CN102841108A - Polarization secondary target energy dispersion type X-ray fluorescent spectrograph - Google Patents
Polarization secondary target energy dispersion type X-ray fluorescent spectrograph Download PDFInfo
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Abstract
The invention discloses a polarization secondary target energy dispersion type X-ray fluorescent spectrograph. According to the spectrograph disclosed by the invention, two planes, namely a secondary target and a sample, are arranged on a spatial stereoscopic light path, an X-ray tube of the spectrograph emits primary X rays, the primary X rays are incident to the secondary target in an angle of 45 degrees, scattered rays of the primary X rays emergent from the secondary target in the angle of 45 degrees are full-polarization X rays with polarization direction vertical to an incident plane, and target characteristic X rays excited on the secondary target by the primary X rays are isotropous circular polarization rays and are discrete spectral lines. By adopting the spectrograph disclosed by the invention, peak-to-background ratio is improved, detection limit of microelement detection is reduced, low-content elements in the sample can be detected, and test accuracy and efficiency are improved.
Description
Technical field
The invention belongs to a kind of spectrometer, particularly a kind of polarization secondary target energy dispersion type Xray fluorescence spectrometer.
Background technology
Advantages such as energy dispersion type X-ray fluorescence spectra technology (EDXRF) is simple and efficient with it, nondestructive analysis; At industry-by-industries such as production, scientific researches application is very widely arranged all, especially more pushed the development and the application of this technology to a unprecedented height in the detection in environmental protection field.
The basic structure of main flow EDXRF instrument two-dimensional design as shown in Figure 1 in the market, X-ray tube are excited and produce ray incident sample, produce fluorescent then and are received by detector; Again through the spectrum Treatment Analysis; Obtain test result, effectively the propagation of X ray is constrained in the two dimensional surface, and such structure has the detection efficiency height; Advantages such as little are disturbed in scattering, are extensively adopted by industry all the time.
Deepen continuously along with what use; The development and application engineers is constantly attempted through changing light pipe output, install optical filter additional, shorten light path, installing means such as vacuum additional and strengthen, reduce scattering background to reach spectrum local, weaken purpose such as air light path interference and obtained certain achievement; But this two-dimentional light channel structure is restricting the development of technology all the time, because the space that can supply operate is limited after all.
Along with the innovation of technology, polarization secondary target light path has appearred at present---and utilize the three-dimensional polarization excitaton source, the geometric layout of X-ray tube, polarization target or secondary target and sample is three-dimensional, uses the technology of polarized light or secondary target activation sample.
At present; For energy-dispersion X-ray fluorescence spectrometer; A problem that often runs into is, the energy that the characteristic X-ray energy of the trace element that some must detect is lower than the characteristic X-ray of certain high-load element in the matrix material just slightly in this case because the low energy hangover of high-load elemental characteristic X ray on detector is (little to the macroelement influence; But it is very big that trace element is measured influence) and/or the influence of escape peak; The detection of trace element is difficulty very, and this has brought great challenge for the application of XRF energy spectrometer, even adopt above-mentioned polarization secondary target light path; Utilize the selective excitation of fluorescence secondary target; The characteristic X-ray energy that also can only solve trace element significantly is lower than the situation of high-load elemental characteristic X ray, and is lower than the situation of high-load elemental characteristic X ray slightly for the characteristic X-ray energy of trace element, because the fluorescent X-ray of fluorescence secondary target outgoing has the intense line of 2 different-energies at least; Be difficult to accomplish only excite micro-fluorescence to be measured and do not excite high-load interference element fluorescence simultaneously; Though a little effect is arranged, can not deal with problems at all, also do not see the effective technology means of handling this situation on the whole at present.
Summary of the invention
The objective of the invention is to solve the deficiency of above-mentioned technology; A kind of polarization secondary target energy dispersion type Xray fluorescence spectrometer is proposed; Fluorescence Spectra to realize spectrometer does not have background and selective excitation function; And can detect the low content element in the sample, improved the accuracy of test and the purpose of efficient.
