Time-resolved ultra-small-angle X-ray scattering beamline(BL10U1)at SSRF

The construction of a new beamline,BL10U1,was completed at the Shanghai synchrotron radiation facility in 2020.This multipurpose beamline was designed to provide X-ray scattering techniques such as ultra-small-angle X-ray scattering(USAXS),small-angle X-ray scattering(SAXS),wide-angle X-ray scattering,and microfocus SAXS(μSAXS)for a broad user community.To realize fast time-resolved USAXS experiments,the beamline adopted an in-vacuum undulator with a total length of 1.6 m as the photon source.An in-house cryogenic-cooled double multilayer monochromator was installed to deliver a photon flux of approximately 10^(13) photons/s at a photon energy of 10 keV.The three-year successful operation of this beamline demonstrated that the monochromator operated smoothly,as expected.BL10U1 has three end stations in succession:USAXS end station,μSAXS end station,and end station for industrial applications.The minimum scattering vector q~0.0042 nm^(-1) at 10 keV can be achieved at the USAXS end station equipped with a 28 m-long and 1.8 m-diameter vacuum flight tube.At theμSAXS end station,a beam spot of less than 10×8μm was achieved for micro-SAXS experiments.In contrast,in situ experimental instruments up to 5 m high and 8 m wide can be mounted at the industrial application end station,which offers industrial scientists the opportunity to use their large industrial equipment.BL10U1 opens up a new capability to investigate phenomena such as non-equilibrium and dynamic processes of materials with a wide length scale from angstroms to micrometers with millisecond time resolution.In this paper,we also report beamline design considerations and commissioning results.

Detection method of forward-scatter signal based on Rényi entropy

The application scope of the forward scatter radar(FSR)based on the Global Navigation Satellite System(GNSS)can be expanded by improving the detection capability.Firstly,the forward-scatter signal model when the target crosses the baseline is constructed.Then,the detection method of the for-ward-scatter signal based on the Rényi entropy of time-fre-quency distribution is proposed and the detection performance with different time-frequency distributions is compared.Simula-tion results show that the method based on the smooth pseudo Wigner-Ville distribution(SPWVD)can achieve the best perfor-mance.Next,combined with the geometry of FSR,the influence on detection performance of the relative distance between the target and the baseline is analyzed.Finally,the proposed method is validated by the anechoic chamber measurements and the results show that the detection ability has a 10 dB improvement compared with the common constant false alarm rate(CFAR)detection.

Temperature and Salinity Dual-parameter Sensing Based on Forward Brillouin Scattering in 1060-XP SMF

A novel temperature and salinity discriminative sensing method based on forward Brillouin scattering(FBS)in 1060-XP single-mode fiber(SMF)is proposed.The measured frequency shifts corresponding to different radial acoustic modes in 1060-XP SMF show different sensitivities to temperature and salinity.Based on the new phenomenon that different radial acoustic modes have different frequency shift-temperature and frequency shift-salinity coefficients,we propose a novel method for simultaneously measuring temperature and salinity by measuring the frequency shift changes of two FBS scattering peaks.In a proof-of-concept experiment,the temperature and salinity measurement errors are 0.12℃and 0.29%,respectively.The proposed method for simultaneously measuring temperature and salinity has the potential applications such as ocean surveying,food manufacturing and pharmaceutical engineering.

BL19U2:Small-angle X-ray scattering beamline for biological macromolecules in solution at SSRF

The BL19U2 at the Shanghai Synchrotron Radiation Facility is a small-angle X-ray scattering beamline dedicated to structural studies pertaining to biological macromolecules in solution.The beamline has been officially opened to users in March 2015,and since then,a series of technological innovations has been developed to optimize beamline performance,thereby significantly improving the data collection efficiency and broadening the application scope of biological small-angle X-ray scattering.BL19U2 is ideal for the high-throughput screening of weakly scattered proteins,protein assemblies,nucleic acids,inorganic nanomaterials,and organic drug molecules.This paper describes the design and overview of the BL19U2 beamline.Versatile sample environments at the experimental station and some recent scientific highlights are presented.

