Classifications

• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
  • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
  • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
  • G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
  • G01N23/2252—Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA]
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/252—Tubes for spot-analysing by electron or ion beams; Microanalysers
  • H01J37/256—Tubes for spot-analysing by electron or ion beams; Microanalysers using scanning beams
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
  • H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
• • G—PHYSICS
  • G01—MEASURING; TESTING
  • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
  • G01N2223/00—Investigating materials by wave or particle radiation
  • G01N2223/40—Imaging
  • G01N2223/418—Imaging electron microscope
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/244—Detection characterized by the detecting means
  • H01J2237/2441—Semiconductor detectors, e.g. diodes
  • H01J2237/24415—X-ray
  • H01J2237/2442—Energy-dispersive (Si-Li type) spectrometer
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/244—Detection characterized by the detecting means
  • H01J2237/2441—Semiconductor detectors, e.g. diodes
  • H01J2237/24415—X-ray
  • H01J2237/24425—Wavelength-dispersive spectrometer
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/26—Electron or ion microscopes
  • H01J2237/28—Scanning microscopes
  • H01J2237/2803—Scanning microscopes characterised by the imaging method
  • H01J2237/2804—Scattered primary beam
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/26—Electron or ion microscopes
  • H01J2237/28—Scanning microscopes
  • H01J2237/2803—Scanning microscopes characterised by the imaging method
  • H01J2237/2807—X-rays

Definitions

• the present invention relates generally to methods and structures for identifying minerals using charged particle beam systems with x-ray spectroscopy.
• a scanning electron microscope is a type of electron microscope that images a sample by scanning it with a focused beam of electrons in a predetermined pattern. The electrons interact with the atoms that make up the sample producing signals that provide information about the sample's surface topography, composition, and other properties.
• the types of signals produced by an SEM include secondary electrons, back- scattered electrons (BSE), characteristic X-rays, light (cathodoluminescence), specimen current and transmitted electrons.
• the signals result from interactions of the electron beam with atoms at or near the surface of the sample.
• SEI secondary electron imaging
• the SEM can produce very high-resolution images of a sample surface, revealing details less than 1 nm in size. Due to the very narrow electron beam, SEM micrographs have a large depth of field yielding a characteristic three-dimensional appearance useful for understanding the surface structure of a sample.
• Wavelength dispersive spectroscopy or “WDS.”
• a high-energy beam of charged particles such as electrons or protons, or a beam of X-rays
• a high-energy beam of charged particles such as electrons or protons, or a beam of X-rays
• an atom within the sample contains ground state (or unexcited) electrons in discrete energy levels or electron shells bound to the nucleus.
• the incident beam may excite an electron in an inner shell, ejecting it from the shell while creating an electron hole where the electron was.
• An electron from an outer, higher-energy shell then fills the hole, and the difference in energy between the higher-energy shell and the lower energy shell may be released in the form of an X-ray.
• each element allows x-rays that are characteristic of an element's atomic structure to be uniquely identified from one another.
• the number and energy of the X-rays emitted from a specimen can be measured by an x-ray spectrometer, such as an EDS or a wavelength dispersive spectrometer, to determine the elemental composition of the specimen to be measured.
• BSE Back-scattered electrons
• BSE signals are typically acquired at a rate of microseconds per pixel.
• EDS systems have a longer acquisition time, typically requiring on the order of several seconds per pixel to produce a spectrum having sufficient resolution to uniquely identify a mineral. The longer time required to collect an x-ray spectrum to uniquely identify a mineral substantially limits the number of pixels that can be measured.
• EDS systems are also typically insensitive to light atoms. Because of the advantages of both EDS detectors and BSE detectors, it is sometimes useful to use both BSE and x-ray spectra to accurately identify minerals, which requires more time and becomes a difficult problem to solve with a commercially viable approach.
• the Qemscan® and MLA® systems comprise an SEM, one or more EDS detectors, and software for controlling data acquisition. These systems identify and quantify elements represented within an acquired spectrum, and then match this elemental data against a list of mineral definitions with fixed elemental ranges.
• Some mineral classification systems compare the acquired spectrum of an unknown mineral to a library of known mineral spectrums, and then identify the sample based on which known spectrum that is most similar to the sample's spectrum.
