CN108398450A - Microbeam X-ray fluorescence analytical method based on combination X-ray capillary - Google Patents
Microbeam X-ray fluorescence analytical method based on combination X-ray capillary Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
A kind of Microbeam X-ray fluorescence analytical method based on combination X-ray capillary, includes the following steps:1) systematic optical axis calibration is carried out first with visible laser, the X-ray light pipe for sending out sightless X-ray radiation is moved into systematic optical axis after the completion of calibration;2) fluorescence detection microbeam is formed using based on combination X-ray capillary tube device;3) X-ray light is radiated on the combination X-ray capillary tube device, each X-ray capillary lens positioned at different location respectively focus its incident part X-ray light, the superposition of multiple focal spots ultimately forms X-ray detection microbeam, and is irradiated to the test sample on sample stage;4) X-ray detector is placed close to the sample on sample stage, collects second-order fluorescence caused by X-ray detection microbeam irradiation sample, and is sent into analysis of information collection module and is carried out fluorescence analysis.The present invention is provided simultaneously with high microcell resolution ratio and high detection sensitivity, and can carry out field assay.
Description
Technical field
The present invention relates to X-ray detection and imaging field, especially a kind of microbeam X based on combination X-ray capillary is penetrated
Line fluorescence analysis method.
Background technology
X-ray fluorescence (XRF, X-Ray Fluorescence) analysis system can be under normal pressure to various forms (solid-state/liquid
State/powder etc.) sample carries out simple and quick, high-resolution and lossless element quantitative measurment is analyzed.Numerous industries pair in recent years
More stringent requirements are proposed for the micro-zone analysis ability and detection sensitivity of XRF (for example microcell resolution ratio is required to reach micron, even
Sub-micrometer scale), therefore high-resolution, highly sensitive Microbeam X-ray fluorescence analytical method and system (micro-XRF) become and work as
Preceding research hotspot.
To obtain higher microcell resolution ratio, it usually needs be equipped with X-ray focusing device in system of fluorescence analysis.
It has been proposed that Fluorescence Spectrometer (the patent No. based on X-ray capillary tube device:201010180956.6), because X has been used to penetrate
Line capillary tube device is focused, and microcell resolution ratio obtains a degree of raising, but due to X-ray capillary tube device pair
The absorption of X-ray radiation so that detection counting rate is greatly lowered, and affects the detection of X-ray fluorescence analyzing system in turn
Sensitivity.Separately it has been proposed that a kind of energy-dispersion X-ray fluorescence spectrometer (patent No.:201010004423.2), it is sent out with X-ray
The primary X-ray that generating apparatus generates goes to irradiate secondary target, improves detection sensitivity, but apparatus structure and control device are multiple
Miscellaneous, microcell resolution ratio is not high.How high microcell resolution ratio and high detection sensitivity are obtained simultaneously, is current micro-beam X-ray fluorescence
Analysis method and system need the Key technique problem solved.In addition, using X-ray light pipe as x-ray radiation source, it is main to consider
Be analysis system/instrument miniaturization, therefore when solving above-mentioned Key technique problem, it is also desirable to take into account the light of system and
Ease for use.
