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A diamond anvil cell (DAC) is a
high-pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of t ...
device used in
geology Geology () is a branch of natural science concerned with Earth and other Astronomical object, astronomical objects, the features or rock (geology), rocks of which it is composed, and the processes by which they change over time. Modern geology ...
,
engineering Engineering is the use of scientific principles to design and build machines, structures, and other items, including bridges, tunnels, roads, vehicles, and buildings. The discipline of engineering encompasses a broad range of more speciali ...
, and materials science experiments. It enables the compression of a small (sub-
millimeter 330px, Different lengths as in respect to the electromagnetic spectrum, measured by the metre and its derived scales. The microwave is between 1 meter to 1 millimeter. The millimetre (American and British English spelling differences#-re, -er, ...
-sized) piece of material to extreme pressures, typically up to around 100–200  gigapascals, although it is possible to achieve pressures up to 770  gigapascals (7,700,000  bars or 7.7 million
atmospheres The standard atmosphere (symbol: atm) is a unit of pressure defined as Pa. It is sometimes used as a ''reference pressure'' or ''standard pressure''. It is approximately equal to Earth's average atmospheric pressure at sea level. History The s ...
). The device has been used to recreate the pressure existing deep inside
planet A planet is a large, rounded astronomical body that is neither a star nor its remnant. The best available theory of planet formation is the nebular hypothesis, which posits that an interstellar cloud collapses out of a nebula to create a you ...
s to synthesize materials and phases not observed under normal ambient conditions. Notable examples include the non-molecular
ice X Ice is water frozen into a solid state, typically forming at or below temperatures of 0 degrees Celsius or Depending on the presence of impurities such as particles of soil or bubbles of air, it can appear transparent or a more or less opaq ...
, polymeric nitrogen and metallic phases of
xenon Xenon is a chemical element with the symbol Xe and atomic number 54. It is a dense, colorless, odorless noble gas found in Earth's atmosphere in trace amounts. Although generally unreactive, it can undergo a few chemical reactions such as the ...
,
lonsdaleite Lonsdaleite (named in honour of Kathleen Lonsdale), also called hexagonal diamond in reference to the crystal structure, is an allotrope of carbon with a hexagonal lattice, as opposed to the cubical lattice of conventional diamond. It is found ...
, and potentially
metallic hydrogen Metallic hydrogen is a phase of hydrogen in which it behaves like an electrical conductor. This phase was predicted in 1935 on theoretical grounds by Eugene Wigner and Hillard Bell Huntington. At high pressure and temperatures, metallic hydroge ...
. A DAC consists of two opposing
diamond Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, b ...
s with a sample compressed between the polished
culet {{inline, date=November 2022 In gemology, a culet is a flat face on the bottom of a gemstone. During the 14th century, after the adoption of the table cut, a further facet was added to the bottom of the cut parallel to the surface of the tab ...
s (tips). Pressure may be monitored using a reference material whose behavior under pressure is known. Common pressure standards include ruby fluorescence, and various structurally simple metals, such as
copper Copper is a chemical element with the symbol Cu (from la, cuprum) and atomic number 29. It is a soft, malleable, and ductile metal with very high thermal and electrical conductivity. A freshly exposed surface of pure copper has a pink ...
or
platinum Platinum is a chemical element with the symbol Pt and atomic number 78. It is a dense, malleable, ductile, highly unreactive, precious, silverish-white transition metal. Its name originates from Spanish , a diminutive of "silver". Pla ...
. The uniaxial pressure supplied by the DAC may be transformed into uniform
hydrostatic pressure Fluid statics or hydrostatics is the branch of fluid mechanics that studies the condition of the equilibrium of a floating body and submerged body " fluids at hydrostatic equilibrium and the pressure in a fluid, or exerted by a fluid, on an i ...
using a pressure-transmitting medium, such as
argon Argon is a chemical element with the symbol Ar and atomic number 18. It is in group 18 of the periodic table and is a noble gas. Argon is the third-most abundant gas in Earth's atmosphere, at 0.934% (9340 ppmv). It is more than twice a ...
,
xenon Xenon is a chemical element with the symbol Xe and atomic number 54. It is a dense, colorless, odorless noble gas found in Earth's atmosphere in trace amounts. Although generally unreactive, it can undergo a few chemical reactions such as the ...
,
hydrogen Hydrogen is the chemical element with the symbol H and atomic number 1. Hydrogen is the lightest element. At standard conditions hydrogen is a gas of diatomic molecules having the formula . It is colorless, odorless, tasteless, non-to ...
,
helium Helium (from el, ἥλιος, helios, lit=sun) is a chemical element with the symbol He and atomic number 2. It is a colorless, odorless, tasteless, non-toxic, inert, monatomic gas and the first in the noble gas group in the periodic ta ...
, paraffin oil or a mixture of
methanol Methanol (also called methyl alcohol and wood spirit, amongst other names) is an organic chemical and the simplest aliphatic alcohol, with the formula C H3 O H (a methyl group linked to a hydroxyl group, often abbreviated as MeOH). It is ...
and
ethanol Ethanol (abbr. EtOH; also called ethyl alcohol, grain alcohol, drinking alcohol, or simply alcohol) is an organic compound. It is an alcohol with the chemical formula . Its formula can be also written as or (an ethyl group linked to a ...
. The pressure-transmitting medium is enclosed by a gasket and the two diamond anvils. The sample can be viewed through the diamonds and illuminated by
X-rays An X-ray, or, much less commonly, X-radiation, is a penetrating form of high-energy electromagnetic radiation. Most X-rays have a wavelength ranging from 10 picometers to 10 nanometers, corresponding to frequencies in the range 30&nbs ...
and visible light. In this way,
X-ray diffraction X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles ...
and
fluorescence Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation. It is a form of luminescence. In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, tha ...
;
optical absorption In physics, absorption of electromagnetic radiation is how matter (typically electrons bound in atoms) takes up a photon's energy — and so transforms electromagnetic energy into internal energy of the absorber (for example, thermal energy). A ...
and
photoluminescence Photoluminescence (abbreviated as PL) is light emission from any form of matter after the absorption of photons (electromagnetic radiation). It is one of many forms of luminescence (light emission) and is initiated by photoexcitation (i.e. photo ...
; Mössbauer, Raman and
Brillouin scattering Brillouin scattering (also known as Brillouin light scattering or BLS), named after Léon Brillouin, refers to the interaction of light with the material waves in a medium (e.g. electrostriction and magnetostriction). It is mediated by the refra ...
; positron annihilation and other signals can be measured from materials under high pressure. Magnetic and microwave fields can be applied externally to the cell allowing
nuclear magnetic resonance Nuclear magnetic resonance (NMR) is a physical phenomenon in which nuclei in a strong constant magnetic field are perturbed by a weak oscillating magnetic field (in the near field) and respond by producing an electromagnetic signal with a ...
,
electron paramagnetic resonance Electron paramagnetic resonance (EPR) or electron spin resonance (ESR) spectroscopy is a method for studying materials that have unpaired electrons. The basic concepts of EPR are analogous to those of nuclear magnetic resonance (NMR), but the spin ...
and other magnetic measurements. Attaching
electrodes An electrode is an electrical conductor used to make contact with a nonmetallic part of a circuit (e.g. a semiconductor, an electrolyte, a vacuum or air). Electrodes are essential parts of batteries that can consist of a variety of materials dep ...
to the sample allows electrical and magnetoelectrical measurements as well as heating up the sample to a few thousand degrees. Much higher temperatures (up to 7000 K) can be achieved with laser-induced heating, and cooling down to millikelvins has been demonstrated.


