CN108152313A - The light splitting optical path of Xray fluorescence spectrometer is debugged and correction system and method automatically - Google Patents
The light splitting optical path of Xray fluorescence spectrometer is debugged and correction system and method automatically Download PDFInfo
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- CN108152313A CN108152313A CN201711447124.4A CN201711447124A CN108152313A CN 108152313 A CN108152313 A CN 108152313A CN 201711447124 A CN201711447124 A CN 201711447124A CN 108152313 A CN108152313 A CN 108152313A
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Abstract
It is debugged automatically the present invention relates to a kind of light splitting optical path for sequential wavelength dispersion X-ray fluorescence spectrometer and correction system and method.System includes Operating Interface Module, crystal frame control module, angular instrument θ axis and 2 θ axis high-precision step motor controls modules, detector data acquisition module, data and image processing module；Systematic selection is tested benchmark spectral line of the element spectral line as calibration angular instrument, crystal glancing angle and the detector angle of emergence are calculated by Bragg equation, the θ axis of angular instrument and 2 θ axis are rotated into designated position, adjust automatically of stepper motor, crystal frame, the detector realization to crystal and detector position of θ axis and 2 θ axis is mounted on by control, the crystal correction factor is obtained, so as to be corrected to crystal glancing angle and the detector angle of emergence.The present invention, which realizes, debugs the remote auto of light splitting optical path, and protective debugging personnel reduce the dependence to commissioning staff's commissioning experience, improve debugging efficiency and precision from X-ray radiation.
Description
Technical field
The invention belongs to Xray fluorescence spectrometer technical fields, are related to a kind of for sequential Wavelength Dispersive-X-Ray fluorescence
The light splitting optical path of spectrometer is debugged and correction system and method automatically.
Background technology
Sequential wavelength dispersion X-ray fluorescence spectrometer is a kind of precision instrument that Accurate Analysis is carried out to constituent content,
Short with analysis time, Element detection range is wide, and analysis sample type is more, the features such as not failure analysis sample, extensively using with
The necks such as petrochemical industry, construction material, metal and inorganic non-metallic material, ceramics, verification retrieval, biomaterial, drug semiconductor
Domain.Light splitting optical path is the core component of wavelength dispersion Fluorescence Spectrometer, and the performance quality of instrument is played a crucial role.
Light splitting optical path includes level-one collimator, crystal, secondary collimator and detector, former in the vacuum cavity of spectrometer
Reason is that the excitation of X-rays that light pipe generates is analyzed sample generation x-ray fluorescence, and x-ray fluorescence becomes flat by level-one collimator
Row light, in fixed angular illumination to crystal, incident x-ray fluorescence is become after crystal is divided by secondary collimator
Enter detector for directional light, detector acquisition x-ray fluorescence intensity is analyzed by processing, final to obtain element in sample
Type and content.
Light splitting optical path is designed according to the Bragg diffraction model (as shown in Figure 1) of crystal, crystalline dispersion principle
Meet Bragg's equation：
N λ=2dsin θ
In formula, n is diffraction progression；λ is fluorescent X-ray wavelength；θ is crystal glancing angle；D is interplanar distance.For specific
Element spectral line, diffraction progression n and fluorescent X-ray wavelength X be it is changeless, for specified interplanar distance d be it is fixed not
Become, when crystal glancing angle θ meets Bragg equation, detector can just collect fluorescence intensity at 2 θ of the angle of emergence.
From Bragg diffraction model as can be seen that when measuring x-ray fluorescence 8, the angle of rotation of crystal 7 and detector 6
Degree is respectively θ and 2 θ, and crystal 7 and detector 6 are separately mounted on the θ axis and 2 θ axis of angular instrument, and θ axis and 2 θ axis is controlled to make its beginning
It is 2 times of relationships eventually.
