Sample-specific reference spectra library

Patent metadata

Field	Value
Publication number	US-9719950-B2
Application number	US-201514630704-A
Country	US
Kind code	B2
Filing date	Feb 25, 2015
Priority date	Feb 25, 2015
Publication date	Aug 1, 2017
Grant date	Aug 1, 2017

Abstract

A method and apparatus are provided for identifying a material with a sample-specific reference spectral list or library. A sequential approach to SEM-EDS automated mineralogy classification is carried out by performing two or more material classification analyses. A pre-classification step restricts the processing of spectra deconvolution algorithms to a subset of spectra that pass a dominant mineral criteria resulting in a significantly reduced subset of reference spectra that occur within the measured sample in pure enough form at a given minimum quantity. The following complex classification stages involving deconvolution of multiple constituents within measured spectra is based on this sample relevant subset.

First claim

We claim:

1. A method of identifying materials in a sample, comprising:
collecting from multiple points on the sample measurement data providing information from which the composition of the sample at the multiple points can be determined;
analyzing the measurement data to identify materials present in a pure phase at any of the multiple points in the sample;
forming a sample-specific reference library containing materials identified as present in a pure phase at any of the multiple points in the sample; and
analyzing the measurement data using the sample-specific library to determine the composition of the multiple points on the sample.

2. The method of claim 1 , wherein analyzing the measurement data to identify materials present in a pure phase comprises comparing the measurement data to a global reference library containing spectra of known pure elements and/or minerals.

3. The method of claim 2 , wherein the sample specific reference library comprises less than two thirds of the materials in the global reference library.

4. The method of claim 1 , wherein at least a portion of the step of collecting from multiple points on the sample measurement data and at least a portion of the step of analyzing the measurement data to identify materials present in a pure phase are performed simultaneously.

5. The method of claim 4 in which analyzing the measurement data using the sample-specific library to determine the composition of the multiple points on the sample includes re-analyzing the multiple points when additional materials are added to the sample-specific library.

6. The method of claim 5 in which re-analyzing the multiple points comprises re-analyzing the material using only combinations including the material newly added to the sample-specific library.

7. The method of claim 1 , wherein collecting from multiple points on the sample measurement data comprises directing an electron beam toward the multiple points on the sample and collecting an x-rays spectrum from each of the multiple points.

8. The method of claim 7 in which the sample specific library contains x-ray spectra of pure materials.

9. The method of claim 1 , wherein collecting from multiple points on the sample measurement data comprises collecting diffraction data.

10. The method of claim 1 , wherein collecting from multiple points on the sample measurement data comprises collecting spectral data.

11. The method of claim 1 , wherein collecting measurement data includes collecting x-ray data, electron backscatter diffraction data, electron energy loss data, or light data.

12. The method of claim 1 , wherein analyzing the measurement data includes analyzing the data using x-ray spectroscopy, electron backscatter diffraction analysis, electron energy loss spectroscopy, light spectroscopy, or Raman spectroscopy.

13. The method of claim 1 in which:
collecting from multiple points on the sample measurement data comprises collecting from multiple points on the sample x-ray spectral data;
analyzing the measurement data to identify materials present in a pure phase at any of the multiple points in the sample comprises analyzing the x-ray spectral data to identify materials present in a pure phase at any of the multiple points in the sample; and
analyzing the measurement data using the sample-specific library comprises analyzing the x-ray spectral data and the sample-specific library to determine the composition of the multiple points on the sample.

14. The method of claim 1 further comprising, before analyzing the measurement data using the sample-specific library, adding spectra of a trace mineral to the sample-specific library.

15. The method of claim 1 in which analyzing the measurement data using the sample-specific library to determine the composition of the multiple points on the sample comprises analyzing the same or a subset of the measurement data analyzed to identify materials present in a pure phase.

16. A method of identifying a material in a SEM system, comprising:
directing an electron beam toward multiple points on a sample;
collecting a measured x-ray spectrum from each of the multiple points on the sample;
analyzing the x-ray spectra from the multiple points on the sample to determine materials present in pure form at any of the multiple points on the sample; and
analyzing the x-ray spectra from the multiple points on the sample to determine the composition of the sample at the multiple points.

17. The method of claim 16 in which analyzing the x-ray spectra from the multiple points on the sample to determine materials present in pure form comprises comparing the x-ray spectra with reference spectra from a global reference library to form a sample-specific library of the materials present in pure form and in which analyzing the x-ray spectra from the multiple points on the sample to determine the composition of the sample at the multiple points includes analyzing the x-ray spectra from the multiple points using the sample-specific library.

18. The method of claim 17 in which the global reference library includes more than fifty materials and in which the sample-specific reference library includes less than thirty materials.

19. The method of claim 17 in which the sample-specific library includes reference spectra of about ten to twenty minerals, these minerals being selected from the group consisting of: albite, anatase, anhydrite, ankerite, annite, anorthite, apatite, aragonite, augite, barite, beidellite, berthierine, biotite, brookite, calcite, calcium montmorillonite, carbon, chamosite, chlorapatite, clinochlore, dickite, dolomite, feldspar, fluorapatite, fluorite, forsterite, glauconite, goethite, graphite, gypsum, halite, halloysite, hematite, illite, ilmenite, kaolinite, kutnohorite, lepidocrocite, magnesite, magnetite, monazite, montmorillonite, muscovite, orthoclase, phlogopite, potassium feldspar, pyrite, quartz, rectorite, rhodochrosite, rutile, saponite, siderite, sodium montmorillonite, sylvite, talc, xenotime, and zircon.

20. A materials analysis system, comprising:
an electron beam focusing column;
an x-ray detector;
a control system for controlling the scanning electron microscope in accordance with operator instructions or stored instructions;
a computer memory in data communications with the scanning electron microscope and storing computer readable instructions for performing the steps of claim 16 .

21. The materials analysis system of claim 20 in which the computer memory includes a global reference library and a sample specific library.

Assignees

• Fei Co

Inventors

• Owen Michael James
• Donaldson Ashley
• Howell Garth
• Parker Phillip John Christopher

Classifications

• H01J37/252

  Tubes for spot-analysing by electron or ion beams; Microanalysers · CPC title

• H01J2237/2807

  X-rays · CPC title

• G01N23/2252 Primary

  Measuring emitted X-rays, e.g. electron probe microanalysis [EPMA] · CPC title

• H01J37/244

  Detectors; Associated components or circuits therefor · CPC title

• G01J3/44

  Raman spectrometry; Scattering spectrometry {; Fluorescence spectrometry} · CPC title