De-mixing dynamics of a binary liquid system in a controlled-pore glass

The European Physical Journal E - The temperature-induced microphase separation of the binary liquid system iso-butyric acid+heavy water (iBA + D2O) in a mesoporous silica glass (CPG-10-75) of...     

Contrast variation in spin-echo small angle neutron scattering

The use of contrast variation in spin-echo small angle neutron scattering (SESANS) experiments is discussed for the case of colloidal structural investigation. On the basis of calculations for several model systems, we find that the contrast variation SESANS technique, in terms of the measured SESANS correlation function G(z), is not sensitive to the structural characteristics of colloidal suspensions consisting of particles with uniform scattering length density profiles. However, its ability to resolve structural heterogeneity, at both intra-colloidal and inter-colloidal length scales, is clearly demonstrated. The prospect of using this new technique to investigate structural information that is difficult to probe in other ways is also explored.     

Phase separation of a binary liquid in anodic aluminium oxide templates: a structural study by small angle neutron scattering

The radial nanostructure of the binary liquid triethylamine/water confined in 60 nm diameter independent cylindrical pores of anodic aluminium oxide membranes is studied by small angle neutron scattering. It is shown that composition inhomogeneities are present in the confined mixtures well below the bulk critical point. An analysis of the neutron scattering form factor reveals the existence of an adsorbed water layer of a few nanometers at the liquid/alumina interface, coexisting with a TEA-rich phase in the core.     

Phase transitions in 8CB liquid crystal confined to a controlled-pore glass: Deuteron NMR and small angle X-ray scattering studies

We present results of the deuteron nuclear magnetic resonance (NMR) and small-angle X-ray scattering (SAXS) study of ordering and phase transition behavior of octylcyanobiphenyl (8CB) liquid crystal confined to a controlled-pore glass (CPG) with nontreated and silanes-treated pore surfaces. The deuteron NMR spectra allowed to determine the degree of nematic liquid crystal ordering and also provided an indirect information on the confined 8CB smectic ordering via its influence on the nematic ordering. For the smectic phase these data are supplemented with measurements of the temperature dependence of the first-order SAXS diffraction pattern. The NMR results indicate that the average nematic and smectic order parameters of 8CB in the nontreated CPG are only weakly perturbed by the confinement. The SAXS data further suggest that in confined 8CB for both nontreated and silane-treated CPG a domainlike pattern appears in accordance with the Imry-Ma theorem.     

Light scattering and small angle neutron scattering experiments with an aggregating binary liquid mixture of critical composition

Results of light scattering and small angle neutron scattering experiments with a 2-butoxyethanol (2-C₄E₁)/D₂O mixture of critical composition (stoichiometric mole fraction of 2-C₄E₁x = 0.0598; critical temperature T_c (visual) = 42.714 °C) are reported. They are carried out with the aim to find out whether the temperature dependence of the correlation length ξ characterizing the extension of concentration fluctuations near T_c is different from that characterizing the size of aggregates of the 2-C₄E₁ molecules which appear to exist at temperatures away from T_c. The experiments show that the temperature dependence of ξ near T_c is the same as that away from T_c within the uncertainty of the measurements. – As a by-product of this study, neutron scattering data were collected corresponding to a wide range of values of the scaling variable x (3 < x < 2100; x = qξ q is the absolute value of the scattering vector). They are analysed in terms of the limiting form of the universal correlation scaling function gξ(x) = C₁x^?(2-η) to determine the value of the universal critical exponent η. A value of η = 0.039 ± 0.004 is found. It is considered consistent with the theoretically expected values.     

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.      

Structure and dynamics of water confined in a nanoporous sol-gel silica glass: a neutron scattering study

During recent years, the understanding of the modification of the structure and dynamics of water confined in different environments has been the focus of much interest in scientific research. This topic is in fact of great relevance in a lot of technological areas and, in living systems, essential water-related phenomena occur in restricted geometries in cells, and active sites of proteins and membranes, or at their surface. In this paper we report on the most recent up to date account of structural and dynamical properties of confined water in comparison with the bulk state. In particular, as far as structure is concerned, we present new neutron diffraction results on heavy water confined in a fully hydrated sol-gel silica glass (GelSil) as a function of the temperature. At low T, the nucleation of cubic ice superimposed to liquid water, already observed for water within Vycor glasses, is discussed. As far as the dynamics is concerned, we report results of a detailed spectroscopic analysis of diffusive relaxation and vibrational properties of water confined in nanopores of Gelsil glass, at different temperatures and hydration percentages, performed by our research group during recent years by means of incoherent quasi-elastic (IQENS) and inelastic (IINS) neutron scattering. IQENS spectra are analysed in the framework of the relaxing cage model (RCM). IINS spectra show the evolution of the one-phonon-amplitude weighted proton vibrational density of states (VDOS), Z(ω), when water loses its peculiar bulk properties and originates new structural environments due to its surface interactions.     

