KR101769709B1 - Method for aligning for spectrum module of wavelength dispersive x-ray fluorescence analyzer - Google Patents

Abstract

According to the present invention, a method of aligning a spectrum module of a wavelength dispersive X-ray fluorescence analyzer comprises: a standard specimen preparation step of fixating a standard specimen; a detector fixating step of fixating a detector; an X-ray generation step of irradiating X-ray with the standard specimen using an X-ray tube after the standard specimen preparation step and the detector fixating step are completed; a spectrum crystal angle adjustment step of detecting energy of fluorescence X-ray by the detector to correspond to a rotation angle while rotating a spectrum crystal; a spectrum crystal alignment step of fixating the spectrum crystal at an angle of the spectrum crystal by which maximum energy of the standard specimen checked in the spectrum crystal angle adjustment step is detected; a detector angle adjustment step of detecting the energy of the fluorescence X-ray by the detector to correspond to the rotation angle while rotating the detector; and a detector alignment step of fixating the detector at an angle of the detector by which maximum energy of the standard specimen checked in the detector angle adjustment step is detected.

Description

METHOD FOR ALIGNING FOR SPECTRUM MODULE OF WAVELENGTH DISPERSIVE X-RAY FLUORESCENCE ANALYZER FIELD OF THE INVENTION [0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a wavelength dispersive X-ray fluorescence analyzer, and more particularly, to a method of aligning a spectral module included in a wavelength dispersive X-ray fluorescence analyzer.

X-ray fluorescence analysis (XRF) is a method of qualitative and quantitative analysis of an element by using an X-ray (characteristic fluorescent X-ray) generated by irradiating the sample with X-rays. Because of its non-destructive and rapid measurement, fluorescent X-ray analysis is widely used for process control. In addition, it is the most simple analysis to investigate the composition of element in general material evaluation. It analyzes valuable materials such as archeology, It is also used to perform outdoor analysis with devices.

Spectrometers of fluorescent X-rays from a sample are classified into two types, one is spectroscopic spectroscopy (Wavelength Dispersive XRF; WD-XRF) using Bragg's law and the other is a spectrometer (Energy Dispersive XRF, ED-XRF) using semiconductor detectors.

The ED-XRF has the advantage of analyzing the X-rays generated from the X-ray generator to the specimen, and analyzing the X-rays at short time by simultaneously inputting the characteristic X-rays and braking radiation generated from the specimen to the detector. However, WD-XRF has the limitation of precise measurement due to interferences between the characteristic fluorescent X-rays. However, since the angle resolution of the spectral crystal is directly related to the detection resolution, the resolution can be increased up to 10 eV, So that more accurate measurement can be performed.

Korean Patent Laid-Open Publication No. 10-2015-0088833 entitled " Method for Performing X-Ray Fluorescence Analysis and X-ray Fluorescence Analysis Apparatus ", 2015.08.03.

An object of the present invention is to provide a method for efficiently aligning a spectroscopic module provided in a wavelength dispersive X-ray fluorescence analysis apparatus.

According to an aspect of the present invention,

A front collimator through which a fluorescent X-ray generated in the sample passes by an X-ray irradiated from an X-ray tube, a spectral crystal in which a specific wavelength of a fluorescent X-ray passing through the front collimator is reflected, and an incident angle and an angle of reflection of the fluorescent X- A spectroscopic crystal angle adjuster for rotating the spectroscopic crystal around a center of rotation (O) positioned at a center of the reflection surface of the spectroscopic crystal so as to change the spectroscopic crystal, a rear collimator through which the X- A method of aligning a spectroscopic module of a wavelength dispersive X-ray fluorescence analyzer having a detector for analyzing a fluorescent X-ray passing through a collimator, the method comprising: preparing a standard specimen; A detector fixing step of fixing the detector; An X-ray generating step of irradiating an X-ray to the standard sample using the X-ray tube after completing the standard specimen preparation step and the detector fixing step; A spectroscopic crystal angle adjusting step in which the spectroscopic crystal angle adjusting unit rotates the spectroscopic crystal around the rotation center and the energy of the fluorescent X-rays is detected by the detector according to the rotation angle; A spectral crystal alignment step in which the spectral crystal is fixed at an angle of the spectral crystal at which the maximum energy of the standard specimen identified in the spectral crystal angle adjustment step is detected; A detector angle adjusting step of detecting the energy of the fluorescent X-rays by the detector corresponding to the rotation angle while the detector is rotating about the rotation center using the detector angle adjusting unit; And a detector aligning step of fixing the detector to an angle of the detector at which the maximum energy of the standard specimen identified in the detector angle adjusting step is detected. Is provided.