Principle

The operation of the diamond anvil cell relies on a simple principle: :p=\frac where is the pressure, the applied force, and the area. Typical culet sizes for diamond anvils are 100–250 micron (µm), such that a very high pressure is achieved by applying a moderate
force In physics, a force is an influence that can change the motion of an object. A force can cause an object with mass to change its velocity (e.g. moving from a state of rest), i.e., to accelerate. Force can also be described intuitively as a ...
on a sample with a small area, rather than applying a large force on a large area.
Diamond Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, b ...
is a very hard and virtually incompressible material, thus minimising the deformation and failure of the
anvil An anvil is a metalworking tool consisting of a large block of metal (usually forged or cast steel), with a flattened top surface, upon which another object is struck (or "worked"). Anvils are as massive as practical, because the higher ...
s that apply the force.


History

The first diamond anvil cell in the NIST museum at Gaithersburg. Shown in the image above is the part which compresses the central assembly. The study of materials at extreme conditions, high pressure and high temperature uses a wide array of techniques to achieve these conditions and probe the behavior of material while in the extreme environment.
Percy Williams Bridgman Percy Williams Bridgman (April 21, 1882 – August 20, 1961) was an American physicist who received the 1946 Nobel Prize in Physics for his work on the physics of high pressures. He also wrote extensively on the scientific method and on other as ...
, the great pioneer of high-pressure research during the first half of the 20th century, revolutionized the field of high pressures with his development of an opposed anvil device with small flat areas that were pressed one against the other with a lever-arm. The anvils were made of
tungsten carbide Tungsten carbide (chemical formula: WC) is a chemical compound (specifically, a carbide) containing equal parts of tungsten and carbon atoms. In its most basic form, tungsten carbide is a fine gray powder, but it can be pressed and formed into ...
(WC). This device could achieve
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
of a few gigapascals, and was used in
electrical resistance The electrical resistance of an object is a measure of its opposition to the flow of electric current. Its reciprocal quantity is , measuring the ease with which an electric current passes. Electrical resistance shares some conceptual parallel ...
and
compressibility In thermodynamics and fluid mechanics, the compressibility (also known as the coefficient of compressibility or, if the temperature is held constant, the isothermal compressibility) is a measure of the instantaneous relative volume change of a f ...
measurements. The first diamond anvil cell was created in 1957-1958. The principles of the DAC are similar to the Bridgman anvils, but in order to achieve the highest possible pressures without breaking the anvils, they were made of the hardest known material: a single crystal
diamond Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, b ...
. The first prototypes were limited in their pressure range and there was not a reliable way to
calibrate In measurement technology and metrology, calibration is the comparison of measurement values delivered by a device under test with those of a calibration standard of known accuracy. Such a standard could be another measurement device of known ...
the pressure. The diamond anvil cell became the most versatile pressure generating device that has a single characteristic that sets it apart from the other pressure devices – its optical transparency. This provided the early
high pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of th ...
pioneers with the ability to directly observe the properties of a material while under
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
. With just the use of an
optical microscope The optical microscope, also referred to as a light microscope, is a type of microscope that commonly uses visible light and a system of lenses to generate magnified images of small objects. Optical microscopes are the oldest design of micro ...
, phase boundaries, color changes and recrystallization could be seen immediately, while
x-ray diffraction X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles ...
or spectroscopy required time to expose and develop photographic film. The potential for the diamond anvil cell was realized by Alvin Van Valkenburg while he was preparing a sample for
IR spectroscopy Infrared spectroscopy (IR spectroscopy or vibrational spectroscopy) is the measurement of the interaction of infrared radiation with matter by absorption, emission, or reflection. It is used to study and identify chemical substances or function ...
and was checking the alignment of the diamond faces. The diamond cell was created at the
National Bureau of Standards The National Institute of Standards and Technology (NIST) is an agency of the United States Department of Commerce whose mission is to promote American innovation and industrial competitiveness. NIST's activities are organized into physical sci ...
(NBS) by Charles E. Weir, Ellis R. Lippincott, and Elmer N. Bunting. Within the group, each member focused on different applications of the diamond cell. Van Valkenburg focused on making visual observations, Weir on XRD, Lippincott on
IR Spectroscopy Infrared spectroscopy (IR spectroscopy or vibrational spectroscopy) is the measurement of the interaction of infrared radiation with matter by absorption, emission, or reflection. It is used to study and identify chemical substances or function ...
. The group members were well experienced in each of their techniques before they began outside collaboration with university researchers such as William A. Bassett and Taro Takahashi at the