Time of flight grazing incidence small angle neutron scattering

Grazing incidence small angle neutron scattering (GISANS) overcomes the limitations of conventional small angle scattering with respect to extremely small sample volumes in the thin film geometry. In time of flight (TOF) mode neutrons with a broad range of wavelengths are used simultaneously and recorded as a function of their respective times of flight. The combination of both, TOF-GISANS, enables the simultaneous performance of several GISANS measurements, which differ in wavelength. As a consequence, within one measurement a full set of GISANS pattern related to different scattering vectors, different scattering depths and resolutions result. This allows the detection of nanostructures with a chemical sensitivity. The possibilities of TOF-GISANS are demonstrated by the simple example of polymer nano-dots located on top of a silicon surface. As probed with atomic force microscopy (AFM) the nano-dots exhibit a large characteristic nearest neighbour distance of 545 nm and a surface coverage of 28%. From the analysis of the wavelength dependent data in combination with AFM the mass density of the polymer nano-dots is determined to be equal to the bulk value. A comparison to common single wavelength GISANS experiments is shown.     

Absence of voids in fast neutron irradiated zirconium by small angle neutron scattering

Abstract

The aim of this research was to resolve a difference of opinion in the literature on the presence of voids in fast neutron irradiated zirconium. There is a great interest in the study of zirconium, since zirconium and its alloys are used extensively in modern power reactors, for example in the fuel rods as a containment material for enriched uranium. A polycrystalline sample of zirconium was irradiated in the HERALD reactor at 40°C with 10²⁰ fast neutrons per cm^?2. The neutron scattering from irradiated and unirradiated standard samples was studied over a wide Q range from 0.001 to 1.12 Å^?1 on a D11 Spectrometer at the ILL (France). The defect cross-section (the difference between the scattering of the standard zirconium crystal and irradiated crystal) was nearly flat as a function of Q (momentum transfer vector) with an average value of 8.5 mb/Str/atom. This indicates a point defect concentration of about 1.8%. Thus the absence of any small angle (Q dependent) defect scattering indicates that large damage regions (e.g. voids) are not produced in zirconium by fast neutron irradiation.     

Structure of Co-Zn ferrite ferrofluid: A small angle neutron scattering analysis

A hydrothermal synthesis route is used to synthesize nanomagnetic particles of Co_0.3Zn_0.7Fe₂O₄ ferrite ferrofluids with particle diameter ranging from 5.5–9 nm. XRD analysis shows the formation of a single phase spinel structure. EDX results confirm the stoichiometric composition of the cations. Small angle neutron scattering technique is used to determine the size and size distribution of Co_0.3Zn_0.7Fe₂O₄ ferrofluid. The sizes thus obtained are in the range of 5.4 to 8.4 nm. These results are in agreement with magnetic measurements.      

Effect of heat treatment on pore structure in nanocrystalline NiO: A small angle neutron scattering study

Nanocrystalline nickel oxide powders were calcined at 300, 600 and 900°C and pore structure evolution was followed by small angle neutron scattering (SANS). Pore size distributions at two widely separated size ranges have been revealed. Shrinkage of larger-sized pore with reduction in polydispersity has been observed with increasing heat treatment temperature. The pore structures at various heat treatment temperatures do not scale. This has been attributed to the grain boundary diffusion leading to an asymmetric shrinkage of the pores.      

A small angle neutron scattering study on the mixtures of pluronic L121 and anionic surfactant AOT

Small angle neutron scattering (SANS) experiments have been carried out on the micellar solutions containing mixtures of a hydrophobic triblock copolymer (L121, EO₅PO₆₈EO₅) and a hydrophobic anionic surfactant (AOT, sodium bis(2-ethylhexyl)sulphosuccinate) in water with varying ratio (R) of AOT to L121 for R = 0.15, 0.2, 0.3, 0.5 and 0.6. It is known that either L121 or AOT alone forms vesicles in water, but in the mixture with appropriate ratio of the two components a thermodynamically stable, isotropic solution of apparently small micelle-like aggregates is formed. We find that these micelles are prolate ellipsoidal.      

