CN202330315U - X-ray fluorescence spectrum quantitative analysis device - Google Patents
X-ray fluorescence spectrum quantitative analysis device Download PDFInfo
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- CN202330315U CN202330315U CN2011203302664U CN201120330266U CN202330315U CN 202330315 U CN202330315 U CN 202330315U CN 2011203302664 U CN2011203302664 U CN 2011203302664U CN 201120330266 U CN201120330266 U CN 201120330266U CN 202330315 U CN202330315 U CN 202330315U
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- magnetic force
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Abstract
The utility model discloses an X-ray fluorescence spectrum quantitative analysis device. The theoretical calculation and the standard sample comparison process of a math correction method and an experiment correction method in the prior art are complicated. The device disclosed by the utility model comprises a high energy pulse laser, a laser reflective mirror, a laser lead-in window, a solid sample, a solid sample table, a solid sample magnetic transmission rod, a transmission rod flange, a magnet transmission slide block, a magnetic transmission rod sleeve, a magnetic transmission rod flange, a graphite sedimentation table, a graphite sedimentation table support rod, a graphite sedimentation table flange, an X-ray tube, an X-ray tube cable, an X-fluorescence detector, a metal ceramic electrode, an X- fluorescence detector support rod, a vacuum unit and a vacuum cavity. According to the utility model, factors generating a matrix effect are eliminated from the source through a thin film deposition technology, the elimination process affected by the matrix effect in an XRF (X-ray fluorescence) quantitative analysis is simplified, and the detection efficiency and the test accuracy are improved.
Description
Technical field
The utility model belongs to the testing of materials analysis field, relates to a kind of device of X-ray fluorescence spectra quantitative test.
Background technology
XRF is a kind of nondestructive elemental analysis method.It makes the atomic radiation characteristic fluorescence X ray in the sample, just so-called secondary x rays by the primary X-ray excited sample that X ray light sends.Wavelength and intensity distributions according to the radiation spectral line realize the qualitative and quantitative analysis to the sample component.Yet often cause very big error when the existence of (component in the sample beyond the analytical element just coexistence elements is referred to as matrix) because matrix effect, no standard specimen XRF quantitative test.
Matrix effect is mainly proofreaied and correct through mathematics correction method and experiment correction method at present.The mathematics correction method comprises empirical coefficient method, fundamental parameters method, theoretical influence coefficient method etc.The general error of mathematics correction method is very big, and program is complicated, and what have also need provide standard model.The experiment correction method mainly is that internal standard method, standard addition method, dilution method etc. are arranged, but these methods directly are not suitable for solid sample.Above-mentioned the whole bag of tricks all is to eliminate the precision of the influence of matrix effect with raising XRF quantitative test through theory or laboratory facilities, needs complicated Theoretical Calculation or standard specimen relatively, and process is quite loaded down with trivial details, and the sample preparation program is loaded down with trivial details.
Summary of the invention
The purpose of the utility model is exactly the deficiency to prior art, and a kind of device of X-ray fluorescence spectra quantitative test is provided.
The utility model adopts following technical scheme:
The utility model comprises that high energy pulse laser, laser reflective mirror, laser guide-in window, solid sample, solid sample platform, solid sample magnetic drives bar, drive link flange, magnet driving block, magnetic force transmit rod sleeve, magnetic force transmits bar flange, graphite deposition table, graphite deposition table support bar, graphite deposition table flange, X-ray pipe, X-ray pipe cable, X fluorescent probe, cermet electrodes, X fluorescent probe support bar, vacuum unit and vacuum cavity.
The laser guide-in window is arranged on the vacuum cavity outside, and an end of X-ray pipe passes vacuum cavity, and is fixed on the vacuum cavity, and the other end is connected with X-ray pipe cable.
The upper end of X fluorescent probe is unsettled; Be connected with an end of X-ray fluorescent probe support bar in the middle of the lower end; Be connected with the electrode of cermet electrodes flange around in the middle of the lower end, the other end of X-ray fluorescent probe support bar is threaded with the cermet electrodes flange.
