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Structural analysis in the range of characteristic sizes from 1 nm to ~1.5 µm was performed for SiO2–TiO2 aerogels prepared in supercritical CO2, isopropanol, hexafluoroisopropanol, or methyl-tert-butyl ether using small-angle X-ray scattering and neutron scattering complementary methods. A two-level model that accounts for scattering by individual inhomogeneities and their aggregates, which have fractal properties, satisfactorily describes the aerogel structures over the entire range of scales. It is shown for the first time that the titania concentration is the key factor in the small-angle neutron and X-ray scattering by SiO2–TiO2 aerogels. The phase composition of an aerogel does not significantly affect the aerogel structure in the range of scales from 1 nm to ~1.5 µm, as probed by small-angle X-ray and neutron scattering. [ABSTRACT FROM AUTHOR]

Fullerenols C60(OH)X and C70(OH)X (X ∼ 30) have been studied in aqueous solutions at the concentrations 0.05–22wt% by X-ray and neutron scattering and using modeling hydroxyls' arrangements on carbon cages to explain the molecular assembly defined by hydrophobic and hydrophilic interactions of molecules. In the case of C60 quantum chemical calculations minimizing molecular energy for different configurations of OH-groups on the carbon cages showed their preferred localization at C60 spheroids' equatorial zone and at the opposite poles. However, less symmetric hydroxyls' localization on C70 molecules was found since hydroxyls do not create closed chains on them. As a result, the molecules C60(OH)X are associated into primary chain-like aggregates (∼20 units, few nanometers in size) more likely in water than the fullerenols C70(OH)X forming similar groups of lower aggregation degree. For C60(OH)X and C70(OH)X the peculiarities in hydroxyls' grafting affected a coordination of primary groups integrated into secondary and tertiary structures at the distances R ∼ 5 nm and R ∼ 30 nm at the concentrations C > 5wt% and C > 10wt%, respectively. The discovered mechanism of fullerenols' assembly in water will facilitate their use in chemistry and biomedicine. [ABSTRACT FROM AUTHOR]

The parameters of the mesostructure of amorphous zirconium dioxide and their evolution at different stages of heat treatment are determined by small-angle neutron scattering. Particles of amorphous zirconium dioxide, which form mass fractals with the dimension Dv = 2.21, are rearranged into surface fractals with a surface dimension of Ds = 2.52 upon annealing at a temperature of 400°C or higher. In the resulting system, a shell with a fractal structure is formed over a dense core (a cluster of nanoparticles of zirconium dioxide with a constant density). Transformation of the fractal system from a mass fractal into a surface one is characterized by the appearance of a core, and its growth is due to the crystallization of hydrated zirconia particles at high temperatures. A model for the formation of a fractal particle, implying the existence of a core–shell surface fractal system, is proposed. The characteristic radius of ZrO2 nanoparticles increases from 14 to 200 Å with an increase in the annealing temperature from 400 to 600°C. [ABSTRACT FROM AUTHOR]

We report on the investigation of a transformer oil-based magnetic nanofluid exposed to an electric field by means of synchrotron small angle X-ray scattering. Two types of small angle X-ray scattering experiments were carried out. In the first one, the electric field up to 6 kV/cm was generated in the nanofluid between two immersed electrodes. The other experiment focused on the nanofluid in an external electric field up to 10 kV/cm, when the electrodes were not in a direct electrical contact with the nanofluid. In the available range (0.02-4.5 nm-1) of scattering vector q, the non-contact mode has no effect on the scattering intensity. The contact mode yielded noticeable low-q intensity variations. In comparison to small angle neutron scattering, the small angle X-ray scattering study did not prove the proportional increase in the low q scattering intensity with increasing electric field, but rather stochastic variations. The observed intensity variations reflect the local structural nanofluid changes caused by the induced electrohydrodynamics. The electrical conductivity and relaxation processes are pointed out as favorable conditions for electrohydrodynamics in the magnetic nanofluid. [ABSTRACT FROM AUTHOR]

