a nonionic surfactant C₁₆E₇/D₂O system in a Couette shear cell ( 0.001 < < 10 s^-1, : shear rate) has been investigated by using a small angle neutron scattering technique. In the lamellar phase, the steady shear flow having > 0.01 s^-1 suppresses undulation fluctuations of lamellae (Maxwell effect). This suppression of fluctuations brings two effects; 1) shear-induced lamellae ordering toward a parallel orientation and 2) obstruction of a lamellar↦gyroid transition. It is quite interesting to note that there is a characteristic shear rate range ( 0.01 < < 0.3 s^-1), where both effects take place. We have also investigated the shear effects on the gyroid phase. Below the characteristic shear rate range, the gyroid structure keeps three-dimensional network lattice, while above the characteristic shear rate range, the gyroid structure transforms to the parallel orientation lamellae (shear-induced gyroid-lamellar transition). Thus the shear flow having the characteristic shear rate plays very important roles in shear ordering phenomena. Received 26 June 2000 and Received in final form 12 January 2001     

Coarsening in a driven Ising chain with conserved dynamics

We study the low-temperature coarsening of an Ising chain subject to spin-exchange dynamics and a small driving force. This dynamical system reduces to a domain diffusion process, in which entire domains undergo nearest-neighbor hopping, except for the shortest domains-dimers-which undergo long-range hopping. This system exhibits anomalous ordering dynamics due to the existence of two characteristic length scales: the average domain length L(t) approximately t(1/2) and the average dimer hopping distance l(t) approximately square root[L(t)] approximately t(1/4). As a consequence of these two scales, the density of short domains decays as t(-5/4), instead of the t(-3/2) decay that would arise from pure domain diffusion.     

Probing polymer nanocomposite morphology by small angle neutron scattering

Polyamide nanocomposite films were prepared from nanometer-sized silica particles having particle radius of gyration (R _g) of about 66 Å and trimesoyl chloride-m-phenylene diamine-based polyamides having macromolecular units of about 100–140 Å. The nanoscale morphology of the samples was characterized using small angle neutron scattering (SANS). SANS reveals that silica nanoparticles interact well with the polyamide units only at limited silica loading.     

Modifications of the mesoscopic structure of cellulose in paper degradation

Paper is the main component of a huge quantity of cultural heritage. It is primarily composed of cellulose that undergoes significant degradation with the passage of time. By using small angle neutron scattering (SANS), we investigated cellulose's supramolecular structure, which allows access to degradation agents, in ancient and modern samples. For the first time, SANS data were interpreted in terms of water-filled pores, with their sizes increasing from 1.61 nm up to 1.97 nm in natural and artificially aged papers. The protective effect of gelatine sizing was also observed.     

A kinetics study of vacancy cluster evolution under VVER-type reactor condition

The vacancy clusters (VC) evolution in the neutron-irradiated VVER-type reactor pressure vessel steels is investigated, beginning at the nucleation stage and finishing in the coarsening stage. For this, characteristic VVER-type reactor conditions are considered. VC evolution in the nucleation stage is analysed on the basis of the computer simulation data. During the deterministic and the coarsening stage, elastic interaction between iron matrix and VC is accounted, that provides the stability of the peak of the size distribution function under the condition of increasing neutron fluence in correspondence to the experiments. The results are compared with the results of SANS experiments which were carried out on specimens irradiated at surveillance positions of VVER reactors. The presented approach may be used for analyses of the small inhomogeneities (about 1 nm) in the irradiated damage structure of the VVER-type steels.     

Small angle neutron scattering and small angle X-ray scattering studies of platinum-loaded carbon foams

The morphology of carbon nanofoam samples comprising platinum nanoparticles dispersed in the matrix was characterized by small angle neutron scattering (SANS) and small angle X-ray scattering (SAXS) techniques. Results show that the structure of pores of carbon matrix exhibits a mass (pore) fractal nature and the average radius of the platinum particles is about 2.5 nm. The fractal dimension as well as the size distribution parameters of platinum particles varies markedly with the platinum content and annealing temperature. Transmission electron micrographs of the samples corroborate the SANS and SAXS results.      

Small angle neutron scattering study of pore microstructure in ceria compacts

Ceria powders were prepared by gel combustion process using cerium nitrate and hitherto unexplored amino acids such as aspartic acid, arginine and valine as fuels. The powders have been characterized by X-ray and laser diffraction. Cold pressed compacts of these powders have been sintered at 1250°C for 2 h. Internal pore microstructure of the sintered compacts has been investigated by small angle neutron scattering (SANS) over a scattering wave vector q range of 0.003–0.17 nm⁻¹. The SANS profiles indicate surface fractal morphology of the pore space with fractal dimensionality lying between 2.70 and 2.76.      

