Small-angle neutron scattering study on the stability of oxide nanoparticles in long-term thermally aged 9Cr-oxide dispersion strengthened steel

A 9 Cr-oxide dispersion strengthened(ODS)steel was thermally aged at 873 K for up to 5000 h.The size distribution and chemical composition of the dispersed oxide nanoparticles were analyzed by small-angle neutron scattering under a magnetic field.Combined with transmission electron microscopy,Vickers micro-hardness tests and electron backscattered diffraction measurements,all the results showed that the thermal treatment had little or no effect on the size distributions and volume fractions of the oxide nanoparticles in the ferromagnetic matrix,which suggested excellent thermal stability of the 9 Cr-ODS steel.

SMALL ANGLE NEUTRON SCATTERING INVESTIGATION OF Ni_(50)Mo(50)ALLOY AND ITS FRACTAL PROPERTIES

Small angle neutron scattering(SANS) technique has been used to investigate the Ni_(50)Mo_(50) system prepared by mechanical alloying(MA). Significant changes of the scattering intensity have been observed among the samples with different milling time.Interesting fractal-like behavior of the sample system have been found and attempts have been made to determine the fractal dimensions. It is expected that the fractal dimension can be related to the different stages of MA to some extent.

Study on porosity of ceramic SiC using small angle neutron scattering

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In-Situ Measuring the Particle Mean Size and Dust Concentration by Near-Forward Small Angle Light Scattering

This paper presents a method of measuring the particle mean size and dust concentration by small angle near forward light scattering optics and the extinction theory. Its theory is based on Fraunhofer diffraction theory which is the approximation of Mie scattering within the forward Fraunhofer diffraction lobe, and Rosin Rammler function is introduced to describe the particle size distribution in two phase flow in advance. Compared with the values by the sample weight method, the measurement results have a reasonable agreement. The present work has demonstrated that this method will be probably used to monitor the parameters of two phase flow.

Small Angle X-ray Scattering Study of Precipitation Kinetics in Al-Zn-Mg-Cu Alloys

The evolution of microstructure parameters （precipitate size and volume fraction） for two types of Al-Zn-Mg-Cu alloys （7075 and 7055） during aging has been studied by synchrotron-radiation small angle X-ray scattering （SAXS）.The results show that the precipitates are only a few nanorneters for both alloys ageing even at higher temperature of 160℃ for 72 h （4.44 and 5.82 nm, respectively）. The maximum of the precipitate volume fraction increases with in creasing Zn content and is about 0.023-0.028 and 0.052-0.054, respectively. The coarsening of precipitate is consistent with LSW （Lifshitz-Slyozov-Wagner） model even at the initial stage where volume fraction is still varying.The activation energy of coarsening regime has been determined to be about 1.22±0.02 eV and 1.25±0.02 eV for alloys 7075 and 7055, respectively.

Small-angle X-ray scattering investigation of aging behavior of Al-Cu-Mg-Ag alloys using synchrotron radiation

The aging behavior of Al-Cu-Mg-Ag alloys with high Cu/Mg was studied by transmission electron microscopy (TEM) and small-angle X-ray scattering (SAXS) using synchrotron radiation. TEM study reveals that the major strengthening phases of the alloy after aging at 160?C for 10 h are Ω and less θ′. SAXS study shows that the scattering patterns are composed of several concentric circles at the beginning of aging process, which is replaced by the butterfly-wings scattering patterns with the increase of aging time. The butterfly-wings scattering patterns are composed of several branches. The angles between the branches are roughly equal to that between the habit planes of precipitates. The evolution of Guinier radius with aging time indicates the good coarsening resistance of the precipitates. The evolution of integrated intensity is consistent with the classical two-step precipitation process.

Growth Kinetics of Nanocrystals and Nanorods by Employing Small-angle X-ray Scattering (SAXS) and Other Techniques

In this article, we report the results of our detailed investigations of the growth kinetics of zero-dimensional nanocrystals as well as one-dimensional nanorods by the combined use of small angel X-ray scattering （SAXS）, transmission electron microscopy （TEM） along with other physical techniques. The study includes growth kinetics of gold nanocrystals formed by the reduction of HAuCl4 by tetrakis（hydroxymethyl） phosphonium chloride in aqueous solution, of CdSe nanocrystals formed by the reaction of cadmium stearate and selenium under solvothermal conditions, and of ZnO nanorods formed by the reaction of zinc acetate with sodium hydroxide under solvothermal conditions in the absence and presence of capping agents. The growth of gold nanocrystals does not follow the diffusion-limited Ostwald ripening, and instead follows a Sigmoidal rate curve. The heat change associated with the growth determined by isothermal titration calorimetry is about 10 kcal·mol^-1 per I nm increase in the diameter of the nanocrystals. In the case of CdSe nanocrystals also, the growth mechanism deviates from diffusion-limited growth and follows a combined model containing both diffusion and surface reaction terms. Our study of the growth kinetics of uncapped and poly（vinyl pyrollidone） （PVP）-capped ZnO nanorods has yielded interesting insights. We observe small nanocrystals next to the ZnO nanorods after a lapse of time in addition to periodic focusing and defocusing of the width of the length distribution. These observations lend support to the diffusion-limited growth model for the growth of uncapped ZnO nanorods. Accordingly, the time dependence on the length of uncapped nanorods follows the L3 law as required for diffusion-limited Ostwald ripening. The PVP-capped nanorods, however, show a time dependence, which is best described by a combination of diffusion （L^3） and surface reaction （L^2） terms.