The two-level organization of C60 fullerene clusters in solutions of C60 in pure toluene and toluene/N-methyl-2-pyrrolidone solvent mixtures is studied by small-angle X-ray scattering (SAXS). The SAXS data for freshly prepared solutions are compared with the data obtained by dynamic light scattering, a technique we use to assess the temporal stability of the prepared solutions. For all solutions in the mixed solvent, regardless of the ratio between the polar and nonpolar components, the UV−Vis absorption spectra tend to become featureless with time. We attribute this behavior primarily to the presence of the polar component in the molecular environment of fullerene molecules. [ABSTRACT FROM AUTHOR]

A newly developed high-pressure rheometer for in situ X-ray scattering experiments is described. A commercial rheometer was modified in such a way that X-ray scattering experiments can be performed under different pressures and shear. First experiments were carried out on hyaluronan, a ubiquitous biopolymer that is important for different functions in the body such as articular joint lubrication. The data hint at a decreased electrostatic interaction at higher pressure, presumably due to the increase of the dielectric constant of water by 3% and the decrease of the free volume at 300 bar. [ABSTRACT FROM AUTHOR]

The development of a dedicated small-angle X-ray scattering setup for the investigation of complex fluids at different controlled shear conditions is reported. The setup utilizes a microfluidics chip with a narrowing channel. As a consequence, a shear gradient is generated within the channel and the effect of shear rate on structure and interactions is mapped spatially. In a first experiment small-angle X-ray scattering is utilized to investigate highly concentrated protein solutions up to a shear rate of 300000 s−1. These data demonstrate that equilibrium clusters of lysozyme are destabilized at high shear rates. [ABSTRACT FROM AUTHOR]

The article discusses a study which investigated the magnetic properties and physical characteristics of iron oxide nanoparticles in magnetoferritin. Topics highlighted include the role of brain ferritin in patients with Alzheimer's disease, the structure, quality and quantity of the iron core composition in the brain ferritin and the advantages of magnetoferritin for biotechnological applications. Also discussed is the mechanism of in vitro chemical synthesis of magnetoferritin.

The Sr2FeMoO6− δ compound attracts the attention of researchers due to a high Curie temperature, large values of negative magnetoresistance at room temperature and a practically 100% spin polarization of conduction electrons. We have studied the role of grain boundaries on the electrical transport in Sr2FeMoO6− δ in applied magnetic fields up to 8 T. The compound was synthesized out of partially reduced SrFeO3− x, SrMoO4− y precursors (sample I). At the first oxidation stage upon annealing at 700 K in argon with a partial oxygen pressure p(O2) = 10 Pa for 15 h (sample II), the internal structure of the Sr2FeMoO5.82 grains did not change. Sample II exhibits a mixed type of electrical conduction. In a magnetic field B its resistivity decreases without changing the mixed regime of charge transport, only shifting the temperature of minimum resistivity ( TmB) to lower values. At temperatures above TmB the conductivity is predominantly metallic, whereas below TmB down to 4.2 K it is of semiconductor type. The increase of the annealing time up to 30 h (sample III) brings about an increase of the resistivity and the appearance of semiconductor-type conductivity at T = 300-4.2 K, which indicates the formation of a continuous insulating interlayer between the grains. In a magnetic field, the resistivity decreases, with the conductivity changing from the semiconducting to a mixed one. In the latter case the charge transport can occur both through point metallic contacts and by means of spin-dependent tunneling across dielectric interlayers between Sr2FeMoO5.82 grains. [ABSTRACT FROM AUTHOR]

UV-Vis spectroscopy and small-angle neutron scattering experiments are performed on the cluster solution of fullerene C60 in N-methyl-2-pyrrolidone before and after dilution of the system with pure solvent. Some changes in the UV-Vis spectra showing solvatochromism at dilution are observed, while the neutron scattering signal does not change. The effect is discussed with respect to the relation between solvatochromism and cluster formation for fullerene solutions in nitrogen-containing solvents. [ABSTRACT FROM AUTHOR]