Characterization of nanoparticles of lidocaine in w/o micro emulsions using small-angle neutron scattering and dynamic light scattering

Microemulsions (MEs) are of special interest because a variety of reactants can be introduced into the nanometer-sized aqueous domains, leading to materials with controlled size and shape [1,2]. In the past few years, significant research has been conducted in the reverse ME-mediated synthesis of organic nanoparticles [3,4]. In this study, a w/o ME medium was employed for the synthesis of lidocaine by direct precipitation in w/o microemulsion systems: water/isopropylpalmitat/Tween80/Span80. The particle size as well as the location of nanoparticles in the ME droplet were characterized by means of dynamic light scattering (DLS) and small angle neutron scattering (SANS). It is observed that lidocaine precipitated in the aqueous cores because of its insolubility in water. Hydrodynamic radius and gyration radius of microemulsion droplets were estimated as ∼15 nm and ∼4.50 nm from DLS and SANS respectively. Furthermore, different size parameters obtained by DLS and SANS experiments were compared     

Small angle neutron scattering from micellar solutions

Small angle neutron scattering (SANS) is an ideal tool for studying structures of macromolecules and colloidal solutions. A number of micellar solutions have been studied in our laboratory using a home built SANS spectrometer. This paper gives an introduction to the technique of SANS and gives a brief survey of the results obtained at Trombay.     

Antiferromagnetic domains in nickel oxide by magnetic neutron laue diffraction

Two kinds of domains had been observed in antiferromagnetic nickel oxide: T-domains, associated with the four 〈111〉 propagation vectors and S-domains, associated with the three equivalent antiferromagnetic directions within a T-domain. Taking advantage of the direct interaction of neutrons with the arrangement and direction of magnetic moments, the T and S antiferromagnetic domain distributions are investigated in several single crystal samples by magnetic neutron Laue diffraction (MNLD). The T-domain behaviour when a stress is applied is qualitatively investigated. In white beam a direct topographic observation and identification of T-domains are presented. By simultaneously measuring the relative intensities of magnetic Bragg reflections from a sample with preferential domain population it is possible to confirm the direction of sublattice magnetization which had been obtained by an optical method. The S-domain distribution is studied as a function of the magnetic field on the one hand, and as a function of time on the other. This last phenomenon is very similar to the well-known magnetic after-effect which occurs in most ferromagnets. It is concluded that MNLD could be a very valuable technique to investigate many topics of magnetism.     

Vortex imaging in Co-doped BaFe2As2

We review superconducting vortex imaging in Co-doped BaFe₂As₂ by Bitter decoration and small-angle neutron scattering (SANS). At all measured fields a highly disordered vortex configuration is observed, which is attributed to strong pinning. Further support of this conclusion comes from the absence of a Meissner rim in decoration images obtained close to the sample edge. The evolution of the SANS scattering vector with increasing applied field indicates vortex lattice domains of (distorted) hexagonal symmetry. This is consistent with the decoration images which show small, six fold coordinated ordered vortex domains. The SANS scattered intensity is found to decrease rapidly with increasing field, exceeding the rate expected from estimates of the upper critical field. This is consistent with the large degree of vortex “lattice” disorder.     

Accuracy of stress measurement by Laue microdiffraction (Laue‐DIC method): the influence of image noise,calibration errors and spot number

Laue microdiffraction, available at several synchrotron radiation facilities, is well suited for measuring the intragranular stress field in deformed materials thanks to the achievable submicrometer beam size. The traditional method for extracting elastic strain (and hence stress) and lattice orientation from a microdiffraction image relies on fitting each Laue spot with an analytical function to estimate the peak position on the detector screen. The method is thus limited to spots exhibiting ellipsoidal shapes, thereby impeding the study of specimens plastically deformed. To overcome this difficulty, the so‐called Laue‐DIC method introduces digital image correlation (DIC) for the evaluation of the relative positions of spots, which can thus be of any shape. This paper is dedicated to evaluating the accuracy of this Laue‐DIC method. First, a simple image noise model is established and verified on the data acquired at beamline BM32 of the European Synchrotron Radiation Facility. Then, the effect of image noise on errors on spot displacement measured by DIC is evaluated by Monte Carlo simulation. Finally, the combined effect of the image noise, calibration errors and the number of Laue spots used for data treatment is investigated. Results in terms of the uncertainty of stress measurement are provided, and various error regimes are identified.     

Form-factors for different aggregation models of micelles

Spherical micelles in ionic micellar solutions, often aggregate to form spherical, cylindrical or chain-like aggregates on addition of salt to the solution. It is known that the technique of small angle neutron scattering (SANS) can be used to distinguish spherical and cylindrical aggregates. To examine if SANS can be used to distinguish the latter two aggregation processes, we have calculated the angular distribution of scattered neutrons from 0.002 M CTAB solutions. These calculations show that aggregation of CTAB micelles results in large changes in SANS spectra. The shapes of SANS spectra are different for the above three types of aggregates, suggesting that technique of SANS can indeed be used to distinguish the three aggregation processes. The size of the aggregate can also be obtained from such studies.     

Vortex lattice transitions in YNi2B2C

We have performed extensive small-angle neutron scattering (SANS) diffraction studies of the vortex lattice in single crystal YNi₂B₂C for B‖c. High-resolution SANS, combined with a field-oscillation vortex lattice preparation technique, allows us to separate Bragg scattered intensities from two orthogonal domains and accurately determine the unit cell angle, β. The data suggest that upon increasing field there is a finite transition width where both low- and high-field distorted hexagonal vortex lattice phases, mutually rotated by 45°, coexist. The smooth variation of diffracted intensity from each phase through the transition corresponds to a redistribution of populations between the two types of domains.