• the MLA uses a chi-squared statistical test to compare the value at each energy channel of the measured spectrum to the value at the corresponding channel of the known mineral spectrum.
• the MLA assigns the unknown spectrum to the element having the "best match" to the spectrum, as long as a minimum similarity is met.
• QEMSCAN uses a system of rules or criteria that, if met, classify the spectrum. This is typically applied in a "first match" manner, that is, the spectrum is compared sequentially to the criteria for each possible mineral, and when the spectra meets a criteria, the system assigns that element to the spectrum.
• An object of the invention is to efficiently classify mineral samples analyzed by x- ray spectroscopy.
• the invention combines a rules-based approach with a similarity metric approach.
• the combination provides synergistic benefits beyond those that would be expected from the approach applied individually.
• Embodiments of the invention simplify the mineral identification process so that it can be automated.
• FIG. 1 is a scanning electron microscope suitable for implementing a mineral analysis system of the present invention.
• FIG. 2 is a flow chart of an embodiment of the invention.
• FIG. 3 is a flow chart of the first match algorithm portion of the embodiment of
• FIG. 2 The first figure.
• FIG. 4 is a flow chart of the best match algorithm portion of the embodiment of FIG. 2.
• Embodiments of the present invention are directed towards a method for efficiently and easily classifying minerals based on an x-ray spectrum.
• This invention describes a robust method that can be automated to identify a mineral from SEM-EDS data without human intervention.
• Combining a rules-based approach with a best match approach provides the unexpected benefit of decreasing the analysis time and increasing the robustness of the analysis.
• a first match, rules-based approach is used to eliminate data points that are not of interest, such as data points that represent the resin between mineral samples or data points that represent a crack in a sample, which provides unreliable readings.
• a "data point" corresponds to a position on the sample, either a single dwell point or multiple, grouped dwell points, and can include one or more types of information, such as an x-ray spectrum and back scattered electron information, from that position on the sample.
• the rules applied for such preliminary screening are typically different from the rules typically applied when the rules- based, first match, system is used alone. The different rules provide benefits that would not accrue from merely applying prior art systems in sequence.
• One embodiment uses in the "Best Match” analysis, the similarity metric described in 'Mineral Identification Using Mineral Definitions Including Variability' as described in U.S. Pat. Appl. No. 13/661,774, filed October 26, 2012, where is hereby incorporated by reference.
• This analysis when used with the present invention, eliminates the need for expert users to locate and collect examples of minerals to compare measured data against for determining a similarity metric or formulating a list of rules that are applied sequentially to identify a mineral. This system allows untrained operators to use it, as opposed to previous systems that required extensive training and expertise.
• FIG. 1 is an example of a scanning electron beam system 100 with an x-ray detector 140 suitable for analyzing samples prepared according to the present invention.
• a scanning electron microscope 141 along with power supply and control unit 145, is provided with system 100.
• An electron beam 132 is emitted from a cathode 153 by applying voltage between cathode 153 and an anode 154.
• Electron beam 132 is focused to a fine spot by means of a condensing lens 156 and an objective lens 158.
• Electron beam 132 is scanned two-dimensionally on the specimen by means of a deflection coil 160. Operation of condensing lens 156, objective lens 158, and deflection coil 160 is controlled by power supply and control unit 145.
• a system controller 133 controls the operations of the various parts of scanning electron beam system 100.
• the vacuum chamber 110 is evacuated with ion pump 168 and mechanical pumping system 169 under the control of vacuum controller 132.
• Electron beam 132 can be focused onto sample 102, which is on movable X-Y stage 104 within lower vacuum chamber 110.
• sample 102 When the electrons in the electron beam strike sample 102, the sample gives off x-rays whose energy correlated to the elements in the sample. X-rays having energy inherent to the elemental composition of the sample are produced in the vicinity of the electron beam incident region.
• Emitted x-rays are collected by x-ray detector 140, preferably an energy dispersive detector of the silicon drift detector type, although other types of detectors could be employed, which generates a signal having an amplitude proportional to the energy of the detected x-ray.