The detector includes a scintillation detector for detecting a fluorescent X-ray in a high energy region, and a proportional counter for detecting a fluorescent X-ray in a low-energy region, wherein the scintillation detector and the proportional counter can rotate together have.

Wherein the rear collimator comprises a first rear collimator positioned between the spectroscopic crystal and the progression detector and a second rear collimator positioned between the spectroscopic crystal and the proportional counter, The first rear collimator rotates together with the scintillation detector, and the second rear collimator rotates together with the proportional counter.

According to the present invention, all of the objects of the present invention described above can be achieved. Specifically, a spectral crystal alignment step in which a spectral crystal is fixed at an angle at which a maximum energy of a standard specimen is detected in a state where the detector is fixed, and a spectral crystal alignment step in which, at an angle at which the maximum energy of the standard specimen is detected while the spectral crystal is fixed The alignment of the spectroscopic module of the wavelength dispersive X-ray fluorescence spectrometer is efficiently performed.

FIG. 1 is a schematic view showing a configuration of a wavelength dispersive X-ray fluorescence analysis apparatus in which a spectroscopic module alignment method of a wavelength dispersive X-ray fluorescence analysis apparatus according to an embodiment of the present invention is used.
FIG. 2 is a flowchart illustrating a method of aligning a spectroscopic module of a wavelength dispersive X-ray fluorescence spectrometer according to an embodiment of the present invention.

Hereinafter, the configuration and operation of an embodiment of the present invention will be described in detail with reference to the drawings.

FIG. 1 schematically shows a configuration of a wavelength dispersive X-ray fluorescence analysis apparatus in which an alignment method of a spectroscopic module according to an embodiment of the present invention is used. Prior to describing the alignment method of the spectroscopic module, a schematic configuration of the wavelength dispersive X-ray fluorescence analysis apparatus will be described with reference to FIG. 1, the wavelength dispersive X-ray fluorescence analysis apparatus 100 includes an X-ray tube 110 for generating an X-ray to irradiate a specimen S, a specimen fixing unit 120 for fixing the specimen S, And a spectroscopy module 130 for spectroscopically analyzing the characteristic fluorescent X-rays generated from the specimen S. In the wavelength dispersive X-ray fluorescence analysis apparatus 100, the entire optical path shown by the one-dot chain line is kept in vacuum tightness. To this end, although not shown, the wavelength dispersive X-ray fluorescence analysis apparatus 100 further includes a vacuum chamber.

The X-ray tube 110 generates an X-ray and irradiates the specimen S fixed to the sample fixing unit 120. The x-ray tube 110 must generate x-rays of uniform intensity for a long time for accurate x-ray fluorescence analysis. Although not shown, the wavelength dispersive X-ray fluorescence analysis apparatus 100 further includes a high voltage generator for driving the X-ray tube 110.

The specimen fixing unit 120 fixes the specimen S to be analyzed. The specimen S fixed to the specimen fixing part 120 when the alignment of the spectroscopic module 130 is performed is a standard specimen. The specimen S fixed to the specimen fixing unit 120 generates the characteristic fluorescent X-rays by the X-rays irradiated from the X-ray tube 110 and the characteristic X-rays generated in the specimen S are irradiated to the spectroscopic module 130 .

The spectroscopy module 130 spectroscopically analyzes the characteristic fluorescent X-rays generated from the specimen S. The spectroscopy module 130 includes a front collimator 140, a spectroscopic crystal 150, a spectroscopic crystal angle adjuster 160, a rear collimator 170, a detector 180, (Not shown).

The front collimator 140 is positioned between the specimen S and the spectroscopic crystal 150 fixed to the specimen holder 120 on the optical path. The front collimator 140 forms a parallel ray so that the characteristic fluorescent X-rays generated in the specimen S are irradiated only to the spectroscopic crystal 150.

The spectroscopic crystal 150 is used to detect the wavelength of the characteristic fluorescent X-rays passing through the front collimator 140. A specific wavelength of the characteristic fluorescent X-ray is reflected or filtered by the spectral crystal 150 to be selected. The spectroscopic crystal 150 is rotatable around a rotation center O positioned at the center of the reflection surface to change the incident angle and reflection angle of the characteristic fluorescent X-ray to the spectroscopic crystal 150.