Understanding fluorine-free electrolytes via small-angle X-ray scattering

Fluorine-free electrolytes have attracted great attention because of its low-cost and environmental friendliness. However, so far, little is known about the solution structures of these electrolytes. Here,we compare the solvation phenomenon of sodium tetraphenylborate(NaBPh_(4)) salt dissolved in organic solvents of propylene carbonate(PC), 1,2-dimethoxyethane(DME), acetonitrile(ACN) and tetrahydrofuran(THF). Small-angle X-ray scattering(SAXS) reveals a unique two-peak structural feature in this saltconcentrated PC electrolyte, while solutions using other solvents only have one scattering peak.Molecular dynamics(MD) simulations further reveal that there are anion-based clusters in addition to the short-range charge ordering in the concentrated NaBPh4/PC electrolyte. Raman spectroscopy confirms the existence of considerable contact ion pairs(CIPs). This work emphasizes the importance of global and local structural analysis, which will provide valuable clues for understanding the structureperformance relationship of electrolytes.

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.

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.

Investigation of the topological shape of bovine serum albumin in solution by small-angle x-ray scattering at Beijing synchrotron radiation facility

This paper reports that at a newly constructed small-angle x-ray scattering station of Beijing Synchrotron Radia- tion Facility, the topological shape of ligand-free bovine serum albumin in solution has been investigated. An appropriate scattering curve is obtained and the calculated value of the gyration radius is 31.2~=t=0.25 ~_ （11=0.1 nm） which is co- incident with other ones＇ results. It finds that the low-resolution structure models obtained by making use of ab initio reconstruction methods are fitting the crystal structure of human serum albumin very well. All of these results perform the potential of the beamline to apply to structural biology studies. The characteristics, the defects, and the improving measures of the station in future are also discussed.

Small-Angle X-Ray Scattering of Amorphous Germanium: Numerical Modeling

The present work deals with a detailed analysis of the small-angle X-ray scattering of nanoporous atomistic models for amorphous germanium. Structures with spherical nanovoids, others with arbitrarily oriented ellipsoidal ones, with monodisperse and polydisperse size distributions, were first generated. After relaxing the as-generated structure, we compute its radial distribution function, and then we deduce by the Fourier transform technique its X-ray scattering pattern. Using a smoothing procedure, the computed small-angle X-ray scattering patterns are corrected for the termination errors due to the finite size of the model, allowing so, for the first time at our best knowledge, a rigorous quantitative analysis of this scattering. The Guinier’s law is found to be valid irrespective of size and shape of the nanovoids over a scattering vector-range extending beyond the expected limit. A weighted combination of the Guinier’s forms accounts for well the nanovoid size distribution in the amorphous structure. The invariance of the Q-factor and its relationship to the void volume fraction are also confirmed. Our findings support then the quantitative analyses of available small-angle X-ray scattering data for amorphous germanium.

The Significance of Solutions Obtained from Ill-Posed Systems of Linear Equations Constituted by Synchrotron Radiation Based Anomalous Small-Angle X-Ray Scattering

Synchrotron radiation based experimental techniques known as Anomalous Small-Angle X-ray Scattering (ASAXS) provide deep insight into the nanostructure of uncountable material systems in condensed matter research i.e. solid state physics, chemistry, engineering and life sciences thereby rendering the origin of the macroscopic functionalization of the various materials via correlation to its structural architecture on a nanometer length scale. The techniques constitute a system of linear equations, which can be treated by matrix theory. The study aims to analyze the significance of the solutions of the stated matrix equations by use of the so-called condition numbers first introduced by A. Turing, J. von Neumann and H. Goldstine. Special attention was given for the comparison with direct methods i.e. the Gaussian elimination method. The mathematical roots of ill-posed ASAXS equations preventing matrix inversion have been identified. In the framework of the theory of von Neumann and Goldstine the inversion of certain matrices constituted by ASAXS gradually becomes impossible caused by non-definiteness. In Turing’s theory which starts from more general prerequisites, the principal minors of the same matrices approach singularity thereby imposing large errors on inversion. In conclusion both theories recommend for extremely ill-posed ASAXS problems avoiding inversion and the use of direct methods for instance Gaussian elimination.