In order to directly observe neutron scattering by heavy fermion quasiparticles at low temperatures, a CeRu2Si2 single crystal has been studied by the small-angle neutron scattering method. In the experiment, neutron scattering is observed at T = 0.85 K for momentum transfers q ≤ 0.04Å–1, which is treated as the orbital component of magnetic scattering by heavy fermion quasiparticles. It has been found that the application of a magnetic field H = 1 T leads to both an increase in the observed scattering and its anisotropy with respect to the field direction. Moreover, measurements in the magnetic field reveal additional scattering for q > 0.04 Å–1, which is well described by a Lorentzian and is interpreted as neutron magnetic scattering by spin-density fluctuations with a correlation radius Rc ≈ 30 Å. © 2005 Pleiades Publishing, Inc. [ABSTRACT FROM AUTHOR]

Poly(ethylene glycol) is used for coating of colloidal particles and other surfaces for gaining biocompatibility. Particularly, it can be introduced into magnetic fluids. The aim of the current study was to reveal the structural characteristics of poly(ethylene glycol) in neat D2O using small-angle neutron scattering technique. Solutions of poly(ethylene glycol) (at temperature of 37°C) with different molecular weights in an interval of 400-20000 were investigated. It is concluded that at low concentrations (less than 2% of mass fraction) poly(ethylene glycol) molecules behave as Gaussian coils. [ABSTRACT FROM AUTHOR]

The structural stability of magnetoferritin, a synthetic analogue of ferritin, at various pH levels is assessed here. The structural and electrical properties of the complexes were determined by small-angle X-ray scattering (SAXS), dynamic light scattering (DLS) and zeta potential measurements. At pH 3-6 a reduction of electrostatic repulsion on the suspended colloids resulted in aggregation and sedimentation of magnetoferritin. At neutral to slightly alkaline conditions (pH 7-9) the magnetoferritin structure was stable for lower iron loadings. Higher solution pH 10-12 induced destabilization of the protein structure and dissociation of subunits. Increasing the loading factor in the MFer complex leads to decrease of the stability versus pH changes., (Copyright © 2017 Elsevier B.V. All rights reserved.)

Multi-drug resistant bacteria are currently undermining our health care system worldwide. While novel antimicrobial drugs, such as antimicrobial peptides, are urgently needed, identification of new modes of action is money and time consuming, and in addition current approaches are not available in a high throughput manner. Here we explore how small angle X-ray scattering (SAXS) as high throughput method can contribute to classify the mode of action for novel antimicrobials and therefore supports fast decision making in drug development. Using data bases for natural occurring antimicrobial peptides or predicting novel artificial peptides, many candidates can be discovered that will kill a selected target bacterium. However, in order to narrow down the selection it is important to know if these peptides follow all the same mode of action. In addition, the mode of action should be different from conventional antibiotics, in consequence peptide candidates can be developed further into drugs against multi-drug resistant bacteria. Here we used one short antimicrobial peptide with unknown mode of action and compared the ultrastructural changes of Escherichia coli cells after treatment with the peptide to cells treated with classic antibiotics. The key finding is that SAXS as a structure sensitive tool provides a rapid feedback on drug induced ultrastructural alterations in whole E. coli cells. We could demonstrate that ultrastructural changes depend on the used antibiotics and their specific mode of action. This is demonstrated using several well characterized antimicrobial compounds and the analysis of resulting SAXS curves by principal component analysis. To understand the result of the PCA analysis, the data is correlated with TEM images. In contrast to real space imaging techniques, SAXS allows to obtain nanoscale information averaged over approximately one million cells. The measurement takes only seconds, while conventional tests to identify a mode of action require days or weeks per single substance. The antimicrobial peptide showed a different mode of action as all tested antibiotics including polymyxin B and is therefore a good candidate for further drug development. We envision SAXS to become a useful tool within the high-throughput screening pipeline of modern drug discovery. This article is part of a Special Issue entitled: Antimicrobial peptides edited by Karl Lohner and Kai Hilpert., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Synthetic biological macromolecule of magnetoferritin containing an iron oxide core inside a protein shell (apoferritin) is prepared with different content of iron. Its structure in aqueous solution is analysed by small-angle synchrotron X-ray (SAXS) and neutron (SANS) scattering. The loading factor (LF) defined as the average number of iron atoms per protein is varied up to LF=800. With an increase of the LF, the scattering curves exhibit a relative increase in the total scattered intensity, a partial smearing and a shift of the match point in the SANS contrast variation data. The analysis shows an increase in the polydispersity of the proteins and a corresponding effective increase in the relative content of magnetic material against the protein moiety of the shell with the LF growth. At LFs above ∼150, the apoferritin shell undergoes structural changes, which is strongly indicative of the fact that the shell stability is affected by iron oxide presence., (Copyright © 2014 Elsevier B.V. All rights reserved.)