University of Rochester The University of Rochester (U of R, UR, or U of Rochester) is a private research university in Rochester, New York. The university grants undergraduate and graduate degrees, including doctoral and professional degrees. The University of ...
. During the first experiments using diamond anvils, the sample was placed on the flat tip of the diamond (the
culet {{inline, date=November 2022 In gemology, a culet is a flat face on the bottom of a gemstone. During the 14th century, after the adoption of the table cut, a further facet was added to the bottom of the cut parallel to the surface of the tab ...
) and pressed between the diamond faces. As the diamond faces were pushed closer together, the sample would be pressed and extrude out from the center. Using a
microscope A microscope () is a laboratory instrument used to examine objects that are too small to be seen by the naked eye. Microscopy is the science of investigating small objects and structures using a microscope. Microscopic means being invisi ...
to view the sample, it could be seen that a smooth pressure gradient existed across the sample with the outermost portions of the sample acting as a kind of gasket. The sample was not evenly distributed across the diamond culet but localized in the center due to the "cupping" of the diamond at higher pressures. This cupping
phenomenon A phenomenon ( : phenomena) is an observable event. The term came into its modern philosophical usage through Immanuel Kant, who contrasted it with the noumenon, which ''cannot'' be directly observed. Kant was heavily influenced by Gottfrie ...
is the
elastic Elastic is a word often used to describe or identify certain types of elastomer, elastic used in garments or stretchable fabrics. Elastic may also refer to: Alternative name * Rubber band, ring-shaped band of rubber used to hold objects togethe ...
stretching of the edges of the diamond
culet {{inline, date=November 2022 In gemology, a culet is a flat face on the bottom of a gemstone. During the 14th century, after the adoption of the table cut, a further facet was added to the bottom of the cut parallel to the surface of the tab ...
, commonly referred to as the "shoulder height". Many diamonds were broken during the first stages of producing a new cell or any time an experiment is pushed to higher
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
. The NBS group was in a unique position where almost endless supplies of diamonds were available to them. Customs officials occasionally confiscated diamonds from people attempting to smuggle them into the country. Disposing of such valuable confiscated materials could be problematic given rules and regulations. One solution was simply to make such materials available to people at other government agencies if they could make a convincing case for their use. This became an unrivaled resource as other teams at the
University of Chicago The University of Chicago (UChicago, Chicago, U of C, or UChi) is a private research university in Chicago, Illinois. Its main campus is located in Chicago's Hyde Park neighborhood. The University of Chicago is consistently ranked among the b ...
,
Harvard University Harvard University is a private Ivy League research university in Cambridge, Massachusetts. Founded in 1636 as Harvard College and named for its first benefactor, the Puritan clergyman John Harvard, it is the oldest institution of highe ...
, and
General Electric General Electric Company (GE) is an American multinational conglomerate founded in 1892, and incorporated in New York state and headquartered in Boston. The company operated in sectors including healthcare, aviation, power, renewable ene ...
entered the high pressure field. During the following decades DACs have been successively refined, the most important innovations being the use of
gasket Some seals and gaskets A gasket is a mechanical seal which fills the space between two or more mating surfaces, generally to prevent leakage from or into the joined objects while under compression. It is a deformable material that is used to ...
s and the
ruby A ruby is a pinkish red to blood-red colored gemstone, a variety of the mineral corundum ( aluminium oxide). Ruby is one of the most popular traditional jewelry gems and is very durable. Other varieties of gem-quality corundum are called ...
pressure calibration. The DAC evolved to be the most powerful lab device for generating static high pressure. The range of static pressure attainable today extends to 640 GPa, much higher than the estimated pressures at the Earth's center (~360 GPa).


Components

There are many different DAC designs but all have four main components:


Force-generating device

Relies on the operation of either a
lever A lever is a simple machine consisting of a beam or rigid rod pivoted at a fixed hinge, or '' fulcrum''. A lever is a rigid body capable of rotating on a point on itself. On the basis of the locations of fulcrum, load and effort, the lever is d ...
arm, tightening
screw A screw and a bolt (see '' Differentiation between bolt and screw'' below) are similar types of fastener typically made of metal and characterized by a helical ridge, called a ''male thread'' (external thread). Screws and bolts are used to ...
s, or
pneumatic Pneumatics (from Greek ‘wind, breath’) is a branch of engineering that makes use of gas or pressurized air. Pneumatic systems used in industry are commonly powered by compressed air or compressed inert gases. A centrally located and ...
or
hydraulic Hydraulics (from Greek: Υδραυλική) is a technology and applied science using engineering, chemistry, and other sciences involving the mechanical properties and use of liquids. At a very basic level, hydraulics is the liquid counte ...
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
applied to a membrane. In all cases the
force In physics, a force is an influence that can change the motion of an object. A force can cause an object with mass to change its velocity (e.g. moving from a state of rest), i.e., to accelerate. Force can also be described intuitively as a ...
is uniaxial and is applied to the tables (bases) of the two anvils.


