CN108152313B - Automatic debugging and correcting system and method for light-splitting light path of X-ray fluorescence spectrometer - Google Patents
Automatic debugging and correcting system and method for light-splitting light path of X-ray fluorescence spectrometer Download PDFInfo
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Abstract
The invention relates to an automatic debugging and correcting system and method for a spectroscopic light path of a sequential wavelength dispersion X-ray fluorescence spectrometer. The system comprises an operation interface module, a crystal frame control module, a high-precision step motor control module for a theta axis and a 2 theta axis of the goniometer, a detector data acquisition module and a data image processing module; the system selects the measured element spectral line as the reference spectral line of the calibration goniometer, calculates the glancing angle of the crystal and the exit angle of the detector through a Bragg equation, rotates the theta axis and the 2 theta axis of the goniometer to a specified position, and realizes automatic adjustment of the positions of the crystal and the detector by controlling a stepping motor, a crystal frame and the detector which are arranged on the theta axis and the 2 theta axis to obtain a crystal correction factor, thereby correcting the glancing angle of the crystal and the exit angle of the detector. The invention realizes remote automatic debugging of the beam splitting optical path, protects debugging personnel from X-ray radiation, reduces the dependence on the debugging experience of the debugging personnel, and improves the debugging efficiency and precision.
Description
Technical Field
The invention belongs to the technical field of X-ray fluorescence spectrometers, and relates to an automatic debugging and correcting system and method for a spectroscopic light path of a sequential wavelength dispersion X-ray fluorescence spectrometer.
Background
The sequential wavelength dispersion X-ray fluorescence spectrometer is a precise instrument for precisely analyzing the element content, has the characteristics of short analysis time, wide element detection range, multiple analysis sample types, no damage to analysis samples and the like, and can be widely applied to the fields of petrochemical industry, building materials, metal and inorganic nonmetallic materials, ceramics, cultural relics identification, biological materials, pharmaceutical semiconductors and the like. The light splitting optical path is a core component of the wavelength dispersion fluorescence spectrometer, and plays a vital role in the performance of the instrument. The light splitting optical path comprises a primary collimator, a crystal, a secondary collimator and a detector, and is arranged in a vacuum cavity of the spectrometer.
The spectroscopic optical path is designed according to a Bragg diffraction model (shown in figure 1) of the crystal, and the crystal dispersion principle accords with Bragg law:
nλ＝2dsinθ
wherein n is a diffraction order; lambda is the fluorescent X-ray wavelength; θ is the crystal glancing angle; d is the interplanar spacing. For a specific elemental line, the diffraction order n and the fluorescent X-ray wavelength λ are fixed, and for a specified interplanar spacing d, the detector can only acquire the fluorescent intensity at the exit angle 2θ when the crystal glancing angle θ satisfies the bragg equation.
As can be seen from the bragg diffraction model, when measuring the X-ray fluorescence 8, the rotation angles of the crystal 7 and the detector 6 are θ and 2θ, respectively, and the crystal 7 and the detector 6 are mounted on the θ axis and the 2θ axis of the goniometer, respectively, and the θ axis and the 2θ axis are controlled to be always in a 2-fold relationship.
The sequential wavelength dispersion X-ray fluorescence spectrometer is different from the fixed-channel wavelength dispersion X-ray fluorescence spectrometer, when different elements are measured, a proper spectroscopic crystal is required to be selected, the crystal is switched into a spectroscopic light path through a crystal switching device, and the crystal and a detector in the spectroscopic light path are required to rotate according to the angle calculated by a Bragg equation, so that the angle meter theta axis of the crystal and the angle meter 2 theta axis of the detector are required to be calibrated. The traditional debugging method is to calibrate the theta axis and the 2 theta axis of the goniometer through a horizontal angle measuring instrument, and then to accurately calibrate the theta axis through rotating a crystal adjusting screw, and the 2 theta axis is not accurately calibrated any more. When the X-ray is started, the protective cover must be closed, otherwise, the escaping X-ray can cause injury to human body. The crystal is installed in the cavity of spectrum appearance, need close X ray when rotatory crystal adjustment screw and open the protective cover, close the protective cover after the crystal angle adjustment is accomplished, open X ray fluorescence intensity that X ray observation detector gathered and record, find the biggest position of intensity and accomplish the debugging after repeating above adjustment process repeatedly.