Stability of the Dividing Distribution Function Method for ParticleSize Distribution Analysis in Small Angle X－Ray Scattering

The Dividing Distribution Function (DDF) method is one of the methods by which the particle size distribution of ultrafine powder can be evaluated from its small angle X-ray scattering data. In this paper, the stability of the solution obtained from DDF method has been investigated through optimizing the coefficient matrix, introducing a damping factor and a least square treatment. All calculations were accomplished with a microcomputer. It was shown that the average deviations of the size distribution obtained are not larger than the assigned random errors to the scattering intensities as long as the corresponding requirements are satisfied.

Small Angle X-ray Scattering Study of PS Conformation in Tetrahydrofuran Solvent with Gas Anti-solvent

Small angle X-ray scattering (SAXS) was used to study the effect of dissolved CO2 on the conformation of polystyrene (PS) in PS/tetrahydrofuran(THF) solution at 308.15 K and at pressures up to 3 MPa. The cloud pressure and the expansion curve of the solution were also determined. The dependence of the conformation on pressure was discussed.

Small angle X-ray scattering beamline at SSRF

Beamline BL16B1 at Shanghai Synchrotron Radiation Facility(SSRF) is dedicated to studying the microstructure and dynamic processes of polymers, nanomaterials, mesoporous materials, colloids, liquid crystals,metal materials, etc. At present, SAXS, wide angle X-ray scattering(WAXS), simultaneous SAXS/WAXS,grazing incident SAXS, and anomalous SAXS techniques are available for end user to conduct diverse experiments at this beamline. The sample-to-detector distance is adjustable from 0.2 m to 5 m. The practicable q-range is 0.03–3.6 nm-1at incident X-ray of 10 ke V for conventional SAXS whilst a continuous q-region of0.06–33 nm-1can be achieved in simultaneous SAXS/WAXS mode. Time-resolved SAXS measurements in sub-second level was achieved by the beamline upgrating in 2013. This paper gives detailed descriptions about the status, performance and applications of the SAXS beamline.

A new package:MySAS for small angle scattering data analysis

In this paper,A MySAS package,which is verified on Windows XP,can easily convert two-dimensional data in small angle neutron and X-ray scattering analysis,operate individually and execute one particular operation as numerical data reduction or analysis,and graphical visualization.This MySAS package can implement the input and output routines via scanning certain properties,thus recalling completely sets of repetition input and selecting the input files.On starting from the two-dimensional files,the MySAS package can correct the anisotropic or isotropic data for physical interpretation and select the relevant pixels.Over 50 model functions are fitted by the POWELL code using x^2 as the figure of merit function.

Studies on microdomain structure in segmented polyether polyurethaneureas by positron annihilation lifetime and small-angle X-ray scattering

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Quantitative evaluation of equatorial small-angle X-ray scattering for cylindrical fibers

Elongated microvoids, internal fibrillar structure, and edge scattering from both surface refraction cause an equatorial streak in small angle X-ray scattering. A model for analyzing the edge scattering of fibers is proposed. Simulation results indicate that the intensity of edge scattering from surface refraction of a cylindrical fiber is strong and makes an important contribution to the equatorial streak. Two factors influence edge scattering intensity. One is the sample-to-detector distance （D）; edge scattering intensity increases with increasing D. The equatorial streak becomes weak when D is shortened. The other factor is the refraction index. Edge scattering intensity increases as the real component of the refraction index decreases. In experiment, weak or even no equatorial streaks were found for samples measured in a roughly index-matching fluid. Edge scattering can be eliminated or weakened, and it can be calculated by comparing the intensities of a cylindrical fiber when it is measured in air and in index-matching fluid. The simulation data are basically in agreement with the experimental data.

Scanning Microfocus Small Angle X-ray Scattering Study of the Avian Eggshell

Synchrotron microfocus small angle X-ray scattering was used to investigate the nanostructure and microscopic variation of eggshells. It uses a microbeam allowing the ability to probe interactions between the organic and inorganic components at nanometer level and is ideal for mapping over small areas to obtain a detailed analysis of structural variations. Thin sections of eggshells were scanned from the shell membrane （inner） to the cuticle （outer） surface. The data collected was used to produce two-dimensional maps showing microscopic changes within the different layers of the eggshell. The structural alterations ap- parently could have implications at the macroscopic level of the resulting eggshell. As the organic matrix is embedded within the eggshell this may contribute to the variations observed in calcite crystal form and texture, Structural information obtained about a biomaterial at different length scales is important in relating the structure to its functional properties. This knowledge and the principles behind the formation of biomaterials could be used in the attempt of bioengineering new systems.