The vacuum unit is arranged on the vacuum cavity outside.
Solid sample is placed in the graphite sample platform; One end of graphite sample platform is unsettled, and the other end is connected with an end of solid sample platform magnetic drives bar, and the other end of solid sample platform magnetic drives bar passes magnetic force and transmits the bar flange; Get into magnetic force and transmit rod sleeve; The end that magnetic force transmits the bar flange is threaded with vacuum cavity, and magnetic force transmits the other end and the magnetic force transmission rod sleeve of bar flange and fixes, and has through hole in the middle of the magnet driving block; One end of magnetic force transmission rod sleeve runs through the through hole of magnet driving block, and magnetic force transmits rod sleeve and the magnet driving block is slidingly matched.
The upper end of graphite deposition table is fixed on an end of graphite deposition table support bar; Graphite deposition table lower end is unsettled; The other end of graphite deposition table support bar passes graphite deposition table flange, and is slidingly matched with graphite deposition table flange, and graphite deposition table flange is threaded with vacuum cavity.
The pulse laser that high energy pulse laser is launched gets into the laser guide-in window through the reflection of laser reflective mirror.
Described X fluorescent probe, solid sample, solid sample platform and graphite deposition table all are arranged in the vacuum cavity.
The beneficial effect of the utility model: the utility model converts solid sample to be measured to the film sample identical with its component through the pulsed laser deposition method, fundamentally eliminates matrix effect.As long as just can obtain composition in the sample through basic X ray parameters such as theoretical XRF yield, Theoretical Mass absorption coefficients.
Description of drawings
Fig. 1 is the utility model structural representation;
The stainless steel alloy component that Fig. 2 records for the utility model is with the Thickness Variation curve.
Embodiment
Like Fig. 1, the utility model device comprises that high energy pulse laser 1, laser reflective mirror 2, laser guide-in window 3, solid sample 4, solid sample platform 5, solid sample platform magnetic drives bar 6, magnetic force transmit rod sleeve 7, magnetic force transmits bar flange 8, magnet driving block 9, graphite deposition table 10, graphite deposition table support bar 11, graphite deposition table flange 12, X-ray pipe 13, X-ray pipe cable 14, XRF detector 15, cermet electrodes flange 16, X-ray fluorescent probe support bar 17, vacuum unit 18 and vacuum cavity 19.
Laser guide-in window 3 is arranged on the vacuum cavity 19, and an end of X-ray pipe 13 passes vacuum cavity 19, and is fixed on the vacuum cavity 19, and the other end of X-ray pipe 13 is connected with X-ray pipe cable 14.
The upper end of X fluorescent probe 15 is unsettled; Be connected with an end of X-ray fluorescent probe support bar 17 in the middle of the lower end; Be connected with the electrode of cermet electrodes flange 16 around in the middle of the lower end, the other end of X-ray fluorescent probe support bar 17 is threaded with cermet electrodes flange 16.
Vacuum unit 18 is arranged on the vacuum cavity 19.
The upper end of graphite deposition table 10 is fixed on an end of graphite deposition table support bar 11; Graphite deposition table 10 lower ends are unsettled; The other end of graphite deposition table support bar 11 passes graphite deposition table flange 12; And be slidingly matched with graphite deposition table flange 12, graphite deposition table flange 12 is threaded with vacuum cavity 19.
The pulse laser that high energy pulse laser 1 is launched gets into laser guide-in window 3 through 2 reflections of laser reflective mirror and is radiated on the solid sample 4, and solid sample 4 is placed in solid sample platform 5, and the move left and right of transmitting bar slide block 9 through magnetic force can move the solid sample platform.
The method of utilizing said apparatus to analyze may further comprise the steps:
Step 1: slide into the end to magnet driving block 9 to the right, open magnetic force and transmit bar flange 8, be placed on solid sample 4 on the solid sample platform 5, tighten magnetic force and transmit bar flange 8.Be moved to the left magnet driving block 9, move on to graphite deposition table below to solid sample platform 5.