A sequential wavelength dispersion X-ray fluorescence spectrometer is generally matched with 5-10 unequal crystals to meet the measurement of various elements, and each crystal is debugged and needs to be continuously switched on and off for X-rays, so that a protective cover is detached, time and labor are very consumed, and loss is generated on an X-ray source. Because the X-ray intensity acquisition is discrete, the experience requirement of debugging personnel is very high when searching the maximum intensity of X-rays, the debugging can be completed by repeated operation, and the precision can not be ensured.
Disclosure of Invention
The invention aims to provide an automatic debugging and correcting system for a light-splitting light path of a sequential wavelength dispersion X-ray fluorescence spectrometer, which improves the debugging efficiency and the debugging precision of the light-splitting light path of the sequential wavelength dispersion X-ray fluorescence spectrometer, reduces the labor intensity of debugging personnel and reduces the dependence on the debugging experience of the debugging personnel.
Another object of the present invention is to provide an automatic tuning and calibration method for a spectroscopic path of a sequential wavelength dispersive X-ray fluorescence spectrometer.
In order to achieve the above object, the present invention provides the following technical solutions:
firstly, selecting a spectral line of a measured element as a reference spectral line of a calibration goniometer, and calculating a crystal glancing angle theta through a Bragg equation 0 Angle of emergence 2 theta with detector 0 And (3) rotating the theta axis and the 2 theta axis of the goniometer to a specified position obtained by calculation, and after manually adjusting the crystal, controlling a high-precision stepping motor, a crystal frame and a detector which are arranged on the theta axis and the 2 theta axis of the goniometer by upper computer software to realize high-precision automatic adjustment of the positions of the crystal and the detector, so as to obtain a group of crystal correction factors, and correcting the glancing angle theta of the crystal and the emergence angle 2 theta of the detector by the correction factors of the crystal.
An automatic debugging and correcting system for a spectroscopic light path of an X-ray fluorescence spectrometer, wherein the X-ray fluorescence spectrometer is a sequential wavelength dispersion X-ray fluorescence spectrometer, and comprises a detector 6, a goniometer, a crystal frame and a plurality of crystals for spectroscopic, and a theta axis and a 2 theta axis of the goniometer are respectively provided with a selected crystal and a detector, and the system comprises: the device comprises an operation interface module 1, a crystal frame control module 2, a goniometer theta axis and 2 theta axis high-precision stepper motor control module 3, a detector data acquisition module 4 and a data image processing module 5;
the crystal frame control module 2 switches the selected crystal into a beam splitting optical path;
the user sets the scanning range of the theta axis and the 2 theta axis of the goniometer, the scanning interval and the acquisition time of the detector through the operation interface module 1;
the theta axis and 2 theta axis high-precision stepper motor control module 3 of the angle meter adjusts the theta axis and 2 theta axis, and rotates the crystal and the detector to a specified position in sequence according to the scanning range;
the detector data acquisition module 4 acquires the X-ray intensity of the designated position, sends acquired information to the data image processing module 5 for processing, finally establishes a visual and stereoscopic three-dimensional data model, calculates a corresponding correction factor, and returns the information to the interface module 1 for display.
The operation interface module 1 comprises a user parameter setting interface, a detector data acquisition interface and a three-dimensional data display interface; the user parameter setting interface sets the scanning range and the scanning interval of the high-precision stepper motor of the theta axis and the 2 theta axis of the goniometer, and selects a debugging crystal; the detector data acquisition interface sets detector acquisition parameters and displays acquisition spectrograms and X-ray intensity values; the three-dimensional data display interface displays the final three-dimensional data model obtained by analysis.
The motor used by the crystal frame control module 2 for driving the crystal frame to move is a low-energy-consumption direct current motor which can be used under vacuum conditions; 10-20 different crystals are arranged on the crystal frame; the fine adjustment of the crystal angle is realized by adjusting the crystal adjusting screw.
