Convergent beam electron diffraction (CBED) is an electron diffraction technique where a convergent or divergent beam (conical electron beam) of electrons is used to study materials.
CBED was first introduced in 1939 by Kossel and Möllenstedt. [1] The development of the Field Emission Gun (FEG) in the 1970s, [2] the Scanning Transmission Electron Microscopy (STEM), energy filtering devices and so on, made possible smaller probe diameters and larger convergence angles, and all this made CBED more popular. In the seventies, CBED was being used for the determination of the point group and space group symmetries by Goodman and Lehmpfuh, [3] and Buxton, [4] and starting in 1985, CBED was used by Tanaka et al. for studying crystals structure. [5] [6] [7] [8] [9]
By using CBED, the following information can be obtained:
where is the distance between the crystallographic planes , is the Bragg angle, is an integer, and is the wavelength of the probing electrons.
Since the diameter of the probing convergent beam is smaller than in the case of a parallel beam, most of the information in the CBED pattern is obtained from very small regions, which other methods cannot reach. For example, in Selected Area Electron Diffraction (SAED), where a parallel beam illumination is used, the smallest area that can be selected is 0.5 μm at 100 kV, whereas in CBED, it is possible to go to areas smaller than 100 nm. [41] Also, the amount of information that is obtained from a CBED pattern is larger than that from a SAED pattern. Nonetheless, CBED also has its disadvantages. The focused probe may generate contamination, which can cause localized stresses. But this was more of a problem in the past, and now, with the high vacuum conditions, one should be able to probe a clean region of the specimen in minutes to hours. Another disadvantage is that the convergent beam may heat or damage the chosen region of the specimen. [42] Since 1939, CBED has been mainly used to study thicker materials.
Recently, CBED was applied to study graphene [43] and other 2D monolayer crystals and van der Waals structures. For 2D crystals, the analysis of CBED patterns is simplified, because the intensity distribution in a CBED disk is directly related to the atomic arrangement in the crystal. The deformations at a nanometer resolution have been retrieved, the interlayer distance of a bilayer crystal has been reconstructed, and so on, by using CBED. [44]
An electron microscope is a microscope that uses a beam of electrons as a source of illumination. They use electron optics that are analogous to the glass lenses of an optical light microscope to control the electron beam, for instance focusing them to produce magnified images or electron diffraction patterns. As the wavelength of an electron can be up to 100,000 times smaller than that of visible light, electron microscopes have a much higher resolution of about 0.1 nm, which compares to about 200 nm for light microscopes. Electron microscope may refer to:
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.
Electron diffraction is a generic term for phenomena associated with changes in the direction of electron beams due to elastic interactions with atoms. It occurs due to elastic scattering, when there is no change in the energy of the electrons. The negatively charged electrons are scattered due to Coulomb forces when they interact with both the positively charged atomic core and the negatively charged electrons around the atoms. The resulting map of the directions of the electrons far from the sample is called a diffraction pattern, see for instance Figure 1. Beyond patterns showing the directions of electrons, electron diffraction also plays a major role in the contrast of images in electron microscopes.
The Ewald sphere is a geometric construction used in electron, neutron, and x-ray diffraction which shows the relationship between:
In physics, the phase problem is the problem of loss of information concerning the phase that can occur when making a physical measurement. The name comes from the field of X-ray crystallography, where the phase problem has to be solved for the determination of a structure from diffraction data. The phase problem is also met in the fields of imaging and signal processing. Various approaches of phase retrieval have been developed over the years.
Electron backscatter diffraction (EBSD) is a scanning electron microscopy (SEM) technique used to study the crystallographic structure of materials. EBSD is carried out in a scanning electron microscope equipped with an EBSD detector comprising at least a phosphorescent screen, a compact lens and a low-light camera. In the microscope an incident beam of electrons hits a tilted sample. As backscattered electrons leave the sample, they interact with the atoms and are both elastically diffracted and lose energy, leaving the sample at various scattering angles before reaching the phosphor screen forming Kikuchi patterns (EBSPs). The EBSD spatial resolution depends on many factors, including the nature of the material under study and the sample preparation. They can be indexed to provide information about the material's grain structure, grain orientation, and phase at the micro-scale. EBSD is used for impurities and defect studies, plastic deformation, and statistical analysis for average misorientation, grain size, and crystallographic texture. EBSD can also be combined with energy-dispersive X-ray spectroscopy (EDS), cathodoluminescence (CL), and wavelength-dispersive X-ray spectroscopy (WDS) for advanced phase identification and materials discovery.
Electron crystallography is a subset of methods in electron diffraction focusing just upon detailed determination of the positions of atoms in solids using a transmission electron microscope (TEM). It can involve the use of high-resolution transmission electron microscopy images, electron diffraction patterns including convergent-beam electron diffraction or combinations of these. It has been successful in determining some bulk structures, and also surface structures. Two related methods are low-energy electron diffraction which has solved the structure of many surfaces, and reflection high-energy electron diffraction which is used to monitor surfaces often during growth.
A scanning transmission electron microscope (STEM) is a type of transmission electron microscope (TEM). Pronunciation is [stɛm] or [ɛsti:i:ɛm]. As with a conventional transmission electron microscope (CTEM), images are formed by electrons passing through a sufficiently thin specimen. However, unlike CTEM, in STEM the electron beam is focused to a fine spot which is then scanned over the sample in a raster illumination system constructed so that the sample is illuminated at each point with the beam parallel to the optical axis. The rastering of the beam across the sample makes STEM suitable for analytical techniques such as Z-contrast annular dark-field imaging, and spectroscopic mapping by energy dispersive X-ray (EDX) spectroscopy, or electron energy loss spectroscopy (EELS). These signals can be obtained simultaneously, allowing direct correlation of images and spectroscopic data.