Step 2: open graphite deposition table flange 12, change the graphite deposition table 10 of cleaning, tighten graphite deposition table flange 12.
Step 3: the open vacuum unit, vacuumize, make that the pressure in the vacuum chamber is lower than 1.0Pa.
Step 4: open high energy pulse laser 1, laser beam is passed laser guide-in window 3 and is radiated on the solid sample 4 after reflecting through laser reflective mirror 2.The control laser pulse number makes the film thickness that is deposited on the solid sample 4 on the graphite sample platform 5 less than 100nm.
Step 6: close high energy pulse laser.
Step 7: move on to magnet driving block 9 to the right, remove solid sample platform 5 from X fluorescent probe 15 tops.
Step 8: open X-ray pipe 13, open X fluorescent probe 15 and measure, the record spectral line.
Step 9: close the power supply of X fluorescent probe 13, close X-ray pipe power supply, close general supply.
The laser beam that the utility model sends from high energy pulse laser is incided on the solid sample in the vacuum cavity by the laser guide-in window after through reflective mirror, and the solid sample surface is heated and discharges the composition particle identical with it.The particle that discharges from solid sample is deposited on the graphite deposition table that is positioned at the solid sample top and forms film.The x-ray bombardment that the X-ray pipe sends is to this film, and the XRF that film sends is surveyed by the XRF detector that is positioned at its below.
Suppose incident X bundle for monochromatic X ray, then for a certain element i that is positioned at depth d, the intensity of the characteristic X fluorescent x ray that it sends
I 0 With incident X-rays intensity
0, incident angle
, this element is to the mass absorption coefficient of incident X-rays
i, sample density
, this characteristic X fluorescent x ray yield
iConcentration c with this element
iThese factors are relevant, promptly
Matrix effect is exactly that incident X-rays stands the Strength Changes that the absorption of other atoms causes in the solid sample to the characteristic X fluorescence of sample interior motion and outgoing from sample interior when sample surfaces moves.When this characteristic fluorescence ray during to apparent motion, it also will receive, and the degree of depth is less than the absorption of the upper strata atom of d in the solid sample, and its situation and incident X-rays are similar.The emergence angle of supposing characteristic X fluorescent x ray does
, solid sample is to the mass absorption coefficient of this characteristic X fluorescence
j, then the absorption of characteristic X fluorescence is proportional to during outgoing
Therefore, the X-ray fluorescence that sends of the element i intensity that finally arrives detector is proportional to
.For film sample; D is very little; The numerical value of
and
is also very little; Two exponential terms in the formula are all near 1 so, and this moment, matrix effect can be ignored.Therefore,, the influence of matrix effect can be eliminated, the higher no standard specimen XRF quantitative test of precision can be obtained thus as long as process film sample to solid sample.
Because the component of the film that the pulsed laser deposition technology is processed and the component of solid sample itself are very approaching, we utilize the pulsed laser deposition technology to process the precision of film sample to guarantee to measure to solid sample in the utility model.Simultaneously, we combine the pulsed laser deposition device with the XRF spectrometer, so not only can utilize the pulsed laser deposition technology to process film sample to solid sample, can the time avoid absorption and the interference to X fluorescence such as argon gas element in the air in test again.
As shown in Figure 2, utilize the utility model device that the composition of a certain stainless steel material is tested.Utilize the pulsed laser deposition technology to deposit 7 Thin Stainless Steel membrane samples respectively, thickness is respectively 10nm, 20nm, 50nm, 100nm, 200nm, 500nm, 1000nm.The content that records Fe, Cr, three kinds of elements of Ni in the Thin Stainless Steel membrane sample of different-thickness is such as shown in the accompanying drawing 2.When the Thin Stainless Steel film thickness less than 200nm in, composition is constant basically, and consistent with standard value, explains that matrix effect is not obvious.But after the stainless steel thickness surpassed 200nm, component was along with the increase of thickness departs from standard value rapidly.This shows that thickness eliminated the matrix effect in the XRF quantitative test effectively less than the film stainless steel sample of 200nm.