The stepping motor controlled by the high-precision stepping motor control module 3 of the angle meter theta axis and 2 theta axis is a five-phase stepping motor, so that acceleration during starting, uniform speed during running and gradual deceleration movement during stopping of the theta axis and 2 theta axis can be realized; meanwhile, the theta axis and the 2 theta axis can respectively move and simultaneously link; and is provided with an anti-collision emergency treatment function.
The detector data acquisition module 4 is provided with a fluid proportional counter for measuring light elements and a scintillator counter for measuring heavy elements, and the communication mode between the detector data acquisition module and an upper computer is USB or Ethernet.
An X-ray fluorescence spectrometer beam splitting light path debugging and correcting method using the system comprises the following steps:
a. closing the X-rays of the sequential wavelength dispersion X-ray fluorescence spectrometer, opening a protective cover, installing a plurality of different crystals on a crystal frame, and switching the selected crystals into a light splitting optical path through a crystal frame control module 2;
b. the angle measuring instrument theta axis is moved to a position convenient for adjusting the angle of the crystal by the angle measuring instrument theta axis and 2 theta axis high-precision stepping motor control module 3, a horizontal angle measuring instrument is placed on the surface of the crystal to measure the horizontal angle of the crystal, the crystal angle is adjusted by rotating a crystal adjusting screw, and the horizontal angle measurement shows that the adjustment of the crystal adjusting screw is completed when the specified angle is reached;
c. closing a protective cover, opening X rays, setting acquisition parameters of a detector and scanning ranges and scanning intervals of a theta axis stepping motor and a 2 theta axis stepping motor of an angle meter through an operation interface module 1, and sending a command to start automatic correction;
d. the theta axis and 2 theta axis high-precision stepper motor control module 3 of the goniometer adjusts the theta axis and 2 theta axis, and rotates the crystal and the detector to a specified position in sequence according to the scanning range; the detector data acquisition module 4 acquires the X-ray intensity of the designated position, sends acquired information to the data image processing module 5 for processing, finally establishes a visual three-dimensional data model, and selects theta corresponding to the maximum X-ray intensity p And 2 theta p ；(θ p -θ 0 ，2θ p -2θ 0 ) Namely, the correction factors of the theta axis and the 2 theta axis of the goniometer corresponding to the crystal;
e. after automatic correction is completed on all crystals, a group of crystal correction factor list is obtained; and correcting the glancing angle theta of the crystal and the emergence angle 2 theta of the detector by inquiring correction factors of the corresponding crystal.
The precision of the horizontal angle measuring instrument is not lower than 0.1 degrees.
Compared with the prior art, the invention has the beneficial effects that:
the automatic debugging and correcting system of the beam-splitting optical path is different from the traditional debugging system (the traditional debugging system only carries out fine adjustment on the crystal), can simultaneously realize accurate fine adjustment on the crystal and the detector, and improves the acquisition intensity of the detector signals; the debugging and correcting system adopts the high-precision stepping motor to realize high-precision control on the theta axis and the 2 theta axis of the goniometer, thereby improving the debugging precision; the upper computer software of the debugging and correcting system is communicated with the system control module in an Ethernet mode, so that remote and rapid operation can be realized, a protective cover is not required to be opened, repeated opening of X rays and repeated disassembly of the protective cover are avoided, time and manpower are saved, loss of an X ray source is reduced, and debugging personnel are protected from X ray radiation; the debugging and correcting system can realize one-key operation of the whole debugging process through the operation interface, reduces the dependence on the debugging experience of a debugging person and improves the debugging efficiency.
The automatic debugging and correcting system for the beam-splitting optical path has the remarkable advantages of high reliability, high precision, high speed, high instantaneity and the like, and can be widely applied to instruments with the same requirements.
Drawings
FIG. 1 is a schematic diagram of a crystalline Bragg diffraction model;
FIG. 2 is a schematic diagram of an automatic debugging and correction system for a spectroscopic path of a sequential wavelength dispersive X-ray fluorescence spectrometer according to the present invention;
FIG. 3 is a graph showing the X-ray fluorescence intensity values corresponding to different positions of θ and 2θ of the crystal according to the embodiment of the present invention.
