Energy-dispersive X-ray spectroscopy (also known as EDS, EDX, or EDXA) is a powerful technique that enables the user to analyze the elemental composition of a desired sample. The major operating principle that allows EDS to function is the capacity of high energy electromagnetic radiation (X-rays) to eject 'core' electrons (electrons that are. The Energy Dispersive X-ray (EDX) microanalysis is a technique of elemental analysis associated to electron microscopy based on the generation of characteristic Xrays that reveals the presence of.
Interaction of an electron beam with a sample target produces a variety of emissions, including x-rays. An energy-dispersive (EDS) detector is used to separate the characteristic x-rays of different elements into an energy spectrum, and EDS system software is used to analyze the energy spectrum in order to determine the abundance of specific elements. EDS can be used to find the chemical composition of materials down to a spot size of a few microns, and to create element composition maps over a much broader raster area. Together, these capabilities provide fundamental compositional information for a wide variety of materials.
How it Works - EDS
EDS systems are typically integrated into either an SEM or EPMA instrument. EDS systems include a sensitive x-ray detector, a liquid nitrogen dewar for cooling, and software to collect and analyze energy spectra. The detector is mounted in the sample chamber of the main instrument at the end of a long arm, which is itself cooled by liquid nitrogen. The most common detectors are made of Si(Li) crystals that operate at low voltages to improve sensitivity, but recent advances in detector technology make availabale so-called 'silicon drift detectors' that operate at higher count rates without liquid nitrogen cooling.
An EDS detector contains a crystal that absorbs the energy of incoming x-rays by ionization, yielding free electrons in the crystal that become conductive and produce an electrical charge bias. The x-ray absorption thus converts the energy of individual x-rays into electrical voltages of proportional size; the electrical pulses correspond to the characteristic x-rays of the element.
Energy Dispersive X-ray Spectroscopy Pdf
Strengths
- When used in 'spot' mode, a user can acquire a full elemental spectrum in only a few seconds. Supporting software makes it possible to readily identify peaks, which makes EDS a great survey tool to quickly identify unknown phases prior to quantitative analysis.
- EDS can be used in semi-quantitative mode to determine chemical composition by peak-height ratio relative to a standard.
Limitations
- There are energy peak overlaps among different elements, particularly those corresponding to x-rays generated by emission from different energy-level shells (K, L and M) in different elements. For example, there are close overlaps of Mn-Kα and Cr-Kβ, or Ti-Kα and various L lines in Ba. Particularly at higher energies, individual peaks may correspond to several different elements; in this case, the user can apply deconvolution methods to try peak separation, or simply consider which elements make 'most sense' given the known context of the sample.
- Because the wavelength-dispersive (WDS) method is more precise and capable of detecting lower elemental abundances, EDS is less commonly used for actual chemical analysis although improvements in detector resolution make EDS a reliable and precise alternative.
- EDS cannot detect the lightest elements, typically below the atomic number of Na for detectors equipped with a Be window. Polymer-based thin windows allow for detection of light elements, depending on the instrument and operating conditions.
X-ray Minecraft
Results
A typical EDS spectrum is portrayed as a plot of x-ray counts vs. energy (in keV). Energy peaks correspond to the various elements in the sample. Generally they are narrow and readily resolved, but many elements yield multiple peaks. For example, iron commonly shows strong Kα and Kβ peaks. Elements in low abundance will generate x-ray peaks that may not be resolvable from the background radiation.
References
- Severin, Kenneth P., 2004, Energy Dispersive Spectrometry of Common Rock Forming Minerals. Kluwer Academic Publishers, 225 p.--Highly recommended reference book of representative EDS spectra of the rock-forming minerals, as well as practical tips for spectral acquisition and interpretation.
- Goldstein, J. (2003) Scanning electron microscopy and x-ray microanalysis. Kluwer Adacemic/Plenum Pulbishers, 689 p.
- Reimer, L. (1998) Scanning electron microscopy : physics of image formation and microanalysis. Springer, 527 p.
- Egerton, R. F. (2005) Physical principles of electron microscopy : an introduction to TEM, SEM, and AEM. Springer, 202.
- Clarke, A. R. (2002) Microscopy techniques for materials science. CRC Press (electronic resource)
Related Links
- Petroglyph--An atlas of images using electron microscope, backscattered electron images, element maps, energy dispersive x-ray spectra, and petrographic microscope-- Eric Chrisensen, Brigham Young University
Teaching Activities
- Argast, Anne and Tennis, Clarence F., III, 2004, A web resource for the study of alkali feldspars and perthitic textures using light microscopy, scanning electron microscopy and energy dispersive X-ray spectroscopy, Journal of Geoscience Education 52, no. 3, p. 213-217.
Physical Underpinnings
In the quantum mechanical model of the atom, an electron’s energy state is defined by a set of quantum numbers. The primary quantum number, n, provides the coarsest description of the electron’s energy level, and all the sublevels that share the same primary quantum number are sometimes said to comprise an energy “shell.” Instead of describing the lowest-energy shell as the “n = 1 shell,” it is more common in spectroscopy to use alphabetical labels: The K shell has n = 1, the L shell has n = 2, the M shell has n = 3, and so on. Subsequent quantum numbers divide the shells into subshells: one for K, three for L, and five for M. Increasing primary quantum numbers correspond with increasing average distance from the nucleus and increasing energy (Figure (PageIndex{1})). An atom’s core shells are those with lower primary quantum numbers than the highest occupied shell, or valence shell.
Transitions between energy levels follow the law of conservation of energy. Excitation of an electron to a higher energy state requires an input of energy from the surroundings, and relaxation to a lower energy state releases energy to the surroundings. One of the most common and useful ways energy can be transferred into and out of an atom is by electromagnetic radiation. Core shell transitions correspond to radiation in the X-ray portion of the spectrum; however, because the core shells are normally full by definition, these transitions are not usually observed.
X-ray spectroscopy uses a beam of electrons or high-energy radiation (see instrument variations, below) to excite core electrons to high energy states, creating a low-energy vacancy in the atoms’ electronic structures. This leads to a cascade of electrons from higher energy levels until the atom regains a minimum-energy state. Due to conservation of energy, the electrons emit X-rays as they transition to lower energy states. It is these X-rays that are being measured in X-ray spectroscopy. The energy transitions are named using the letter of the shell where ionization first occurred, a Greek letter denoting the group of lines that transition belongs to, in order of decreasing importance, and a numeric subscript ranking the peak's the intensity within that group. Thus, the most intense peak resulting from ionization in the K shell would be Kα1 (Figure (PageIndex{2})). Since each element has a different nuclear charge, the energies of the core shells and, more importantly, the spacing between them vary from one element to the next. While not every peak in an element’s spectrum is exclusive to that element, there are enough characteristic peaks to be able to determine composition of the sample, given sufficient resolving power.