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Wavelength-dispersive X-ray spectroscopy (WDXS or WDS) is a method used to count the number of X-rays of a specific wavelength diffracted by a crystal. The wavelength of the impinging X-ray and the crystal's lattice spacings are related by Bragg's law and produce constructive interference if they fit the criteria of Bragg's law. Unlike the related technique of energy-dispersive X-ray spectroscopy (EDS), WDS reads or counts only the X-rays of a single wavelength at a time, not producing a broad spectrum of wavelengths or energies simultaneously. WDS is primarily used in chemical analysis, in an X-ray fluorescence spectrometer, in an electron microprobe, and may also be used in a scanning electron microscope.
X-rays make up X-radiation, a form of high-energy electromagnetic radiation. Most X-rays have a wavelength ranging from 0.01 to 10 nanometers, corresponding to frequencies in the range 30 petahertz to 30 exahertz (3×1016 Hz to 3×1019 Hz) and energies in the range 100 eV to 100 keV. X-ray wavelengths are shorter than those of UV rays and typically longer than those of gamma rays. In many languages, X-radiation is referred to as Röntgen radiation, after the German scientist Wilhelm Röntgen, who discovered it on November 8, 1895. He named it X-radiation to signify an unknown type of radiation. Spelling of X-ray(s) in the English language includes the variants x-ray(s), xray(s), and X ray(s).
In physics, the wavelength is the spatial period of a periodic wave—the distance over which the wave's shape repeats. It is the distance between consecutive corresponding points of the same phase on the wave, such as two adjacent crests, troughs, or zero crossings, and is a characteristic of both traveling waves and standing waves, as well as other spatial wave patterns. The inverse of the wavelength is called the spatial frequency. Wavelength is commonly designated by the Greek letter lambda (λ). The term wavelength is also sometimes applied to modulated waves, and to the sinusoidal envelopes of modulated waves or waves formed by interference of several sinusoids.
Diffraction refers to various phenomena that occur when a wave encounters an obstacle or a slit. It is defined as the bending of waves around the corners of an obstacle or through an aperture into the region of geometrical shadow of the obstacle/aperture. The diffracting object or aperture effectively becomes a secondary source of the propagating wave. Italian scientist Francesco Maria Grimaldi coined the word "diffraction" and was the first to record accurate observations of the phenomenon in 1660.
The X-rays emitted by the sample being analyzed are collimated by parallel copper blades (called collimator or Soller slits), and irradiate a known single crystal at a precise angle. The single crystal diffracts the photons (Bragg's law) which are collected by a detector, usually a scintillation counter or a proportional counter.
A collimator is a device which narrows a beam of particles or waves. To narrow can mean either to cause the directions of motion to become more aligned in a specific direction, or to cause the spatial cross section of the beam to become smaller.
A crystal or crystalline solid is a solid material whose constituents are arranged in a highly ordered microscopic structure, forming a crystal lattice that extends in all directions. In addition, macroscopic single crystals are usually identifiable by their geometrical shape, consisting of flat faces with specific, characteristic orientations. The scientific study of crystals and crystal formation is known as crystallography. The process of crystal formation via mechanisms of crystal growth is called crystallization or solidification.
In physics, Bragg's law, or Wulff–Bragg's condition, a special case of Laue diffraction, gives the angles for coherent and incoherent scattering from a crystal lattice. When X-rays are incident on an atom, they make the electronic cloud move, as does any electromagnetic wave. The movement of these charges re-radiates waves with the same frequency, blurred slightly due to a variety of effects; this phenomenon is known as Rayleigh scattering. The scattered waves can themselves be scattered but this secondary scattering is assumed to be negligible.
The single crystal, the specimen, and the detector are mounted precisely on a goniometer with the distance from the source of X-rays (the specimen) and the crystal equal to the distance from the crystal to 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).
A goniometer is an instrument that either measures an angle or allows an object to be rotated to a precise angular position. The term goniometry is derived from two Greek words, gōnia, meaning angle, and metron, meaning measure.
