CN113848224A - A system for the identification of elements contained in a sample - Google Patents
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- CN113848224A CN113848224A CN202111191279.2A CN202111191279A CN113848224A CN 113848224 A CN113848224 A CN 113848224A CN 202111191279 A CN202111191279 A CN 202111191279A CN 113848224 A CN113848224 A CN 113848224A
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- 239000007787 solid Substances 0.000 claims abstract description 33
- 230000003287 optical effect Effects 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims description 20
- 238000003384 imaging method Methods 0.000 claims description 16
- 230000003595 spectral effect Effects 0.000 claims description 4
- 238000001228 spectrum Methods 0.000 abstract description 12
- 238000001514 detection method Methods 0.000 abstract description 10
- 230000001066 destructive effect Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 238000000921 elemental analysis Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000010884 ion-beam technique Methods 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010422 painting Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000002405 diagnostic procedure Methods 0.000 description 1
- 238000012631 diagnostic technique Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2255—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident ion beams, e.g. proton beams
- G01N23/2258—Measuring secondary ion emission, e.g. secondary ion mass spectrometry [SIMS]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/081—Investigating materials by wave or particle radiation secondary emission incident ion beam, e.g. proton
- G01N2223/0813—Investigating materials by wave or particle radiation secondary emission incident ion beam, e.g. proton incident ion beam and measuring X-rays [PIXE]
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/107—Different kinds of radiation or particles protons
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Abstract
本发明涉及一种样品所含元素的鉴定系统，包括：设置在同一光路的激光器、聚焦模块、固体靶、样品和X射线探测器；所述聚焦模块设置在所述激光器和所述固体靶之间；所述聚焦模块用于将所述激光器发出的激光进行聚焦；所述固体靶用于与经过所述聚焦模块聚焦后的激光发生相互作用，产生质子束；所述样品设置在所述固体靶和所述X射线探测器之间；所述样品用于在所述质子束轰击下，激发出X射线；所述X射线探测器用于根据所述X射线确定能量谱线以确定所述样品的元素种类。本发明能够实现对样品所含元素的无损和高质量检测。
The invention relates to an identification system for elements contained in a sample, comprising: a laser, a focusing module, a solid target, a sample and an X-ray detector arranged in the same optical path; the focusing module is arranged between the laser and the solid target the focusing module is used for focusing the laser light emitted by the laser; the solid target is used for interacting with the laser focused by the focusing module to generate a proton beam; the sample is arranged on the solid between the target and the X-ray detector; the sample is used to excite X-rays under the bombardment of the proton beam; the X-ray detector is used to determine energy spectrum lines according to the X-rays to determine the sample type of element. The invention can realize non-destructive and high-quality detection of the elements contained in the sample.
Description
Technical Field
The invention relates to the field of ion beam analysis, in particular to an identification system for elements contained in a sample.
Background
Ion beam analysis techniques are one of the powerful tools used in the field of material science, and although they are gaining importance in more and more fields, most ion beam analysis equipment still rely on conventional accelerator technology and have serious limitations in terms of portability, flexibility and detection performance. Particularly, in the field of cultural heritage, since the lack of technology and diagnostic method suitable for protecting and preserving cultural relics such as art works and monuments is currently hindered, the development of new technology and method capable of protecting or restoring the cultural heritage is urgently needed. These techniques need to be inexpensive and widely applicable to museums or repair centers, and solve special problems that conventional diagnostic techniques cannot solve.
Since the proton beams generated by the conventional accelerator are all of single energy, the dose is mainly deposited at a certain depth in the depth direction of the sample, and the elemental analysis method by using the single-energy proton beams to excite X-rays can only analyze the elements contained in the sample at the position. Analysis of a historical relic sample (such as ancient calligraphy and painting) with a multilayer structure by a traditional accelerator may lack a part of information.
Disclosure of Invention
The invention aims to provide an identification system for elements contained in a sample, so as to realize nondestructive and high-quality detection of the elements contained in the sample.
