同步辐射技术在核材料研究中的应用

先进同步辐射光源具有高通量、高相干性、高脉冲重复率等优点,将基于其的X射线衍射、小角散射、成像、谱学等表征方法与原位环境(如温度场、应力场、气氛、溶液介质等)实验装置配合,可为系统表征与评价核能系统用材料与部件的服役行为和损伤机制提供重要技术手段.核材料在高温/应力/介质/中子辐照等复杂多场环境下的服役损伤行为长期以来...     

New opportunities for 3D materials science of polycrystalline materials at the micrometre lengthscale by combined use of X-ray diffraction and X-ray imaging

Non-destructive, three-dimensional (3D) characterization of the grain structure in mono-phase polycrystalline materials is an open challenge in material science. Recent advances in synchrotron based X-ray imaging and diffraction techniques offer interesting possibilities for mapping 3D grain shapes and crystallographic orientations for certain categories of polycrystalline materials. Direct visualisation of the three-dimensional grain boundary network or of two-phase (duplex) grain structures by means of absorption and/or phase contrast techniques may be possible, but is restricted to specific material systems. A recent extension of this methodology, termed X-ray diffraction contrast tomography (DCT), combines the principles of X-ray diffraction imaging, three-dimensional X-ray diffraction microscopy (3DXRD) and image reconstruction from projections. DCT provides simultaneous access to 3D grain shape, crystallographic orientation and local attenuation coefficient distribution. The technique applies to the larger range of plastically undeformed, polycrystalline mono-phase materials, provided some conditions on grain size and texture are fulfilled. The straightforward combination with high-resolution microtomography opens interesting new possibilities for the observation of microstructure related damage and deformation mechanisms in these materials.     

Synchrotron‐Based Micro‐CT and Refraction‐Enhanced Micro‐CT for Non‐Destructive Materials Characterisation

X‐ray computed tomography is an important tool for non‐destructively evaluating the 3‐D microstructure of modern materials. To resolve material structures in the micrometer range and below, high brilliance synchrotron radiation has to be used. The Federal Institute for Materials Research and Testing (BAM) has built up an imaging setup for micro‐tomography and ‐radiography (BAMline) at the Berliner storage ring for synchrotron radiation (BESSY). In computed tomography, the contrast at interfaces within heterogeneous materials can be strongly amplified by effects related to X‐ray refraction. Such effects are especially useful for materials of low absorption or mixed phases showing similar X‐ray absorption properties that produce low contrast. The technique is based on ultra‐small‐angle scattering by microstructural elements causing phase‐related effects, such as refraction and total reflection. The extraordinary contrast of inner surfaces is far beyond absorption effects. Crack orientation and fibre/matrix debonding in plastics, polymers, ceramics and metal‐matrix‐composites after cyclic loading and hydro‐thermal aging can be visualized. In most cases, the investigated inner surface and interface structures correlate to mechanical properties. The technique is an alternative to other attempts on raising the spatial resolution of CT machines.     

A new bridge technique for neutron tomography and diffraction measurements

An attractive feature of neutron techniques is the ability to identify hidden materials and structures inside engineering components and objects of art and archaeology. Bearing this in mind we are investigating a new technique, “Tomography Driven Diffraction” (TDD), that exploits tomography data to guide diffraction experiments on samples with complex structures and shapes. The technique can be used utilising combinations of individual tomography and diffraction instruments, such as NEUTRA (PSI, CH) and ENGIN-X (ISIS, UK), but is also suitable for new combined imaging and diffraction instruments such as the JEEP synchrotron engineering instrument (DIAMOND, UK) and the proposed IMAT neutron imaging and diffraction instrument (ISIS, UK).     

Direct tomography with chemical-bond contrast

Three-dimensional (3D) X-ray imaging methods have advanced tremendously during recent years. Traditional tomography uses absorption as the contrast mechanism, but for many purposes its sensitivity is limited. The introduction of diffraction, small-angle scattering, refraction, and phase contrasts has increased the sensitivity, especially in materials composed of light elements (for example, carbon and oxygen). X-ray spectroscopy, in principle, offers information on element composition and chemical environment. However, its application in 3D imaging over macroscopic length scales has not been possible for light elements. Here we introduce a new hard-X-ray spectroscopic tomography with a unique sensitivity to light elements. In this method, dark-field section images are obtained directly without any reconstruction algorithms. We apply the method to acquire the 3D structure and map the chemical bonding in selected samples relevant to materials science. The novel aspects make this technique a powerful new imaging tool, with an inherent access to the molecular-level chemical environment.     

