# US 10,371,651 B2 · Method for analyzing an object by X-ray diffraction

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- Number: US 10,371,651 B2
- Document ID: US10371651B2
- Status: Granted
- Kind: B2
- Application number: 15/389,819
- Filed: 2016-12-23
- Published: 2017-06-29
- Granted: 2019-08-06
- Earliest claimed: 2015-12-24
- Assignees: Commissariat A L'energie Atomique Et Aux Energies Alternatives
- Applicants: Commissariat a L'Energie Atomique et aux Energies Alternatives
- Inventors: Damien Barbes; Caroline Paulus; Joachim Tabary
- Web page: https://patentgrep.com/patent/US10371651B2

## CPC

- G01N 23/2076: {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}
- G01N 23/20025: Sample holders or supports therefor
- G01N 23/20091: Measuring the energy-dispersion spectrum [EDS] of diffracted radiation
- G01N 2223/316: collimators
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The invention is a method for analysing an object by x-ray diffraction spectroscopy, in which a spectroscopic detector comprising a plurality of adjacent pixels is placed facing an object irradiated by an x-ray beam. Each pixel is able to acquire an energy spectrum of radiation elastically scattered by the object, the radiation propagating in a direction making an acute angle to the propagation direction of the collimated beam. The method allows, on the basis of each measured spectrum, a nature of the materials composing various portions of the object to be determined.

## Claims

### Claim 1

A Method for analysing an object comprising:
a) placing the object facing an irradiation source emitting ionising electromagnetic radiation and irradiating the object using the irradiation source, through a first collimator, so as to form a collimated incident beam propagating towards the object along a propagation axis;
b) placing a detector comprising a plurality of pixels, so that each pixel is configured to detect radiation scattered by the object thus irradiated, the scattered radiation propagating in a direction making an acute scattering angle to the propagation axis;
c) acquiring, with a plurality of pixels of the detector, a scattering spectrum representative of an energy distribution of the scattered radiation, each scattering spectrum being associated with one pixel;
d) decomposing the object into elementary volumes and associating, with each pixel, a spatial dispersion function representing a contribution of each elementary volume to the scattered radiation detected by each pixel;
e) on the basis of the acquired scattering spectra and of the spatial dispersion functions associated with respective pixels, determining a scattering signature associated with each elementary volume, the signature being representative of a material forming the elementary volume; and
f) on the basis of the scattering signatures associated with each elementary volume, estimating a nature of the material forming the various elementary volumes of the object;
wherein:
a second collimator is interposed between the object and the detector, the second collimator defining an aperture extending between the object and the detector, along a median axis that is inclined with respect to the propagation axis, so that at least one elementary volume emits scattered radiation, through the aperture, towards various pixels of the plurality of pixels;
the method comprises determining, for each pixel, a spatial dispersion function;
each spatial dispersion function being established with respect to elementary volumes; and
each spatial dispersion function representing an intensity of radiation, reaching the pixel, the radiation being respectively scattered by the elementary volumes.

### Claim 2 (depends on 1)

The Method according to claim 1, wherein e) comprises, on the basis of the scattering spectrum acquired by each pixel, determining a scattering function associated with the pixel, the scattering function being obtained by combining the scattering spectrum with a reference spectrum acquired by the pixel while a reference material is placed in the place of the object.

### Claim 3 (depends on 2)

The Method according to claim 2, wherein determining the scattering function associated with each pixel comprises taking into account a reference scattering function, which is established, for each pixel, relatively to the reference material.

### Claim 4 (depends on 3)

The Method according to claim 3, wherein determining the scattering function associated with each pixel comprises:
establishing a ratio, term by term, of the scattering spectrum, acquired by the pixel, to the reference spectrum, and
multiplying, term by term, the ratio by the reference scattering function established for the pixel.

### Claim 5 (depends on 2)

The Method according to claim 2, wherein e) comprises taking into account an attenuation spectral function of the object and an attenuation spectral function of the reference object.

### Claim 6 (depends on 2)

The Method according to claim 2, wherein e) comprises:
establishing a response matrix with the spatial scattering functions associated with each pixel;
establishing a spatial dispersion matrix on the basis of with the spatial dispersion functions associated with each pixel; and
estimating a matrix of the scattering signatures of each elementary volume, wherein a product of the spatial dispersion matrix by the matrix of scattering signatures of each elementary volume substantially corresponds to the response matrix.

### Claim 7 (depends on 1)

The Method according to claim 1, wherein the spatial dispersion function associated with each pixel is elaborated by
placing a calibration object successively in various positions, along the propagation axis; and
carrying out, in each position:
i) irradiating the calibration object and acquiring, with said pixel, a calibration spectrum, of the radiation scattered by said calibration object placed in the position;
ii) in each calibration spectrum, identifying a calibration peak that is characteristic of the calibration object; and
iii) determining the intensity of the calibration peak;
the spatial dispersion function being obtained from the intensities of the calibration peaks respectively determined, for the pixel, in each position of the calibration object.

### Claim 8 (depends on 1)

The Method according to claim 1, wherein f) comprises, for each elementary volume, comparing the scattering signature, obtained in e), associated with the elementary volume with pre-established scattering signatures, each pre-established scattering signatures corresponding to a known material.

### Claim 9 (depends on 1)

The Method according to claim 1, wherein the pixels are virtual pixels obtained by a sub-pixelation of physical pixels of the detector.

### Claim 10 (depends on 1)

A processor-readable data storage medium comprising instructions for executing d) to f) of a method according to claim 1, on the basis of scattering spectra respectively acquired by pixels of a detector, each scattering spectrum being representative of an energy distribution of a scattered radiation, each scattering spectrum being associated with one pixel.

### Claim 11 (depends on 1)

A Device for analysing an object comprising:
an irradiation source, configured to produce ionising electromagnetic radiation propagating towards a holder of the object;
a first collimator, placed between the irradiation source and the holder, the first collimator having an aperture configured to form a collimated beam propagating along a propagation axis, towards the holder; and
a second collimator, placed between the holder and a detector, the second collimator having an aperture extending between the holder and the detector, along a median axis that is inclined with respect to the propagation axis;
the detector comprising pixels, each pixel being configured to detect electromagnetic radiation scattered by the object through the aperture, and to acquire a scattering spectrum;
wherein
the device comprises a microprocessor configured to carry out, on the basis of the scattering spectrum acquired by each pixel, steps d) to f) of the method according to claim 1.

### Claim 12 (depends on 11)

The Device according to claim 11, wherein the median axis makes a collimating angle, to the propagation axis, the collimating angle being strictly larger than 0° and smaller than 20°.

### Claim 13 (depends on 11)

The Device according to claim 11, comprising an auxiliary detector configured to acquire a transmission spectrum of radiation transmitted by the object, held on the holder, along the propagation axis.