Another object of the present invention is on the emitting light path of secondary target, optical filter to be installed, and reaches can the fluorescent line (2 intense line) of secondary target outgoing be filled into only surplus intense line at least, and other intense line is absorbed very low purpose by optical filter.
For achieving the above object, the technical scheme that the present invention adopts is:
A kind of polarization secondary target energy dispersion type Xray fluorescence spectrometer; Spectrometer with secondary target and two floor plan of sample on the space multistory light path; The X-ray pipe of spectrometer penetrates simple X ray; Described simple X ray incides on the secondary target with 45; Scattered ray with the simple X ray of 45 ° of outgoing from the secondary target is the full polarization X ray of polarization direction perpendicular to plane of incidence, and the target characteristic X-ray that simple X ray excites on the secondary target is isotropic circular polarization line, and is discrete spectral line.
The scattered ray of secondary target is pressed the space multistory light path; Incide on the sample with 45; Scattered portion polarization direction in the incident ray is parallel to this plane of incidence; During through the outgoing of polarization once more of sample plane, can on sample, not produce the scattered ray of 45 outgoing, i.e. polarization extinction at the scattered ray of the simple X ray of 45 ° of full polarizations; The target characteristic X-ray that simple X ray excites on the secondary target is isotropic circular polarization line, and is discrete spectral line; Target characteristic spectrum in the incident ray is full polarization after by sample scattering, and the characteristic X-ray that sample is excited is circularly polarized line spectrum;
The characteristic X-ray that sample is excited is received by detector and analyzes, and detector receives only the characteristic X-ray that the element in the sample is excited and the scattered ray of secondary target characteristic X-ray at 45.
Further, simple X ray is that continuous a piece of wood serving as a brake to halt a carriage of X-ray pipe outgoing causes that good fortune is penetrated and discrete target characteristic curve, is isotropic circular polarization X ray.
Further; The scattered ray of secondary target is pressed the space multistory light path; Incide on the sample with 45, the scattered portion polarization direction in the incident ray is parallel to this plane of incidence, and promptly scattered portion can not occur when outgoing again comprises continuous spectrum and target characteristic spectrum.
Further, the target characteristic spectrum comprises Compton scattering and Rayleigh scattering after by sample scattering, is the discrete spectrum of full polarization.
Further, the secondary target adopts Bark to draw target, and described Bark draws target to come excited sample with the scattered ray of secondary target.
Further, the secondary target adopts fluorescence secondary target, and described fluorescence secondary target adopts the fluorescent line excited sample of secondary target outgoing.
Further, simple X ray comprises the discrete characteristic X-ray of continuous spectrum and target material.
Further, on the emitting light path of secondary target, be added with optical filter, described optical filter is filled into only surplus intense line with the fluorescent line of secondary target outgoing, and other intense line is absorbed very low by optical filter.
Further, the material of optical filter and thickness are through calculating, making many characteristic fluorescence X ray of secondary target outgoing become accurate homogeneous X-ray.
Adopt above-mentioned technology; Beneficial effect of the present invention has: the primary X-ray that produces with X-ray generator removes to shine the secondary target; Monochromatic excitation source with the secondary target produces under the irradiation of primary X-ray is shone sample, realizes that the fluorescence Spectra of spectrometer does not have background and selective excitation function, can go up and remove and the upward very big continuous scattering background that reduces the detected fluorescence power spectrum of detector of practice; Improve peak back of the body ratio; Reduce the detection limit that trace element detects, and can detect the low content element in the sample, improved the accuracy and the efficient of test.
Second beneficial effect of the present invention is on the emitting light path of secondary target, optical filter to be installed; Can the fluorescent line (2 intense line) of secondary target outgoing be filled into only surplus intense line at least; Other intense line is absorbed very low by optical filter, through this technology, reach with accurate monochromatic excitation source irradiation sample; Realize the selective excitation function of spectrometer, can detect the element to be measured of the trace in the sample that contains the high-load interference element.
