小角X射线散射表征非晶合金纳米尺度结构非均匀

表征纳米尺度结构非均匀对于理解非晶合金的变形、弛豫等动力学行为至关重要.受时空尺度限制,非晶合金纳米尺度结构非均匀的实验表征具有很大的挑战性.本文针对一种典型的锆基非晶合金,开展了同步辐射小角X射线散射原位拉伸实验.通过对散射曲线的定量分析,揭示了非晶合金在纳米尺度的非均匀结构图像.首先,Porod散射曲线呈现正偏离行为,表明非晶合金属于非理想两相散射体系,两相界面弥散且任一相内都存在电子密度涨落.基于散射曲线的Guinier定律分析,进一步揭示非晶合金中散射体形状远偏离球形,其特征尺度主要分布在0.8—1.6 nm之间,且在弹性变形阶段几乎不变.最后,通过Debye相关函数分析,发现这些纳米尺度散射体仅在1 nm之内存在强关联,符合非晶合金短程有序、长程无序的结构特征.研究结果表明非晶合金中存在具有复杂空间分布的纳米尺度非均匀结构.     

Investigation of craze development using small-angle X-ray scattering of synchrotron radiation

The development of crazes in polycarbonate was investigated with the method of ultra-small-angle X-ray scattering (USAXS) of synchrotron radiation. Measurements at different temperatures and with different draw rates were carried out. The two-dimensional scattering patterns were analyzed by means of a fibrillar model of the craze. The geometrical parameters of the craze as a function of the macroscopic draw ratio were determined by using a curve-fitting procedure. From the measured values of the diameter and the mean distance of the fibrils, it is possible to calculate the volume fraction v_f of the fibrils directly. Additional scattering caused by submicrocracks is discussed.     

Small-angle neutron scattering study of structural evolution of different phases in protein solution

Small-angle neutron scattering (SANS) has been used to study the structural evolution of different phases in protein solution leading to crystallization, denaturation and gelation. The protein solution under crystallization mostly consists of monomers and dimers, and higher-mers are not observed as they are perhaps formed in very small numbers. The onset and the rate of crystallization strongly depend on the salt concentration. Protein denaturation on addition of surfactant occurs due to the formation of micelle-like clusters along the unfolded polypeptide chains of the protein. The structure of such protein-surfactant complex is found to be independent of the size of the micelles in their pure surfactant solutions. The structure of temperature-induced protein gels shows a fractal structure. Rheology of these gels shows a strong dependence on varying pH or protein concentration, whereas the structure of such gels is found to be similar.      

Small-angle neutron scattering study of dynamically polarized polyethylenes

We carried out a small-angle neutron scattering (SANS) study of dynamically polarized polyethylene (PE) samples doped with 2,2,6,6-tetramethylpiperidine 1-oxyl (TEMPO). The transmission of the PE with almost fully polarized neutrons (98.5%) increased with increasing the proton polarization, P. The incoherent scattering cross section decreased with increasing P. The effect of P on the polarized neutrons’ transmission and the incoherent scattering cross section agreed well with the theory. The q-dependence of the coherent scattering, which reflects a two-phase structure of PE composed of crystalline and amorphous domains, was kept unchanged by the proton polarization, but the intensity increased by a factor of 3 and 6 for P=+23% and −23%, respectively. The results mean that the contrast between the two phases was successfully enhanced by a dynamic nuclear polarization (DNP) technique. However, the enhancement is only 1/13–1/16 of the enhancement calculated by assuming a homogeneous polarization through the PE sample. The discrepancy suggests that P in amorphous domains (25%) should be higher than that in crystalline domains (22%) by 3%, which in turn may suggest the partial depolarization of proton spins on the way of the spin diffusion from amorphous domains, where TEMPO radicals localize, to crystalline domains.     

Small-angle neutron scattering studies of nonionic surfactant: Effect of sugars

Micellar solution of nonionic surfactantn-dodecyloligo ethyleneoxide surfactant, decaoxyethylene monododecyl ether [CH₃(CH₂)₁₁(OCH₂CH₂)₁₀OH], C₁₂E₁₀ in D₂O solution have been analysed by small-angle neutron scattering (SANS) at different temperatures (30, 45 and 60° C) both in the presence and absence of sugars. The structural parameters like micelle shape and size, aggregation number and micellar density have been determined. It is found that the micellar structure significantly depends on the temperature and concentration of sugars. The micelles are found to be prolate ellipsoids at 30° C and the axial ratio of the micelle increases with the increase in temperature. The presence of lower concentration of sugar reduces the size of micelles and it grows at higher concentration of sugar. The structure of micelles is almost independent of the different types of sugars used.     

Small-angle neutron scattering studies on water soluble complexes of poly(ethylene glycol)-based cationic random copolymer and SDS

The interaction of cationic random copolymers of methoxy poly(ethylene glycol) monomethacrylate and (3-(methacryloylamino)propyl) trimethylammonium chloride with oppositely charged surfactant, sodium dodecyl sulphate, and the influence of surfactant association on the polymer conformation have been investigated by small-angle neutron scattering. SANS data showed a positive indication of the formation of RCPSDS complexes. Even though the complete structure of the polyion complexes could not be ascertained, the results obtained give us the information on the local structure in these polymer-surfactant systems. The data were analysed using the log-normal distribution of the polydispersed spherical aggregate model for the local structure in these complexes. For all the systems the median radius and the polydispersity were found to be in the range of 20 ± 2 Å and 0.6 ± 0.05, respectively.     

