Sensitive high-resolution ion microprobe
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The sensitive high-resolution ion microprobe (also sensitive high mass-resolution ion microprobe or SHRIMP) is a large-diameter, double-focusing secondary ion mass spectrometer (SIMS) sector instrument produced by Australian Scientific Instruments in Canberra, Australia. Similar to the IMS 1270-1280-1300 large-geometry ion microprobes produced by CAMECA, Gennevilliers, France and like other SIMS instruments, the SHRIMP
microprobe A microprobe is an instrument that applies a stable and well-focused beam of charged particles (electrons or ions) to a sample. Types When the primary beam consists of accelerated electrons, the probe is termed an electron microprobe, when the prim ...
bombards a sample under vacuum with a beam of primary
ions An ion () is an atom or molecule with a net electrical charge. The charge of an electron is considered to be negative by convention and this charge is equal and opposite to the charge of a proton, which is considered to be positive by conven ...
that sputters secondary ions that are focused, filtered, and measured according to their energy and mass. The SHRIMP is primarily used for geological and geochemical applications. It can measure the isotopic and elemental abundances in minerals at a 10 to 30 μm-diameter scale and with a depth resolution of 1–5 μm. Thus, SIMS method is well-suited for the analysis of complex minerals, as often found in
metamorphic Metamorphic rocks arise from the transformation of existing rock to new types of rock in a process called metamorphism. The original rock (protolith) is subjected to temperatures greater than and, often, elevated pressure of or more, causin ...
terrains, some
igneous rock Igneous rock (derived from the Latin word ''ignis'' meaning fire), or magmatic rock, is one of the three main The three types of rocks, rock types, the others being Sedimentary rock, sedimentary and metamorphic rock, metamorphic. Igneous rock ...
s, and for relatively rapid analysis of statistical valid sets of detrital minerals from sedimentary rocks. The most common application of the instrument is in uranium-thorium-lead
geochronology Geochronology is the science of determining the age of rocks, fossils, and sediments using signatures inherent in the rocks themselves. Absolute geochronology can be accomplished through radioactive isotopes, whereas relative geochronology is ...
, although the SHRIMP can be used to measure some other
isotope Isotopes are two or more types of atoms that have the same atomic number (number of protons in their nuclei) and position in the periodic table (and hence belong to the same chemical element), and that differ in nucleon numbers (mass numbers) ...
ratio measurements (e.g., δ7Li or δ11B) and trace element abundances.


