X-ray analyzing apparatus and method

Patent metadata

Field	Value
Publication number	US-9146204-B2
Application number	US-201214350866-A
Country	US
Kind code	B2
Filing date	Aug 6, 2012
Priority date	Nov 14, 2011
Publication date	Sep 29, 2015
Grant date	Sep 29, 2015

Abstract

An X-ray analyzing apparatus is such that a diffraction pattern, in which the intensity of secondary X-rays ( 4 ) is associated with the angle of rotation of a sample (S), is stored; while the pattern is scanned by a line of the secondary X-rays ( 4 ) intensity in a direction of highness and lowness, points on the pattern having not higher intensity than the line are taken as candidate points; respective angles of rotation of the candidate points, when the maximum value of the difference in angle of rotation between the neighboring candidate points attains a predetermined angle, are stored; depending on coordinates of a point of measurement, the angle of rotation proximate to the coordinates is read out from the stored angles; and the sample (S) is set to the read out angle and the point of measurement is arranged within the field of view (V) of a detector ( 7 ).

First claim

What is claimed is:

1. An X-ray analyzing apparatus which comprises:
a sample table to support a disc-shaped sample of a kind having a crystalline structure, which has been placed on such sample table;
an X-ray source to radiate monochromated primary X-rays towards the sample;
a detector to detect secondary X-rays emitted from the sample;
a parallel shifting unit to move in parallel the sample table to enable an arbitrary point of measurement of a measuring surface of the sample to be arranged within a field of view of the detector;
a rotating unit to rotate the sample table about an axis perpendicular to the measuring surface of the sample; and
a control unit to control the X-ray source, the parallel shifting unit and the rotating unit;
in which with respect to a certain arbitrary point of measurement lying in the neighborhood of an edge of the sample, measurement is carried out by positioning the certain arbitrary point of measurement so that the monochromated primary X-rays are radiated from a region above the sample and reflected towards outside of the region;
in which the control unit stores a predetermined angle of a value which is equal to or smaller than an angle 2θ1 determined by the following equation (1) on the basis of the radius R of the sample and the radius T of the field of view of the detector in the measuring surface of the sample, but not smaller than 4°;
sin θ1=( R−T )/ R   (1)

in which by the control unit, the monochromated primary X-rays are radiated from the X-ray source while the sample is rotated 360° by the rotating unit about a predetermined point of the sample, and a diffraction pattern, in which the intensity of the secondary X-rays of a wavelength of the monochromated primary X-rays detected by the detector is associated with the angle of rotation of the sample, is acquired and stored;
in which by the control unit, while the diffraction pattern is scanned by a linear line representative of the intensity of the secondary X-rays in a direction of highness and lowness of the intensity, points on the diffraction pattern having the intensity not higher than the intensity represented by the linear line are taken as candidate points, and respective angles of rotation of the candidate points, when the maximum value of the difference in angle of rotation among the neighboring candidate points becomes to be the predetermined angle, are stored; and
in which depending on coordinates of the point of measurement of the sample, the angle of rotation most proximate to coordinates of the point of measurement is read out from the stored respective angles of rotation of the candidate points, the rotating unit and the parallel shifting unit are controlled so that the sample is set at the angle of rotation so read out and the point of measurement of the sample is arranged within the field of view of the detector.

2. An X-ray analyzing apparatus which comprises:
a sample table to support a disc-shaped sample of a kind having a crystalline structure, which has been placed on such sample table;
an X-ray source to radiate monochromated primary X-rays towards the sample;
a detector to detect secondary X-rays emitted from the sample;
a parallel shifting unit to move in parallel the sample table to enable an arbitrary point of measurement of a measuring surface of the sample to be arranged within a field of view of the detector;
a rotating unit to rotate the sample table about an axis perpendicular to the measuring surface of the sample; and
a control unit to control the X-ray source, the parallel shifting unit and the rotating unit;
in which with respect to a certain arbitrary point of measurement lying in the neighborhood of an edge of the sample, measurement is carried out by positioning the certain arbitrary point of measurement so that the monochromated primary X-rays are radiated from a region above the sample and reflected towards outside of the region;
in which the control unit stores a predetermined angle of a value which is equal to or smaller than an angle 2θ1 determined by the following equation (1) on the basis of the radius R of the sample and the radius T of the field of view of the detector in the measuring surface of the sample, but not smaller than 4°;
sin θ1=( R−T )/ R   (1)