Sequential wavelength dispersion X-ray fluorescence spectrometer is different from fixed road wavelength dispersion X-ray fluorescence spectrometer, works as survey
It when measuring different elements, needs to select suitable analyzing crystal, and passes through crystal switching device and crystal is switched to light splitting optical path
In, crystal and detector needs in light splitting optical path are rotated according to the angle that Bragg equation is calculated, so needing
The angular instrument θ axis for carrying crystal is demarcated with carrying the 2 θ axis of angular instrument of detector.Traditional adjustment method is to pass through water
Flat angel measuring instrument demarcates angular instrument θ axis and 2 θ axis, then adjusts accurate mark of the screw realization to θ axis by rotating crystal
Fixed, 2 θ axis then no longer carry out Accurate Calibration.Protective cover is must shut off when opening X ray, the X ray otherwise escaped can make human body
Into injury.Crystal is mounted in the cavity of spectrometer, and rotating crystal needs to close X ray opening protective cover when adjusting screw, brilliant
Body angle closes protective cover after adjusting, open the x-ray fluorescence intensity and record of X ray observation detector acquisition, repeatedly
The completion debugging of maximum intensity position is found after repeating more than adjustment process.
The crystal that the 5-10 blocks that can generally arrange in pairs or groups on one sequential wavelength dispersion X-ray fluorescence spectrometer do not wait is each to meet
The measurement of kind element, often debugging one piece of crystal needs continuous switch X ray, and dismounting protective cover very expends time and people
Power generates loss to x-ray source.Since X-ray intensity acquisition is discrete, when finding X ray maximum intensity to debugging people
The skill requirement of member is very high, needs operation repeatedly that could complete to debug, precision can not ensure.
Invention content
The object of the present invention is to provide a kind of light splitting optical path for sequential wavelength dispersion X-ray fluorescence spectrometer is automatic
Debugging and correction system, improve the debugging efficiency and adjustment accuracy of sequential wavelength dispersion X-ray fluorescence spectrometer light splitting optical path,
Mitigate the labor intensity of commissioning staff, reduce the dependence of the commissioning experience to mode personnel.
It is a further object to provide a kind of light splitting light for sequential wavelength dispersion X-ray fluorescence spectrometer
Road debugging and bearing calibration automatically.
To achieve these goals, the present invention provides following technical solutions：
Benchmark spectral line of the spectral line of tested element as calibration angular instrument is selected first, and crystalline substance is calculated by Bragg equation
Body glancing angle θ0With 2 θ of the detector angle of emergence0, the θ axis of angular instrument and 2 θ axis are rotated to the designated position being calculated, to crystal
After being manually adjusted, upper computer software is by control mounted on angular instrument θ axis and high-precision stepper motor, the crystal of 2 θ axis
Frame, detector realize the High Precision Automatic adjustment to crystal and detector position, obtain one group of crystal correction factor, pass through crystal
Correction factor crystal glancing angle θ and 2 θ of the detector angle of emergence are corrected.
Automatically debugging is a kind of light splitting optical path of Xray fluorescence spectrometer with correction system, the Xray fluorescence spectrometer
Sequential wavelength dispersion X-ray fluorescence spectrometer, including detector 6, angular instrument, crystal frame and multiple light splitting crystal, angle measurement
The θ axis of instrument and 2 θ axis carry selected crystal and detector respectively, which includes：Operating Interface Module 1, crystal frame control mould
Block 2, angular instrument θ axis and 2 θ axis high-precision step motor controls modules 3, detector data acquisition module 4 and data image processing
Module 5；
Selected crystal is switched in light splitting optical path by the crystal frame control module 2；
Scanning range and sweep spacing and detection of the user by the setting angular instrument θ axis of Operating Interface Module 1 and 2 θ axis
Device acquisition time；
The angular instrument θ axis and 2 θ axis high-precision step motor controls modules 3 adjust the θ axis and 2 θ axis, according to scanning
Crystal and detector are rotated to designated position by range successively；
The detector data acquisition module 4 is acquired the X-ray intensity of the designated position, and acquisition information is sent
Enter the data image processing module 5 to be handled, it is final to establish intuitive three-dimensional three-dimensional data model, calculate corresponding school
Positive divisor, and information back is shown to interface module 1 is made.