Invention content
For the defect for overcoming the microcell resolution ratio and detectivity of existing X-ray fluorescence analyzing system not high enough, with
And complicated, bulky dimensions, it can not realize that portable deficiency, the present invention provide one kind and being provided simultaneously with high microcell resolution ratio simultaneously
And high detection sensitivity, and the miniaturization Microbeam X-ray fluorescence analytical method of field assay can be carried out.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of Microbeam X-ray fluorescence analytical method based on combination X-ray capillary, the system for realizing the method include
X-ray light pipe, visible laser, combination X-ray capillary tube device, sample stage and X-ray detector and its information collection point
Analyse module, the detected sample grade of the X-ray light pipe or visible laser with combination X-ray capillary tube device, sample stage
In in same optical axis, the X-ray detector is placed close to sample;The Microbeam X-ray fluorescence analytical method includes such as
Lower step:
1) because X-ray radiation is invisible, systematic optical axis calibration, the visible light lasers are carried out first with visible laser
Device is for calibrating, and after the completion of calibration, the X-ray light pipe for sending out sightless X-ray radiation is moved into systematic optical axis, while visible
Light laser removes systematic optical axis;
2) fluorescence detection microbeam is formed using based on combination X-ray capillary tube device, the X-ray detector is adopted with information
Set analysis module is connected;The combination X-ray capillary tube device includes 2 or more X-ray capillary lens and combination X-ray hair
Tubule machanical fastener, the X-ray capillary lens are a kind of X-ray light collecting devices based on reflection effect, can be to more
Wavelength X-ray radiation carries out two-dimension focusing, forms dotted focusing spot;X-ray capillary lens entrance end size is more than
Exit end size, the size of exit end to focal spot are known as the back focal length of X-ray capillary lens;The combination X-ray capillary
Pipe machanical fastener plays fixed X-ray capillary lens, and foundation combines the composite configuration of X-ray capillary tube device,
Its positioned inside simultaneously fixes 2 or more X-ray capillary lens;
3) X-ray light is radiated on the combination X-ray capillary tube device, is located at each X-ray hair of different location
Tubule lens respectively focus its incident part X-ray light, and the superposition of multiple focal spots ultimately forms X-ray detection microbeam,
And it is irradiated to the test sample on sample stage;
4) X-ray detector is placed close to the sample on sample stage, and it is tested to collect X-ray detection microbeam irradiation
Second-order fluorescence caused by sample, and be sent into analysis of information collection module and carry out fluorescence analysis.
Further, the system also includes horizontal guide rail and vertical guide rail, the vertical guide rail, combination X-ray capillaries
Device and sample stage are placed on horizontal guide rail successively horizontally moveablely, and the X-ray light pipe and visible laser are placed in vertical
On straight guide, the mechanical axis of the vertical guide rail and horizontal guide rail is mutually perpendicular to;In the step 1), the X-ray light pipe and
Visible laser is alternately moved in and out systematic optical axis by the track movement of vertical guide rail.
Further, include the identical X-ray capillary of (M+1) a parameter in the combination X-ray capillary tube device
Pipe lens, the M are positive integer and M >=1.The combination X-ray capillary tube device is centrosymmetric distribution along its optical axis, described
Combine the optical axis coincidence of zero level X-ray capillary lens in the optical axis and array of X-ray capillary tube device, the combination X-ray
The optical axis of capillary tube device with combine in non-zero order X-ray capillary lens optical axis included angle be θ, all non-zero order X-ray hairs
Tubule lens are arranged on the concentric circles being concentric with the optical axis, and the radius of the concentric circles is calculated according to following equation:
The concentric radius of circle r of incidence end1:r1≥l·tanθ+2a (1)
The concentric radius of circle r of exit end2:r2≥2b (2)
Wherein a is X-ray capillary lens entrance end radius, b is X-ray capillary lens exit end radius, l is X-ray hair
The length of tubule lens.
The layout structure of (M+1) a X-ray capillary lens in the combination X-ray capillary tube device so that all (M+
1) focal spot of a X-ray capillary lens focus is in same position, and is located on optical axis.
Distance of the sample stage away from the combination X-ray capillary tube device, the back focal length ruler with X-ray capillary lens
It is very little identical.The sample stage can be lifted, the translation of two dimensions, the angular deflection of two dimensions, the tune of totally 5 dimensions
Section.The adjusting of 5 dimensions is the accurate adjusting for carrying out position in order to opposed sample thereon so that from combination X-ray
The X-ray detection microbeam irradiation of capillary tube device outgoing is to tested region.
The present invention technical concept be:X-ray capillary lens are a kind of X-ray focusing devices based on reflection effect,
For its focused spot size tens to microns up to a hundred, height can be obtained by being focused to X-ray beam using X-ray capillary lens
Quality detection microbeam improves the microcell resolution ratio of system of fluorescence analysis of the present invention.