Boron is a chemical element with the symbol B and atomic number 5. Produced entirely by cosmic ray spallation and supernovae and not by stellar nucleosynthesis, it is a low-abundance element in the Solar system and in the Earth's crust. Boron is concentrated on Earth by the water-solubility of its more common naturally occurring compounds, the borate minerals. These are mined industrially as evaporites, such as borax and kernite. The largest known boron deposits are in Turkey, the largest producer of boron minerals.
Oxygen is the chemical element with the symbol O and atomic number 8, meaning its nucleus has 8 protons. The number of neutrons varies according to the isotope: the stable isotopes have 8, 9, or 10 neutrons. Oxygen is a member of the chalcogen group on the periodic table, a highly reactive nonmetal, and an oxidizing agent that readily forms oxides with most elements as well as with other compounds. By mass, oxygen is the third-most abundant element in the universe, after hydrogen and helium. At standard temperature and pressure, two atoms of the element bind to form dioxygen, a colorless and odorless diatomic gas with the formula O
2. Diatomic oxygen gas constitutes 20.8% of the Earth's atmosphere. As compounds including oxides, the element makes up almost half of the Earth's crust.
Modern systems contain a small number of crystals of known but differing properties, with automated changing of the crystal depending on the energy being analysed, enabling elements from the entire periodic table to be analyzed, with the exception of hydrogen, helium, and lithium, as their atomic number, and by extension x-ray cross section, is too low to analyze via x-ray methods.
Hydrogen is the chemical element with the symbol H and atomic number 1. With a standard atomic weight of 1.008, hydrogen is the lightest element in the periodic table. Hydrogen is the most abundant chemical substance in the Universe, constituting roughly 75% of all baryonic mass. Non-remnant stars are mainly composed of hydrogen in the plasma state. The most common isotope of hydrogen, termed protium, has one proton and no neutrons.
Helium is a chemical element with the symbol He and atomic number 2. It is a colorless, odorless, tasteless, non-toxic, inert, monatomic gas, the first in the noble gas group in the periodic table. Its boiling point is the lowest among all the elements. Helium is the second lightest and second most abundant element in the observable universe. It is present at about 24% of the total elemental mass, which is more than 12 times the mass of all the heavier elements combined. Its abundance is similar to this in both the Sun and in Jupiter. This is due to the very high nuclear binding energy of helium-4, with respect to the next three elements after helium. This helium-4 binding energy also accounts for why it is a product of both nuclear fusion and radioactive decay. Most helium in the universe is helium-4, the vast majority of which was formed during the Big Bang. Large amounts of new helium are being created by nuclear fusion of hydrogen in stars.
Lithium is a chemical element with the symbol Li and atomic number 3. It is a soft, silvery-white alkali metal. Under standard conditions, it is the lightest metal and the lightest solid element. Like all alkali metals, lithium is highly reactive and flammable, and must be stored in mineral oil. When cut, it exhibits a metallic luster, but moist air corrodes it quickly to a dull silvery gray, then black tarnish. It never occurs freely in nature, but only in compounds, such as pegmatitic minerals, which were once the main source of lithium. Due to its solubility as an ion, it is present in ocean water and is commonly obtained from brines. Lithium metal is isolated electrolytically from a mixture of lithium chloride and potassium chloride.
It is a convenient and sensitive method for determining the chemical constituents and composition of phases on the microscale.
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 and murals.
X-ray spectroscopy is a general term for several spectroscopic techniques for characterization of materials by using x-ray excitation.
Energy-dispersive X-ray spectroscopy, sometimes called energy dispersive X-ray analysis (EDXA) 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.
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Microscopy is the technical field of using microscopes to view objects and areas of objects that cannot be seen with the naked eye. There are three well-known branches of microscopy: optical, electron, and scanning probe microscopy, along with the emerging field of X-ray microscopy.