The Operating Interface Module 1 includes customer parameter setting interface, detector data acquisition interface and three-dimensional data and shows
Show interface；Customer parameter setting interface sets the scanning range and sweep span of angular instrument θ axis and 2 θ axis high-precision stepper motors,
Selected debugging crystal；Detector data acquisition interface sets detector acquisition parameter, display acquisition spectrogram and X-ray intensity value；
The final three-dimensional data model that the display analysis of three-dimensional data display interface obtains.
The motor that the crystal frame control module 2 drives crystal frame movement used is available for the low energy consumption under vacuum condition
Direct current generator；10~20 pieces of different crystal are installed on crystal frame；Screw realization crystal angle fine tuning is adjusted by adjusting crystal.
The angular instrument θ axis is five phase steppings with the stepper motor that 2 θ axis high-precision step motor controls modules 3 are controlled
Motor, can realize accelerate when θ axis and 2 θ axis start, in operation at the uniform velocity with gradual retarded motion when stopping；Meanwhile, it is capable to it realizes
θ axis is moved respectively with 2 θ axis with linking simultaneously；And equipped with anticollision emergency handling function.
The detector data acquisition module 4 is equipped with the fluid-type proportional counter for measuring light element and measures heavy element
Scintillator count device is USB or Ethernet with host computer communication mode.
A kind of debugging of Xray fluorescence spectrometer light splitting optical path and bearing calibration using the system includes the following steps：
A, the X ray of closing sequence formula wavelength dispersion X-ray fluorescence spectrometer opens protective cover, by multiple and different crystalline substances
Body is installed on crystal frame, and passes through crystal frame control module 2 and selected crystal is switched in light splitting optical path；
B, angular instrument θ axis is moved to 2 θ axis high-precision step motor controls modules 3 by angular instrument θ axis and be conveniently adjusted
The position of crystal angle, level angle measurer are placed on plane of crystal and measure its level angle, and spiral shell is adjusted by rotating crystal
Silk is adjusted crystal angle, and level angle measurement is shown to specified angle and completes to adjust crystal the adjustment of screw；
C, protective cover is closed, opens X ray, detector acquisition parameter and angular instrument θ are set by Operating Interface Module 1
The scanning range and sweep span of axis and 2 θ shaft step motors, and send order and start to automatically correct；
D, angular instrument θ axis and 2 θ axis high-precision step motor controls modules 3 adjust the θ axis and 2 θ axis, according to scanning model
It encloses and crystal and detector is rotated into designated position successively；Detector data acquisition module 4 is to the X-ray intensity of the designated position
It is acquired, and acquisition information is sent into the data image processing module 5 and is handled, it is final to establish intuitive three-dimensional three-dimensional
Data model therefrom chooses the corresponding θ of X-ray intensity maximum valuepWith 2 θp；(θp-θ0, 2 θp-2θ0) it is the corresponding survey of the crystal
Angle instrument θ axis and 2 θ axis correction factors；
E, after being automatically corrected to the completion of all crystal, one group of crystal correction is obtained because of sublist；Pass through the corresponding crystal of inquiry
Correction factor crystal glancing angle θ and 2 θ of the detector angle of emergence are corrected.
The precision of the level angle measurer is not less than 0.1 °.
Compared with prior art, the beneficial effects of the present invention are：
The automatic debugging of the light splitting optical path of the present invention and correction system are different from traditional debugging system, and (traditional debugging system is only
Crystal is finely adjusted), the precise fine-adjustment to crystal and detector can be achieved at the same time, the acquisition for improving detector signal is strong
Degree；The debugging, using high-precision control of the high-precision stepper motor realization to angular instrument θ axis and 2 θ axis, is improved with correction system
Adjustment accuracy；The debugging is communicated with correcting the upper computer software of system with system control module by ether net mode, can
It realizes long-range fast operating, without opening protective cover, avoids the repetition unlatching of X ray and the repeated removal of protective cover, save
Time and manpower, reduce the loss of x-ray source, while protective debugging personnel are from X-ray radiation；The debugging and correction system
System can realize a key operation of full debugging flow by operation interface, reduce the dependence to commissioning staff's commissioning experience, improve
Debugging efficiency.