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.

Real-time pore structure evolution difference between deep and shallow coal during gas adsorption:A study based on synchrotron radiation small-angle X-ray scattering

Coal seam CO_(2) sequestration is an important option to address global warming.A better knowledge on coal pore structure evolution during gas adsorption can provide guidance for coal seams CO_(2) seques-tration.However,few investigations on the pore structure evolution differences between the deep and shallow coal were conducted during gas adsorption.In this study,based on the real-time synchrotron radiation small-angle X-ray scattering(SAXS)observation,the average pore diameter and pore surface fractal dimension evolution differences between deep and shallow coal were investigated from the as-pects of coal compositions and stress history.Two types of coal deformation(inner-swelling and outer-swelling)coexist during gas adsorption.Coal compositions have significant impact on the dominance of deformation type.The dominance of inner-swelling in deep coal is induced by the higher ash contents,and there is the decrease of average pore diameter during gas adsorption.The impact of stress-history(burial depth)on adsorption-induced deformation is more prominent than that of gas adsorption ca-pacity.In deep coal,the surface fractal dimension evolution presents a negative correlation with the evolution of pore diameters.In shallow coal,the surface fractal dimension evolution presents a Langmuir-type correlation with the adsorption time.

Small-angle X-ray analysis of the effect of grain size on the thermal damage of octahydro-1, 3, 5, 7-tetranitro-1, 3, 5, 7 tetrazocine-based plastic-bounded expolsives

The microstmcture evolution of plastic-bonded explosives （PBXs） after thermal stimulus plays a key role in PBX performance. In this paper, the nanoscale pores of thermal-treated octahydro-1,3,5,7-tetranitro-1,3,5,7 tetrazocine （HMX）- based PBXs with different HMX particle sizes [approximately 40 （FLIP） and 100 μm （LHP）] were measured using small- angle X-ray scattering （SAXS）. No obvious pore variations were found in the LHP samples heated at 160 ℃ for 6 h, whereas the amount of pores of FHP decreased when subjected to 160 ℃ for 6 h. At 180 ℃, the average pore radii of FHP and LHP decreased from approximately 45 nm to 25 nm, and the total pore volume increased distinctively because of phase transformation. The LHP sample reached a high level of pore content after being held at 180 ℃ for 1 h, whereas FHP required 3 h. Both FHP and LHP had relatively high pore volumes when subjected to 200 ℃ for 1 and 3 h.

Simultaneous detection of the acoustic-field aberration and Doppler shift in forward acoustic scattering

The aberration in the received acoustic field and the Doppler shift in the forward scattered field are simultaneously induced when a submerged target crosses the source–receiver line. Formulations for the two variations are developed upon an ideal forward scattering configuration. Both the field aberration and the Doppler shift are expressed as functions of the same argument — the target motion time. An experimental validation was carried out in a tank, in which the continuous wave was transmitted. The field aberration and the Doppler shift were extracted from the collected data by the simple Hilbert transform and a hybrid technique, respectively. The measured aberration and Doppler shift agree with the theoretical results.Simultaneous detection outputs are beneficial to enhance the reliability on target detection by providing both the aberrations in the received acoustic field and the Doppler shift in the forward scattered field.

