Acronym | WDXS WDS |
---|---|
Classification | Spectroscopy |
Analytes | Elements in solids, liquids, powders and thin films |
Manufacturers | Anton Paar, Bruker AXS, Hecus, Malvern Panalytical, Rigaku Corporation, Xenocs, CAMECA, JEOL, Oxford Instruments |
Other techniques | |
Related | Energy-dispersive X-ray spectroscopy |
Wavelength-dispersive X-ray spectroscopy (WDXS or WDS) is a non-destructive analysis technique used to obtain elemental information about a range of materials by measuring characteristic x-rays within a small wavelength range. The technique generates a spectrum in which the peaks correspond to specific x-ray lines and elements can be easily identified. WDS is primarily used in chemical analysis, wavelength dispersive X-ray fluorescence (WDXRF) spectrometry, electron microprobes, scanning electron microscopes, and high precision experiments for testing atomic and plasma physics.
Wavelength-dispersive X-ray spectroscopy is based on known principles of how the characteristic x-rays are generated by a sample and how the x-rays are measured.
X-rays are generated when an electron beam of high enough energy dislodges an electron from an inner orbital within an atom or ion, creating a void. This void is filled when an electron from a higher orbital releases energy and drops down to replace the dislodged electron. The energy difference between the two orbitals is characteristic of the electron configuration of the atom or ion and can be used to identify the atom or ion. [1]
According to Bragg's law, when an X-ray beam of wavelength "λ" strikes the surface of a crystal at an angle "Θ" and the crystal has atomic lattice planes a distance "d" apart, then constructive interference will result in a beam of diffracted x-rays that will be emitted from the crystal at angle "Θ" if
This means that a crystal with a known lattice size will deflect a beam of x-rays from a specific type of sample at a pre-determined angle. The x-ray beam can be measured by placing a detector (usually a scintillation counter or a proportional counter) in the path of the deflected beam and, since each element has a distinctive x-ray wavelength, multiple elements can be determined by having multiple crystals and multiple detectors. [1]
To improve accuracy the x-ray beams are usually collimated by parallel copper blades called a Söller collimator. The single crystal, the specimen, and the detector are mounted precisely on a goniometer with the distance between the specimen and the crystal equal to the distance between the crystal and the detector. It is usually operated under vacuum to reduce the absorption of soft radiation (low-energy photons) by the air and thus increase the sensitivity for the detection and quantification of light elements (between boron and oxygen). The technique generates a spectrum with peaks corresponding to x-ray lines. This is compared with reference spectra to determine the elemental composition of the sample. [2]
As the atomic number of the element increases so there are more possible electrons at different energy levels that can be ejected resulting in x-rays with different wavelengths. This creates spectra with multiple lines, one for each energy level. The largest peak in the spectrum is labelled Kα, the next Kβ, and so on.
Applications include analysis of catalysts, cement, food, metals, mining and mineral samples, petroleum, plastics, semiconductors, and wood. [3]
Spectroscopy is the field of study that measures and interprets the electromagnetic spectra that result from the interaction between electromagnetic radiation and matter as a function of the wavelength or frequency of the radiation. Matter waves and acoustic waves can also be considered forms of radiative energy, and recently gravitational waves have been associated with a spectral signature in the context of the Laser Interferometer Gravitational-Wave Observatory (LIGO).
Auger electron spectroscopy is a common analytical technique used specifically in the study of surfaces and, more generally, in the area of materials science. It is a form of electron spectroscopy that relies on the Auger effect, based on the analysis of energetic electrons emitted from an excited atom after a series of internal relaxation events. The Auger effect was discovered independently by both Lise Meitner and Pierre Auger in the 1920s. Though the discovery was made by Meitner and initially reported in the journal Zeitschrift für Physik in 1922, Auger is credited with the discovery in most of the scientific community. Until the early 1950s Auger transitions were considered nuisance effects by spectroscopists, not containing much relevant material information, but studied so as to explain anomalies in X-ray spectroscopy data. Since 1953 however, AES has become a practical and straightforward characterization technique for probing chemical and compositional surface environments and has found applications in metallurgy, gas-phase chemistry, and throughout the microelectronics industry.