Claims (1)
1. the device of an X-ray fluorescence spectra quantitative test; Comprise that high energy pulse laser, laser reflective mirror, laser guide-in window, solid sample, solid sample platform, solid sample magnetic drives bar, drive link flange, magnet driving block, magnetic force transmit rod sleeve, magnetic force transmits bar flange, graphite deposition table, graphite deposition table support bar, graphite deposition table flange, X-ray pipe, X-ray pipe cable, X fluorescent probe, cermet electrodes, X fluorescent probe support bar, vacuum unit and vacuum cavity, it is characterized in that:
The laser guide-in window is arranged on the vacuum cavity outside, and an end of X-ray pipe passes vacuum cavity, and is fixed on the vacuum cavity, and the other end is connected with X-ray pipe cable;
The upper end of X fluorescent probe is unsettled; Be connected with an end of X-ray fluorescent probe support bar in the middle of the lower end; Be connected with the electrode of cermet electrodes flange around in the middle of the lower end, the other end of X-ray fluorescent probe support bar is threaded with the cermet electrodes flange;
The vacuum unit is arranged on the vacuum cavity outside;
Solid sample is placed in the graphite sample platform; One end of graphite sample platform is unsettled, and the other end is connected with an end of solid sample platform magnetic drives bar, and the other end of solid sample platform magnetic drives bar passes magnetic force and transmits the bar flange; Get into magnetic force and transmit rod sleeve; The end that magnetic force transmits the bar flange is threaded with vacuum cavity, and magnetic force transmits the other end and the magnetic force transmission rod sleeve of bar flange and fixes, and has through hole in the middle of the magnet driving block; One end of magnetic force transmission rod sleeve runs through the through hole of magnet driving block, and magnetic force transmits rod sleeve and the magnet driving block is slidingly matched;
The upper end of graphite deposition table is fixed on an end of graphite deposition table support bar; Graphite deposition table lower end is unsettled; The other end of graphite deposition table support bar passes graphite deposition table flange, and is slidingly matched with graphite deposition table flange, and graphite deposition table flange is threaded with vacuum cavity;
The pulse laser that high energy pulse laser is launched gets into the laser guide-in window through the reflection of laser reflective mirror;
Described X fluorescent probe, solid sample, solid sample platform and graphite deposition table all are arranged in the vacuum cavity.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203302664U CN202330315U (en) | 2011-09-05 | 2011-09-05 | X-ray fluorescence spectrum quantitative analysis device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011203302664U CN202330315U (en) | 2011-09-05 | 2011-09-05 | X-ray fluorescence spectrum quantitative analysis device |
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| CN202330315U true CN202330315U (en) | 2012-07-11 |
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| CN2011203302664U Expired - Lifetime CN202330315U (en) | 2011-09-05 | 2011-09-05 | X-ray fluorescence spectrum quantitative analysis device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323284A (en) * | 2011-09-05 | 2012-01-18 | 杭州电子科技大学 | A kind of device and method of X-ray fluorescence spectra quantitative test |
| CN102778294A (en) * | 2012-07-18 | 2012-11-14 | 中国工程物理研究院流体物理研究所 | Double-spectrum imaging device driven by laser to generate X-ray source |
-
2011
- 2011-09-05 CN CN2011203302664U patent/CN202330315U/en not_active Expired - Lifetime
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102323284A (en) * | 2011-09-05 | 2012-01-18 | 杭州电子科技大学 | A kind of device and method of X-ray fluorescence spectra quantitative test |
| CN102778294A (en) * | 2012-07-18 | 2012-11-14 | 中国工程物理研究院流体物理研究所 | Double-spectrum imaging device driven by laser to generate X-ray source |
| CN102778294B (en) * | 2012-07-18 | 2015-08-05 | 中国工程物理研究院流体物理研究所 | Laser Driven produces two optical spectrum imaging devices of X-ray source |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20120711 Effective date of abandoning: 20130522 |
|
| AV01 | Patent right actively abandoned |
Granted publication date: 20120711 Effective date of abandoning: 20130522 |
|
| RGAV | Abandon patent right to avoid regrant |