Emerging X-ray imaging technologies for energy materials

With the growing need for sustainable energy technologies, advanced characterization methods become more and more critical for optimizing energy materials and understanding their operation mechanisms. In this review, we focus on the synchrotron-based X-ray imaging technologies and the associated applications in gaining fundamental insights into the physical/chemical properties and reaction mechanisms of energy materials. We will discuss a few major X-ray imaging technologies, including X-ray projection imaging, transmission X-ray microscopy, scanning transmission X-ray microscopy, tender and soft X-ray imaging, and coherent diffraction imaging. Researchers can choose from various X-ray imaging techniques with different working principles based on research goals and sample specifications. With the X-ray imaging techniques, we can obtain the morphology, phase, lattice and strain information of energy materials in both 2D and 3D in an intuitive way. In addition, with the high-penetration X-rays and the high-brilliance synchrotron sources, operando/in-situ experiments can be designed to track the qualitative and quantitative changes of the samples during operation. We expect this review can broaden readers’ view on X-ray imaging techniques and inspire new ideas and possibilities in energy materials research.     

High-speed synchrotron X-ray phase contrast imaging for analysis of low-Z composite microstructure

The study of high performance composites such as plastic-bonded explosives under extreme conditions often requires innovative experimental techniques. Here, static synchrotron X-ray phase-contrast imaging (PCI) of simulated explosive materials has been performed at high speed in an effort to determine feasibility of imaging material response to dynamic, high-strain rate events (10²–10⁷ s^?1). The microstructure of pristine materials, idealized composites and simulated explosive composites has been characterized with synchrotron PCI at the Advanced Photon Source. High spatial resolution (2 μm) of the microstructure was achieved with 5 μs exposures, and features such as interfaces, cracks, voids, and bubbles were clearly observed. The likelihood of obtaining sufficient phase information at even faster exposures (e.g., 0.2–0.5 μs) is shown to be high.     

Application of X-ray refraction topography to fibre reinforced plastics

The effect of X-ray refraction employs an unconventional small angle X-ray scattering (SAXS) technique which has been developed and applied to meet actual problems for improved non-destructive characterisation of advanced materials. The X-ray refraction technique makes use of X-ray optical effects at micro interfaces of composite materials. This method reveals the inner surface and interface concentrations in nanometer dimensions due to the short X-ray wavelength near 10⁻⁴ μm. Sub-micron crack and pore sizes are easily determined by “X-ray refractometry” without destroying the structure by cutting or polishing for microscopic techniques. The non-destructive characterisation of microfailure e.g. voids, fibre debonding, fibre cracks and microcracks of a short glass fibre reinforced polyoximethylene (POM-GF) after mechanical loading and accelerated ageing is investigated. X-ray refraction topographs are illustrated, showing the damage accumulation of POM-GF specimens after the fatigue test.     

高分辨三维成像原位试验机研制进展及应用

先进材料及结构的损伤表征和在役性能评价是重大装备研发与服役中的关键科学问题。目前,依托同步辐射大科学装置的X射线三维成像技术在金属材料细观损伤力学行为研究方面具有独特优势,而兼容于同步辐射光源相应光束线站的各类原位加载装置对材料内部微结构损伤演化的动态高分辨表征具有重要意义。简要介绍了国内外依托世界各大高性能光源的原位加载试验机研制进展与应用成果,重点阐述了可实现单向拉压、循环加载及具备极寒、高温、真空等样品环境的基于同步辐射X射线成像的原位加载装置的设计原理及结构特点。最后,结合第三代高能X射线三维成像技术特点、先进光源线站建设、高通量试验要求等,对材料原位加载条件下的高时空分辨率动态成像进行了展望,指出开发集拉伸、压缩、低周疲劳、高周疲劳和超高周疲劳加载机构于一体的多功能原位试验机是一项重要的工作。     

X射线成像术(上)