X-ray photoelectron spectroscopy (XPS) is a surface-sensitive quantitative spectroscopic technique based on the photoelectric effect that can identify the elements that exist within a material or are covering its surface, as well as their chemical state, and the overall electronic structure and density of the electronic states in the material. XPS is a powerful measurement technique because it not only shows what elements are present, but also what other elements they are bonded to. The technique can be used in line profiling of the elemental composition across the surface, or in depth profiling when paired with ion-beam etching. It is often applied to study chemical processes in the materials in their as-received state or after cleavage, scraping, exposure to heat, reactive gasses or solutions, ultraviolet light, or during ion implantation.
X-ray fluorescence (XRF) is the emission of characteristic "secondary" X-rays from a material that has been excited by being bombarded with high-energy X-rays or gamma rays. The phenomenon is widely used for elemental analysis and chemical analysis, particularly in the investigation of metals, glass, ceramics and building materials, and for research in geochemistry, forensic science, archaeology and art objects such as paintings.
Particle-induced X-ray emission or proton-induced X-ray emission (PIXE) is a technique used for determining the elemental composition of a material or a sample. When a material is exposed to an ion beam, atomic interactions occur that give off EM radiation of wavelengths in the x-ray part of the electromagnetic spectrum specific to an element. PIXE is a powerful yet non-destructive elemental analysis technique now used routinely by geologists, archaeologists, art conservators and others to help answer questions of provenance, dating and authenticity.
The emission spectrum of a chemical element or chemical compound is the spectrum of frequencies of electromagnetic radiation emitted due to an electron making a transition from a high energy state to a lower energy state. The photon energy of the emitted photon is equal to the energy difference between the two states. There are many possible electron transitions for each atom, and each transition has a specific energy difference. This collection of different transitions, leading to different radiated wavelengths, make up an emission spectrum. Each element's emission spectrum is unique. Therefore, spectroscopy can be used to identify elements in matter of unknown composition. Similarly, the emission spectra of molecules can be used in chemical analysis of substances.
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 convert high energy electrons into photons.
In physics, atomic spectroscopy is the study of the electromagnetic radiation absorbed and emitted by atoms. Since unique elements have unique emission spectra, atomic spectroscopy is applied for determination of elemental compositions. It can be divided by atomization source or by the type of spectroscopy used. In the latter case, the main division is between optical and mass spectrometry. Mass spectrometry generally gives significantly better analytical performance, but is also significantly more complex. This complexity translates into higher purchase costs, higher operational costs, more operator training, and a greater number of components that can potentially fail. Because optical spectroscopy is often less expensive and has performance adequate for many tasks, it is far more common. Atomic absorption spectrometers are one of the most commonly sold and used analytical devices.
Energy-dispersive X-ray spectroscopy, sometimes called energy dispersive X-ray analysis or energy dispersive X-ray microanalysis (EDXMA), is an analytical technique used for the elemental analysis or chemical characterization of a sample. It relies on an interaction of some source of X-ray excitation and a sample. Its characterization capabilities are due in large part to the fundamental principle that each element has a unique atomic structure allowing a unique set of peaks on its electromagnetic emission spectrum. The peak positions are predicted by the Moseley's law with accuracy much better than experimental resolution of a typical EDX instrument.
X-ray spectroscopy is a general term for several spectroscopic techniques for characterization of materials by using x-ray radiation.
An electron microprobe (EMP), also known as an electron probe microanalyzer (EPMA) or electron micro probe analyzer (EMPA), is an analytical tool used to non-destructively determine the chemical composition of small volumes of solid materials. It works similarly to a scanning electron microscope: the sample is bombarded with an electron beam, emitting x-rays at wavelengths characteristic to the elements being analyzed. This enables the abundances of elements present within small sample volumes to be determined, when a conventional accelerating voltage of 15-20 kV is used. The concentrations of elements from lithium to plutonium may be measured at levels as low as 100 parts per million (ppm), material dependent, although with care, levels below 10 ppm are possible. The ability to quantify lithium by EPMA became a reality in 2008.