The spectroscopic crystal angle adjuster 160 is mechanically connected to the spectroscopic crystal 150 to adjust the angle of the spectroscopic crystal 150 by rotating the spectroscopic crystal 150 about the center O of rotation. The spectral crystal angle adjuster 160 includes a step motor capable of adjusting the angle of the super precise angle.

The rear collimator 170 is located on the optical path between the spectroscopic crystal 150 and the detector 180. The rear collimator 170 forms a parallel light beam such that the characteristic fluorescent X-rays reflected from the spectroscopic crystal 150 are irradiated only to the detector 180. The rear collimator 170 includes a first rear collimator 171 and a second rear collimator 172 positioned adjacent to each other along the circumferential direction of the rotation center O. [

The detector 180 analyzes the characteristic fluorescent X-rays that have passed through the rear collimator 170. The detector 180 includes a scintillation detector 181 located corresponding to the first rear collimator 171 and a proportional counter 182 located corresponding to the second rear collimator 172 Respectively. The detector 180 is rotatable about the rotation center O together with the rear collimator 170.

The scintillation detector 181 is a detector for detecting a fluorescent X-ray in a high energy region, and includes a scintillator for converting the incident X-rays into visible light and a light pipe for amplifying the incident visible light. The scintillation detector 181 is integrally coupled to the first rear collimator 171 located at the front and rotates together with the rotation about the center O of rotation.

The proportional counter tube 182 is a detector for detecting a fluorescent X-ray in a low energy region. The center electrode is an anode and the cylinder wall is a cathode. The incident X-ray measures the current generated by electrons generated by ionizing the gas inside Measure energy and intensity. The gas used in the proportional gas tube is a P-10 gas composed of 90% argon and 10% methane, and 10% methane is an additional ion by ultraviolet radiation emitted from atoms excited during the course of the reaction with radiation and detection gas And it acts as a quench gas which is added in order to prevent it. The proportional counter tube 182 is integrally coupled to the second rear collimator 172 located at the front and rotates about the center O of rotation.

The detector angle adjuster 190 is mechanically coupled to the detector 180 to adjust the angle of the detector 180 by rotating the detector 190 about the center O of rotation. The detector angle adjusting unit 190 is provided with a step motor capable of adjusting the angle of the super precise angle.

In the wavelength dispersive X-ray fluorescence analysis apparatus 100 having the structure shown in FIG. 1, a fluorescent X-ray emitted from an X-ray tube 110 irradiated with a sample S is irradiated to a front collimator 140, Accurate detection of the spectroscopic module 130 is required since the reflected energy is detected to identify the element of the sample.

FIG. 2 is a flowchart illustrating a method of aligning a spectroscopic module of a wavelength dispersive X-ray fluorescence spectrometer according to an embodiment of the present invention. The alignment method of the spectroscopic module shown in FIG. 2 is used for alignment of the spectroscopic module 130 included in the wavelength dispersive X-ray fluorescence apparatus 100 having the structure as shown in FIG. 2, a method of aligning a spectroscopic module of a wavelength dispersive X-ray fluorescence spectrometer according to an embodiment of the present invention includes a standard specimen preparing step S10, a detector fixing step S20, an X-ray generating step S30 A spectral crystal angle adjustment step S40, a crystal alignment step S50, a detector angle adjustment step S60, and a detector alignment step S70.

In the standard specimen preparation step S10, a standard specimen S previously known for alignment is fixed to the specimen fixing portion 120. [ After the standard specimen preparation step S10 is completed, the detector fixing step S20 is performed.

In the detector fixing step S20, the detector is fixed at a predetermined alignment position for alignment of the spectroscopic crystal 150. [ In this embodiment, it is described that the detector fixing step S20 is performed after the standard specimen preparation step S10, but may alternatively be performed before the standard specimen preparation step S10, or the two steps may be performed simultaneously. After the detector fixing step S20 and the standard specimen preparation step S10 are all completed, the X-ray generating step S30 is performed.