该文着重从衬度的形成讨论了X射线成像。介绍衬度生成的三种机制:吸收、位相变动和衍射。还介绍了成像设备的主要构成部件:X射线源(X射线发生器、直线加速器和同步辐射),各类探测器、像增强器与显示器,机械、控制与数据处理系统等;应用各种衬度形成的一些成像方法也作了简述,如利用吸收衬度的造影成像、数字减影和双色减影成像、计算机断层成像;利用相位衬度的干涉仪法、类同轴全息法和衍射增强法;利用衍射衬度的Lang透射法和Berg-Barrett反射法等,并用少量例子说明。     

X射线成像术(下)

该文的前半部分(本刊上一期)已扼要介绍了X射线成像的三种衬度机制及成像设备各主要组件的构造,下半部分将继续介绍应用各种衬度的不同的成像方法和一些实例。     

Physical properties and biocompatibility of UHMWPE-derived materials modified by synchrotron radiation

The applications of synchrotron radiation (SR) in medical imaging have become of great use, particularly in angiography, bronchography, mammography, computed tomography, and X-ray microscopy. Thanks to recently developed phase contrast imaging techniques non-destructive preclinical testing of low absorbing materials such as polymers has become possible. The focus of the present work is characterization and examination of UHMWPE-derived materials widely used in medicine, before and after their exposure to SR during such testing. Physical properties, such as wettability, surface energy, IR-spectroscopy, roughness, optical microscopy, microhardness measurements of UHMWPE samples were studied before and after SR. The relationship between a growth of UHMWPE surface hydrophilicity after SR and surface colonization by stromal cells was studied in vitro. Obtained results demonstrate that SR may be used as prospective direction to examine bulk (porous) structure of polymer materials and/or to modify polymer surface and volume for tissue engineering.     

Critical assessment 20: on carbon excess in bainitic ferrite

For several decades, the question of carbon supersaturation in bainitic ferrite has attracted the attention of physical metallurgists. Originally, this was associated with excess carbon due to the displacive nature of phase transformation and its subsequent trapping at defects in bainitic ferrite. The development of advanced experimental techniques, such as atom probe tomography and in situ synchrotron and neutron X-ray diffraction, has provided new insights into carbon distribution within bainitic ferrite. Possible explanations for carbon excess in solid solution are discussed, and the pathways for the future advancement of this research question are suggested.     

Probing deformation substructure by synchrotron X-ray diffraction and dislocation dynamics modelling

Materials characterization at the nano-scale is motivated by the desire to resolve the structural aspects and deformation behavior at length scales relevant to those mechanisms that define the novel and unusual properties of nano-structured materials. A range of novel techniques has recently become accessible with the help of synchrotron X-ray beams that can be focused down to spot sizes of less than a few microns on the sample. The unique combination of tunability (energy selection), parallelism and brightness of synchrotron X-ray beams allows their use for high resolution diffraction (determination of crystal structure and transformations, analysis of dislocation sub-structures, orientation and texture analysis, strain mapping); small angle X-ray scattering (analysis of nano-scale voids and defects; orientation analysis) and imaging (radiography and tomography). After a brief review of the state-of-the-art capabilities for monochromatic and white beam synchrotron diffraction, we consider the usefulness of these techniques for the task of bridging the gap between experiment and modeling. Namely, we discuss how the experiments can be configured to provide information relevant to the validation and improvement of modeling approaches, and also how the results of various simulations can be post-processed to improve the possibility of (more or less) direct comparison with experiments. Using the example of some recent experiments carried out on beamline 116 at Diamond Light Source near Oxford, we discuss how such experimental results can be interpreted in view and in conjunction with numerical deformation models, particularly those incorporating dislocation effects, e.g., finite-element based pseudo-continuum strain gradient formulations, and discrete dislocation simulations. Post-processing of FE and discrete dislocation simulations is described, illustrating the kind of information that can be extracted from comparisons between modeling and experimental data.     

Monitoring elastic strain and damage by neutron and synchrotron X-ray beams

Abstract

Large scale neutron and synchrotron X-ray facilities have been providing important information for physicists and chemists for many decades. Increasingly, materials engineers are finding that these facilities can also provide important information non-destructively. Highly penetrating neutron and X-ray synchrotron beams provide the materials engineer with a means of obtaining information about the state of stress and damage deep within materials. The principles underlying the elastic strain measurement and damage characterisation techniques are introduced. The capabilities of the methods are illustrated through a number of practical applications including: mapping damage and stress transfer fibre by fibre in continuous fibre reinforced composites during loading, measurement of residual stresses in welding, the use of measurements to refine finite element models, and creep cavitation cracking in power plant steels.     