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.
Powder diffraction is a scientific technique using X-ray, neutron, or electron diffraction on powder or microcrystalline samples for structural characterization of materials. An instrument dedicated to performing such powder measurements is called a powder diffractometer.
Elastic recoil detection analysis (ERDA), also referred to as forward recoil scattering, is an ion beam analysis technique in materials science to obtain elemental concentration depth profiles in thin films. This technique is known by several different names. These names are listed below. In the technique of ERDA, an energetic ion beam is directed at a sample to be characterized and there is an elastic nuclear interaction between the ions of beam and the atoms of the target sample. Such interactions are commonly of Coulomb nature. Depending on the kinetics of the ions, cross section area, and the loss of energy of the ions in the matter, ERDA helps determine the quantification of the elemental analysis. It also provides information about the depth profile of the sample.
Characterization, when used in materials science, refers to the broad and general process by which a material's structure and properties are probed and measured. It is a fundamental process in the field of materials science, without which no scientific understanding of engineering materials could be ascertained. The scope of the term often differs; some definitions limit the term's use to techniques which study the microscopic structure and properties of materials, while others use the term to refer to any materials analysis process including macroscopic techniques such as mechanical testing, thermal analysis and density calculation. The scale of the structures observed in materials characterization ranges from angstroms, such as in the imaging of individual atoms and chemical bonds, up to centimeters, such as in the imaging of coarse grain structures in metals.
Low-energy ion scattering spectroscopy (LEIS), sometimes referred to simply as ion scattering spectroscopy (ISS), is a surface-sensitive analytical technique used to characterize the chemical and structural makeup of materials. LEIS involves directing a stream of charged particles known as ions at a surface and making observations of the positions, velocities, and energies of the ions that have interacted with the surface. Data that is thus collected can be used to deduce information about the material such as the relative positions of atoms in a surface lattice and the elemental identity of those atoms. LEIS is closely related to both medium-energy ion scattering (MEIS) and high-energy ion scattering, differing primarily in the energy range of the ion beam used to probe the surface. While much of the information collected using LEIS can be obtained using other surface science techniques, LEIS is unique in its sensitivity to both structure and composition of surfaces. Additionally, LEIS is one of a very few surface-sensitive techniques capable of directly observing hydrogen atoms, an aspect that may make it an increasingly more important technique as the hydrogen economy is being explored.
Rutherford backscattering spectrometry (RBS) is an analytical technique used in materials science. Sometimes referred to as high-energy ion scattering (HEIS) spectrometry, RBS is used to determine the structure and composition of materials by measuring the backscattering of a beam of high energy ions (typically protons or alpha particles) impinging on a sample.
Characteristic X-rays are emitted when outer-shell electrons fill a vacancy in the inner shell of an atom, releasing X-rays in a pattern that is "characteristic" to each element. Characteristic X-rays were discovered by Charles Glover Barkla in 1909, who later won the Nobel Prize in Physics for his discovery in 1917.
Resonance ionization is a process in optical physics used to excite a specific atom beyond its ionization potential to form an ion using a beam of photons irradiated from a pulsed laser light. In resonance ionization, the absorption or emission properties of the emitted photons are not considered, rather only the resulting excited ions are mass-selected, detected and measured. Depending on the laser light source used, one electron can be removed from each atom so that resonance ionization produces an efficient selectivity in two ways: elemental selectivity in ionization and isotopic selectivity in measurement.
X-ray emission spectroscopy (XES) is a form of X-ray spectroscopy in which the X-ray line spectra are measured with a spectral resolution sufficient to analyze the impact of the chemical environment on the X-ray line energy and on branching ratios. This is done by exciting electrons out of their shell and then detecting the emitted photons of the recombining electrons.