X-ray analysis device and peak search method

Patent metadata

Field	Value
Publication number	US-11435303-B2
Application number	US-202117170123-A
Country	US
Kind code	B2
Filing date	Feb 8, 2021
Priority date	May 12, 2020
Publication date	Sep 6, 2022
Grant date	Sep 6, 2022

Abstract

The present invention provides an X-ray analysis device and a peak search method capable of realizing highly accurate peak searches without significantly increasing a processing time. Peak search processing includes: a step (S220) for acquiring a profile of a spectrum; a step (S240) for narrowing down a wavelength range where a true value of a peak wavelength (peak intensity) may be present, taking into account statistical fluctuation of a measured value; a step (S250) for measuring the intensity of the X-rays at the long wavelength end, the short wavelength end, and the intermediate wavelength in the narrowed wavelength range; a step (S255) for calculating a quadratic function passing through the respective measured values in the above-described three wavelengths; and a step (S260) for calculating the wavelength of the vertex of the calculated quadratic function as the peak wavelength.

First claim

The invention claimed is:

1. An X-ray analysis device comprising:
a wavelength dispersive spectrometer; and
a processing unit configured to perform peak search processing for detecting a peak wavelength of a spectrum of characteristic X-rays to be diffracted using a spectrometer,
wherein the peak search processing includes
first processing for acquiring a profile of the spectrum by measuring the characteristic X-rays by a time shorter than a counting time when measuring peak intensity of the characteristic X-rays, while actuating the spectrometer so that a wavelength of the characteristic X-rays changes at predetermined intervals,
second processing for calculating a minimum value of a value that a true value of the peak intensity can take, from an intensity value of data indicating maximum intensity in the acquired profile and a statistical fluctuation of a measured value,
third processing for calculating a minimum measured value that a measured value of the peak intensity can take by the statistical fluctuation of the measured value when the true value of the peak intensity is the minimum value,
fourth processing for measuring the intensity of the characteristic X-rays for the counting time which is same as for measuring peak intensity, at the long and short end of the wavelength range in which the measured value in the acquired profile is larger than the minimum measured value, and at an intermediate wavelength between the long and short ends,
fifth processing for calculating a quadratic function passing through each measured value of the long wavelength end, the short wavelength end, and the intermediate wavelength, and
sixth processing for calculating a wavelength of a vertex of the calculated quadratic function as the peak wavelength.

2. The X-ray analysis device as recited in claim 1 ,
wherein the intermediate wavelength is a median value in the wavelength range.

3. The X-ray analysis device as recited in claim 1 ,
wherein the processing unit calculates the intensity of the vertex of the quadratic function as the peak intensity.

4. The X-ray analysis device as recited in claim 1 ,
wherein the processing unit measures the peak intensity for the counting time at the peak wavelength.

5. The X-ray analysis device as recited in claim 1 ,
wherein the processing unit executes the first to third processing at an initial measurement point when a quantitative analysis is performed at a plurality of measurement points on a sample,
wherein the fourth processing includes
processing for continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the long wavelength end,
processing for continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the short wavelength end, and
processing for continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the intermediate wavelength,
wherein the fifth processing includes processing for calculating a quadratic function passing through each measured value of the long wavelength end, the short wavelength end, and the intermediate wavelength for each of the plurality of measurement points, and
wherein the sixth processing includes processing of calculating a wavelength of a vertex of the calculated quadratic function as the peak wavelength for each of the plurality of measurement points.

6. A peak search method for detecting a peak wavelength of a spectrum of characteristic X-rays to be dispersed using a wavelength dispersive spectrometer, the peak search method comprising:
a first step of acquiring a profile of the spectrum by measuring the characteristic X-rays by a time shorter than a counting time when measuring peak intensity of the characteristic X-rays, while actuating the spectrometer so that a wavelength of the characteristic X-rays changes at predetermined intervals:
a second step of calculating a minimum value of a value that a true value of the peak intensity can take, from an intensity value of data indicating maximum intensity in the acquired profile and a statistical fluctuation of a measured value;
a third step of calculating a minimum measured value that a measured value of the peak intensity can take by the statistical fluctuation of the measured value when the true value of the peak intensity is the minimum value;
a fourth step of measuring the intensity of the characteristic X-rays for the counting time which is same as for measuring peak intensity, at the long and short end of the wavelength range in which the measured value in the acquired profile is larger than the minimum measured value, and at an intermediate wavelength between the long and short ends;
a fifth step of calculating a quadratic function passing through each measured value of the long wavelength end, the short wavelength end, and the intermediate wavelength; and
a sixth step of calculating a wavelength of a vertex of the calculated quadratic function as the peak wavelength.

7. The peak search method as recited in claim 6 ,
wherein the intermediate wavelength is a median value in the wavelength range.

8. The peak search method as recited in claim 6 ,
wherein the sixth step includes a step of calculating the intensity of the vertex of the quadratic function as the peak intensity.

9. The peak search method as recited in claim 6 ,
wherein the sixth step includes a step of measuring the peak intensity for the counting time in the peak wavelength.

10. The peak search method as recited in claim 6 ,
wherein in a case where a quantitative analysis is performed at a plurality of measurement points on the sample,
the fourth step includes
a step of continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the long wavelength end,
a step of continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the short wavelength end, and
a step of continuously measuring the intensity of the characteristic X-rays for the counting time sequentially at the plurality of measurement points at the intermediate wavelength,
wherein the fifth step includes a step of calculating the quadratic function passing through each measured value of the long wavelength end, the short wavelength end, and intermediate wavelength for each of the plurality of measurement points, and
wherein the sixth step includes a step of calculating a wavelength of the vertex of the calculated quadratic function as the peak wavelength for each of the plurality of measurement points.

Assignees

• Shimadzu Corp

Inventors

• Sakamae Hiroshi

Classifications

• G01N23/20091

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

• G01N23/2252 Primary

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

• G01N23/2209 Primary

  using wavelength dispersive spectroscopy [WDS] · CPC title

• G01N23/223

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