Wherein the reference numerals are as follows:
n number of diffraction orders
Lambda fluorescent X-ray wavelength
Glancing angle of theta crystal
d-plane spacing
1 operation interface module
2 crystal frame control module
3 angle meter theta axis and 2 theta axis high-precision stepping motor control module
4 detector data acquisition module
5 data image processing module
6 detector
7 crystal
8X-ray fluorescence
Detailed Description
The invention is further illustrated below with reference to examples.
As shown in fig. 2, an automatic debugging and correcting system for a spectroscopic optical path of an X-ray fluorescence spectrometer is a sequential wavelength dispersion X-ray fluorescence spectrometer, and comprises a detector (6), an angle meter, a crystal frame and a plurality of crystals for spectroscopic, wherein a selected crystal and a detector are respectively carried on a theta axis and a 2 theta axis of the angle meter, and the system comprises an operation interface module 1, a crystal frame control module 2, a theta axis and 2 theta axis high-precision stepper motor control module 3, a detector data acquisition module 4 and a data image processing module 5.
The crystal holder control module 2 switches the selected crystal into the spectroscopic optical path.
The user sets the scanning range of the angle meter theta axis and the 2 theta axis, the scanning interval and the acquisition time of the detector through the operation interface module 1.
The theta axis and 2 theta axis high-precision stepper motor control module 3 of the goniometer adjusts the theta axis and 2 theta axis, and rotates the crystal and the detector to specified positions in sequence according to the scanning range.
The detector data acquisition module 4 acquires the X-ray intensity at the designated position, sends acquired information to the data image processing module 5 for processing, finally establishes a visual three-dimensional data model, calculates a corresponding correction factor, and returns the information to the interface module 1 for display.
The operation interface module 1 comprises a user parameter setting interface, a detector data acquisition interface and a three-dimensional data display interface.
The user parameter setting interface can set the scanning range and the scanning interval of the high-precision stepper motor of the theta axis and the 2 theta axis of the goniometer, and select the debugging crystal;
the detector data acquisition interface sets detector acquisition parameters and displays acquisition spectrograms and X-ray intensity values;
the three-dimensional data display interface displays the final three-dimensional data model obtained by analysis.
The motor used by the crystal frame control module 2 for driving the crystal frame to move is a low-energy-consumption direct current motor which can be used under a vacuum condition, at least 10 different crystals can be installed on the crystal frame, and fine adjustment of the angles of the crystals is realized by adjusting crystal adjusting screws.
The stepping motor controlled by the high-precision stepping motor control module 3 of the angle meter theta axis and 2 theta axis is a five-phase stepping motor, so that acceleration during starting, uniform speed during running and gradual deceleration movement during stopping of the theta axis and 2 theta axis can be realized; meanwhile, the theta axis and the 2 theta axis can move respectively and are linked simultaneously, and an anti-collision emergency treatment function is provided.
The detector data acquisition module 4 can set acquisition parameters (acquisition time and acquisition range), is provided with a fluid proportional counter capable of measuring light elements and a scintillator counter capable of measuring heavy elements, and is communicated with an upper computer in a USB or Ethernet mode.
A method for debugging and correcting a spectroscopic path of a sequential wavelength dispersion X-ray fluorescence spectrometer comprises the following steps:
first, the X-rays of the sequential wavelength dispersive X-ray fluorescence spectrometer are turned off, the protective cover is opened, a plurality of different crystals are mounted on the crystal mount, and the selected crystals are switched into the spectroscopic optical path by the crystal mount control module 2.
Secondly, the angle meter theta axis is moved to a position convenient for adjusting the crystal angle through the angle meter theta axis and 2 theta axis high-precision stepping motor control module 3, the horizontal angle meter is placed on the crystal surface to measure the horizontal angle, the crystal angle is adjusted through the crystal frame control module 2 to rotate the crystal adjusting screw, and the horizontal angle measurement shows that the adjustment of the crystal adjusting screw is completed when the specified angle is reached.