Two opposing diamond anvils

Made of high
gem A gemstone (also called a fine gem, jewel, precious stone, or semiprecious stone) is a piece of mineral crystal which, in cut and polished form, is used to make jewelry or other adornments. However, certain rocks (such as lapis lazuli, opal, an ...
quality, flawless diamonds, usually with 16
facet Facets () are flat faces on geometric shapes. The organization of naturally occurring facets was key to early developments in crystallography, since they reflect the underlying symmetry of the crystal structure. Gemstones commonly have facets cut ...
s, they typically weigh to   carat (25 to 70 mg). The culet (tip) is ground and polished to a hexadecagonal surface parallel to the table. The culets of the two
diamond Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, b ...
s face one another, and must be perfectly
parallel Parallel is a geometric term of location which may refer to: Computing * Parallel algorithm * Parallel computing * Parallel metaheuristic * Parallel (software), a UNIX utility for running programs in parallel * Parallel Sysplex, a cluster o ...
in order to produce uniform
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
and to prevent dangerous strains. Specially selected anvils are required for specific measurements – for example, low diamond absorption and luminescence is required in corresponding experiments.


Gasket

A
gasket Some seals and gaskets A gasket is a mechanical seal which fills the space between two or more mating surfaces, generally to prevent leakage from or into the joined objects while under compression. It is a deformable material that is used to ...
used in a diamond anvil cell experiment is a thin metal foil, typically 0.3 mm in thickness, which is placed in between the diamonds. Desirable materials for gaskets are strong, stiff metals such as
rhenium Rhenium is a chemical element with the symbol Re and atomic number 75. It is a silvery-gray, heavy, third-row transition metal in group 7 of the periodic table. With an estimated average concentration of 1 part per billion (ppb), rhenium is one ...
or
tungsten Tungsten, or wolfram, is a chemical element with the symbol W and atomic number 74. Tungsten is a rare metal found naturally on Earth almost exclusively as compounds with other elements. It was identified as a new element in 1781 and first isol ...
.
Steel Steel is an alloy made up of iron with added carbon to improve its strength and fracture resistance compared to other forms of iron. Many other elements may be present or added. Stainless steels that are corrosion- and oxidation-resistan ...
is frequently used as a cheaper alternative for low pressure experiments. The above-mentioned materials cannot be used in radial geometries where the
x-ray An X-ray, or, much less commonly, X-radiation, is a penetrating form of high-energy electromagnetic radiation. Most X-rays have a wavelength ranging from 10 picometers to 10  nanometers, corresponding to frequencies in the range 30&nb ...
beam must pass through the gasket. Since they are not transparent to X-rays, if X-ray illumination through the gasket is required, lighter materials such as
beryllium Beryllium is a chemical element with the symbol Be and atomic number 4. It is a steel-gray, strong, lightweight and brittle alkaline earth metal. It is a divalent element that occurs naturally only in combination with other elements to for ...
,
boron nitride Boron nitride is a thermally and chemically resistant refractory compound of boron and nitrogen with the chemical formula BN. It exists in various crystalline forms that are isoelectronic to a similarly structured carbon lattice. The hexagonal ...
,
boron Boron is a chemical element with the symbol B and atomic number 5. In its crystalline form it is a brittle, dark, lustrous metalloid; in its amorphous form it is a brown powder. As the lightest element of the '' boron group'' it has t ...
or
diamond Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, b ...
are used as a gasket. Gaskets are preindented by the diamonds and a hole is drilled in the center of the indentation to create the sample chamber.


Pressure-transmitting medium

The
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
transmitting medium is the compressible fluid that fills the sample chamber and transmits the applied
force In physics, a force is an influence that can change the motion of an object. A force can cause an object with mass to change its velocity (e.g. moving from a state of rest), i.e., to accelerate. Force can also be described intuitively as a ...
to the sample.
Hydrostatic pressure Fluid statics or hydrostatics is the branch of fluid mechanics that studies the condition of the equilibrium of a floating body and submerged body " fluids at hydrostatic equilibrium and the pressure in a fluid, or exerted by a fluid, on an i ...
is preferred for
high-pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of t ...
experiments because variation in strain throughout the sample can lead to distorted observations of different behaviors. In some experiments stress and strain relationships are investigated and the effects of non-hydrostatic forces are desired. A good
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
medium will remain a soft, compressible fluid to
high pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of th ...
. The full range of techniques that are available has been summarized in a tree diagram by William Bassett. The ability to utilize any and all of these techniques hinges on being able to look through the diamonds which was first demonstrated by visual observations.