In order to achieve the purpose, the invention provides the following scheme:
a system for identifying elements contained in a sample, comprising: the device comprises a laser, a focusing module, a solid target, a sample and an X-ray detector which are arranged on the same optical path;
the focusing module is arranged between the laser and the solid target; the focusing module is used for focusing laser emitted by the laser; the solid target is used for interacting with the laser focused by the focusing module to generate a proton beam; the sample is disposed between the solid target and the X-ray detector; the sample is used for exciting X rays under the bombardment of the proton beam; the X-ray detector is used for determining an energy spectral line according to the X-ray so as to determine the element type of the sample.
Optionally, the X-ray detector is a reflective elliptic curved crystal spectrometer.
Optionally, the reflective elliptic curved crystal spectrometer comprises a crystal and an imaging plate; the crystal is used for reflecting the X-rays with different energies to different positions in space; the imaging plate is used for determining energy spectral lines according to different positions of the space.
Optionally, the focusing module is an off-axis parabolic mirror.
Optionally, the off-axis parabolic mirror is configured to focus a spot of the laser to 5 microns.
Optionally, the laser is a high-power femtosecond laser.
Optionally, the sample is disposed on an output optical path of a proton beam of the solid target; the distance between the solid target and the sample was 4 cm.
Optionally, the focused laser bombards the solid target at an angle of 30 degrees.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
according to the system for identifying the elements contained in the sample, the focusing module is arranged between the laser and the solid target; the focusing module is used for focusing laser emitted by the laser; the solid target is used for interacting with the laser focused by the focusing module to generate a proton beam; the sample is arranged between the solid target and the X-ray detector; the sample is used for exciting X rays under the bombardment of proton beams; the X-ray detector is used to determine an energy line from the X-rays to determine the elemental species of the sample. The method can acquire element information of different depths of a sample at one time by utilizing the characteristics of a specific wide energy spectrum of a proton beam accelerated by laser, and realize the chromatographic scanning of the sample. The proton beam accelerated by the laser is a pulse beam, enough X rays can be generated by one or more laser pulses, so that the elemental composition of the sample can be determined, the elemental analysis can be completed in a short time, and the sample is prevented from being damaged.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic diagram of a system for identifying elements contained in a sample according to the present invention;
FIG. 2 is an X-ray energy spectrum obtained from raw data and unscrambling acquired data from an imaging panel;
FIG. 3 is a flow chart of the operation of the system for identifying elements contained in a sample according to the present invention.
Description of the symbols:
1-laser, 2-laser, 3-off-axis paraboloidal mirror, 4-solid target, 5-proton beam, 6-sample, 7-X-ray, 8-reflection type elliptic curved crystal spectrometer, 9-crystal and 10-imaging plate.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide an identification system for elements contained in a sample, so as to realize nondestructive and high-quality detection of the elements contained in the sample.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1, the present invention provides a system for identifying elements contained in a sample, comprising: the device comprises a laser 1, a focusing module, a solid target 4, a sample 6 and an X-ray detector which are arranged on the same optical path.
The focusing module is arranged between the laser 1 and the solid target 4; the focusing module is used for focusing the laser 2 emitted by the laser 1; the solid target 4 is used for interacting with the laser focused by the focusing module to generate a proton beam 5; the sample 6 is arranged between the solid target 4 and the X-ray detector; the sample 6 is used for exciting X-rays 7 under the bombardment of the proton beam 5; the X-ray detector is arranged to determine an energy line from the X-rays 7 to determine the elemental species of the sample 6. Wherein the thickness of the solid target 4 is in the order of micrometers.
In practical application, the X-ray detector is a reflective elliptic curved crystal spectrometer 8; for detecting X-rays 7 excited by the proton beam 5. The reflection type elliptic curved crystal spectrometer 8 comprises a crystal 9 and an imaging plate 10; the crystal 9 is used for reflecting the X-rays 7 with different energies to different positions in space; the crystal 9 in the reflective elliptic curved crystal spectrometer 8 reflects the X-ray 7 with different energy to different positions in space, and the intensity of the X-ray 7 at different positions is recorded to obtain the energy spectrum information of the X-ray 7. The imaging plate 10 is used to determine energy lines from different positions of the space. The imaging plate 10 is an X-ray detection medium for recording signals of the X-rays 7 at different spatial positions.