in which by the control unit, the monochromated primary X-rays are radiated from the X-ray source while the sample is rotated 360° by the rotating unit about a predetermined point of the sample, and a diffraction pattern, in which an intensity ratio, which is the intensity of the secondary X-rays of a wavelength of the monochromated primary X-rays detected by the detector, divided by the intensity of fluorescent X-rays from a principal component of the sample detected by the detector, is associated with the angle of rotation of the sample, is acquired and stored;
in which by the control unit, while the diffraction pattern is scanned by a linear line representative of the intensity ratio of the secondary X-rays in a direction of highness and lowness of the intensity ratio, points on the diffraction pattern having the intensity ratio not higher than the intensity ratio represented by the linear line are taken as candidate points, and respective angles of rotation of the candidate points, when the maximum value of the difference in angle of rotation among the neighboring candidate points becomes to be the predetermined angle, are stored; and
in which depending on coordinates of the point of measurement of the sample, the angle of rotation most proximate to coordinates of the point of measurement is read out from the stored respective angles of rotation of the candidate points, the rotating unit and the parallel shifting unit are controlled so that the sample is set at the angle of rotation so read out and the point of measurement of the sample is arranged within the field of view of the detector.

3. An X-ray analyzing method using an X-ray analyzing apparatus which comprises:
a sample table to support a disc-shaped sample of a kind having a crystalline structure, which has been placed on such sample table;
an X-ray source to radiate monochromated primary X-rays towards the sample;
a detector to detect secondary X-rays emitted from the sample;
a parallel shifting unit to move in parallel the sample table to enable an arbitrary point of measurement of a measuring surface of the sample to be arranged within a field of view of the detector; and
a rotating unit to rotate the sample table about an axis perpendicular to the measuring surface of the sample;
in which with respect to a certain arbitrary point of measurement lying in the neighborhood of an edge of the sample, measurement is carried out by positioning the certain arbitrary point of measurement so that the monochromated primary X-rays are radiated from a region above the sample and reflected towards outside of the region;
in which a predetermined angle of a value which is equal to or smaller than an angle 2θ1 determined by the following equation (1) on the basis of the radius R of the sample and the radius T of the field of view of the detector in the measuring surface of the sample, but not smaller than 4°, is stored;
sin θ1=( R−T )/ R   (1)

in which the monochromated primary X-rays are radiated from the X-ray source while the sample is rotated 360° by the rotating unit about a predetermined point of the sample, and a diffraction pattern, in which the intensity of the secondary X-rays of a wavelength of the monochromated primary X-rays detected by the detector is associated with the angle of rotation of the sample, is acquired and stored;
in which while the diffraction pattern is scanned by a linear line representative of the intensity of the secondary X-rays in a direction of highness and lowness of the intensity, points on the diffraction pattern having the intensity not

Assignees

• Fukuda Tomoyuki
• Shimizu Kosuke
• Ikeshita Akihiro
• Rigaku Denki Co Ltd

Inventors

• Fukuda Tomoyuki
• Shimizu Kosuke
• Ikeshita Akihiro

Classifications

• G21K1/06

  using diffraction, refraction or reflection, e.g. monochromators (G21K1/10, G21K7/00 take precedence) · CPC title

• G01N23/20

  by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials · 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

• G01N23/2204

  Specimen supports therefor; Sample conveying means therefore · CPC title

• G01N23/20016

  Goniometers · CPC title