Measuring pressure

The two main pressure scales used in
static Static may refer to: Places *Static Nunatak, a nunatak in Antarctica United States * Static, Kentucky and Tennessee *Static Peak, a mountain in Wyoming **Static Peak Divide, a mountain pass near the peak Science and technology Physics *Static el ...
high-pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of t ...
experiments are
X-ray diffraction X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles ...
of a material with a known
equation of state In physics, chemistry, and thermodynamics, an equation of state is a thermodynamic equation relating state variables, which describe the state of matter under a given set of physical conditions, such as pressure, volume, temperature, or intern ...
and measuring the shift in ruby
fluorescence Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation. It is a form of luminescence. In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, tha ...
lines. The first began with NaCl, for which the compressibility has been determined by first principles in 1968. The major pitfall of this method of measuring pressure is that you need X-rays. Many experiments do not require X-rays and this presents a major inconvenience to conduct both the intended experiment and a diffraction experiment. In 1971, the NBS high pressure group was set in pursuit of a
spectroscopic 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 wa ...
method for determining
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
. It was found that the
wavelength 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, tr ...
of ruby
fluorescence Fluorescence is the emission of light by a substance that has absorbed light or other electromagnetic radiation. It is a form of luminescence. In most cases, the emitted light has a longer wavelength, and therefore a lower photon energy, tha ...
emissions Emission may refer to: Chemical products * Emission of air pollutants, notably: **Flue gas, gas exiting to the atmosphere via a flue ** Exhaust gas, flue gas generated by fuel combustion ** Emission of greenhouse gases, which absorb and emit radi ...
change with pressure; this was easily calibrated against the NaCl scale. Once pressure could be generated and measured it quickly became a competition for which cells can go the highest. The need for a reliable
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
scale became more important during this race. Shock-wave data for the compressibilities of Cu, Mo, Pd, and Ag were available at this time and could be used to define equations of states up to Mbar
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
. Using these scales these pressures were reported: Both methods are continually refined and in use today. However, the ruby method is less reliable at high temperature. Well defined equations of state are needed when adjusting
temperature Temperature is a physical quantity that expresses quantitatively the perceptions of hotness and coldness. Temperature is measured with a thermometer. Thermometers are calibrated in various temperature scales that historically have relied o ...
and
pressure Pressure (symbol: ''p'' or ''P'') is the force applied perpendicular to the surface of an object per unit area over which that force is distributed. Gauge pressure (also spelled ''gage'' pressure)The preferred spelling varies by country a ...
, two parameters that affect the lattice parameters of materials.


Uses

Prior to the invention of the diamond anvil cell, static high-pressure apparatus required large hydraulic presses which weighed several tons and required large specialized laboratories. The simplicity and compactness of the DAC meant that it could be accommodated in a wide variety of experiments. Some contemporary DACs can easily fit into a
cryostat A cryostat (from ''cryo'' meaning cold and ''stat'' meaning stable) is a device used to maintain low cryogenic temperatures of samples or devices mounted within the cryostat. Low temperatures may be maintained within a cryostat by using various r ...
for low-temperature measurements, and for use with a
superconducting Superconductivity is a set of physical properties observed in certain materials where electrical resistance vanishes and magnetic flux fields are expelled from the material. Any material exhibiting these properties is a superconductor. Unlike ...
electromagnet An electromagnet is a type of magnet in which the magnetic field is produced by an electric current. Electromagnets usually consist of wire wound into a coil. A current through the wire creates a magnetic field which is concentrated in ...
. In addition to being hard,
diamonds Diamond is a solid form of the element carbon with its atoms arranged in a crystal structure called diamond cubic. Another solid form of carbon known as graphite is the chemically stable form of carbon at room temperature and pressure, ...
have the advantage of being transparent to a wide range of the
electromagnetic spectrum The electromagnetic spectrum is the range of frequencies (the spectrum) of electromagnetic radiation and their respective wavelengths and photon energies. The electromagnetic spectrum covers electromagnetic waves with frequencies ranging fro ...
from
infrared Infrared (IR), sometimes called infrared light, is electromagnetic radiation (EMR) with wavelengths longer than those of Light, visible light. It is therefore invisible to the human eye. IR is generally understood to encompass wavelengths from ...
to
gamma rays A gamma ray, also known as gamma radiation (symbol γ or \gamma), is a penetrating form of electromagnetic radiation arising from the radioactive decay of atomic nuclei. It consists of the shortest wavelength electromagnetic waves, typically ...
, with the exception of the far
ultraviolet Ultraviolet (UV) is a form of electromagnetic radiation with wavelength from 10 nm (with a corresponding frequency around 30  PHz) to 400 nm (750  THz), shorter than that of visible light, but longer than X-rays. UV radiation ...
and
soft X-rays An X-ray, or, much less commonly, X-radiation, is a penetrating form of high-energy electromagnetic radiation. Most X-rays have a wavelength ranging from 10  picometers to 10 nanometers, corresponding to frequencies in the range 30  ...
. This makes the DAC a perfect device for
spectroscopic 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 wa ...
experiments and for crystallographic studies using hard
X-rays An X-ray, or, much less commonly, X-radiation, is a penetrating form of high-energy electromagnetic radiation. Most X-rays have a wavelength ranging from 10 picometers to 10 nanometers, corresponding to frequencies in the range 30&nbs ...
. A variant of the diamond anvil, the hydrothermal diamond anvil cell (HDAC) is used in experimental petrology/geochemistry for the study of aqueous fluids, silicate melts, immiscible liquids, mineral solubility and aqueous fluid speciation at geologic pressures and temperatures. The HDAC is sometimes used to examine aqueous complexes in solution using the synchrotron light source techniques
XANES X-ray absorption near edge structure (XANES), also known as near edge X-ray absorption fine structure (NEXAFS), is a type of absorption spectroscopy that indicates the features in the X-ray absorption spectra ( XAS) of condensed matter due to the ...
and
EXAFS Extended X-ray absorption fine structure (EXAFS), along with X-ray absorption near edge structure (XANES), is a subset of X-ray absorption spectroscopy ( XAS). Like other absorption spectroscopies, XAS techniques follow Beer's law. The X-ray ...
. The design of HDAC is very similar to that of DAC, but it is optimized for studying liquids.