Description of drawings
Fig. 1 is the basic light path synoptic diagram of two-dimentional EDXRF;
Fig. 2 is the polarisation of light synoptic diagram;
Fig. 3 is the Brewster example schematic;
Fig. 4 is that polarization secondary target space multistory light path principle is resolved synoptic diagram;
Fig. 5 is that polarization secondary target space multistory light path principle is resolved schematic flow diagram;
Fig. 6 is ordinary two dimensional light path and polarization secondary target optical test path EC680K sample spectrogram contrast synoptic diagram;
Fig. 7 is the high Br sample spectra contrast of an ordinary two dimensional light path and polarization secondary target optical test path synoptic diagram;
Embodiment
Below in conjunction with specific embodiment the present invention is described further, but the present invention is not limited to following examples.
As shown in Figure 2; Brewster is thought; When reflection and refraction took place on two kinds of isotropic dielectric interfaces circularly polarized light, reflected light and refract light all were partial poolarized lights, and direction of vibration is preponderated than the composition that is parallel to the plane of incidence perpendicular to the composition of the plane of incidence in the reflected light; Light is n from refractive index
1Medium incident refractive index be n
2Medium the time, as incident angle i
bSatisfy
The time, reflected light becomes full-polarization, incident angle i
bBe called Brewster angle.With regard to X ray, the refractive index n in air and medium
1And n
2All be about 1, so Brewster angle is about 45 degree.We are set to space multistory light path as shown in Figure 3 with secondary target and two planar cloth of sample in instrument; Circularly polarized simple X ray (the discrete characteristic X-ray that comprises continuous spectrum and target material) incides on the secondary target with 45; From the secondary target with the scattered ray of 45 ° of outgoing; Be the full polarization X ray of polarization direction, and the target fluorescence that simple X ray excites on the secondary target is isotropic circular polarization line perpendicular to plane of incidence.
, incide on the sample with 45 ° by space optical path shown in Figure 3 from the spectral line of secondary target outgoing, the scattered portion in the incident ray (polarization direction is parallel to this plane of incidence) can not occur when outgoing again; And the fluorescent X-ray of the secondary target target in the incident ray by sample scattering after (comprising Compton scattering and Rayleigh scattering) be full polarization; The characteristic X-ray that sample is excited is circularly polarized.
Can find out that from the process of top elaboration in theory, the continuous spectrum of X-ray pipe outgoing and the characteristic X-ray of light pipe target are can not get into detector, promptly eliminate in the spectrum of EDXRF instrument test the continuous scattering background that spectrum unscrambling and measuring accuracy are had the greatest impact.In practical application, can not satisfy the condition that desirable full polarization disappears mutually, but the purpose that reduces scattering background significantly can reach.
Comprehensive above the description, the background peaks that in the spectrum of ordinary two dimensional EDXRF instrument test spectrum unscrambling and measuring accuracy is had the greatest impact owing to mainly be derived from the continuous part of X-ray tube outgoing in composing, can be eliminated by twice polarization in three-dimensional light path fully; Secondary target in the three-dimensional structure can be changed or switch eaily, and this maybe with regard to providing for the selective excitation of element.
More than be the basic light path of our seen polarization secondary target instrument, going out is the basic light path that the present invention adopts, and the present invention can adopt Bark to draw target to make the secondary target, also can adopt fluorescence secondary target.Bark draws target to come excited sample with the scattered ray of secondary target, and fluorescence secondary target adopts the fluorescent line excited sample of secondary target outgoing.
Patent of the present invention; Be employed in the way that adds optical filter on the emitting light path of secondary target, make to go up and remove and the continuous scattering background that greatly reduces the detected fluorescence power spectrum of detector is gone up in practice, improve peak back of the body ratio; Reduce the problem of the detection limit of trace element detection, obtain solving very effectively.Through selecting suitable material and having the optical filter of suitable thickness; Can the fluorescent line (2 intense line) of secondary target outgoing be filled into only surplus intense line at least; Through reasonable disposition secondary target and optical filter; Make this intense line that remains just in time be fit to excite the characteristic fluorescence X ray of trace element to be measured; And just in time can not excite high-load elemental characteristic X ray, and so just can eliminate or significantly reduce of the interference of high-load elemental characteristic X ray the characteristic X-ray of trace element, the detection limit of trace element is significantly reduced.Our monochromatic selective excitation that is referred to as to be as the criterion.With such configuration; We to C1 element in the plastic cement sample that contains high-load Ti, contain in the plastic material of high-load Br (fire retardant) that the Pb element detects in the semiconductor material that C1 element in Pb, Hg element, the soldering tin material (main composition is Sn) contains high-load Bi; Detection limit is reduced to below the 10ppm to thousands of ppm by the hundreds of of the XRF energy spectrometer of routine, detects precision and accuracy and also is significantly improved.