In practical application, the focusing module is an off-axis parabolic mirror 3. Wherein the off-axis paraboloidal mirror 3 is used for focusing the light spot of the laser to 5 microns.
In practical applications, the laser 1 is a high power femtosecond laser. The laser 1 serves as a drive source for the proton beam 5 of the entire apparatus.
In practical application, the sample 6 is arranged on the output light path of the proton beam 5 of the solid target 4; the distance between the solid target 4 and the sample 6 is 4 cm.
In practical applications, the focused laser strikes the solid target 4 at an angle of 30 degrees.
As shown in FIG. 3, the steps of analyzing the elements of the sample by using the system for identifying the elements contained in the sample provided by the present invention are as follows:
step 1: laser accelerated proton beam
Laser generated by a high-power femtosecond laser focuses a light spot to 5 microns through an off-axis paraboloid mirror and bombards the solid target in the figure 1 at 30 degrees, and the laser interacts with the solid to generate a proton beam with energy of MeV magnitude. The proton beam has the characteristics of large divergence angle and wide energy spectrum.
Step 2: proton beam excitation of X-rays
A sample needing element component identification is placed at a position 4cm right behind a solid target, and is generally a metal product, a ceramic product and the like in a cultural relic archaeology. The MeV-level proton beam accelerated by the front laser is incident on the sample and collides with atoms in the sample, in the collision, the proton can excite K shell layer electrons of atoms of the sample to generate holes on an electron track, and the L shell layer electrons of the atoms emit characteristic X rays when filling the holes.
And step 3: x-ray detection
In the present invention, a reflection-type elliptic curved crystal spectrometer is used as an X-ray detector. The reflection type elliptic curved crystal spectrometer consists of a crystal and an imaging plate. During detection, the position of the proton beam spot (namely the position of generating the X-ray) is positioned at one focus of the ellipse, and the X-ray is converged at the other focus of the ellipse after being reflected by the crystal. According to the bragg formula 2dsin θ ═ n λ (n ═ 1,2,3, …), where d is the interplanar spacing, θ is the angle between the incident X-ray and the corresponding interplanar, λ is the wavelength of the X-ray, and n is the number of diffraction orders. X-rays with different wavelengths are reflected by the crystal from different angles, so that the X-rays are scattered behind the focus point, and the X-rays are received at different positions of the imaging plate by selecting the imaging plate as an X-ray detection medium.
And 4, step 4: analysis of elemental composition from X-ray energy spectra
As shown in fig. 2(a), a stripe-shaped characteristic line is formed on the imaging plate, and the position of the line on the imaging plate corresponds to the energy of the characteristic X-ray, and the imaging plate corresponds to the energy from low to high from top to bottom, and the detectable energy is in the range of 1keV to 10 keV. The imaging plate is scanned to obtain a pixel matrix, an X-ray energy spectrum as shown in fig. 2(b) can be drawn according to the pixel values, the peak corresponds to the characteristic X-ray, and then the energy of the characteristic X-ray is analyzed to determine what element is contained in the sample. It can be seen from fig. 2 that the energy values corresponding to the two characteristic X-rays are 4.5keV and 4.9keV, which are consistent with the empirical value of the characteristic X-ray of titanium element, indicating that the sample detected this time contains titanium element. The types of the contained elements are identified by comparing the energy value of the characteristic X-ray on the X-ray energy spectrum with the empirical value of each element, and the element information of different depths of the sample can be obtained at one time by combining the characteristic that the proton beam accelerated by the laser has a wide energy spectrum, so that the chromatographic scanning of the sample to be detected is realized.
The analysis technology using the traditional accelerator is that the beam current with the magnitude of mum or mm is generally scanned, the divergence angle of the proton beam accelerated by laser is large, and the proton beam spot with the magnitude of cm is generated on a sample to be measured by irradiation. In practical archaeological applications, such a large area of the beam spot may enable large scale scanning of the sample. For example, a cultural relic of a certain dynasty is screened from a stack of cultural relics to be detected, the cultural relics contain certain specific elements, and the target cultural relics can be quickly found by using the large-area beam spot to exclude other irrelevant cultural relics.
