Dark-field X-ray microscopy

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Dark-field X-ray microscopy (DFXM [1] or DFXRM [2] ) is an imaging technique used for multiscale structural characterisation. It is capable of mapping deeply embedded structural elements with nm-resolution using synchrotron X-ray diffraction-based imaging. The technique works by using scattered X-rays to create a high degree of contrast, and by measuring the intensity and spatial distribution of the diffracted beams, it is possible to obtain a three-dimensional map of the sample's structure, orientation, and local strain.

Contents

History

The first experimental demonstration of dark-field X-ray microscopy was reported in 2006 by a group at the European Synchrotron Radiation Facility in Grenoble, France. Since then, the technique has been rapidly evolving and has shown great promise in multiscale structural characterization. [1] Its development is largely due to advances in synchrotron X-ray sources, which provide highly collimated and intense beams of X-rays. The development of dark-field X-ray microscopy has been driven by the need for non-destructive imaging of bulk crystalline samples at high resolution, and it continues to be an active area of research today. However, dark-field microscopy, [3] [4] dark-field scanning transmission X-ray microscopy, [5] and soft dark-field X-ray microscopy [6] has long been used to map deeply embedded structural elements.

Principles and instrumentation

A monochromatic beam from a synchrotron source illuminates the sample. Objective is the objective lens and Detector is the 2D area detector Principle of dark-field X-ray microscopy.webp
A monochromatic beam from a synchrotron source illuminates the sample. Objective is the objective lens and Detector is the 2D area detector

In this technique, a synchrotron light source is used to generate an intense and coherent X-ray beam, which is then focused onto the sample using a specialized objective lens. The objective lens acts as a collimator to select and focus the scattered light, which is then detected by the 2D detector to create a diffraction pattern. [1] The specialized objective lens in DFXM, referred to as an X-ray objective lens, is a crucial component of the instrumentation required for the technique. It can be made from different materials such as beryllium, silicon, and diamond, depending on the specific requirements of the experiment. [8] The objective enables one to enlarge or reduce the spatial resolution and field of view within the sample by varying the number of individual lenses and adjusting and (as in the figure) correspondingly. The diffraction angle is typically 10–30°. [9] [10]

The sample is positioned at an angle such that the direct beam is blocked by a beam stop or aperture, and the diffracted beams from the sample are allowed to pass through a detector. [11]

An embedded crystalline element (for example, a grain or domain) of choice (green) is aligned such that the detector is positioned at a Bragg angle that corresponds to a particular diffraction peak of interest, which is determined by the crystal structure of the sample. The objective magnifies the diffracted beam by a factor and generates an inverted 2D projection of the grain. Through repeated exposures during a 360° rotation of the element around an axis parallel to the diffraction vector, , several 2D projections of the grain are obtained from various angles. [12] A 3D map is then obtained by combining these projections using reconstruction algorithms [13] similar to those developed for CT scanning. If the lattice of the crystalline element exhibits an internal orientation spread, this procedure is repeated for a number of sample tilts, indicated by the angles and . [1]

The current implementation of DFXM at ID06, ESRF, uses a compound refractive lens (CRL) as the objective, giving spatial resolution of 100 nm and angular resolution of 0.001°. [14] [15]

Applications, limitations and alternatives

Current and potential applications

Multiscale mapping of 10% tensile deformed aluminium. (a) Part of the X-ray mapping of all grains in the specimen. (b) Zooming in on one embedded grain and mapping the intrinsic variation in orientation. A vertical section through the grain is shown for ease of inspection of the spatial heterogeneity. (c) Condensing the incoming beam vertically defines a sub-micron layer within the grain. Below: The corresponding keys for the orientation maps Multiscale mapping of 10%25 tensile deformed aluminium.webp
Multiscale mapping of 10% tensile deformed aluminium. (a) Part of the X-ray mapping of all grains in the specimen. (b) Zooming in on one embedded grain and mapping the intrinsic variation in orientation. A vertical section through the grain is shown for ease of inspection of the spatial heterogeneity. (c) Condensing the incoming beam vertically defines a sub-micron layer within the grain. Below: The corresponding keys for the orientation maps