Iing is proposed novel combination X-ray capillary tube device, each X-ray capillary lens in combination focus respectively,
By combining the structure design of X-ray capillary tube device, can to combine (M+1) a capillary in X-ray capillary tube device
Pipe lens focus effectively improves the intensity of focal spot in identical focal spot position, and improves the counting rate of detection in turn, that is, improves this
The detectivity of invention system of fluorescence analysis.
In addition, X-ray capillary lens have and can carry out that two-dimension focusing and manufacture craft be simple, robustness to X-ray
It is good, can batch machining the advantages of, therefore be formed by that system of fluorescence analysis is compact-sized, average weight, be suitble to structure miniaturization
Analytical instrument can carry out field assay.
Beneficial effects of the present invention are mainly manifested in:1, using combination X-ray capillary tube device as X-ray fluorescence spectra
The focus device of instrument, while realizing high microcell resolution ratio and high detection sensitivity, wherein high microcell resolution ratio is by the list in combining
A X-ray capillary lens are realized, high detection sensitivity is then the Overlay that is focused by combination X-ray capillary to realize;
2, X-ray capillary lens can carry out two-dimension focusing to X-ray, be suitable for carrying out sample the applied field of spot scan analysis
Scape;3, combination X-ray capillary tube device have the advantages that manufacture craft is simple, robustness is good, can batch machining, therefore formed
System of fluorescence analysis is compact-sized, average weight, be suitble to structure miniaturized analytical instrument, field assay can be carried out.
Description of the drawings
Fig. 1 is that the present invention is based on the used analysis systems of Microbeam X-ray fluorescence analytical method of combination X-ray capillary
Structural schematic diagram, wherein 1 be X-ray light pipe, 2 be visible laser, 3 be horizontal guide rail, 4 be vertical guide rail, 5 be combination X
Ray capillary tube device, 6 be sample, 7 be sample stage, 8 be X-ray detector, 9 be analysis of information collection module.
Fig. 2 is that the present invention is based on X-ray capillary is combined in the Microbeam X-ray fluorescence analytical method of combination X-ray capillary
The structural schematic diagram of tube device and its machanical fastener (by taking M=4 as an example).
Fig. 3 is the A-A sectional views of Fig. 2.
Specific implementation mode
The invention will be further described below in conjunction with the accompanying drawings.
Referring to Fig.1~Fig. 3, a kind of Microbeam X-ray fluorescence analytical method based on combination X-ray capillary, described in realization
The system of method includes that X-ray light pipe 1, visible laser 2, combination X-ray capillary tube device 5, sample stage 7 and X-ray are visited
Survey device 8 and its analysis of information collection module 9, the X-ray light pipe or visible laser are equal and combine X-ray capillary device
Part, sample stage sample 6 be located in same optical axis, the X-ray detector close to sample place;The microbeam X
Ray fluorescence analysis method includes the following steps:
1) because X-ray radiation is invisible, systematic optical axis calibration, the visible light lasers are carried out first with visible laser
Device is for calibrating, and after the completion of calibration, the X-ray light pipe for sending out sightless X-ray radiation is moved into systematic optical axis, while visible
Light laser removes systematic optical axis;
2) fluorescence detection microbeam is formed using based on combination X-ray capillary tube device, the X-ray detector is adopted with information
Set analysis module is connected;The combination X-ray capillary tube device includes 2 or more X-ray capillary lens and combination X-ray hair
Tubule machanical fastener, the X-ray capillary lens are a kind of X-ray light collecting devices based on reflection effect, can be to more
Wavelength X-ray radiation carries out two-dimension focusing, forms dotted focusing spot;X-ray capillary lens entrance end size is more than
Exit end size, the size of exit end to focal spot are known as the back focal length of X-ray capillary lens;The combination X-ray capillary
Pipe machanical fastener plays fixed X-ray capillary lens, and foundation combines the composite configuration of X-ray capillary tube device,
Its positioned inside simultaneously fixes 2 or more X-ray capillary lens;
3) X-ray light is radiated on the combination X-ray capillary tube device, is located at each X-ray hair of different location
Tubule lens respectively focus its incident part X-ray light, and the superposition of multiple focal spots ultimately forms X-ray detection microbeam,
And it is irradiated to the test sample on sample stage;
4) X-ray detector is placed close to the sample on sample stage, and it is tested to collect X-ray detection microbeam irradiation
Second-order fluorescence caused by sample, and be sent into analysis of information collection module and carry out fluorescence analysis.