In the X-ray generating step S30, an X-ray is generated by the X-ray tube 110 and irradiated to the standard specimen S. The fluorescent X-rays generated in the standard specimen S by the X-rays are passed through the front collimator 140, the spectral crystal 150 and the rear collimator 170 in order and then incident on the detector 180. After the X-ray generating step S30 is completed, the spectral crystal angle changing step S40 is performed.

The spectroscopic crystal 150 is rotated about the rotation center O by the spectroscopic crystal angle adjuster 160 so that the incident angle and the reflection angle of the fluorescent X-ray relative to the spectroscopic crystal 150 are changed in the spectroscopic crystal angle adjustment step S40 At the same time, the energy is detected in accordance with the rotation angle in the detector 180. During the spectral crystal angle change step (S40), the angle of the spectral crystal 150 at which the maximum energy of the standard specimen S is detected is confirmed. After the spectroscopic crystal angle change step S40 is completed, the spectroscopic crystal alignment step S50 is performed.

In the spectroscopic crystal alignment step S50, the spectroscopic crystal 150 is fixed at an angle of the spectroscopic crystal 150 at which the maximum energy of the standard sample S detected in the spectroscopic crystal angle adjustment step S40 is detected. After the spectroscopic crystal alignment step (S50) is completed, the detector angle adjustment step (S60) is performed.

In the detector angle adjusting step S60, the detector 180 rotates about the rotation center O by the detector angle adjusting unit 190, and at the same time, the energy is detected by the detector 180 in accordance with the rotation angle. In the course of performing the detector angle adjustment step (S60), the angle of the detector 180 at which the maximum energy of the standard specimen S is detected is confirmed. After the detector angle adjustment step (S60) is completed, the detector alignment step (S70) is performed.

In the detector alignment step S70, the detector 180 is fixed to the angle of the detector 180 at which the maximum energy of the standard specimen S detected in the detector angle adjustment step S60 is detected, All sorting is completed.

Although the present invention has been described with reference to the above embodiments, the present invention is not limited thereto. It will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined by the appended claims.

100: wavelength dispersive X-ray fluorescence analyzer
110: X-ray tube
120:
130: Spectral module
140: front collimator
150: Spectral Crystal
160: Spectroscopic crystal angle adjusting section
170: rear collimator
180:
190: Detection part angle adjusting part

Claims (3)

A front collimator through which a fluorescent X-ray generated in the sample passes by an X-ray irradiated from an X-ray tube, a spectral crystal in which a specific wavelength of a fluorescent X-ray passing through the front collimator is reflected, and an incident angle and an angle of reflection of the fluorescent X- A spectroscopic crystal angle adjuster for rotating the spectroscopic crystal around a center of rotation (O) positioned at a central portion of the reflection surface of the spectroscopic crystal so as to change the spectroscopic crystal, A scintillation detector for detecting a fluorescent X-ray in a high energy region by analyzing a fluorescent X-ray that has passed through the first rear collimator, and a second rear collimator By analyzing the fluorescent X-rays, A proportional counter and a method of aligning the spectral module of wavelength-dispersive X-ray fluorescence analysis device having call and the scintillation detector the proportional counter control detector angle to rotate about the center of rotation for detecting fluorescent X-rays in the energy region,
A standard specimen preparation step to fix a standard specimen;
A detector fixing step of fixing the scintillation detector and the proportional counter tube;
An X-ray generating step of irradiating the X-ray to the standard specimen using the X-ray tube after completion of the standard specimen preparation step and the detector fixing step;
A spectral crystal angle adjusting step of detecting the energy of the fluorescent X-rays by the scintillation detector and the proportional counter according to the rotation angle while the spectral crystal is rotated about the rotation center by the spectral crystal angle adjusting unit;
A spectral crystal alignment step in which the spectral crystal is fixed at an angle of the spectral crystal at which the maximum energy of the standard specimen identified in the spectral crystal angle adjustment step is detected;
A detector angle adjusting step of detecting the energy of the fluorescent X-rays by the scintillation detector and the proportional counter according to the rotation angle while the scintillation detector and the proportional counter are rotated together with the rotation center using the detector angle adjusting unit; And
And a detector aligning step in which the scintillation detector and the proportional counter are fixed at an angle of the scintillation detector and the proportional counter to which the maximum energy of the standard specimen detected in the detector angle adjustment step is detected,
Wherein the first rear collimator rotates together with the scintillation detector and the second rear collimator rotates together with the proportional counter tube in the detector angle adjustment step. Way. delete delete

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