An investigation of mortars affected by alkali-silica reaction by X-ray synchrotron microtomography: a preliminary study

A first attempt to investigate samples affected by alkali-silica reaction (ASR) by synchrotron X-ray microtomography has been made. The setup available at the SYRMEP beamline, at the third generation synchrotron Elettra (Trieste, Italy), allowed collecting phase-contrast enhanced images, with a detectability approaching that of optical microscopy (a few microns). In this study, mortar cylinders were prepared and immersed in a 1-M NaOH solution at 80 °C for 14 days to enhance the ASR. The weathered samples were studied using the traditional 2D techniques such as optical microscopy and scanning electron microscopy as well as using the 3D micro-CT. Over the aged samples, the 3D imaging allows the ASR weathering to be studied, showing the reactive aggregate progressive dissolution with subsequent deposition of gel and microcracks development. This technique has proven to be a valuable, non-destructive, method which allows the rendering of the microstructural features in specimen affected by ASR.     

Void growth and coalescence in model materials investigated by high-resolution X-ray microtomography

The influences of work hardening behavior of materials on ductile fracture, and especially on void growth and coalescence, have been investigated in model materials by in-situ X-ray computed tomography (XCT) coupled with tensile deformation. The model materials contain an artificial void array embedded in a metal matrix. By producing such materials with different metal matrices (pure copper, brass, Glidcop = copper strengthened by $\text{ Al}_{2}\text{ O}_{3}$ nanoparticles), the influences of the work hardening behaviors on void growth and coalescence/linkage process are analyzed. This set of experiments were performed at Japanese synchrotron radiation facility SPring-8 BL20XU beamline, whereby the X-ray tomography setup with one of the highest spatial resolution in the world is available. This beamline however provides less brilliant X-rays compared to the ESRF ID15 beamline where the our previous experiments were performed Hosokava et al. (Acta Mater, 60:2829–2839, 2012), (Acta Mater, 61:1021–1036, 2013). To compensate for the X-ray absorption problems, the specimens to be tested have to be much smaller, making the experiments more difficult. Nevertheless, the growth and linkage behaviors of the artificial voids were successfully visualized, and the plastic strain whereby the linkage takes place (referred to as the linkage strain, hereafter) were quantitatively captured. The models for void coalescence developed by Thomason and by Pardoen and Hutchinson both predict coalescence rather well for both brass and Glidcop, even though the linkage events were found to be dominated by the meso/macro shear localization process.     

同步辐射小角X射线散射及其在材料研究中的应用

小角X射线散射(small angle X-ray scattering,SAXS)是研究物质内部一纳米到数百纳米甚至到微米尺度级别微观结构的有力工具.近年来随着我国同步辐射技术的不断发展,同步辐射SAXS技术被越来越多地应用到各种材料的研究领域.然而,由于SAXS图谱是倒空间的信号,并不像显微镜那么直观,也不如X射线...     

X-ray tomography applied to the characterization of cellular materials. Related finite element modeling problems

The analyses of several materials exhibiting a cellular structure have been carried out using X-ray tomography. This new technique allows the three dimensional and non destructive visualisation of the studied materials at the scale of their cellular microstructure. Qualitative examples are given for metal foams, bread and cellular concrete. The similarity between these materials is striking. It has been measured by quantitative 3D image processing. The different Finite Element Methods available today to produce meshes from these images are presented and discussed in the final part of this paper.     

On coherence in neutron imaging

The variety of imaging signals in neutron radiography and tomography became quite large compared to the pure absorption and scattering contrast in neutron radiographies and topographies in the early sixties or seventies of the last century. The diversity of absorption based techniques for neutron radiography and tomography is comparable to coherence based imaging techniques such as phase contrast, differential phase contrast, dark field imaging, diffraction enhanced contrast, refraction contrast, ultra small angle scattering contrast, grating interferometry and crystal interferometry, also the spin of the neutron was successfully used for imaging [1], [2], [3], [4], [5], [6], [7], [8], [9], [10], [11] and [12]. We show which effects (total reflection, diffraction, refraction) contribute to e.g. a step boundary or a phase boundary. Taking this simple object, one can learn to understand the imaging procedure and what is displayed in a radiograph.