Further, the system also includes horizontal guide rail 3 and vertical guide rail 4, the vertical guide rail, combination X-ray capillarys
Tube device and sample stage are placed on horizontal guide rail successively horizontally moveablely, and the X-ray light pipe and visible laser are placed in
On vertical guide rail, the mechanical axis of the vertical guide rail and horizontal guide rail is mutually perpendicular to;In the step 1), the X-ray light pipe
And visible laser, systematic optical axis is alternately moved in and out by the track movement of vertical guide rail.
Further, include the identical X-ray capillary of (M+1) a parameter in the combination X-ray capillary tube device
Pipe lens, the M are positive integer and M >=1.The combination X-ray capillary tube device is centrosymmetric distribution along its optical axis, described
Combine the optical axis coincidence of zero level X-ray capillary lens in the optical axis and array of X-ray capillary tube device, the combination X-ray
The optical axis of capillary tube device with combine in non-zero order X-ray capillary lens optical axis included angle be θ, all non-zero order X-ray hairs
Tubule lens are arranged on the concentric circles being concentric with the optical axis, and the radius of the concentric circles is calculated according to following equation:
The concentric radius of circle r of incidence end1:r1 ≥l·tanθ+2a (1)
The concentric radius of circle r of exit end2:r2≥2b (2)
Wherein a is X-ray capillary lens entrance end radius, b is X-ray capillary lens exit end radius, l is X-ray hair
The length of tubule lens.
The layout structure of (M+1) a X-ray capillary lens in the combination X-ray capillary tube device so that all (M+
1) focal spot of a X-ray capillary lens focus is in same position, and is located on optical axis.
Distance of the sample stage away from the combination X-ray capillary tube device, the back focal length ruler with X-ray capillary lens
It is very little identical.The sample stage can be lifted, the translation of two dimensions, the angular deflection of two dimensions, the tune of totally 5 dimensions
Section.The adjusting of 5 dimensions is the accurate adjusting for carrying out position in order to opposed sample thereon so that from combination X-ray
The X-ray detection microbeam irradiation of capillary tube device outgoing is to tested region.
The X-ray detector is placed close to the sample on sample stage, collects X-ray detection microbeam irradiation detected sample
Second-order fluorescence caused by product, and be sent into analysis of information collection module and carry out fluorescence analysis, described information collection analysis module is logical
Interface is crossed with X-ray detector to be connected.
Claims (5)
1. a kind of Microbeam X-ray fluorescence analytical method based on combination X-ray capillary, which is characterized in that realize the method
System include X-ray light pipe, visible laser, combination X-ray capillary tube device, sample stage and X-ray detector and its
Analysis of information collection module, the X-ray light pipe or visible laser are and combination X-ray capillary tube device, sample stage
Sample is located in same optical axis, and the X-ray detector is placed close to sample;The MICRO-BEAM XRF ANALYSIS
Method includes the following steps:
1) because X-ray radiation is invisible, systematic optical axis calibration is carried out first with visible laser, the visible laser is used
After the completion of calibration, calibration, the X-ray light pipe for sending out sightless X-ray radiation is moved into systematic optical axis, while visible light swashs
Light device removes systematic optical axis;
2) fluorescence detection microbeam, the X-ray detector and information collection point are formed using based on combination X-ray capillary tube device
Module is analysed to be connected;The combination X-ray capillary tube device includes 2 or more X-ray capillary lens and combination X-ray capillary
Machanical fastener, the X-ray capillary lens are a kind of X-ray light collecting devices based on reflection effect, can be to multi-wavelength X
Ray radiation carries out two-dimension focusing, forms dotted focusing spot;X-ray capillary lens entrance end size is more than exit end
Size, the size of exit end to focal spot are known as the back focal length of X-ray capillary lens;The combination X-ray capillary machinery
Fastener plays fixed X-ray capillary lens, according to the composite configuration of combination X-ray capillary tube device, inside it
Position and hold 2 or more X-ray capillary lens;
3) X-ray light is radiated on the combination X-ray capillary tube device, is located at each X-ray capillary of different location
Lens respectively focus its incident part X-ray light, and the superposition of multiple focal spots ultimately forms X-ray detection microbeam, and shines
The test sample being mapped on sample stage;
4) X-ray detector is placed close to the sample on sample stage, collects X-ray detection microbeam irradiation sample
Generated second-order fluorescence, and be sent into analysis of information collection module and carry out fluorescence analysis.