Thirdly, closing the protective cover, opening the X-ray, setting acquisition parameters of the detector, the scanning range and the scanning interval of the theta axis and 2 theta axis stepping motors of the goniometer through the operation interface module 1, and sending a command to start automatic correction;
fourth, the detector sequentially collects X-ray fluorescence intensity values corresponding to different positions of theta and 2 theta to obtain a group of X-ray fluorescence intensity values, and theta corresponding to the maximum X-ray intensity value is selected from the X-ray fluorescence intensity values p And 2 theta p 。(θ p -θ 0 ，2θ p -2θ 0 ) The correction factors of the theta axis and the 2 theta axis of the goniometer corresponding to the crystal are obtained.
Fifthly, after automatic correction is completed on all the crystals, a group of correction factor lists are obtained, and the glancing angle theta of the crystals and the emergence angle 2 theta of the detector are corrected by inquiring the correction factors of the corresponding crystals.
As shown in FIG. 3, the X-ray fluorescence intensity values corresponding to different positions of theta and 2 theta are acquired by the detector, the horizontal axis represents different positions of 2 theta, each line in the graph represents different positions of theta, and the corresponding theta of the highest point (maximum X-ray intensity) in the graph is found p And 2 theta p Obtaining θ from nλ=2dsinθ 0 ，(θ p -θ 0 ，2θ p -2θ 0 ) And when the correction factors of the angle meter theta axis and the angle meter 2 theta axis corresponding to the crystal are automatically corrected, the detector acquires the X-ray fluorescence intensity values corresponding to all the crystals, a group of correction factor lists are obtained after the correction is completed, and the glancing angle theta of the crystal and the emergence angle 2 theta of the detector are corrected by inquiring the correction factors of the corresponding crystals.
Claims (7)
1. An automatic debugging and correcting system of a beam splitting light path of an X-ray fluorescence spectrometer, wherein the X-ray fluorescence spectrometer is a sequential wavelength dispersion X-ray fluorescence spectrometer, and comprises a detector (6), a goniometer, a crystal frame and a plurality of crystals for beam splitting, and a theta axis and a 2 theta axis of the goniometer are respectively provided with a selected crystal and a detector, and the automatic debugging and correcting system is characterized in that: the system comprises: the device comprises an operation interface module (1), a crystal frame control module (2), a goniometer theta axis and 2 theta axis high-precision stepper motor control module (3), a detector data acquisition module (4) and a data image processing module (5);
the crystal frame control module (2) switches the selected crystal into a light splitting light path;
the user sets the scanning range of the theta axis and the 2 theta axis of the goniometer and the scanning interval and the acquisition time of the detector through an operation interface module (1);
the theta axis and 2 theta axis high-precision stepper motor control module (3) of the angle meter adjusts the theta axis and 2 theta axis, and sequentially rotates the crystal and the detector to a designated position according to a scanning range, so that acceleration during starting, uniform speed during running and gradual deceleration during stopping of the theta axis and 2 theta axis can be realized; meanwhile, the theta axis and the 2 theta axis can respectively move and simultaneously link; and is provided with an anti-collision emergency treatment function;
the detector data acquisition module (4) acquires the X-ray intensity of the appointed position, sends acquired information to the data image processing module (5) for processing, finally establishes a visual three-dimensional data model, calculates a corresponding correction factor, and transmits the information back to the operation interface module (1) for display;
wherein, the sending the collected information to the data image processing module (5) for processing specifically comprises: establishing a visual three-dimensional data model, and selecting theta corresponding to the maximum X-ray intensity from the model p And 2 theta p ；θ p -θ 0 ，2θ p -2θ 0 Respectively correcting factors of a theta axis and a 2 theta axis of the goniometer corresponding to the crystal; obtaining a group of crystal correction factor lists based on the obtained correction factors; and correcting the glancing angle theta of the crystal and the emergence angle 2 theta of the detector by inquiring correction factors of the corresponding crystal.
2. The automated tuning and calibration system for the spectroscopic path of an X-ray fluorescence spectrometer of claim 1, wherein:
the operation interface module (1) comprises a user parameter setting interface, a detector data acquisition interface and a three-dimensional data display interface; the user parameter setting interface sets the scanning range and the scanning interval of the high-precision stepper motor of the theta axis and the 2 theta axis of the goniometer, and selects a debugging crystal; the detector data acquisition interface sets detector acquisition parameters and displays acquisition spectrograms and X-ray intensity values; the three-dimensional data display interface displays the final three-dimensional data model obtained by analysis.
