X-ray spectrometer and methods for use

Patent metadata

Field	Value
Publication number	US-11796490-B2
Application number	US-202117366759-A
Country	US
Kind code	B2
Filing date	Jul 2, 2021
Priority date	Sep 15, 2016
Publication date	Oct 24, 2023
Grant date	Oct 24, 2023

Abstract

A spectrometer includes a crystal analyzer having a radius of curvature that defines a Rowland circle, a sample stage configured to support a sample such that the sample is offset from the Rowland circle, x-ray source configured to emit unfocused x-rays toward the sample stage, and a position-sensitive detector that is tangent to the Rowland circle. A method performed via a spectrometer includes emitting, via an x-ray source, unfocused x-rays toward a sample that is mounted on a sample stage such that the sample is offset from the Rowland Circle, thereby causing the sample to emit x-rays that impinge on the crystal analyzer or transmit a portion of the unfocused x-rays to impinge on the crystal analyzer; scattering, via the crystal analyzer, the x-rays that impinge on the crystal analyzer; and detecting the scattered x-rays via a position-sensitive detector that is tangent to the Rowland circle.

First claim

The invention claimed is:

1. A spectrometer comprising:
a crystal analyzer having a radius of curvature that defines a Rowland circle;
a sample stage configured to support a sample such that the sample is inside the Rowland circle;
an x ray tube inside the Rowland circle configured to emit x-rays toward the sample stage that are unfocused and broadband; and
a position-sensitive detector that is tangent to the Rowland circle.

2. The spectrometer of claim 1 , wherein the spectrometer is configured in an emission mode such that the position-sensitive detector is configured to detect x-rays emitted by the sample.

3. The spectrometer of claim 1 , wherein the spectrometer is configured in a transmission mode such that the position-sensitive detector is configured to detect x-rays transmitted through the sample.

4. The spectrometer of claim 1 , wherein the position-sensitive detector is configured to detect the x-rays after the x-rays are transmitted through the sample after being redirected by the crystal analyzer.

5. The spectrometer of claim 1 , wherein the sample stage is located between the crystal analyzer and the position-sensitive detector.

6. The spectrometer of claim 1 , wherein the spectrometer is integrated into or configured to operate within a glove box or a fume hood.

7. The spectrometer of claim 1 , wherein the x-ray tube is configured to emit x-rays having a spot size on a sample, when present, that is at least 0.1 mm.

8. The spectrometer of claim 1 , wherein the spectrometer is operable to distinguish between x-rays having an energy difference as small as 1 electron-volt (eV).

9. A method performed via a spectrometer having a crystal analyzer with a radius of curvature that defines a Rowland circle, the method comprising:
emitting first x-rays toward a sample that are unfocused and broadband via an x-ray tube that is inside the Rowland circle to cause the sample that is inside the Rowland circle to transmit the first x-rays or to cause the sample to emit second x-rays;
selectively redirecting the first x-rays or the second x-rays via the crystal analyzer; and
detecting, via a position-sensitive detector that is tangent to the Rowland circle, the first x-rays after the first x-rays have transmitted through the sample; or
detecting the second x-rays via the position-sensitive detector.

10. The method of claim 9 , the method comprising detecting the first x-rays via the position-sensitive detector after the first x-rays have transmitted through the sample.

11. The method of claim 9 , the method comprising detecting the second x-rays via the position-sensitive detector.

12. The method of claim 9 , wherein the sample is located between the crystal analyzer and the position-sensitive detector.

13. The method of claim 9 , wherein emitting the first x-rays comprises emitting the first x-rays such that the first x-rays form a spot on the sample having a width of at least 0.1 mm.

14. The method of claim 9 , wherein detecting the first x-rays comprises the spectrometer distinguishing between x-rays having an energy difference as small as 1 electron-volt (eV).

15. The method of claim 9 , wherein detecting the second x-rays comprises the spectrometer distinguishing between x-rays having an energy difference as small as 1 electron-volt (eV).

16. The method of claim 9 , wherein the method is performed to determine a distribution of nominal oxidation states, identify provenance, and/or examine local chemistries of sulfur in oil shales, crude oil solids, crude oil liquids, refined crude oil products, processed or unprocessed oil shale, coal, coal ash, fly ash, biochars, soil, pigments, gem stones, or sulfur-containing materials that react with air.

17. The method of claim 9 , wherein the method is performed to determine a distribution of nominal oxidation states, identify provenance, and/or examine local chemistries of phosphorus in biochars, lubricants, soil, phosphate-rich ores, or phosphorous-containing materials that react with air.

18. The method of claim 9 , wherein the method is performed to determine a distribution of nominal oxidation states, identify provenance, and/or examine local chemistries of technetium in waste stream products from nuclear fuel processing or recovery, environmental samples showing technetium contamination, or technetium-containing materials that react with air.

19. The method of claim 9 , wherein the method is performed to determine a distribution of nominal oxidation states, identify provenance, and/or examine local chemistries of chromium-containing consumer electronic components, soil, paint sludge, industrial waste, ore, or mine tailings.

20. The method of claim 9 , wherein detecting the first x-rays comprises distinguishing x-rays having an energy difference as small as 1 electron-volt (eV) as the spectrometer operates in an x-ray emission spectroscopy (XES) configuration.

21. The method of claim 9 , wherein detecting the second x-rays comprises distinguishing x-rays having an energy difference as small as 1 electron-volt (eV) as the spectrometer operates in an x-ray emission spectroscopy (XES) configuration.

22. A spectrometer comprising:
a crystal analyzer having a radius of curvature that defines a Rowland circle;
a sample stage configured to support a sample such that the sample is inside the Rowland circle;
an x-ray tube configured to emit unfocused x-rays; and
a position-sensitive detector that is tangent to the Rowland circle.

23. The spectrometer of claim 22 , wherein the x-ray tube is configured to emit x-rays having a spot size on a sample, when present, that is at least 0.1 mm.

24. The spectrometer of claim 22 , wherein the spectrometer is operable to distinguish between x-rays having an energy difference as small as 1 electron-volt (eV).

Assignees

• Univ Washington

Inventors

• Seidler Gerald Todd
• Hoidn Oliver
• Holden William

Classifications

• G01N23/2076 Primary

  for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS · CPC title

• G01N23/207

  Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions · CPC title

• G01N23/20008

  Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor (monochromators for X- rays using crystals G21K1/06) · CPC title

• G01N23/20025

  Sample holders or supports therefor · CPC title

• G01N23/20091

  Measuring the energy-dispersion spectrum [EDS] of diffracted radiation · CPC title