Adopt the instrument of patent art exploitation promptly can reach the purpose that significantly reduces scattering background by basic light path work.Also can be by switching the purpose that optical filter reaches accurate monochromatic selective excitation.
The beneficial effect instance: we explain the superiority of polarization secondary target light path through the contrast of actual measurement spectrogram: as shown in Figure 4; Test the same standard model EC680K of European Union respectively with common two-dimentional light path EDXRF instrument and polarization secondary target instrument, and do the contrast of spectrum shape.Can see that the effect of polarization secondary target instrument aspect the background elimination is very obvious, conform to fully with the design original intention with optical principle; What Fig. 4 demonstrated is the effect of the elimination scattering background of polarization secondary target.
As shown in Figure 5; Contain Br10%; The sample test of Pb50ppm through reasonable secondary target and filter material are set, are selected specific target characteristic curve that Pb:La is formed strongly and is excited in polarization secondary target instrument; Thereby realize the accurate test to micro Pb element in the high Br sample, such effect can't be imagined in the power spectrum of ordinary two dimensional light path; What Fig. 5 demonstrated is the effect of the monochromatic selective excitation of standard behind the employing optical filter.
The sharp in sum EDXRF instrument that adopts the 3 D stereo light path to succeed in developing; Have and eliminated scattering background, but selective excitation, and measuring accuracy is high; Can solve the excellent functions such as particular sample test that common power spectrum cann't be solved, have very strong practicality and novelty.
In addition, second characteristic of the present invention is on the emitting light path of secondary target, optical filter to be installed, and can the fluorescent line (2 intense line) of secondary target outgoing be filled into only surplus intense line at least, and other intense line is absorbed very low by optical filter.Through this technology, reach with accurate monochromatic excitation source irradiation sample, realize the selective excitation function of spectrometer, can detect the element to be measured of the trace in the sample that contains the high-load interference element, improved the accuracy and the efficient of test.
Adopt the EDXRF instrument of patent art exploitation, can dispose a plurality of secondary targets (fluorescent target or Bark draw target) that switched by computer controlled automatic, configurable a plurality of optical filters that switched by computer controlled automatic are to be suitable for various application.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and obviously, those skilled in the art can carry out various changes and modification and not break away from the spirit and scope of the present invention the present invention.Like this, belong within the scope of claim of the present invention and equivalent technologies thereof if of the present invention these are revised with modification, then the present invention also is intended to comprise these changes and modification interior.
Claims (9)
1. polarization secondary target energy dispersion type Xray fluorescence spectrometer; Described spectrometer with secondary target and two floor plan of sample on the space multistory light path; The X-ray pipe of spectrometer penetrates simple X ray; Described simple X ray incides on the secondary target with 45; Scattered ray with the simple X ray of 45 ° of outgoing from the secondary target is the full polarization X ray of polarization direction perpendicular to plane of incidence, and the target characteristic X-ray that described simple X ray excites on the secondary target is isotropic circular polarization line, and is discrete spectral line;
The scattered ray of---described secondary target is pressed the space multistory light path; Incide on the sample with 45; Scattered portion polarization direction in the incident ray is parallel to this plane of incidence; During through the outgoing of polarization once more of sample plane, can on sample, not produce the scattered ray of 45 outgoing, i.e. polarization extinction at the scattered ray of the simple X ray of 45 ° of full polarizations; The target characteristic X-ray that simple X ray excites on the secondary target is isotropic circular polarization line, and is discrete spectral line; Target characteristic spectrum in the incident ray is full polarization after by sample scattering, and the characteristic X-ray that sample is excited is circularly polarized line spectrum;
The characteristic X-ray that---described sample is excited is received by detector and analyzes, and described detector receives only the characteristic X-ray that the element in the sample is excited and the scattered ray of secondary target characteristic X-ray at 45.
2. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1 is characterized in that: described simple X ray is that continuous a piece of wood serving as a brake to halt a carriage of X-ray pipe outgoing causes that good fortune is penetrated and discrete target characteristic curve, is isotropic circular polarization X ray.
3. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1; It is characterized in that: the scattered ray of described secondary target is pressed the space multistory light path; Incide on the sample with 45; Scattered portion polarization direction in the incident ray is parallel to this plane of incidence, and promptly scattered portion can not occur when outgoing again comprises continuous spectrum and target characteristic spectrum.
4. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1 is characterized in that: described target characteristic spectrum comprises Compton scattering and Rayleigh scattering after by sample scattering, is the discrete spectrum of full polarization.
5. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1 is characterized in that: described secondary target adopts Bark to draw target, and described Bark draws target to come excited sample with the scattered ray of secondary target.
6. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1 is characterized in that: described secondary target adopts fluorescence secondary target, and described fluorescence secondary target adopts the fluorescent line excited sample of secondary target outgoing.
7. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1, it is characterized in that: described simple X ray comprises the discrete characteristic X-ray of continuous spectrum and target material.
8. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 1; It is characterized in that: on the emitting light path of secondary target, be added with optical filter; Described optical filter is filled into only surplus intense line with the fluorescent line of secondary target outgoing, and other intense line is absorbed very low by optical filter.
9. polarization secondary target energy dispersion type Xray fluorescence spectrometer according to claim 8 is characterized in that: the material of described optical filter and thickness are through calculating, making many characteristic fluorescence X ray of secondary target outgoing become accurate homogeneous X-ray.
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Cited By (5)
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| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
| CN105866157A (en) * | 2016-05-26 | 2016-08-17 | 深圳市华唯计量技术开发有限公司 | X fluorescence spectrometer for PM2.5 heavy metal online detection |
| CN108802081A (en) * | 2017-04-27 | 2018-11-13 | 北京安科慧生科技有限公司 | X-ray fluorescence (XRF) spectroscopy systems and methods |
| CN110083091A (en) * | 2019-04-11 | 2019-08-02 | 成都理工大学 | The EDXRF secondary target automatic control device of multipotency X-ray |
| CN113433142A (en) * | 2021-06-22 | 2021-09-24 | 中国工程物理研究院激光聚变研究中心 | High space-time resolution optical system suitable for X-ray diagnosis |
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Cited By (8)
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| CN105510369A (en) * | 2015-12-22 | 2016-04-20 | 北京安科慧生科技有限公司 | Special X-ray fluorescence energy spectrometer for high-precision cement industry |
| CN105866157A (en) * | 2016-05-26 | 2016-08-17 | 深圳市华唯计量技术开发有限公司 | X fluorescence spectrometer for PM2.5 heavy metal online detection |
| CN105866157B (en) * | 2016-05-26 | 2018-08-10 | 深圳市华唯计量技术开发有限公司 | A kind of PM2.5 heavy metals on-line checking X fluorescence spectrometer |
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| CN108802081B (en) * | 2017-04-27 | 2021-07-30 | 北京安科慧生科技有限公司 | X-ray fluorescence (XRF) spectroscopy systems and methods |
| CN110083091A (en) * | 2019-04-11 | 2019-08-02 | 成都理工大学 | The EDXRF secondary target automatic control device of multipotency X-ray |
| CN113433142A (en) * | 2021-06-22 | 2021-09-24 | 中国工程物理研究院激光聚变研究中心 | High space-time resolution optical system suitable for X-ray diagnosis |
| CN113433142B (en) * | 2021-06-22 | 2022-08-26 | 中国工程物理研究院激光聚变研究中心 | High space-time resolution optical system suitable for X-ray diagnosis |
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