History and scientific impact

The SHRIMP originated in 1973 with a proposal by Prof. Bill Compston, trying to build an ion microprobe at the Research School of Earth Sciences of the
Australian National University The Australian National University (ANU) is a public research university located in Canberra, the capital of Australia. Its main campus in Acton encompasses seven teaching and research colleges, in addition to several national academies and ...
that exceeded the sensitivity and resolution of ion probes available at the time in order to analyse individual mineral grains. Optic designer Steve Clement based the prototype instrument (now referred to as 'SHRIMP-I') on a design by
Matsuda Matsuda (written: lit. "pine ricefield") is a Japanese surname. Notable people with the surname include: *, Japanese badminton athlete *Eiji Matsuda (1894–1978), Mexican botanist *Fujio Matsuda (1924–2020), president of the University of Hawa ...
which minimised aberrations in transmitting ions through the various sectors. The instrument was built from 1975 and 1977 with testing and redesigning from 1978. The first successful geological applications occurred in 1980. The first major scientific impact was the discovery of
Hadean The Hadean ( ) is a Eon (geology), geologic eon of History of Earth, Earth history preceding the Archean. On Earth, the Hadean began with the Formation of the Earth, planet's formation about 4.54 billion years ago (although the start of the H ...
(>4000 million year old)
zircon Zircon () is a mineral belonging to the group of nesosilicates and is a source of the metal zirconium. Its chemical name is zirconium(IV) silicate, and its corresponding chemical formula is Zr SiO4. An empirical formula showing some of the r ...
grains at Mt. Narryer in Western Australia and then later at the nearby
Jack Hills The Jack Hills are a range of hills in Mid West Western Australia. They are best known as the source of the oldest material of terrestrial origin found to date: Hadean zircons that formed around 4.39 billion years ago. These zircons have enable ...
. These results and the SHRIMP analytical method itself were initially questioned but subsequent conventional analysis were partially confirmed. SHRIMP-I also pioneered ion microprobe studies of
titanium Titanium is a chemical element with the symbol Ti and atomic number 22. Found in nature only as an oxide, it can be reduced to produce a lustrous transition metal with a silver color, low density, and high strength, resistant to corrosion in ...
,
hafnium Hafnium is a chemical element with the symbol Hf and atomic number 72. A lustrous, silvery gray, tetravalent transition metal, hafnium chemically resembles zirconium and is found in many zirconium minerals. Its existence was predicted by Dmitri M ...
and
sulfur Sulfur (or sulphur in British English) is a chemical element with the symbol S and atomic number 16. It is abundant, multivalent and nonmetallic. Under normal conditions, sulfur atoms form cyclic octatomic molecules with a chemical formula ...
isotopic systems. Growing interest from commercial companies and other academic research groups, notably Prof. John de Laeter of Curtin University (Perth, Western Australia), led to the project in 1989 to build a commercial version of the instrument, the SHRIMP-II, in association with ANUTECH, the Australian National University's commercial arm. Refined ion optic designs in the mid-1990s prompted development and construction of the SHRIMP-RG (Reverse Geometry) with improved mass resolution. Further advances in design have also led to multiple ion collection systems (already introduced in the market by a French company years before), negative-ion stable isotope measurements and on-going work in developing a dedicated instrument for light stable isotopes. Fifteen SHRIMP instruments have now been installed around the world and SHRIMP results have been reported in more than 2000 peer reviewed scientific papers. SHRIMP is an important tool for understanding early Earth history having analysed some of the oldest terrestrial material including the Acasta Gneiss and further extending the age of zircons from the Jack Hills and the oldest impact crater on the planet. Other significant milestones include the first U/Pb ages for lunar zircon and Martian
apatite Apatite is a group of phosphate minerals, usually hydroxyapatite, fluorapatite and chlorapatite, with high concentrations of OH−, F− and Cl− ions, respectively, in the crystal. The formula of the admixture of the three most common e ...
dating. More recent uses include the determination of
Ordovician The Ordovician ( ) is a geologic period and System (geology), system, the second of six periods of the Paleozoic Era (geology), Era. The Ordovician spans 41.6 million years from the end of the Cambrian Period million years ago (Mya) to the start ...
sea surface temperature Sea surface temperature (SST), or ocean surface temperature, is the ocean temperature close to the surface. The exact meaning of ''surface'' varies according to the measurement method used, but it is between and below the sea surface. Air mass ...
, the timing of
snowball Earth The Snowball Earth hypothesis proposes that, during one or more of Earth's Greenhouse and icehouse Earth, icehouse Climate, climates, the Earth's surface, planet's surface became entirely or nearly entirely Freezing, frozen. It is believed that ...
events and development of stable isotope techniques.


Design and operation


Primary column

In a typical U-Pb geochronology analytical mode, a beam of (O2)1− primary ions are produced from a high-purity oxygen gas discharge in the hollow Ni cathode of a
duoplasmatron The Duoplasmatron is an ion source in which a cathode filament emits electrons into a vacuum chamber. A gas such as argon is introduced in very small quantities into the chamber, where it becomes charged or ionized through interactions with the ...
. The ions are extracted from the plasma and accelerated at 10 kV. The primary column uses
Köhler illumination Köhler illumination is a method of specimen illumination used for transmitted and reflected light (trans- and epi-illuminated) optical microscopy. Köhler illumination acts to generate an even illumination of the sample and ensures that an image o ...
to produce a uniform ion density across the target spot. The spot diameter can vary from ~5 µm to over 30 µm as required. Typical ion beam density on the sample is ~10 pA/µm2 and an analysis of 15–20 minutes creates an ablation pit of less than 1 µm.


Sample chamber

The primary beam is 45° incident to the plane of the sample surface with secondary ions extracted at 90° and accelerated at 10 kV. Three quadrupole lenses focus the secondary ions onto a source slit and the design aims to maximise transmission of ions rather than preserving an ion image unlike other ion probe designs. A Schwarzschild objective lens provides reflected-light direct microscopic viewing of the sample during analysis.