Polymer-mediated interactions of fluid membranes in a lyotropic lamellar phase: a small angle X-ray and neutron scattering study

Small angle X-ray and neutron scattering data on an effective three-component lamellar phase composed of water, a non adsorbing water-soluble polymer (polyvynilpyrolidone), fluid membranes, made from a mixture of a cationic surfactant (cetylpiridiumchloride) and a cosurfactant (hexanol), are presented for various membrane as well as polymer concentrations. The data are fitted with a recently proposed model which takes into account the geometry and the fluctuations of these periodic structures. This allows a quantitative study of the polymer contribution to the smectic compression modulus of the lamellar phase. Four different regimes of polymer confinement are expected. The associated variations in are compared to a recent theoretical model, which predicts the polymer-mediated contribution to the smectic compression modulus. Received 20 January 1998     

Magnetic field and pressure dependence of small angle neutron scattering in MnSi

We report small angle neutron scattering of spontaneous and magnetic field aligned components of the helical spin polarization in MnSi for temperatures T down to 0.35 K, at pressures p up to 21 kbar, and magnetic field B up to 0.7 T. The parameter range of our study spans the first order transition between helical order and partial magnetic order at p{c}=14.6 kbar, which coincides with the onset of an extended regime of non-Fermi liquid resistivity. Our study suggests that MnSi above p{c} is not dominated by the remnants of the first order transition at p{c}, but that an unidentified mechanism favors stabilization of a new ground state other than helical order.     

Investigation on pore structure and small-scale agglomeration behaviour in liquid phase sintered SiC using small angle neutron scattering

Mesoscopic density fluctuations in liquid phase sintered silicon carbide have been investigated using small angle neutron scattering (SANS). The increase in the additives results in the modification in the pore size distribution and to some extent the total porosity. SANS revealed a mass fractal nature of the agglomerated matrix microstructure. The fractal dimension of the matrix does not change appreciably with the additives although the upper cut-off value of the fractal decreases significantly with the increase in the additives. The liquid phase sintering due to the presence of additives helps to achieve higher level of densification. However, the agglomeration hinders achievement of the fully dense pellets.      

In-situ neutron scattering study of crystallization in a Zr-based bulk metallic glass

In this paper, we report the structure, optical, and gas-sensing properties of Co-doped ZnO nanocrystals prepared by a simple solvothermal route. The red-shift of the band-gap edge is attributed to a merging of donor and conduction bands due to Co doping. Photoluminescence (PL) spectra were used to study the dependence of doping on the deep-level emission, which show obvious enhanced blue-green emission after Co doping. Gas sensors were prepared and tested for the detection of C₂H₅OH in air. It is found that the Co-doped nanocrystals have a significantly better sensing performance than pure ZnO, which is comparable to the Au-functionalized ZnO sensors. We provide a possible explanation in terms of the sensing mechanism of the surface reaction process.     

Quasi-elastic neutron scattering study of dynamics in condensed matter

Quasi-elastic neutron scattering (QENS) technique, known to study stochastic motions has been successfully used to elucidate the molecular motions and physical properties related to them, in a variety of systems. QENS is a unique technique that provides information on the time-scale of the motion as well as the geometry of the motions. In this paper, results of some of the systems studied using the facility available at Dhruva, Trombay and other mega-facilities are discussed. Emphasis is given on the results obtained from three different systems studied using QENS, namely, (1) alkyl chain motions in monolayer protected metal clusters, (2) molecular motions of propane in Na-Y zeolitic systems and (3) the study of reorientational motions of liquid crystal innO.m series in different mesophases.     

Anisotropy and temperature dependence of small angle neutron scattering from silicon-oxide precipitates in silicon

Czochralski grown silicon crystals contain interstitially dissolved oxygen which diffuses on heating to form precipitates of silica. We have examined these precipitates by small angle neutron scattering (SANS) in the Q-range 0.05 Å^–1<Q<0.4 Å^–1. The obtained SANS patterns reveal pronounced anisotropic intensity distributions which resemble the symmetry of the host crystal. The SANS spectra show an anisotropic central peak at Q<0.1 Å^–1 due to the single particle shape and a number of weak intensities for larger Q-values. These weak side maxima are considered correlation peaks or quasi-elastic interference peaks. They show, however, an unexpected and distinct temperature dependence: with decreasing temperature below values of 220 K their intensity is lost slowly, but reversibly. At T = 50 K only the central peak from the single-particle scattering remains unchanged. Upon heating, the correlation peaks regain their former value of intensity and Q-position without any evidence of thermal hysteresis.     

Nature of the structural heterogeneity in SiH films by small angle neutron scattering

The density and small angle neutron scattering of a variety of silicon hydride films have been measured as function of heat treatment. Anode deposited samples have previously been shown to have a columnar morphology with a dominant column diameter of ～60 Å. This is confirmed and the new studies establish that the matrix separating the columns is of very low density - essentially comprising voids. The mechanism of hydrogen evolution during heat treatment depends on the void morphology. Both plasma deposited and sputtered films may be made which are structurally homogeneous on a scale of ? 10 Å.     

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.