Innovative uses

An innovative use of the diamond anvil cell is testing the sustainability and durability of life under
high pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of th ...
s, including the search for life on
extrasolar planets An exoplanet or extrasolar planet is a planet outside the Solar System. The first possible evidence of an exoplanet was noted in 1917 but was not recognized as such. The first confirmation of detection occurred in 1992. A different planet, in ...
. Testing portions of the theory of
panspermia Panspermia () is the hypothesis, first proposed in the 5th century BCE by the Greek philosopher Anaxagoras, that life exists throughout the Universe, distributed by space dust, meteoroids, asteroids, comets, and planetoids, as well as by spacec ...
(a form of
interstellar travel Interstellar travel is the hypothetical travel of spacecraft from one star system, solitary star, or planetary system to another. Interstellar travel is expected to prove much more difficult than interplanetary spaceflight due to the vast diffe ...
) is one application of DAC. When interstellar objects containing life-forms impact a planetary body, there is high pressure upon impact and the DAC can replicate this pressure to determine if the organisms could survive. Another reason the DAC is applicable for testing life on extrasolar planets is that planetary bodies that hold the potential for life may have incredibly high pressure on their surface. In 2002, scientists at the
Carnegie Institution of Washington The Carnegie Institution of Washington (the organization's legal name), known also for public purposes as the Carnegie Institution for Science (CIS), is an organization in the United States established to fund and perform scientific research. Th ...
examined the pressure limits of life processes. Suspensions of bacteria, specifically ''
Escherichia coli ''Escherichia coli'' (),Wells, J. C. (2000) Longman Pronunciation Dictionary. Harlow ngland Pearson Education Ltd. also known as ''E. coli'' (), is a Gram-negative, facultative anaerobic, rod-shaped, coliform bacterium of the genus '' Esc ...
'' and '' Shewanella oneidensis'', were placed in the DAC, and the pressure was raised to 1.6 GPa, which is more than 16,000 times
Earth Earth is the third planet from the Sun and the only astronomical object known to harbor life. While large volumes of water can be found throughout the Solar System, only Earth sustains liquid surface water. About 71% of Earth's sur ...
's surface pressure (985 hPa). After 30 hours, only about 1% of the bacteria survived. The experimenters then added a dye to the solution. If the cells survived the squeezing and were capable of carrying out life processes, specifically breaking down
formate Formate (IUPAC name: methanoate) is the conjugate base of formic acid. Formate is an anion () or its derivatives such as ester of formic acid. The salts and esters are generally colorless.Werner Reutemann and Heinz Kieczka "Formic Acid" in ''Ull ...
, the dye would turn clear. 1.6 GPa is such great pressure that during the experiment the DAC turned the solution into ice-IV, a room-temperature ice. When the bacteria broke down the formate in the ice, liquid pockets would form because of the chemical reaction. The bacteria were also able to cling to the surface of the DAC with their tails. Skeptics debated whether breaking down formate is enough to consider the bacteria living. Art Yayanos, an oceanographer at the
Scripps Institute of Oceanography The Scripps Institution of Oceanography (sometimes referred to as SIO, Scripps Oceanography, or Scripps) in San Diego, California, US founded in 1903, is one of the oldest and largest centers for ocean and Earth science research, public servi ...
in La Jolla, California, believes an organism should only be considered living if it can reproduce. Subsequent results from independent research groups have shown the validity of the 2002 work. This is a significant step that reiterates the need for a new approach to the old problem of studying environmental extremes through experiments. There is practically no debate whether microbial life can survive pressures up to 600 MPa, which has been shown over the last decade or so to be valid through a number of scattered publications. Similar tests were performed with a low-pressure (0.1–600 MPa) diamond anvil cell, which has better imaging quality and signal collection. The studied microbes, ''
Saccharomyces cerevisiae ''Saccharomyces cerevisiae'' () (brewer's yeast or baker's yeast) is a species of yeast (single-celled fungus microorganisms). The species has been instrumental in winemaking, baking, and brewing since ancient times. It is believed to have b ...
'' (baker's yeast), withstood pressures of 15–50 MPa, and died at 200 MPa.


Single crystal X-ray diffraction

Good single crystal
X-ray diffraction X-ray crystallography is the experimental science determining the atomic and molecular structure of a crystal, in which the crystalline structure causes a beam of incident X-rays to diffract into many specific directions. By measuring the angles ...
experiments in diamond anvil cells require sample stage to rotate on the vertical axis,
omega Omega (; capital: Ω, lowercase: ω; Ancient Greek ὦ, later ὦ μέγα, Modern Greek ωμέγα) is the twenty-fourth and final letter in the Greek alphabet. In the Greek numeric system/ isopsephy ( gematria), it has a value of 800. The ...
. Most diamond anvil cells do not feature a large opening that would allow the cell to be rotated to high angles, a 60  degrees opening is considered sufficient for most
crystals A crystal or crystalline solid is a solid material whose constituents (such as atoms, molecules, or ions) are arranged in a highly ordered microscopic structure, forming a crystal lattice that extends in all directions. In addition, macros ...
but larger angles are possible. The first cell to be used for single crystal experiments was designed by a graduate student at the
University of Rochester The University of Rochester (U of R, UR, or U of Rochester) is a private research university in Rochester, New York. The university grants undergraduate and graduate degrees, including doctoral and professional degrees. The University of ...
, Leo Merrill. The cell was triangular with
beryllium Beryllium is a chemical element with the symbol Be and atomic number 4. It is a steel-gray, strong, lightweight and brittle alkaline earth metal. It is a divalent element that occurs naturally only in combination with other elements to for ...
seats that the diamonds were mounted on; the cell was pressurized with screws and guide pins holding everything in place.