Solution of scattering from rough surface with a 2D target above it by a hybrid method based on the reciprocity theorem and the forward-backward method

This paper proposes a hybrid method based on the forward-backward method （FBM） and the reciprocity theorem （RT） for evaluating the scattering field from dielectric rough surface with a 2D target above it. Here, the equivalent electric/magnetic current densities on the rough surface as well as the scattering field from it are numerically calculated by FBM, and the scattered field from the isolated target is obtained utilizing the method of moments （MOM）. Meanwhile, the rescattered coupling interactions between the target and the surface are evaluated employing the combination of FBM and RT. Our hybrid method is first validated by available MOM results. Then, the functional dependences of bistatic and monostatic scattering from the target above rough surface upon the target altitude, incident and scattering angles are numerically simulated and discussed. This study presents a numerical description for the scattering mechanism associated with rescattered coupling interactions between a target and an underlying randomly rough surface.

Physical model of acoustic forward scattering by cylindrical shell and its experimental validation

Research on the underwater target scattering can provide important theoretical support for target detection. The scattering model of cylindrical shell is established in this paper. It is found that the forward target strength is much stronger and varies with angles of incident wave less significantly than backward target strength. The received forward signal strength fluctuates with the target moving due to the interference between direct signal and scattering signal, which is most significant when the target approaches the baseline. An experiment is carried out in an anechoic tank to validate the scattering model. The method of acquisiting forward scattering in the tank is proposed. The forward and the backward target strengths are achieved by using the pulse compression technology, and they axe about 3dB less than the modeling results. The forward scattering phenomena of quiescent and moving targets are measured, which are similar to modeling results with different target types.

Forward scattering bistatic radar imaging method and practice data processing

A new forward scattering bistatic radar motion compensation method based on spectral analysis and minimum waveform entropy is proposed. In order to demonstrate effectiveness of the presented method and ground vehicles imaging function of forward scattering radar, a simple bistatic forward scattering radar experiment system is set up on both sides of a road to collection ground vehicles experimental data. Finally, experimental ground vehicles imaging results confirm validity of the proposed motion compensation method and the experimental imaging results are identical with computer simulation results in the same parameter and condition.

Distributed analysis of forward stimulated Brillouin scattering for acoustic impedance sensing by extraction of a 2nd-order local spectrum

Distributed fiber sensors based on forward stimulated Brillouin scattering(F-SBS)have attracted special attention because of their capability to detect the acoustic impedance of liquid material outside fiber.However,the reported results were based on the extraction of a 1st-order local spectrum,causing the sensing distance to be restricted by pump depletion.Here,a novel post-processing technique was proposed for distributed acoustic impedance sensing by extracting the 2nd-order local spectrum,which is beneficial for improving the sensing signal-to-noise ratio(SNR)significantly,since its pulse energy penetrates into the fiber more deeply.As a proof-of-concept,distributed acoustic impedance sensing along~1630 m fiber under moderate spatial resolution of~20 m was demonstrated.

基于GNSS的前向散射雷达网目标穿越特性研究

前向散射雷达可通过捕获目标穿越基线时引起的信号扰动实现目标检测,在隐身飞机目标探测方面具有一定潜力,目标穿越特性的研究对信号检测和参数估计具有重要意义。首先构建了基于全球导航卫星系统(global navigation satellite system,GNSS)的前向散射雷达网模型,分析了构成前向散射观测的条件和探测范围。然后,基于前向散射动态信号模型,提出采用时频域统计特征描述目标穿越基线的信号特性。最后,通过仿真分析了目标穿越位置和运动参数对散射信号及其统计特征的影响,揭示了前向散射信号的特征变化规律,对后续提高穿越事件检测概率和参数估计精度具有参考价值。

以全球导航卫星系统为辐射源的前向散射雷达发展综述

前向散射雷达(FSR)可获得高水平雷达截面积(RCS)的特性使其在反隐身中占据重要地位。利用全球导航卫星系统(GNSS)作为辐射源,具有全天时全天候全地域覆盖的优势,通过部署多个接收节点可构建地面/海上/空中目标监视网络。该文针对基于GNSS的FSR发展现状,从目标检测、目标参数估计、阴影逆合成孔径雷达(SISAR)成像及目标分类识别等方面对关键技术和现存问题进行概述,并从组网探测、多目标定位、布站优化和极化信息获取等方面对基于GNSS的FSR发展趋势提出展望。