3. The automated tuning and calibration system for the spectroscopic path of an X-ray fluorescence spectrometer of claim 1, wherein:
the motor used by the crystal frame control module (2) for driving the crystal frame to move is a low-energy-consumption direct current motor which can be used under vacuum conditions; 10-20 different crystals are arranged on the crystal frame; the fine adjustment of the crystal angle is realized by adjusting the crystal adjusting screw.
4. The automated tuning and calibration system for the spectroscopic path of an X-ray fluorescence spectrometer of claim 1, wherein:
the stepping motors controlled by the high-precision stepping motor control module (3) of the angle meter theta axis and 2 theta axis are five-phase stepping motors.
5. The automated tuning and calibration system for the spectroscopic path of an X-ray fluorescence spectrometer of claim 1, wherein:
the detector data acquisition module (4) is provided with a fluid proportional counter for measuring light elements and a scintillator counter for measuring heavy elements, and the communication mode between the detector data acquisition module and an upper computer is USB or Ethernet.
6. An X-ray fluorescence spectrometer spectral light path tuning and correction method using the system of claim 1, wherein: the method comprises the following steps:
a. closing the X-rays of the sequential wavelength dispersion X-ray fluorescence spectrometer, opening a protective cover, installing a plurality of different crystals on a crystal frame, and switching the selected crystals into a light splitting optical path through a crystal frame control module (2);
b. the angle measuring instrument theta axis is moved to a position convenient for adjusting the angle of the crystal by a high-precision stepping motor control module (3) of the angle measuring instrument theta axis and the 2 theta axis, a horizontal angle measuring instrument is placed on the surface of the crystal to measure the horizontal angle of the crystal, the angle of the crystal is adjusted by rotating a crystal adjusting screw, and the horizontal angle measurement shows that the adjustment of the crystal adjusting screw is completed when the specified angle is reached;
c. closing a protective cover, opening X rays, setting acquisition parameters of a detector and scanning ranges and scanning intervals of a theta axis stepping motor and a 2 theta axis stepping motor of an angle meter through an operation interface module (1), and sending a command to start automatic correction;
d. a theta axis and 2 theta axis high-precision stepper motor control module (3) of the goniometer adjusts the theta axis and the 2 theta axis, and sequentially rotates a crystal and a detector to a specified position according to a scanning range; the detector data acquisition module (4) acquires the X-ray intensity of the designated position, sends acquired information to the data image processing module (5) for processing, finally establishes a visual three-dimensional data model, and selects theta corresponding to the maximum X-ray intensity p And 2 theta p ；θ p -θ 0 ，2θ p -2θ 0 Respectively correcting factors of a theta axis and a 2 theta axis of the goniometer corresponding to the crystal;
e. obtaining a group of crystal correction factor lists based on the obtained correction factors; and correcting the glancing angle theta of the crystal and the emergence angle 2 theta of the detector by inquiring correction factors of the corresponding crystal.
7. The method for adjusting and correcting the spectroscopic path of the X-ray fluorescence spectrometer according to claim 6, wherein: the precision of the horizontal angle measuring instrument is not lower than 0.1.
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| US4577338A (en) * | 1982-11-01 | 1986-03-18 | Xertex Corporation | X-Ray fluorescence spectrometer and method of calibrating the same |
| JP2004191122A (en) * | 2002-12-10 | 2004-07-08 | Rigaku Industrial Co | Fluorescence x-ray analyzer |
| JP2007255932A (en) * | 2006-03-20 | 2007-10-04 | Fujitsu Ltd | Sample position adjusting method of x-ray device, and the x-ray device |
| CN104655663A (en) * | 2013-11-25 | 2015-05-27 | 株式会社理学 | Optical axis adjustment device for X-ray analyzer |
| CN104020184A (en) * | 2014-04-04 | 2014-09-03 | 苏州三值精密仪器有限公司 | Upward-lighting type X-ray fluorescence spectrophotometer and control method thereof |
| CN106200686A (en) * | 2015-05-04 | 2016-12-07 | 宝山钢铁股份有限公司 | X fluorescence spectrometer analyzing crystal adjusting apparatus and method is fixed for Wavelength dispersion type |
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