Laser plasma acceleration is an emerging accelerator discipline that has developed vigorously in the last fifty years. The traditional particle acceleration is to accelerate and focus charged particles by using a radio frequency electromagnetic field, and the development is slow in recent years because materials have the limit of an ionization breakdown threshold. Compared with the traditional accelerator, the laser plasma accelerating method generates a MeV-magnitude proton beam, the accelerating gradient of the laser plasma accelerating is improved by more than 3 magnitude orders, the size of the accelerator can be reduced, the miniaturization and the mesa are realized, and the construction cost is greatly reduced.
The conventional accelerator usually needs to irradiate the cultural relic sample for a long time, so that the sample is easy to damage. The proton beam accelerated by the laser is a pulse beam which can generate 10 as soon as13The proton can generate enough X-rays through one or more laser pulses, and the elemental composition of the sample is judged by measuring the characteristic X-ray energy, so that the elemental analysis of the cultural relic is realized in a short time, and the cultural relic is not damaged.
Since the proton beams generated by the conventional accelerator are all of single energy, the dose is mainly deposited at a certain depth in the depth direction of the sample, and the elemental analysis method by using the single-energy proton beams to excite X-rays can only analyze the elements contained in the sample at the position. Analysis of a historical relic sample (such as ancient calligraphy and painting) with a multilayer structure by a traditional accelerator may lack a part of information. The laser accelerated proton beam has the characteristic of wide energy spectrum, and can obtain the element information of samples at different depths at one time, thereby realizing the chromatographic scanning of the sample to be detected.
In the detection of X-rays, a conventional accelerator continuously bombards a sample, and a semiconductor detector is used to detect the X-ray energy spectrum excited by a proton beam. Laser-accelerated proton beams have an ultrafast temporal behavior, so conventional semiconductor detectors are not suitable in such settings due to the time response limitations of the electronics. The X-ray detector adopts a reflection type elliptic curved crystal spectrometer, and is specially used for exciting X-ray energy spectrum detection by a proton beam accelerated by laser.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (8)
1. A system for identifying elements contained in a sample, comprising: the device comprises a laser, a focusing module, a solid target, a sample and an X-ray detector which are arranged on the same optical path;
the focusing module is arranged between the laser and the solid target; the focusing module is used for focusing laser emitted by the laser; the solid target is used for interacting with the laser focused by the focusing module to generate a proton beam; the sample is disposed between the solid target and the X-ray detector; the sample is used for exciting X rays under the bombardment of the proton beam; the X-ray detector is used for determining an energy spectral line according to the X-ray so as to determine the element type of the sample.
2. The system of claim 1, wherein the X-ray detector is a reflection ellipsometer.
3. The system for identifying elements contained in a sample according to claim 2, wherein said reflective ellipsometer comprises a crystal and an imaging plate; the crystal is used for reflecting the X-rays with different energies to different positions in space; the imaging plate is used for determining energy spectral lines according to different positions of the space.
4. The system of claim 1, wherein the focusing module is an off-axis parabolic mirror.
5. The system of claim 4, wherein the off-axis parabolic mirror is configured to focus a spot of the laser light to 5 microns.
6. The system for identifying elements contained in a sample according to claim 1, wherein said laser is a high power femtosecond laser.
7. The system for identifying elements contained in a sample according to claim 1, wherein the sample is provided on an output optical path of a proton beam of the solid target; the distance between the solid target and the sample was 4 cm.
8. The system of claim 1, wherein the focused laser strikes the solid target at an angle of 30 degrees.
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2021
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| GB908182A (en) * | 1958-03-26 | 1962-10-17 | Nat Res Dev | Improvements in the analysis of specimens by electromagnetic radiation |
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| CN202522529U (en) * | 2011-12-21 | 2012-11-07 | 上海激光等离子体研究所 | High-resolution X-ray elliptical bent crystal spectrometer |
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