The light splitting optical path of the present invention is debugged automatically with correction system with reliability is high, precision is high, speed is fast, real-time is high
Remarkable advantages are waited, can be widely applied in the instrument of similary demand.
Description of the drawings
Fig. 1 is crystal Bragg diffraction model schematic；
For the present invention, for sequential wavelength dispersion X-ray fluorescence spectrometer light splitting optical path, debugging is Fig. 2 with correction automatically
System schematic diagram；
Fig. 3 is the corresponding θ of crystal of embodiment of the present invention x-ray fluorescence intensity value curve graphs corresponding with 2 θ different locations.
Reference numeral therein is：
N diffraction progressions
λ fluorescent X-ray wavelength
θ crystal glancing angles
D interplanar distances
1 Operating Interface Module
2 crystal frame control modules
3 angular instrument θ axis and 2 θ axis high-precision step motor control modules
4 detector data acquisition modules
5 data image processing modules
6 detectors
7 crystal
8X ray fluorescences
Specific embodiment
The present invention is further described with reference to embodiment.
As shown in Fig. 2, a kind of Xray fluorescence spectrometer light splitting optical path is debugged and correction system, the x-ray fluorescence automatically
Spectrometer is sequential wavelength dispersion X-ray fluorescence spectrometer, is used including detector (6), angular instrument, crystal frame and multiple light splitting
Crystal, the θ axis of angular instrument and 2 θ axis carry selected crystal and detector respectively, and the system comprises Operating Interface Module 1, crystalline substances
Body frame control module 2, angular instrument θ axis and 2 θ axis high-precision step motor controls modules 3,4 sum number of detector data acquisition module
According to image processing module 5.
Selected crystal is switched in light splitting optical path by crystal frame control module 2.
Scanning range and sweep spacing and detection of the user by the setting angular instrument θ axis of Operating Interface Module 1 and 2 θ axis
Device acquisition time.
Angular instrument θ axis and 2 θ axis high-precision step motor controls modules 3 adjust the θ axis and 2 θ axis, according to scanning range
Crystal and detector are rotated into designated position successively.
Detector data acquisition module 4 is acquired the X-ray intensity of the designated position, and acquisition information is sent into number
It is handled according to image processing module 5, it is final to establish intuitive three-dimensional three-dimensional data model, corresponding correction factor is calculated,
And information back is shown to interface module 1 is made.
The Operating Interface Module 1 includes customer parameter setting interface, detector data acquisition interface and three-dimensional data and shows
Show interface.
Customer parameter setting interface can set scanning range and the scanning of angular instrument θ axis and 2 θ axis high-precision stepper motors
Spacing selectes debugging crystal；
Detector data acquisition interface sets detector acquisition parameter, display acquisition spectrogram and X-ray intensity value；
The final three-dimensional data model that the display analysis of three-dimensional data display interface obtains.
The motor that the crystal frame control module 2 drives crystal frame movement used is available for the low energy consumption under vacuum condition
Direct current generator, crystal frame can mount to few 10 pieces of different crystal, and screw realization crystal angle fine tuning is adjusted by adjusting crystal.
The angular instrument θ axis is five phase steppings with the stepper motor that 2 θ axis high-precision step motor controls modules 3 are controlled
Motor, can realize accelerate when θ axis and 2 θ axis start, in operation at the uniform velocity with gradual retarded motion when stopping；Meanwhile it can realize
θ axis is moved respectively with 2 θ axis with linking simultaneously, and equipped with anticollision emergency handling function.