• Backscattered electrons are detected by backscatter electron detector 147, which can comprise, for example, a microchannel plate or solid state detector.
• Output from x-ray detector 140 is amplified and sorted by the processor 120, which counts and sorts the total number of X-rays detected during a specified period of time, at a selected energy and energy resolution, and a channel width (energy range) of preferably between 10-20 eV per channel.
• output from BSE detector 147 is amplified and processed by processor 120.
• Processor 120 can comprise a computer processor; operator interface means (such as a keyboard or computer mouse); program memory 122 for storing data and executable instructions; interface means for data input and output; executable software instructions embodied in executable computer program code; and display 144 for displaying backscattered electron images and the results of a multivariate spectral analysis by way of video circuit 142.
• Processor 120 can be a part of a standard laboratory personal computer, and is typically coupled to at least some form of computer-readable media.
• Computer-readable media which include both volatile and nonvolatile media, removable and non-removable media, may be any available medium that can be accessed by processor 120.
• Computer-readable media comprise computer storage media and communication media.
• Computer storage media include volatile and nonvolatile, removable and non-removable media implemented in any method or technology for storage of information such as computer-readable instructions, data structures, program modules or other data.
• computer storage media include RAM, ROM, EEPROM, flash memory or other memory technology, CD-ROM, digital versatile disks (DVD) or other optical disk storage, magnetic cassettes, magnetic tape, magnetic disk storage or other magnetic storage devices, or any other medium that can be used to store the desired information and that can be accessed by processor 120.
• Program memory 122 can include computer storage media in the form of removable and/or non-removable, volatile and/or nonvolatile memory and can provide storage of computer-readable instructions, data structures, program modules and other data.
• the processor 120 is programmed by means of instructions stored at different times in the various computer-readable storage media of the computer.
• Programs and operating systems are typically distributed, for example, on floppy disks or CD-ROMs. From there, they are installed or loaded into the secondary memory of a computer. At execution, they are loaded at least partially into the computer's primary electronic memory.
• the invention described herein includes these and other various types of computer-readable storage media when such media contain instructions or programs for implementing the steps described below in conjunction with a microprocessor or other data processor.
• the invention also includes the computer itself when programmed according to the methods and techniques described herein.
• An x-ray spectrum obtained from the system can be stored in a portion of memory 122, such as the measured spectra memory portion 123.
• Data template memory portion 124 stores data templates, such as definitions of known spectra of elements or, in some embodiments, known diffraction patterns of materials.
• the embodiment shown includes a scanning electron microscope
• related embodiment could use a transmission electron microscope or a scanning transmission electron microscope to generate x-rays from the sample.
• An x-ray fluorescence system could also be used to generate x-rays from the sample.
• Other embodiments may detect other characteristic radiation, such as gamma rays, from a sample.
• FIG. 2 shows an overview of a preferred embodiment of a mineral analyzer in accordance with the invention.
• a user of the system indicates the origin of the sample, such as being from a Copper-Lead-Zinc deposit. Knowing the origin reduces the number of minerals that are likely to be in sample, reducing the number of comparisons required and thereby reducing analysis time.
• the system retrieves a pre- determined list of mineral definitions suitable for the sample.
• mineral definition is meant an analysis protocol that when followed will determine the minerals present in the sample, thereby defining the minerals in terms of analysis rules.
• the list of mineral definitions is comprised of one or more analysis sections, where in one embodiment each analysis section is either a 'First Match' or 'Best Match' section.
• step 206 the system determines which analysis section is to be applied to the data point.
• the first analysis section applied uses a rules-based, first match analysis in step 208.
• decision step 210 if the analysis section has identified the mineral composition of the data point, then the data point is assigned its mineral
• step 218 If it is determined in decision block 212 that there are additional data points to be analyzed, the next data point is read in step 214 and the analysis repeats the analysis from step 206.
• step 210 the analysis section fails to identify the composition of the data point, the system determines in decision step 211 if additional analysis sections are available. If available, then the system selects a different analysis section in step 206. For example, if the data point did not meet the criteria for any mineral under the rules-based analysis, then a best match analysis is performed in step 207. If it is determined in step 210 that the best match analysis in step 207 determined the mineral composition of the data point, then the analysis of that data point is complete. If it is then determined in decision block 212 that there are additional data points, the next data point is read in step 214 and the analysis repeats the analysis from step 206.