Characteristics of AOT Microemulsion Structure: a Small Angle X-ray Scattering Study

The method of synchrotron radiation small-angle X-ray scattering (SR-SAXS) has been used to obtain structural information on the system of bis (2-ethylhexyl) sulfosuccinate (AOT)/H2O/isooctane. By using the Guinier plot (Ln I (q) versus q(2)) on the data sets in a defined small q range (0.03-0.06 Angstrom (-1)), the gyration radius at different water/surfactant molar ratio, W-0, was obtained. With the increase of W-0, the gyration radius (R-g) increased at the range of 23.2 similar to 52.7 Angstrom.

SMALL ANGLE LIGHT SCATTERING MEASUREMENT OF THE ISOTROPIC TO NEMATIC TRANSITION OF A SIDE CHAIN NEMATIC POLYMETHACRYLATE

The kinetics of I-->N transition of a side chain nematic polymethacrylate has been studied by small angle depolarized light scattering intensity measurements using a charge coupled device linear image sensor. The polymer shows the transition temperatures K52N79I in degreesC, The H-v scattering intensity T(q,t) during the transition I (at 80.2degreesC)-->N (at 75.8degreesC) shows that T(q) is independent of q for all t, and during the initial stage (in 6 s) T(t) increases exponentially with t. In the later stage of the transition T(t) approaches a saturation value in 2 min. This experimental result indicates that the I-->N transition of a liquid crystalline polymer is a spinodal type of phase transition mediated by orientation fluctuation.

Probing Nanoscale Morphology of PS/PMMA/CdS &PS/PVC/CdS Polymeric Nanocomposites through Small Angle X-Ray Scattering Analysis

Polymeric nanocomposites of PS/PMMA/CdS and PS/PVC/CdS samples have been synthesized through dispersion solution casting technique. The nanoparrticles of CdS were prepared by simple chemical method using CdCl2 and H2S gas produced from thiourea. The nanoscale morphology of the prepared polymeric nanocomposite samples is probed through small angle X-ray scattering (SAXS). The SAXS study reveals that CdS nanoparticles take place at voids position in the respective plymer blend matrix and exhibit their nano nature with very little tendency to agglomerates.

In-situ study of precipitates in Al–Zn–Mg–Cu alloys using anomalous small-angle x-ray scattering

In the present work,the precipitate compositions and precipitate amounts of these elements（including the size distribution,volume fraction,and inter-precipitate distance） on the Cu-containing 7000 series aluminum alloys（7150 and 7085 Al alloys）,are investigated by anomalous small-angle x-ray scattering（ASAXS） at various energies.The scattering intensity of 7150 alloy with T6 aging treatment decreases as the incident x-ray energy approaches the Zn absorption edge from the lower energy side,while scattering intensity does not show a noticeable energy dependence near the Cu absorption edge.Similar results are observed in the 7085 alloy in an aging process（120℃） by employing in-situ ASAXS measurements,indicating that the precipitate compositions should include Zn element and should not be strongly related to Cu element at the early stage after 10 min.In the aging process,the precipitate particles with an initial average size of ~ 8 ？A increase with aging time at an energy of 9.60 ke V,while the increase with a slower rate is observed at an energy of 9.65 ke V as near the Zn absorption edge.

Structural modeling of proteins by integrating small-angle x-ray scattering data

Elucidating the structure of large biomolecules such as multi-domain proteins or protein complexes is challenging due to their high flexibility in solution. Recently, an ＂integrative structural biology＂ approach has been proposed, which aims to determine the protein structure and characterize protein flexibility by combining complementary high- and lowresolution experimental data using computer simulations. Small-angle x-ray scattering（SAXS） is an efficient technique that can yield low-resolution structural information, including protein size and shape. Here, we review computational methods that integrate SAXS with other experimental datasets for structural modeling. Finally, we provide a case study of determination of the structure of a protein complex formed between the tandem SH3 domains in c-Cb1-associated protein and the proline-rich loop in human vinculin.

INVESTIGATION ON THE CONFORMATION OF THE MAIN-CHAIN NEMATIC POLYMER BY SMALL ANGLE X-RAY SCATTERING

The experimental investigation on the conformation of a thermotropic main-chain nematic polymer by small-angle X-ray scattering (SAXS) has been carried out. The average radius of gyration of the polymer has been determined in nematic and isotropic state respectively. The experiment shows that the boundary between domains is not sharp but diffuse, and the diffuse-boundary thickness of the polymer as a function of temperature has been given.