X-ray fluorescence spectrometer and X-ray fluorescence analyzing method

Patent metadata

Field	Value
Publication number	US-9746433-B2
Application number	US-201615391156-A
Country	US
Kind code	B2
Filing date	Dec 27, 2016
Priority date	Jul 1, 2014
Publication date	Aug 29, 2017
Grant date	Aug 29, 2017

Abstract

An X-ray fluorescence spectrometer includes: an X-ray source ( 3 ) to irradiate, with primary X-rays ( 6 ), a sample ( 1 ) that is multiple nanoparticles placed on a substrate ( 10 ); an irradiation angle adjustment unit ( 5 ) to adjust an irradiation angle at which a surface ( 10 a ) of the substrate is irradiated; a detection unit ( 8 ) to measure an intensity of fluorescent X-rays ( 7 ) from the sample ( 1 ); a peak position calculation unit ( 11 ) to generate a sample profile representing change of the intensity of the fluorescent X-rays ( 7 ) against change of the irradiation angle, and to calculate a peak irradiation angle position; a particle diameter calibration curve generation unit ( 21 ) to generate a calibration curve; and a particle diameter calculation unit ( 22 ) to calculate a particle diameter of nanoparticles of an unknown sample ( 1 ) by applying the peak irradiation angle position of the unknown sample ( 1 ) to the calibration curve.

First claim

What is claimed is:

1. An X-ray fluorescence spectrometer comprising:
an X-ray source configured to irradiate, with primary X-rays, a sample that is multiple nanoparticles placed on a substrate;
an irradiation angle adjustment unit configured to adjust an irradiation angle at which a surface of the substrate is irradiated with the primary X-rays;
a detection unit configured to measure an intensity of fluorescent X-rays generated from the sample;
a peak position calculation unit configured to measure, by using the detection unit, an intensity of the fluorescent X-rays generated from the sample each time the irradiation angle is adjusted by the irradiation angle adjustment unit, generate a sample profile representing change of the intensity of the fluorescent X-rays against change of the irradiation angle, and calculate a peak irradiation angle position at which the fluorescent X-rays indicate a highest intensity in the sample profile;
a particle diameter calibration curve generation unit configured to generate a calibration curve for a plurality of standard samples each of which includes nanoparticles having a known uniform particle diameter, and among which the uniform particle diameter is different, the calibration curve representing a correlation between the peak irradiation angle position calculated by the peak position calculation unit and the particle diameter of the nanoparticles; and
a particle diameter calculation unit configured to calculate a particle diameter of nanoparticles of an unknown sample by applying the peak irradiation angle position calculated for the unknown sample by the peak position calculation unit, to the calibration curve generated by the particle diameter calibration curve generation unit.

2. The X-ray fluorescence spectrometer as claimed in claim 1 , comprising a display unit configured to display a warning when the particle diameter of the nanoparticles of the unknown sample is outside a predetermined particle diameter range of the calibration curve.

3. The X-ray fluorescence spectrometer as claimed in claim 1 , comprising:
a half value width calculation unit configured to calculate a half value width of the sample profile generated by the peak position calculation unit; and
a display unit configured to display a warning when the half value width calculated for the unknown sample by the half value width calculation unit is greater than a predetermined upper limit half value width.

4. The X-ray fluorescence spectrometer as claimed in claim 1 , comprising:
an identification unit configured to identify an element of nanoparticles of a sample, and
an exciting line automatic selection unit configured to automatically select, as the primary X-rays, exciting line corresponding to the element identified by the identification unit.

5. An X-ray fluorescence analyzing method comprising preparing: an X-ray source configured to irradiate, with primary X-rays, a sample that is multiple nanoparticles placed on a substrate; an irradiation angle adjustment unit configured to adjust an irradiation angle at which a surface of the substrate is irradiated with the primary X-rays; a detection unit configured to measure an intensity of fluorescent X-rays generated from the sample; and a plurality of standard samples each of which includes nanoparticles having a known uniform particle diameter, and among which the uniform particle diameter is different,
irradiating each standard sample with the primary X-rays for which an irradiation angle is adjusted by using the irradiation angle adjustment unit, and measuring, by the detection unit, an intensity of fluorescent X-rays generated from the standard sample each time the irradiation angle is adjusted,
generating a sample profile representing change of the intensity of the fluorescent X-rays against change of the irradiation angle, and calculating a peak irradiation angle position at which the fluorescent X-rays indicate a highest intensity in the sample profile,
generating a particle diameter calibration curve representing a correlation between the peak irradiation angle position calculated for each standard sample, and the particle diameter of the nanoparticles,
preparing an unknown sample,
irradiating the unknown sample with the primary X-rays for which an irradiation angle is adjusted by using the irradiation angle adjustment unit, and measuring, by the detection unit, an intensity of fluorescent X-rays generated from the unknown sample each time irradiation is performed,
generating a sample profile representing change of the intensity of the fluorescent X-rays against change of the irradiation angle, and calculating a peak irradiation angle position at which the fluorescent X-rays indicate a highest intensity in the sample profile, and
calculating a particle diameter of nanoparticles of the unknown sample by applying the peak irradiation angle position calculated for the unknown sample, to the particle diameter calibration curve.

6. The X-ray fluorescence analyzing method as claimed in claim 5 , wherein
an element of nanoparticles of a sample is identified, and
exciting line corresponding to the identified element is selected as the primary X-rays.

7. The X-ray fluorescence analyzing method as claimed in claim 5 , wherein samples which include nanoparticles having particle diameters of 1 nm to 100 nm are analyzed.

Assignees

• Rigaku Denki Co Ltd

Inventors

• Yamada Takashi
• Shimizu Yuichiro

Classifications

• G01N2223/641

  particle sizing · CPC title

• G01N15/0211

  Investigating a scatter or diffraction pattern · CPC title

• G01N15/02

  Investigating particle size or size distribution (by measuring osmotic pressure G01N7/10; investigating sedimentation of particle suspensions G01N15/04; investigating individual particles G01N15/10) · CPC title

• G01N2223/076

  X-ray fluorescence · CPC title

• G01N23/223 Primary

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