Electrostatic analyzer

The secondary ions are filtered and focussed according to their kinetic energy by a 1272 mm radius 90° electrostatic sector. A mechanically-operated slit provides fine-tuning of the energy spectrum transmitted into the magnetic sector and an electrostatic quadrupole lens is used to reduce aberrations in transmitting the ions to the magnetic sector.


Magnetic sector

The electromagnet has a 1000 mm radius through 72.5° to focus the secondary ions according to their mass/charge ratio according to the principles of the
Lorentz force In physics (specifically in electromagnetism) the Lorentz force (or electromagnetic force) is the combination of electric and magnetic force on a point charge due to electromagnetic fields. A particle of charge moving with a velocity in an elect ...
. Essentially, the path of a less massive ion will have a greater curvature through the magnetic field than the path of a more massive ion. Thus, altering the current in the electromagnet focuses a particular mass species at the detector.


Detectors

The ions pass through a collector slit in the focal plane of the magnetic sector and the collector assembly can be moved along an axis to optimise the focus of a given isotopic species. In typical U-Pb zircon analysis, a single secondary
electron multiplier An electron multiplier is a vacuum-tube structure that multiplies incident charges. In a process called secondary emission, a single electron can, when bombarded on secondary-emissive material, induce emission of roughly 1 to 3 electrons. If an el ...
is used for ion counting.


Vacuum system

Turbomolecular pump A turbomolecular pump is a type of vacuum pump, superficially similar to a turbopump, used to obtain and maintain high vacuum. These pumps work on the principle that gas molecules can be given momentum in a desired direction by repeated collisi ...
s evacuate the entire beam path of the SHRIMP to maximise transmission and reduce contamination. The sample chamber also employs a
cryopump A cryopump or a "cryogenic pump" is a vacuum pump that traps gases and vapours by condensing them on a cold surface, but are only effective on some gases. The effectiveness depends on the freezing and boiling points of the gas relative to the cryop ...
to trap contaminants, especially water. Typical pressures inside the SHRIMP are between ~7 x 10−9 mbar in the detector and ~1 x 10−6 mbar in the primary column.


Mass resolution and sensitivity

In normal operations, the SHRIMP achieves
mass resolution In mass spectrometry, resolution is a measure of the ability to distinguish two peaks of slightly different mass-to-charge ratios ''ΔM'', in a mass spectrum. Resolution and resolving power There are two different definitions of resolution an ...
of 5000 with sensitivity >20 counts/sec/ppm/nA for lead from zircon.


Applications


Isotope dating

For U-Th-Pb geochronology a beam of primary ions (O2)1− are accelerated and
collimated A collimated beam of light or other electromagnetic radiation has parallel rays, and therefore will spread minimally as it propagates. A perfectly collimated light beam, with no divergence, would not disperse with distance. However, diffraction p ...
towards the target where it sputters "secondary" ions from the sample. These secondary ions are accelerated along the instrument where the various isotopes of
uranium Uranium is a chemical element with the symbol U and atomic number 92. It is a silvery-grey metal in the actinide series of the periodic table. A uranium atom has 92 protons and 92 electrons, of which 6 are valence electrons. Uranium is weak ...
,
lead Lead is a chemical element with the symbol Pb (from the Latin ) and atomic number 82. It is a heavy metal that is denser than most common materials. Lead is soft and malleable, and also has a relatively low melting point. When freshly cu ...
and
thorium Thorium is a weakly radioactive metallic chemical element with the symbol Th and atomic number 90. Thorium is silvery and tarnishes black when it is exposed to air, forming thorium dioxide; it is moderately soft and malleable and has a high me ...
are measured successively, along with reference peaks for Zr2O+, ThO+ and UO+. Since the sputtering yield differs between ion species and relative sputtering yield increases or decreases with time depending on the ion species (due to increasing crater depth, charging effects and other factors), the measured relative isotopic abundances do not relate to the real relative isotopic abundances in the target. Corrections are determined by analysing unknowns and reference material (matrix-matched material of known isotopic composition), and determining an analytical-session specific calibration factor.


SHRIMP instruments around the world


References


External links


Founding SHRIMP Lab at Australian National University

Australian Scientific Instruments
{{DEFAULTSORT:Sensitive High Resolution Ion Microprobe Geochronological dating methods Mass spectrometry