DFXM has been used for the non-destructive investigation of polycrystalline materials and composites, revealing the 3D microstructure, [16] phases, [17] orientation of individual grains, [18] [19] and local strains. [20] [21] It has also been used for in situ studies of materials recrystallisation, [22] dislocations [23] [24] and other defects, and the deformation [20] and fracture mechanisms in materials, such as metals [11] and composites. [25] DFXM can provide insights into the 3D microstructure and deformation of geological materials such as minerals and rocks, [1] and irradiated materials. [26]

DFXM has the potential to revolutionise the field of nanotechnology by providing non-destructive, high-resolution 3D imaging of nanostructures and nanomaterials. It has been used to investigate the 3D morphology of nanowires and to detect structural defects in nanotubes. [27] [28]

DFXM has shown potential for imaging biological tissues and organs with high contrast and resolution. It has been used to visualize the 3D microstructure of cartilage and bone, as well as to detect early-stage breast cancer in mouse model. [1] [29]

Limitations

The intense X-ray beams used in DFXM can damage delicate samples, particularly biological specimens. [1] DFXM can suffer from imaging artefacts such as ring artefacts, which can affect image quality and limit interpretation. [11]

The instrumentation required for DFXM is expensive and typically only available at synchrotron facilities, making it inaccessible to many researchers. Although DFXM can achieve high spatial resolution, it is still not as high as the resolution achieved by other imaging techniques such as transmission electron microscopy (TEM) or X-ray crystallography. [11]

Preparation of samples for DFXM imaging can be challenging, especially for samples that are not crystalline. There are also limitations on the sample size that can be imaged as the technique works best with thin samples, typically less than 100 microns thick, due to the attenuation of the X-ray beam by thicker samples. [1] DFXM still suffers from long integration times, which can limit its practical applications. This is due to the low flux density of X-rays emitted by synchrotron sources and the high sensitivity required to detect scattered X-rays. [11]

Alternatives

There are several alternative techniques to DFXM, depending on the application, some of which are:

Related Research Articles

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<span class="mw-page-title-main">Transmission electron microscopy</span> Imaging and diffraction using electrons that pass through samples

Transmission electron microscopy (TEM) is a microscopy technique in which a beam of electrons is transmitted through a specimen to form an image. The specimen is most often an ultrathin section less than 100 nm thick or a suspension on a grid. An image is formed from the interaction of the electrons with the sample as the beam is transmitted through the specimen. The image is then magnified and focused onto an imaging device, such as a fluorescent screen, a layer of photographic film, or a detector such as a scintillator attached to a charge-coupled device or a direct electron detector.

<span class="mw-page-title-main">Synchrotron light source</span> Particle accelerator designed to produce intense x-ray beams

A synchrotron light source is a source of electromagnetic radiation (EM) usually produced by a storage ring, for scientific and technical purposes. First observed in synchrotrons, synchrotron light is now produced by storage rings and other specialized particle accelerators, typically accelerating electrons. Once the high-energy electron beam has been generated, it is directed into auxiliary components such as bending magnets and insertion devices in storage rings and free electron lasers. These supply the strong magnetic fields perpendicular to the beam that are needed to stimulate the high energy electrons to emit photons.

<span class="mw-page-title-main">X-ray microscope</span> Type of microscope that uses X-rays

An X-ray microscope uses electromagnetic radiation in the X-ray band to produce magnified images of objects. Since X-rays penetrate most objects, there is no need to specially prepare them for X-ray microscopy observations.

<span class="mw-page-title-main">Electron backscatter diffraction</span> Scanning electron microscopy technique

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<span class="mw-page-title-main">Scanning transmission electron microscopy</span> Scanning microscopy using thin samples and transmitted electrons

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<span class="mw-page-title-main">Low-energy electron microscopy</span>

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