Phase-contrast imaging is a method of imaging that has a range of different applications. It measures differences in the refractive index of different materials to differentiate between structures under analysis. In conventional light microscopy, phase contrast can be employed to distinguish between structures of similar transparency, and to examine crystals on the basis of their double refraction. This has uses in biological, medical and geological science. In X-ray tomography, the same physical principles can be used to increase image contrast by highlighting small details of differing refractive index within structures that are otherwise uniform. In transmission electron microscopy (TEM), phase contrast enables very high resolution (HR) imaging, making it possible to distinguish features a few Angstrom apart.
Selected area (electron) diffraction is a crystallographic experimental technique typically performed using a transmission electron microscope (TEM). It is a specific case of electron diffraction used primarily in material science and solid state physics as one of the most common experimental techniques. Especially with appropriate analytical software, SAD patterns (SADP) can be used to determine crystal orientation, measure lattice constants or examine its defects.
Low-energy electron microscopy, or LEEM, is an analytical surface science technique used to image atomically clean surfaces, atom-surface interactions, and thin (crystalline) films. In LEEM, high-energy electrons are emitted from an electron gun, focused using a set of condenser optics, and sent through a magnetic beam deflector. The “fast” electrons travel through an objective lens and begin decelerating to low energies near the sample surface because the sample is held at a potential near that of the gun. The low-energy electrons are now termed “surface-sensitive” and the near-surface sampling depth can be varied by tuning the energy of the incident electrons. The low-energy elastically backscattered electrons travel back through the objective lens, reaccelerate to the gun voltage, and pass through the beam separator again. However, now the electrons travel away from the condenser optics and into the projector lenses. Imaging of the back focal plane of the objective lens into the object plane of the projector lens produces a diffraction pattern at the imaging plane and recorded in a number of different ways. The intensity distribution of the diffraction pattern will depend on the periodicity at the sample surface and is a direct result of the wave nature of the electrons. One can produce individual images of the diffraction pattern spot intensities by turning off the intermediate lens and inserting a contrast aperture in the back focal plane of the objective lens, thus allowing for real-time observations of dynamic processes at surfaces. Such phenomena include : tomography, phase transitions, adsorption, reaction, segregation, thin film growth, etching, strain relief, sublimation, and magnetic microstructure. These investigations are only possible because of the accessibility of the sample; allowing for a wide variety of in situ studies over a wide temperature range. LEEM was invented by Ernst Bauer in 1962; however, not fully developed until 1985.
Coherent diffractive imaging (CDI) is a "lensless" technique for 2D or 3D reconstruction of the image of nanoscale structures such as nanotubes, nanocrystals, porous nanocrystalline layers, defects, potentially proteins, and more. In CDI, a highly coherent beam of X-rays, electrons or other wavelike particle or photon is incident on an object.
Kikuchi lines are patterns of electrons formed by scattering. They pair up to form bands in electron diffraction from single crystal specimens, there to serve as "roads in orientation-space" for microscopists uncertain of what they are looking at. In transmission electron microscopes, they are easily seen in diffraction from regions of the specimen thick enough for multiple scattering. Unlike diffraction spots, which blink on and off as one tilts the crystal, Kikuchi bands mark orientation space with well-defined intersections as well as paths connecting one intersection to the next.
Ptychography is a computational method of microscopic imaging. It generates images by processing many coherent interference patterns that have been scattered from an object of interest. Its defining characteristic is translational invariance, which means that the interference patterns are generated by one constant function moving laterally by a known amount with respect to another constant function. The interference patterns occur some distance away from these two components, so that the scattered waves spread out and "fold" into one another as shown in the figure.
Precession electron diffraction (PED) is a specialized method to collect electron diffraction patterns in a transmission electron microscope (TEM). By rotating (precessing) a tilted incident electron beam around the central axis of the microscope, a PED pattern is formed by integration over a collection of diffraction conditions. This produces a quasi-kinematical diffraction pattern that is more suitable as input into direct methods algorithms to determine the crystal structure of the sample.
This is a timeline of crystallography.
There are a variety of technologies available for detecting and recording the images, diffraction patterns, and electron energy loss spectra produced using transmission electron microscopy (TEM).
CrysTBox is a suite of computer tools designed to accelerate material research based on transmission electron microscope images via highly accurate automated analysis and interactive visualization. Relying on artificial intelligence and computer vision, CrysTBox makes routine crystallographic analyses simpler, faster and more accurate compared to human evaluators. The high level of automation together with sub-pixel precision and interactive visualization makes the quantitative crystallographic analysis accessible even for non-crystallographers allowing for an interdisciplinary research. Simultaneously, experienced material scientists can take advantage of advanced functionalities for comprehensive analyses.
4D scanning transmission electron microscopy is a subset of scanning transmission electron microscopy (STEM) which utilizes a pixelated electron detector to capture a convergent beam electron diffraction (CBED) pattern at each scan location. This technique captures a 2 dimensional reciprocal space image associated with each scan point as the beam rasters across a 2 dimensional region in real space, hence the name 4D STEM. Its development was enabled by evolution in STEM detectors and improvements computational power. The technique has applications in visual diffraction imaging, phase orientation and strain mapping, phase contrast analysis, among others.
Dark-field X-ray microscopy 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.