• the third analysis section may be a second, first match, rules-based analysis system in step 208, with different rules than the first analysis section.
• the third analysis section may be another best match analysis section in section 207 using a different matching algorithm or a lower threshold. Again, if the mineral composition of the data point was found to be determined in block 210, then the data point is assigned its mineral identification in step 218.
• step 214 the analysis repeats the analysis from step 206. If the mineral composition of the data point is not identified, and it is determined in step 211 that there is an additional analysis section, then the process returns to step 206 to apply another analysis section. If no additional analysis sections are available, the data point may be classified as "unknown" in step 216.
• the rules in the third analysis section are less stringent than the rules in the first analysis section or the matching threshold in the best match section, so the third analysis section is likely to find at least a general classification for the data point.
• FIG. 3 shows a 'first match' analysis section in more detail.
• This analysis is similar to a QEMSCAN Species Identification Protocol (SIP) rule, described, for example, in U.S. Pat. Publication No. 2011/0144922 is a Method and System for Spectrum Data Analysis, which is assigned to the assignee of the present invention.
• a first match analysis section uses a number of entries in a rules table. Each rule consists of one or more criteria, such as the height of an x-ray peak at a specific energy range, or a backscatter electron intensity value, that must be met to classify the data point as a particular mineral.
• one rule may state that if the BSE value is less than 30, the data point represents the resin used to embed the mineral sample, and so that data point may be discarded. Another rule may indicate that if the BSE value is less than 1000 counts per second, the electron beam is positioned at a crack in the sample, and the data point can be discarded. Another rule may state that if the composition of silicon is between 45% and 47% and oxygen is between 52% and 55%, then the mineral is quartz.
• step 302 a set of rules in a particular sequence is provided.
• step 304 a data point is compared to the first rule in the set. If the data point meets the criteria, decision block 306 shows that the composition of the data point is considered to be the mineral corresponding to the rule and the identification process is complete. If in step 306, the analysis section fails to identify the composition of the data point, the system determines in decision step 308 if additional rules are available. If available, then the next rule is applied to the data point in step 304. The process continues until either the mineral is identified in step 310, or all rules have been applied, and the data point does not meet the criteria of any rule in step 312. If the mineral is identified, then the system continues to process the next data point in step 214 of FIG. 2. If not, then the system continues to process the next analysis section in step 206 of FIG. 2.
• the process of FIG. 3 may be used to remove bad data points, or quickly identify areas that are definitely not of interest such as the resin used to mount the sample.
• the process of FIG. 3 may also be used as a final analysis section that classifies a mineral into a broad category, if it was not possible to specifically identify the mineral using more specific rules or matching.
• the data point that is, the unknown spectrum, is checked sequentially against each of the rules until either a match is found or all the rules have been checked. If the 'First Match' section provides a positive result, the result is taken as the mineral identification. If the 'First Match section does not result in a match, then the process determines if the 'Best Match' section can be used.
• a "Best Match” analysis section consists of mineral definitions and a threshold value.
• a preferred similarity metric is described in "Mineral Identification Using Mineral Definitions Including Variability" as described in U.S. Pat. Appl. No. 13/661,774.
• FIG. 4 shows that the steps of a "Best Match” analysis section.
• step 402 a library of mineral definitions is provided.
• step 404 the data point is compared to each of the mineral definitions in the library, and a similarity metric between the data point and each mineral definition in a library is calculated.
• the mineral definition that has the highest similarity metric with the data point is taken as the best match.
• step 408 the similarity metric of the best match is compared to a pre-specified threshold value, and, if the threshold is met, the best matching mineral definition is taken as the mineral identification in step 410. And the system continues to process the next data point in step 214 of FIG. 2. If the metric falls below the threshold, then no mineral identification is assigned in step 412 and, as described in step 206 of FIG. 2, another analysis section is applied. For example, the third section might be another "first match" section using different rules than the first "first match” section.