The detector data acquisition module 4 can set acquisition parameter (acquisition time, acquisition range), light equipped with can measure
The fluid-type proportional counter of element and the scintillator count device for measuring heavy element, are USB or ether with host computer communication mode
Net.
One kind is debugged for sequential wavelength dispersion X-ray fluorescence spectrometer light splitting optical path and bearing calibration, step are：
First, the X ray of closing sequence formula wavelength dispersion X-ray fluorescence spectrometer opens protective cover, will be multiple and different
Crystal is installed on crystal frame, and passes through crystal frame control module 2 and selected crystal is switched in light splitting optical path.
Second, angular instrument θ axis is moved to 2 θ axis high-precision step motor controls modules 3 by angular instrument θ axis and is convenient for
The position of crystal angle is adjusted, level angle measurer is placed on plane of crystal and measures its level angle, controlled by crystal frame
2 rotating crystal of module adjustment screw is adjusted crystal angle, and level angle measurement is shown to specified angle and completes to crystal
Adjust the adjustment of screw.
Third closes protective cover, opens X ray, and detector acquisition parameter, angular instrument θ are set by Operating Interface Module 1
The scanning range and sweep span of axis and 2 θ shaft step motors, and send order and start to automatically correct；
4th, detector acquires θ x-ray fluorescence intensity values corresponding with 2 θ different locations successively, and it is glimmering to obtain one group of X ray
Light intensity value therefrom chooses the corresponding θ of X-ray intensity maximum valuepWith 2 θp。(θp-θ0, 2 θp-2θ0) it is the corresponding survey of the crystal
Angle instrument θ axis and 2 θ axis correction factors.
5th, after being automatically corrected to the completion of all crystal, one group of correction factor list is obtained, passes through the corresponding crystal of inquiry
Correction factor is corrected crystal glancing angle θ and 2 θ of the detector angle of emergence.
As shown in figure 3, the collected one of corresponding θ of crystal of detector X ray corresponding with 2 θ different locations is glimmering
Light intensity value, horizontal axis represent the different location of 2 θ, and every line all represents the different location of θ in figure, and finding peak in figure, (X is penetrated
Line maximum of intensity) corresponding θpWith 2 θp, θ is obtained according to n λ=2dsin θ0, (θp-θ0, 2 θp-2θ0) it is that the crystal is corresponding
Angular instrument θ axis and 2 θ axis correction factors, when automatically correcting, detector acquires the corresponding x-ray fluorescence intensity value of all crystal, complete
Into one group of correction factor list of rear acquisition, crystal glancing angle θ and detector are emitted by the correction factor of the corresponding crystal of inquiry
2 θ of angle is corrected.
Claims (7)
1. debugging and correction system, the Xray fluorescence spectrometer are suitable to a kind of light splitting optical path of Xray fluorescence spectrometer automatically
Sequence formula wavelength dispersion X-ray fluorescence spectrometer, including detector (6), angular instrument, crystal frame and multiple light splitting crystal, angle measurement
The θ axis of instrument and 2 θ axis carry selected crystal and detector respectively, it is characterised in that：The system includes：Operating Interface Module
(1), crystal frame control module (2), angular instrument θ axis and 2 θ axis high-precision step motor control modules (3), detector data acquisition
Module (4) and data image processing module (5)；
Selected crystal is switched in light splitting optical path by the crystal frame control module (2)；
The scanning range and sweep spacing and detector that user passes through Operating Interface Module (1) setting angular instrument θ axis and 2 θ axis
Acquisition time；
The angular instrument θ axis and 2 θ axis high-precision step motor control modules (3) adjust the θ axis and 2 θ axis, according to scanning model
It encloses and crystal and detector is rotated into designated position successively；
The detector data acquisition module (4) is acquired the X-ray intensity of the designated position, and acquisition information is sent into
The data image processing module (5) is handled, final to establish intuitive three-dimensional three-dimensional data model, calculates corresponding school
Positive divisor, and information back is shown to interface module (1) is made.