2. the Microbeam X-ray fluorescence analytical method as described in claim 1 based on combination X-ray capillary, which is characterized in that
The system also includes horizontal guide rail and vertical guide rail, the vertical guide rail, combination X-ray capillary tube device and sample stage are successively
It is placed on horizontal guide rail horizontally moveablely, the X-ray light pipe and visible laser are placed on vertical guide rail, described vertical
The mechanical axis of guide rail and horizontal guide rail is mutually perpendicular to;In the step 1), the X-ray light pipe and visible laser pass through
The track movement of vertical guide rail is alternately moved in and out systematic optical axis.
3. the Microbeam X-ray fluorescence analytical method as claimed in claim 1 or 2 based on combination X-ray capillary, feature exist
In including the identical X-ray capillary lens of (M+1) a parameter in the combination X-ray capillary tube device, the M is
Positive integer and M >=1.The combination X-ray capillary tube device is centrosymmetric distribution along its optical axis, the combination X-ray capillary
The optical axis coincidence of zero level X-ray capillary lens in the optical axis and array of tube device, the light of the combination X-ray capillary tube device
Axis with combine in the optical axis included angles of non-zero order X-ray capillary lens be θ, all non-zero order X-ray capillary lens are arranged in
On the concentric circles being concentric with the optical axis, the radius of the concentric circles is calculated according to following equation:
The concentric radius of circle r of incidence end1:r1≥l·tanθ+2a (1)
The concentric radius of circle r of exit end2:r2≥2b (2)
Wherein a is X-ray capillary lens entrance end radius, b is X-ray capillary lens exit end radius, l is X-ray hair
The length of tubule lens.
4. the Microbeam X-ray fluorescence analytical method as claimed in claim 3 based on combination X-ray capillary, which is characterized in that
The layout structure of (M+1) a X-ray capillary lens in the combination X-ray capillary tube device so that all (M+1) a X are penetrated
The focal spot of line capillary lens focus is located in same position on optical axis.
5. the Microbeam X-ray fluorescence analytical method as claimed in claim 1 or 2 based on combination X-ray capillary, feature exist
In, distance of the sample stage away from the combination X-ray capillary tube device, the back focal length size phase with X-ray capillary lens
Together.The sample stage can be lifted, the translation of two dimensions, the angular deflection of two dimensions, the adjusting of totally 5 dimensions.
The adjusting of 5 dimensions is the accurate adjusting for carrying out position in order to opposed sample thereon so that from combination X-ray hair
The X-ray detection microbeam irradiation of tubule device outgoing is to tested region.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111473749A (en) * | 2020-04-22 | 2020-07-31 | 中国科学院上海应用物理研究所 | Online characterization method for inner surface shape of single capillary |
CN115389538A (en) * | 2022-08-09 | 2022-11-25 | 深圳市埃芯半导体科技有限公司 | X-ray analysis apparatus and method |
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Effective date of registration: 20230829 Address after: Room 2308, Building 8, Dream Apartment, Century City, Hangzhou Bay New Area, Ningbo, Zhejiang Province, 315400 Patentee after: Ningbo Shunshi Technology Co.,Ltd. Address before: The city Zhaohui six districts Chao Wang Road Hangzhou City, Zhejiang province 310014 18 Patentee before: JIANG University OF TECHNOLOGY |
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