High-temperature techniques

Heating in diamond-anvil cells is typically done by two means, external or internal heating. External heating is defined as heating the anvils and would include a number of resistive heaters that are placed around the diamonds or around the cell body. The complementary method does not change the temperature of the anvils and includes fine resistive heaters placed within the sample chamber and laser heating. The main advantage to resistive heating is the precise measurement of temperature with thermocouples, but the temperature range is limited by the properties of the diamond which will oxidize in air at 700 °C The use of an inert atmosphere can extend this range above 1000 °C. A tungsten wire resistive heater inside a BX90 DAC was reported to reach 1400 °C. With laser heating the sample can reach temperature above 5000 °C, but the minimum temperature that can be measured when using a laser-heating system is ~1200 °C and the measurement is much less precise. Advances in resistive heating are closing the gap between the two techniques so that systems can be studied from room temperature to beyond 5700 °C with the combination of the two.


Gas loading


Principle

The pressure transmitting medium is an important component in any high-pressure experiment. The medium fills the space within the sample 'chamber' and applies the pressure being transmitted to the medium onto the sample. In a good high-pressure experiment, the medium should maintain a homogeneous distribution of pressure on the sample. In other words, the medium must stay hydrostatic to ensure uniform compressibility of the sample. Once a pressure transmitting medium has lost its hydrostaticity, a pressure gradient forms in the chamber that increases with increasing pressure. This gradient can greatly affect the sample, compromising results. The medium must also be inert, as to not interact with the sample, and stable under high pressures. For experiments with laser heating, the medium should have low thermal conductivity. If an optical technique is being employed, the medium should be optically transparent and for x-ray diffraction, the medium should be a poor x-ray scatterer – as to not contribute to the signal. Some of the most commonly used pressure transmitting media have been sodium chloride, silicone oil, and a 4:1 methanol-ethanol mixture. Sodium chloride is easy to load and is used for high-temperature experiments because it acts as a good thermal insulator. The methanol-ethanol mixture displays good hydrostaticity to about 10 GPa and with the addition of a small amount of water can be extended to about 15 GPa. For pressure experiments that exceed 10 GPa, noble gases are preferred. The extended hydrostaticity greatly reduces the pressure gradient in samples at high pressure. Noble gases, such as helium, neon, and argon are optically transparent, thermally insulating, have small X-ray scattering factors, and have good hydrostaticity at high pressures. Even after solidification, noble gases provide quasihydrostatic environments. Argon is used for experiments involving laser heating because it is chemically insulating. Since it condenses at a temperature above that of liquid nitrogen, it can be loaded cryogenically. Helium and neon have low X-ray scattering factors and are thus used for collecting X-ray diffraction data. Helium and neon also have low shear moduli; minimizing strain on the sample. These two noble gases do not condense above that of liquid nitrogen and cannot be loaded cryogenically. Instead, a high-pressure gas loading system has been developed that employs a gas compression method.


Techniques

In order to load a gas as a sample of pressure transmitting medium, the gas must be in a dense state, as to not shrink the sample chamber once pressure is induced. To achieve a dense state, gases can be liquefied at low temperatures or compressed. Cryogenic loading is a technique that uses liquefied gas as a means of filling the sample chamber. The DAC is directly immersed into the cryogenic fluid that fills the sample chamber. However, there are disadvantages to cryogenic loading. With the low temperatures indicative of cryogenic loading, the sample is subjected to temperatures that could irreversibly change it. Also, the boiling liquid could displace the sample or trap an air bubble in the chamber. It is not possible to load gas mixtures using the cryogenic method due to the different boiling points of most gases. Gas compression technique densifies the gases at room temperature. With this method, most of the problems seen with cryogenic loading are fixed. Also, loading gas mixtures becomes a possibility. The technique uses a vessel or chamber in which the DAC is placed and is filled with gas. Gases are pressurized and pumped into the vessel with a compressor. Once the vessel is filled and the desired pressure is reached the DAC is closed with a clamp system run by motor driven screws.


Components

* High-pressure vessel: Vessel in which the diamond anvil cell is loaded. * Clamp device seals the DAC; which is tightened by closure mechanism with motor driven screws. * PLC (programmable logic controller): Controls air flow to the compressor and all valves. The PLC ensures that valves are opened and closed in the correct sequence for accurate loading and safety. * Compressor: Responsible for compression of the gas. The compressor employs a dual-stage air-driven diaphragm design that creates pressure and avoids contamination. Able to achieve 207 MPa of pressure. * Valves: Valves open and close via the PLC to regulate which gases enter the high-pressure vessel. * Burst disks: Two burst disks in the system – one for the high-pressure system and one for the low-pressure system. These disks act as a pressure relief system that protects the system from over-pressurization * Pressure transducers: A pressure sensor for the low- and high-pressure systems. Produces a 0–5 V output over their pressure range. * Pressure meters: Digital displays connected to each pressure transducer and the PLC system. * Vacuum pump and gauges: Cleans the system (by evacuation) before loading. * Optical system: Used visual observation; allowing in situ observations of gasket deformation. * Ruby fluorescence system: Pressure in the sample chamber can be measured during loading using an online ruby fluorescence system. Not all systems have an online ruby fluorescence system for in situ measuring. However, being able to monitor the pressure within the chamber while the DAC is being sealed is advantageous – ensuring the desired pressure is reached (or not over-shot). Pressure is measured by the shift in the laser induced luminescence of rubies in the sample chamber.