2. debugging exists the light splitting optical path of Xray fluorescence spectrometer according to claim 1 with correction system, feature automatically
In：
The Operating Interface Module (1) shows including customer parameter setting interface, detector data acquisition interface and three-dimensional data
Interface；Customer parameter setting interface sets the scanning range and sweep span of angular instrument θ axis and 2 θ axis high-precision stepper motors, choosing
It sets the tone and tries crystal；Detector data acquisition interface sets detector acquisition parameter, display acquisition spectrogram and X-ray intensity value；Three
The final three-dimensional data model that the display analysis of dimension data display interface obtains.
3. debugging exists the light splitting optical path of Xray fluorescence spectrometer according to claim 1 with correction system, feature automatically
In：
Crystal frame control module (2) driving crystal frame movement motor used is straight available for the low energy consumption under vacuum condition
Galvanic electricity machine；10~20 pieces of different crystal are installed on crystal frame；Screw realization crystal angle fine tuning is adjusted by adjusting crystal.
4. debugging exists the light splitting optical path of Xray fluorescence spectrometer according to claim 1 with correction system, feature automatically
In：
The angular instrument θ axis is five phase steppings electricity with the stepper motor that 2 θ axis high-precision step motor control modules (3) are controlled
Machine, can realize accelerate when θ axis and 2 θ axis start, in operation at the uniform velocity with gradual retarded motion when stopping；Meanwhile, it is capable to realize θ
Axis is moved respectively with 2 θ axis with linking simultaneously；And equipped with anticollision emergency handling function.
5. debugging exists the light splitting optical path of Xray fluorescence spectrometer according to claim 1 with correction system, feature automatically
In：
The detector data acquisition module (4) is equipped with the sudden strain of a muscle of fluid-type proportional counter and measurement heavy element for measuring light element
Bright body counter is USB or Ethernet with host computer communication mode.
6. a kind of debugging of Xray fluorescence spectrometer light splitting optical path and bearing calibration using system described in claim 1, feature
It is：This method comprises the following steps：
A, the X ray of closing sequence formula wavelength dispersion X-ray fluorescence spectrometer opens protective cover, and multiple and different crystal is pacified
It is attached on crystal frame, and passes through crystal frame control module (2) and selected crystal is switched in light splitting optical path；
B, angular instrument θ axis is moved to and is conveniently adjusted crystalline substance by angular instrument θ axis and 2 θ axis high-precision step motor control modules (3)
The position of body angle, level angle measurer are placed on plane of crystal and measure its level angle, and screw is adjusted by rotating crystal
Crystal angle is adjusted, level angle measurement is shown to specified angle and completes to adjust crystal the adjustment of screw；
C, protective cover is closed, opens X ray, detector acquisition parameter and angular instrument θ axis are set by Operating Interface Module (1)
With the scanning range and sweep span of 2 θ shaft step motors, and send order and start to automatically correct；
D, angular instrument θ axis and 2 θ axis high-precision step motor control modules (3) adjust the θ axis and 2 θ axis, according to scanning range
Crystal and detector are rotated into designated position successively；Detector data acquisition module (4) is to the X-ray intensity of the designated position
It is acquired, and the information feeding data image processing module (5) will be acquired and handled, it is final to establish the three of intuitive solid
D Data Model therefrom chooses the corresponding θ of X-ray intensity maximum valuepWith 2 θp；(θp-θ0, 2 θp-2θ0) it is that the crystal is corresponding
Angular instrument θ axis and 2 θ axis correction factors；
E, after being automatically corrected to the completion of all crystal, one group of crystal correction is obtained because of sublist；Pass through the school of the corresponding crystal of inquiry
Positive divisor is corrected crystal glancing angle θ and 2 θ of the detector angle of emergence.
7. Xray fluorescence spectrometer light splitting optical path debugging according to claim 6 and bearing calibration, it is characterised in that：Institute
The precision for stating level angle measurer is not less than 0.1 °.
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