Fundamental relationships between deformation-induced surface roughness,critical strain localisation and failure in AA5754-O

This research employs two approaches to characterise the apparent structure observed in localised strain maps constructed from surface topography data acquired from AA5754-O sheet stock that was deformed in three in-plane stretching modes. The first uses a conventional two-point autocorrelation function (ACF), while the second uses the combination of the eigenvalue spectrum associated with each map and information theory. The results from the ACF analysis are inconclusive, implying that this technique lacks the sensitivity necessary to quantify the relationships between multi-point clustering and strain localisation. The information theory-based approach reveals that the relative spectral entropy increases monotonically, attains a maximum and then decreases sharply to the failure strain. This behaviour occurs in all three strain modes and results from two competing processes: one where the formation of structure is favourable and one where it is not. The crossover point is a clear indicator of the onset of critical strain localisation and, therefore, can be regarded as a precursor to failure because once the dominant process shifts, additional strain results in the precipitate formation of a critical strain localisation event.     

Ti-Mo合金氢化物微观缺陷的小角X射线散射研究

采用小角X射线散射(SAXS)方法对Ti-Mo合金氢化物的微观缺陷进行了研究.结果表明,氢化物样品中Mo含量为5at％时,所测定的SAXS强度在高散射角区明显低于其他样品的SAXS强度.氢化物中的晶粒及其内部的亚结构是引起SAXS现象的散射体,而这些亚结构是由合金氢化时引入的大量位错所产生.Mo 含量为5at％合金主要为hcp结构而其他合金为bcc结构,但两种合金氢化后都成为fcc结构的氢化物.据此,认为hcp结构与bcc结构Ti-Mo合金在氢化时氢化物结构相同但引入的位错缺陷特征不同. 关键词： Ti-Mo合金氢化物 小角X射线散射 微观缺陷     

Three-dimensional characterization of fatigue-relevant intermetallic particles in high-strength aluminium alloys using synchrotron X-ray nanotomography

Second-phase particles and small porosities are known to favour fatigue crack initiation in high-strength aluminium alloys 2050-T8 and 7050-T7451. Using high-resolution X-ray tomography (320 nm voxel size), with Paganin reconstruction algorithms, the probability that large clusters of particles contain porosities could be measured for the first time in 3D, as well as precise 3D size distributions. Additional holotomography imaging provided improved spatial resolution (50 nm voxel size), allowing to estimate the probability of finding cracked particles in the as-received material state. The extremely precise 3D shape (including cracks) as well as local chemistry of the particles has been determined. This experiment enabled unprecedented 3D identification of detrimental stress risers relevant for fatigue in as-received aluminium alloys.     

Small-angle polarized neutron scattering study of spherical Fe16N2 nano-particles for magnetic recording tape

We have performed small-angle polarized neutron scattering experiments of spherical Fe₁₆N₂ nano-particles, which are potential candidate materials for high density magnetic recording tape. The results were analyzed based on a core-shell model, and we evaluated the magnetic structure of the particles. The correlation between the magnetic structure and magnetic stability of the particles were discussed in terms of high density recordings.     

Fractal morphology in porous membranes: A small-angle X-Ray scattering investigation

This paper reports the small-angle X-ray scattering (SAXS) study and flow- rate measurements of semipermeable porous polysulfone (PS) and sulfonated polycarbonate-doped polysulfone (SPC-PS) membranes. Flow rates of sodium chloride, sodium sulfate, and polyethylene glycol solutions through these membranes have been measured. For all the solutions, the flux through the SPC-PS membrane was found to be close to 1.65 times that through the PS membrane. SAXS measurements show that the pore morphologies of two membranes are mass fractal in nature with different fractal dimensions. The difference in flow rates through these membranes is explained in terms of porosity and fractal dimension.     

Carbide precipitates in solution-quenched PH13-8 Mo stainless steel: A small-angle neutron scattering investigation

This paper deals with the small-angle neutron scattering (SANS) investigation on solution-quenched PH13-8 Mo stainless steel. From the nature of the variation of the functionality of the profiles for varying specimen thickness and also from the transmission electron microscopy (TEM), it has been established that the small-angle scattering signal predominantly originates from the block-like metallic carbide precipitates in the specimen. The contribution due to double Bragg reflection is not significant in the present case. The single scattering profile has been extracted from the experimental profiles corresponding to different values of specimen thickness. In order to avoid complexity and non-uniqueness of the multi-parameter minimization for randomly oriented polydisperse block-like precipitate model, the data have been analyzed assuming randomly oriented polydisperse cylindrical particle model with a locked aspect ratio.     

