System and method for x-ray absorption spectroscopy using spectral information from two orthogonal planes

Patent metadata

Field	Value
Publication number	US-12429437-B2
Application number	US-202418937615-A
Country	US
Kind code	B2
Filing date	Nov 5, 2024
Priority date	Nov 7, 2023
Publication date	Sep 30, 2025
Grant date	Sep 30, 2025

Abstract

An apparatus includes an x-ray source configured to generate x-rays, at least some of which impinge a sample and at least one diffractor configured to concurrently diffract at least some of the x-rays from the sample in a first direction and in a second direction substantially orthogonal to the first direction. The apparatus further includes at least one two-dimensional (2D) position-sensitive x-ray detector configured to receive at least some of the diffracted x-rays and to concurrently generate first spectral information of the x-rays diffracted in the first direction and second spectral information of the x-rays diffracted in the second direction. The apparatus further includes circuitry configured to receive the first and second spectral information and to generate a single x-ray absorption spectroscopy (XAS) spectrum using the first and second spectral information.

First claim

What is claimed is:

1. An apparatus comprising:
an x-ray source configured to generate x-rays diverging in a first direction and diverging in a second direction substantially orthogonal to the first direction, the x-rays having a spectral intensity variation less than 10% over an energy bandwidth greater than 25 eV with at least one x-ray energy between 1 keV and 30 keV, at least some of the x-rays impinging a sample;
at least one diffractor that is substantially flat, the at least one diffractor configured to receive and concurrently diffract at least some of the x-rays as a function of x-ray energy in the first direction and in the second direction;
at least one two-dimensional (2D) position-sensitive x-ray detector configured to receive at least some of the x-rays diffracted in the first direction by the at least one diffractor and at least some of the x-rays diffracted in the second direction by the at least one diffractor and to concurrently generate first spectral information of the x-rays diffracted in the first direction and second spectral information of the x-rays diffracted in the second direction;
an electromechanical subsystem configured to position the x-ray source, the at least one diffractor, and/or the at least one 2D position-sensitive x-ray detector relative to one another;
circuitry configured to receive the first and second spectral information from the at least one 2D position-sensitive x-ray detector and to generate a single x-ray absorption spectroscopy (XAS) spectrum using the first and second spectral information; and
a sample holder configured to hold the sample between the x-ray source and the at least one diffractor or between the at least one diffractor and the at least one 2D position-sensitive x-ray detector.

2. The apparatus of claim 1 , wherein the electromechanical subsystem is configured to controllably position the x-ray source, the at least one diffractor, and/or the at least one 2D position-sensitive x-ray detector such that the at least one 2D position-sensitive x-ray detector concurrently generates the first spectral information with a first predetermined energy resolution over a first energy bandwidth and generates the second spectral information with a second predetermined energy resolution over a second energy bandwidth in the second direction.

3. The apparatus of claim 1 , wherein the x-rays generated by the x-ray source have an angular divergence greater than 5 mrad.

4. The apparatus of claim 1 , wherein the x-ray source comprises an x-ray focusing optic.

5. The apparatus of claim 1 , wherein the at least one diffractor comprises a plurality of crystals arranged along an incident x-ray beam axis such that the x-rays from the sample impinge the crystals sequentially, a plurality of mosaic crystals, or a single crystal comprising a material selected from the group consisting of: diamond; graphite; quartz; LiF; silicon; germanium.

6. The apparatus of claim 1 , wherein the electromechanical subsystem is configured to controllably position the at least one diffractor and to change Bragg angles of the at least one diffractor.

7. The apparatus of claim 1 , wherein the at least one diffractor comprises:
a first diffractor configured to receive the x-rays from the sample and to concurrently diffract at least some of the received x-rays as a function of x-ray energy in the first direction and in the second direction; and
a second diffractor configured to receive second x-rays from the sample and to concurrently diffract at least some of the received second x-rays as a function of x-ray energy in the first direction and in the second direction.

8. The apparatus of claim 1 , wherein the sample holder is configured to position a substantially flat sample such that an incidence angle of the x-rays relative to a surface of the sample is less than 45 degrees.

9. The apparatus of claim 1 , wherein the sample holder is configured to hold the sample between the at least one diffractor and the at least one 2D position-sensitive x-ray detector and the at least one 2D position-sensitive x-ray detector is positioned at a distance less than 15 millimeters from an area of the sample illuminated by the x-rays.

10. The apparatus of claim 1 , wherein the sample holder is configured to hold the sample between the x-ray source and the at least one diffractor,
the at least one diffractor comprising a plurality of crystal diffractors distributed along at least one x-ray propagation axis of x-rays from the sample, at least one crystal diffractor of the plurality of crystal diffractors having an energy resolution better than 30 eV, wherein
each crystal diffractor of the plurality of crystal diffractors concurrently diffracts a corresponding portion of the x-rays from the sample in the first direction and in the second direction.

11. The apparatus of claim 10 , wherein the spectrum comprises an absorption edge of the sample within an x-ray spectral range having a pre-edge range greater than 5 eV and a post-edge range greater than 30 eV.

12. The apparatus of claim 10 , wherein the spectrum comprises an XANES portion and an EXAFS portion.

13. The apparatus of claim 10 , wherein each crystal diffractor of the plurality of crystal diffractors has a corresponding Bragg angle along the x-ray propagation axis, and the Bragg angles of different crystal diffractors are different from one another.

14. The apparatus of claim 13 , wherein an energy difference corresponding to the different Bragg angles of different crystal diffractors is greater than an energy resolution of an upstream-most crystal diffractor of the plurality of crystal diffractors.

15. An apparatus comprising:
an x-ray source configured to generate x-rays diverging in a first direction and diverging in a second direction substantially orthogonal to the first direction, the x-rays having a spectral intensity variation less than 10% over an energy bandwidth greater than 25 eV with at least one x-ray energy between 1 keV and 30 keV, at least some of the x-rays impinging a sample;
at least one diffractor configured to receive and to concurrently diffract at least some of the x-rays as a function of x-ray energy in the first direction and in the second direction, wherein the at least one diffractor comprises:
a first diffractor configured to receive the x-rays from the sample and to concurrently diffract at least some of the received x-rays as a function of x-ray energy in the first direction and in the second direction; and
a second diffractor configured to receive second x-rays transmitted through the first diffractor and to concurrently diffract at least some of the received second x-rays as a function of x-ray energy in the first direction and in the second direction;

at least one two-dimensional (2D) position-sensitive x-ray detector configured to receive at least some of the x-rays diffracted in the first direction by the at least one diffractor and at least some of the x-rays diffracted in the second direction by the at least one diffractor and to concurrently generate first spectral information of the x-rays diffracted in the first direction and second spectral information of the x-rays diffracted in the second direction;
an electromechanical subsystem configured to position the x-ray source, the at least one diffractor, and/or the at least one 2D position-sensitive x-ray detector relative to one another;
circuitry configured to receive the first and second spectral information from the at least one 2D position-sensitive x-ray detector and to generate a single x-ray absorption spectroscopy (XAS) spectrum using the first and second spectral i

Assignees

• Sigray Inc

Inventors

• Yun Wenbing
• Kirz Janos
• Lewis Sylvia Jia Yun

Classifications

• G01N2223/076

  X-ray fluorescence · CPC title

• G01N23/223

  by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence · CPC title

• G01N2223/0563

  measure of energy-dispersion spectrum of diffracted radiation · CPC title

• G01N2223/0568

  spectro-diffractometry · CPC title

• G01N23/2076

  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