We report the solvent-driven assembly of a polyelectrolytic polyfluorene-polythiophene diblock copolymer-poly[9,9-bis(2-ethylhexyl)fluorene]-b-poly[3-(6-trimethylammoniumhexyl)thiophene] (PF2/6-b-P3TMAHT)-in tetrahydrofuran (THF), water, their 1:1 mixture and in subsequently prepared thin films, as investigated using a combination of scattering, microscopic and photoluminescence techniques. In solution PF2/6-b-P3TMAHT forms large (>100 nm) aggregates which undergo a transition from objects with surface fractal interface (THF) to ones with a significant planar component due to the presence of the 2-dimensionally merged ribbon-like aggregates or fused walls of the observed vesicular aggregates [THF-water (1:1)]. In THF-water and water the blocks are loosely segregated into P3TMAHT and PF2/6 rich domains, with PF2/6 dominating the aggregate interior. Depending on solvent, the spun films contain either aggregates with a crystalline interior (THF) or large 200 nm-2 microm vesicular aggregates embedded in a featureless matrix (THF-water and water). Structural variations are concomitant with distinctive solvatochromic changes in the photophysical properties including a color change from deep red (THF) to pale orange (THF-water and water) in solution, a decrease in fluorescence quantum yield with increasing water content, and a shift from photoluminescence of individual PF2/6 blocks (THF) to efficient PF2/6 --> P3TMAHT energy transfer (THF-water and water).

The structure of ferrofluids (magnetite in decahydronaphtalene) stabilized with saturated mono-carboxylic acids of different chain lengths (lauric, myristic, palmitic and stearic acids) is studied by means of magnetization analysis and small-angle neutron scattering. It is shown that in case of saturated acid surfactants, magnetite nanoparticles are dispersed in the carrier approximately with the same size distribution whose mean value and width are significantly less as compared to the classical stabilization with non-saturated oleic acid. The found thickness of the surfactant shell around magnetite is analyzed with respect to stabilizing properties of mono-carboxylic acids.

We present guidelines on how the solution structure of pi -conjugated hairy-rod polyfluorenes is controlled by the side-chain length and branching. First, the semiquantitative mean-field theory is formulated to predict the phase behavior of the system as a function of side-chain beads (N). The phase transition at N=N{ *} separates a lyotropic phase with solvent coexistence (NN{ *}). The membrane phase transforms into the isotropic phase of dissolved rodlike polymers at the temperature T_{mem}{ *}(N), which decreases both with N and with the degree of side-chain branching. This picture is complemented by polymer demixing with the transition temperature T_{IN}{ *}(N), which decreases with N . For NN{ *}, stable membranes are predicted for T_{IN}{ *}N{ *}. T_{mem}{ *}(N) decreases from 340 K to 280 K for N > or = 8 . For copolymers, the membrane phase is found when the fraction of F8 units is at least 90%, T_{mem}{ *} decreasing with this fraction. The membrane phase contains three material types: loose sheets of two polymer layers, a better packed beta phase, and dissolved polymer. For N > or = 7 and T