软 X射线光学表面散射检测

应用自行研制的软X射线反射率计,分别对不同的反射镜样品,在不同的工作波段以及掠射角下研究了软X射线波段掠入射光学表面的散射。实验结果表明：掠射角增加,波长减小,粗糙度增加,软X射线掠入射表面散射程度加重。     

A simulation study of Tsinghua Thomson scattering X-ray source

Thomson scattering X-ray sources are compact and a?ordable facilities that produce short duration, high brightness X-ray pulses enabling new experimental capacities in ultra-fast science studies, and also medical and industrial applications. Such a facility has been built at the Accelerator Laboratory of Tsinghua University, and upgrade is in progress. In this paper, we present a proposed layout of the upgrade with design parameters by simulation, aiming at high X-ray pulses flux and brightness, and also enabling advanced dynamics studies and applications of the electron beam. Design and construction status of main subsystems are also presented.     

清华汤姆逊散射X射线源初步实验研究

汤姆逊散射X射线源利用高亮度的相对论电子束与超短TW级激光相互作用,能产生能量可调、脉冲长度短（～100飞秒量级）的准单色高能X射线,在超快物理过程研究和医学领域具有广泛的应用前景。清华大学工程物理系加速器实验室正在积极筹建基于光阴极微波电子枪和飞秒强激光的汤姆逊散射实验平台,并利用实验室现有的16MeV返波行波加速器和Nd:YAG纳秒调Q激光系统进行了初步实验研究。在解决实验中出现的电磁干扰和韧致辐射X射线本底干扰等问题后,在实验中测量到了脉宽为6纳秒、脉冲光子产额为1.7x 10^4 的散射光子信号。在本文中将对实验装置和结果进行详细介绍。     

Creep in oriented thermoplastics

Sheets of oriented low-density polyethylene possessing transverse symmetry were prepared by simple tensile drawing at room temperature. The degree of anisotropy was varied by varying the draw ratio. Classic elasticity theory shows that five constants are necessary to characterize the deformation behavior of an elastic material possessing such symmetry. The time-dependent equivalents of these constants have been determined from the simultaneous measurement of longitudinal and lateral strain during tensile creep of specimens cut at 0, 45, and 90 deg to the draw direction. Special creep apparatus, able to handle small, flexible specimens, was developed for this study. The shear compliance obtained from the tensile creep studies was in good agreement with the value obtained from torsional creep measurements on a 0-deg specimen, for the entire range of draw ratios. The contraction measurements have been used to provide additional evidence for deformation mechanisms suggested by the longitudinal strain measurements and, when combined with tensile measurements, have allowed the volume changes occurring during tensile creep to be calculated.     

Small angle X-ray scattering of the colloidal crystal

The monodisperse polystyrene spheres are assembled into the colloidal crystal on the glass substrate by vertical deposition method, which is aimed at the so-called photonic crystal applications. The structural information of the bulk colloidal crystal is crucial for understanding the crystal growth mechanism and devel- oping the various applications of colloidal crystal. Small-angle X-ray scattering （SAXS） technique was used to obtain the bulk structure of the colloidal crystal at Beamline lW2A of BSRF. It is found that the SAXS pattern is sensitive to the relative orientation between the colloidal sample and the incident X-ray direction. The crystal lattice was well distinguished and determined by the SAXS data.     

Small angle X-ray scattering of the colloidal crystal

The monodisperse polystyrene spheres are assembled into the colloidal crystal on the glass substrate by vertical deposition method, which is aimed at the so-called photonic crystal applications. The structural information of the bulk colloidal crystal is crucial for understanding the crystal growth mechanism and developing the various applications of colloidal crystal. Small-angle X-ray scattering (SAXS) technique was used to obtain the bulk structure of the colloidal crystal at Beamline 1W2A of BSRF. It is found that the SAXS pattern is sensitive to the relative orientation between the colloidal sample and the incident X-ray direction. The crystal lattice was well distinguished and determined by the SAXS data.     

A simulation study of Tsinghua Thomson scattering X-ray source

Thomson scattering X-ray sources are compact and affordable facilities that produce short duration, high brightness X-ray pulses enabling new experimental capacities in ultra-fast science studies, and also medical and industrial applications. Such a facility has been built at the Accelerator Laboratory of Tsinghua University, and upgrade is in progress. In this paper, we present a proposed layout of the upgrade with design parameters by simulation, aiming at high X-ray pulses flux and brightness, and also enabling advanced dynamics studies and applications of the electron beam. Design and construction status of main subsystems are also presented.     

X射线汤姆孙散射在温稠密物质研究中的应用

温稠密物质(warm dense matter,WDM)是近年来兴起的一个前沿研究领域,它处于传统的凝聚态与等离子体状态之间的过渡状态.此状态下的物质广泛存在于宇宙和实验室中,如巨行星的内核、惯性约束聚变的内爆燃料等.然而人们对温稠密物质又是陌生的,因为传统的凝聚态和等离子体物理的理论和实验方法难以用于研究这样的物质状态.近几年,随着高功率激光装置以及诊断技术的发展,人们发展出X射线汤姆孙散射方法,对温稠密态物质开展了深入的研究,获得了重要的实验结果.