Laser heating


History

The development of laser heating began only 8 years after Charles Weir, of the
National Bureau of Standards The National Institute of Standards and Technology (NIST) is an agency of the United States Department of Commerce whose mission is to promote American innovation and industrial competitiveness. NIST's activities are organized into physical sci ...
(NBS), made the first diamond anvil cell and Alvin Van Valkenburg, NBS, realized the potential of being able to see the sample while under pressure. William Bassett and his colleague Taro Takahashi focused a laser beam on the sample while under pressure. The first laser heating system used a single 7 
joule The joule ( , ; symbol: J) is the unit of energy in the International System of Units (SI). It is equal to the amount of work done when a force of 1 newton displaces a mass through a distance of 1 metre in the direction of the force appli ...
pulsed
ruby laser A ruby laser is a solid-state laser that uses a synthetic ruby crystal as its gain medium. The first working laser was a ruby laser made by Theodore H. "Ted" Maiman at Hughes Research Laboratories on May 16, 1960. Ruby lasers produce pulses of ...
that heated the sample to 3000 °C while at 260 kilobars. This was sufficient to convert graphite to diamond. The major flaws within the first system related to control and temperature measurement. Temperature measurement was initially done by Basset using an
optical pyrometer A pyrometer is a type of remote-sensing thermometer used to measure the temperature of distant objects. Various forms of pyrometers have historically existed. In the modern usage, it is a device that from a distance determines the temperature of ...
to measure the intensity of the incandescent light from the sample. Colleagues at
UC Berkeley The University of California, Berkeley (UC Berkeley, Berkeley, Cal, or California) is a public land-grant research university in Berkeley, California. Established in 1868 as the University of California, it is the state's first land-grant uni ...
were better able to utilize the black-body radiation and more accurately measure the temperature. The hot spot produced by the laser also created large thermal gradients in between the portions of sample that were hit by the focused laser and those that were not. The solution to this problem is ongoing but advances have been made with the introduction of a double-sided approach.


Double-sided heating

The use of two lasers to heat the sample reduces the axial temperature gradient, this which allows for thicker samples to be heated more evenly. In order for a double-sided heating system to be successful it is essential that the two lasers are aligned so that they are both focused on the sample position. For in situ heating in diffraction experiments, the lasers need to be focused to the same point in space where the X-ray beam is focused.


Laser heating systems at synchrotron facilities

The European Synchrotron Radiation Facility (ESRF) as well as many other synchrotron facilities as the three major
synchrotron A synchrotron is a particular type of cyclic particle accelerator, descended from the cyclotron, in which the accelerating particle beam travels around a fixed closed-loop path. The magnetic field which bends the particle beam into its closed ...
user facilities in the United States all have beamlines equipped with laser heating systems. The respective beamlines with laser heating systems are at the ESRF ID27, ID18, and ID24; at the Advanced Photon Source (APS), 13-ID-D GSECARS and 16-ID-B HP-CAT; at the National Synchrotron Light Source, X17B3; and at the Advanced Light Source, 12.2.2. Laser heating has become a routine technique in high-pressure science but the reliability of temperature measurement is still controversial.


Temperature measurement

In the first experiments with laser heating, temperature came from a calibration of laser power made with known melting points of various materials. When using the pulsed ruby laser this was unreliable due to the short pulse. YAG lasers quickly become the standard, heating for relatively long duration, and allowing observation of the sample throughout the heating process. It was with the first use of YAG lasers that Bassett used an optical pyrometer to measure temperatures in the range of 1000 °C to 1600 °C. The first temperature measurements had a standard deviation of 30 °C from the brightness temperature, but due to the small sample size was estimated to be 50 °C with the possibility that the true temperature of the sample being was 200 °C higher than that of the brightness measurement. Spectrometry of the incandescent light became the next method of temperature measurement used in Bassett's group. The energy of the emitted radiation could be compared to known black-body radiation spectra to derive a temperature. Calibration of these systems is done with published melting points or melting points as measured by resistive heating.


Application of laser heating

Laser heating is used to heat micrograms of sample in diamond-anvil cells when studying matter under extreme conditions. This typically means one of four things: * Thermal equation of states ** Measuring the pressure-volume-temperature state of a material. In DAC work, this is done by applying pressure with the diamond anvils, applying temperature with lasers/resistive heaters, and measuring the volume response with X-ray diffraction. The thermal expansion and compressibility can then be defined in an equation of state with the independent variable of volume. * High-pressure/temperature synthesis ** Using a diamond-anvil cell and laser heating to reach high pressures and temperatures achieve novel synthesis routes not accessible at ambient pressure that can produce unique high-pressure phases. * Phase transition studies ** Providing excess kinetic energy to a sample in order to observe a kinetically unfavorable transition. Developing phase diagrams over the high-pressure range. * High-pressure melting ** Measuring the dependence of the melting point on pressure. Pressure commonly elevates the melting point of solids.


See also

*
Anvil press A multi-anvil press, or anvil press is a type of device related to a machine press that is used to create extraordinarily high pressures within a small volume. Anvil presses are used in materials science and geology for the synthesis and study ...
*
D-DIA The D-DIA or deformation-DIA is an apparatus used for high pressure and high temperature deformation experiments. The advantage of this apparatus is the ability to apply pressures up to approximately 15 GPa while independently creating uniaxial ...
*
Fluid statics Fluid statics or hydrostatics is the branch of fluid mechanics that studies the condition of the equilibrium of a floating body and submerged body " fluids at hydrostatic equilibrium and the pressure in a fluid, or exerted by a fluid, on an im ...
*
High pressure In science and engineering the study of high pressure examines its effects on materials and the design and construction of devices, such as a diamond anvil cell, which can create high pressure. By ''high pressure'' is usually meant pressures of th ...
*
Material properties of diamond Diamond is the allotrope of carbon in which the carbon atoms are arranged in the specific type of cubic lattice called diamond cubic. It is a crystal that is transparent to opaque and which is generally isotropic (no or very weak birefringence ...
*
Pressure experiment Pressure experiments are experiments performed at pressures lower or higher than atmospheric pressure, called low-pressure experiments and high-pressure experiments, respectively. Pressure experiment are necessary because substances behave differ ...


References


External links

* {{DEFAULTSORT:Diamond Anvil Cell Materials science Condensed matter physics Geophysics Physical chemistry High pressure science