• the data point may be compared to Chalcopyrite, having a composition of Fe 30.43%, Cu 34.63%, S 34.94%, and having an average atomic number of 23.54, and to Galena, having a composition of S 13.40%, Pb 86.60% and having an average atomic number of 73.16%. If the data point fails to match Chalcopyrite or Galena with a match of, for example, 95%, then the data point is examined again using a second "first match" section having rules different from the original "first match” section. This second match section, being applied only after a match is not found, can be more generic. For example, a rule can state that if the Si composition is greater than 30%, the mineral is classified as "other silicates" and if the mineral has a composition of greater than 30% sulfur, the mineral is classified as "other sulphides.”
• a method for determining the mineral content of a sample comprising placing a sample in a scanning electron microscope; directing the electron beam to a point on the sample to obtain an x-ray spectrum of the sample and a backscatter electron intensity value, the x-ray spectrum and the backscatter electron intensity value corresponding to a first data point, the data point having an associated mineral composition; sequentially comparing the data point to criteria within a first set of rules, each criterion corresponding to a mineral composition, and identifying the mineral composition of the data point as the mineral composition
• the data point fails to satisfy any of the criteria in the first set of rules, comparing the x-ray spectrum of the data point to x-ray spectra corresponding to minerals in a library of minerals to determine which of the mineral in the library is a best match for the data point; and if the match between the data point x-ray spectrum and the x-ray spectrum in the library meets a predetermined threshold, identifying the mineral composition of the data point as the mineral composition corresponding to the best matching library spectrum.
• a method further comprising if the match between the data point x-ray spectrum and the x-ray spectrum in the library fails to meet the predetermined threshold, sequentially comparing the data point to criteria within a second set of rules, each criterion corresponding to a mineral composition, and identifying the mineral composition of the data point as the mineral composition corresponding to the first satisfied criterion within the second set of rules.
• a method in which comparing the x-ray spectrum of the data point to x-ray spectra corresponding to minerals in a library of minerals to determine which of the mineral in the library is a best match for the data point further comprises comparing a backscatter electron intensity of the data point to a backscatter electron intensity or comprises calculating similarity metrics between the data point and each of the minerals in the library.
• a method in which sequentially comparing the data point to criteria within a first set of rules identifies bad data points or identifies parts of the sample that do not need detailed analysis.
• a method in which calculating similarity metrics includes determining probabilities that the library mineral will produce the values observed for the data point or includes calculating a chi squared value.
• a scanning electron microscope system for determining the mineral content of a sample, comprising an electron beam column for directing an electron beam toward a mineral sample; a detector for measuring the energy or wavelength of x-rays emitted from the mineral sample in response to the impingement of electrons in the electron beam; a processor for executing computer instructions to determine the minerals present in the sample; a computer memory containing computer instructions for sequentially comparing the data point to criteria within a first set of rules, each criterion corresponding to a mineral composition, and identifying the mineral composition of the data point as the mineral composition corresponding to the first satisfied criterion; if the data point fails to satisfy any of the criteria in the first set of rules, comparing the x-ray spectrum of the data point to x-ray spectra corresponding to minerals in a library of minerals to determine which of the mineral in the library is a best match for the data point; and if the match between the data point x-ray spectrum and the x-ray
• a scanning electron microscope system in which the computer instructions further comprise instructions for, if the match between the data point x- ray spectrum and the x-ray spectrum in the library fails to meet the predetermined threshold, sequentially comparing the data point to criteria within a second set of rules, each criterion corresponding to a mineral composition, and identifying the mineral composition of the data point as the mineral composition corresponding to the first satisfied criterion within the second set of rules.
• a scanning electron microscope system in which the computer instructions for comparing the x-ray spectrum of the data point to x-ray spectra corresponding to minerals in a library of minerals to determine which of the mineral in the library is a best match for the data point further comprise computer instructions for comparing a backscatter electron intensity of the data point to a backscatter electron intensity or comprise computer instructions for calculating similarity metrics between the data point and each of the minerals in the library.
• a scanning electron microscope system of in which the computer instructions for sequentially comparing the data point to criteria within a first set of rules comprise computer instructions for identifying bad data points or identifying parts of the sample that do not need detailed analysis.

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• 2012
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