Spectroscopy is the study of the interaction between matter and electromagnetic radiation. Historically, spectroscopy originated through the study of visible light dispersed according to its wavelength, by a prism. Later the concept was expanded greatly to include any interaction with radiative energy as a function of its wavelength or frequency, predominantly in the electromagnetic spectrum, though matter waves and acoustic waves can also be considered forms of radiative energy; recently, with tremendous difficulty, even gravitational waves have been associated with a spectral signature in the context of the Laser Interferometer Gravitational-Wave Observatory (LIGO) and laser interferometry. Spectroscopic data are often represented by an emission spectrum, a plot of the response of interest, as a function of wavelength or frequency.
The emission spectrum of a chemical element or chemical compound is the spectrum of frequencies of electromagnetic radiation emitted due to an atom or molecule 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 the 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 which are needed to convert high energy electrons into photons.
Reflection high-energy electron diffraction (RHEED) is a technique used to characterize the surface of crystalline materials. RHEED systems gather information only from the surface layer of the sample, which distinguishes RHEED from other materials characterization methods that also rely on diffraction of high-energy electrons. Transmission electron microscopy, another common electron diffraction method samples the bulk of the sample due to the geometry of the system. Low-energy electron diffraction (LEED) is also surface sensitive, but LEED achieves surface sensitivity through the use of low energy electrons.
In physics and physical chemistry, time-resolved spectroscopy is the study of dynamic processes in materials or chemical compounds by means of spectroscopic techniques. Most often, processes are studied after the illumination of a material occurs, but in principle, the technique can be applied to any process that leads to a change in properties of a material. With the help of pulsed lasers, it is possible to study processes that occur on time scales as short as 10−16 seconds.
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. The concentrations of elements from beryllium to plutonium can be measured at levels as low as 100 parts per million (ppm). Recent models of EPMAs can accurately measure elemental concentrations of approximately 10 ppm.
Electron backscatter diffraction (EBSD) is a scanning electron microscope–based microstructural-crystallographic characterization technique commonly used in the study of crystalline or polycrystalline materials. The technique can provide information about the structure, crystal orientation, phase, or strain in the material. Traditionally these types of studies have been carried out using X-ray diffraction (XRD), neutron diffraction and/or electron diffraction in a Transmission electron microscope.
Gamma-ray spectroscopy is the quantitative study of the energy spectra of gamma-ray sources, such as in the nuclear industry, geochemical investigation, and astrophysics.
The Davisson–Germer experiment was a 1923-27 experiment by Clinton Davisson and Lester Germer at Western Electric, in which electrons, scattered by the surface of a crystal of nickel metal, displayed a diffraction pattern. This confirmed the hypothesis, advanced by Louis de Broglie in 1924, of wave-particle duality, and was an experimental milestone in the creation of quantum mechanics.
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.
Soft X-ray emission spectroscopy (SXES) is an experimental technique for determining the electronic structure of materials. It is a form of X-ray spectroscopy.
Ultrafast laser spectroscopy is a spectroscopic technique that uses ultrashort pulse lasers for the study of dynamics on extremely short time scales. Different methods are used to examine dynamics of charge carriers, atoms and molecules. Many different procedures have been developed spanning different time scales and photon energy ranges; some common methods are listed below.
Electron spectroscopy is an analytical technique to study the electronic structure and its dynamics in atoms and molecules. In general an excitation source such as x-rays, electrons or synchrotron radiation will eject an electron from an inner-shell orbital of an atom. Detecting photoelectrons that are ejected by x-rays is called x-ray photoelectron spectroscopy (XPS) or electron spectroscopy for chemical analysis (ESCA). Detecting electrons that are ejected from higher orbitals to conserve energy during electron transitions is called Auger electron spectroscopy (AES).
X-ray optics is the branch of optics that manipulates X-rays instead of visible light. It deals with focusing and other ways of manipulating the X-ray beams for research techniques such as X-ray crystallography, X-ray fluorescence, small-angle X-ray scattering, X-ray microscopy, X-ray phase-contrast imaging, X-ray astronomy etc.
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.