CN112924480A - Measuring device for synchronous radiation X-ray and asynchronous infrared light combined use - Google Patents
Measuring device for synchronous radiation X-ray and asynchronous infrared light combined use Download PDFInfo
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- CN112924480A CN112924480A CN202110112178.5A CN202110112178A CN112924480A CN 112924480 A CN112924480 A CN 112924480A CN 202110112178 A CN202110112178 A CN 202110112178A CN 112924480 A CN112924480 A CN 112924480A
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- 230000001360 synchronised effect Effects 0.000 title claims description 12
- 230000005855 radiation Effects 0.000 title abstract description 6
- 230000003287 optical effect Effects 0.000 claims abstract description 80
- 238000006073 displacement reaction Methods 0.000 claims description 23
- 230000005469 synchrotron radiation Effects 0.000 claims description 19
- 239000000463 material Substances 0.000 claims description 13
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 7
- 229910001634 calcium fluoride Inorganic materials 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 239000010409 thin film Substances 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 9
- 238000002474 experimental method Methods 0.000 abstract description 6
- 238000002329 infrared spectrum Methods 0.000 abstract description 6
- 238000004891 communication Methods 0.000 abstract description 3
- 238000000235 small-angle X-ray scattering Methods 0.000 abstract 1
- 238000004566 IR spectroscopy Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 2
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 description 1
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 1
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Classifications
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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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/201—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials by measuring small-angle scattering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention relates to a measuring device for synchronously radiating X rays and asynchronously radiating infrared light, which comprises infrared equipment for emitting infrared light, wherein a first optical assembly, a sample cell, a second optical assembly and an infrared detector are sequentially arranged along the direction of the infrared light, the infrared equipment is connected with an external trigger line, the external trigger line is connected with an X ray detector through a converter, and the infrared detector and the X ray detector are both in communication connection with a control device. The invention can realize the simultaneous radiation SAXS detection and the infrared spectrum detection of the sample under the same external field condition, ensure the intensity of infrared light and improve the reliability of the experiment.
Description
Technical Field
The invention relates to the technical field of in-situ testing, in particular to a measuring device combining synchrotron radiation X rays and asynchronous infrared light, which is used for in-situ measuring related samples.
Background
Synchrotron radiation X-ray small angle scattering (SAXS) refers to a phenomenon that X-rays obtained by electron acceleration enter the surface of a sample at a small angle ranging from 0 DEG to 5 DEG and interact with electrons in the sample to shift in each direction, and a nano-scale microstructure of the sample can be researched. Infrared spectroscopy (IR) refers to the fact that infrared light is irradiated on a sample, when the vibration frequency of a certain group in the sample is the same as the frequency of the irradiated infrared light, resonance is generated, the sample can selectively absorb electromagnetic radiation in an infrared light region with a certain frequency, and the IR is generally used for researching the molecular structure of the sample, and performing qualitative identification, phase analysis and quantitative determination on the sample.
At present, the existing X-ray scatterometer and infrared equipment can finish separate measurement on a sample, but because the synchrotron radiation X-ray has higher intensity, collimation, polarization and resolution compared with the common X-ray, the existing measuring device can not meet the requirements of carrying out synchrotron radiation SAXS detection and infrared spectrum detection on the sample under the same external field condition.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a measuring device combining synchrotron radiation X-rays and asynchronous infrared light, which can perform synchrotron radiation SAXS detection and infrared spectrum detection on a sample under the same external field condition.
The invention provides a measuring device for synchronously radiating X rays and asynchronously radiating infrared light, which comprises infrared equipment for emitting infrared light, wherein a first optical assembly, a sample cell, a second optical assembly and an infrared detector are sequentially arranged along the direction of the infrared light, the infrared equipment is connected with an external trigger line, the external trigger line is connected with an X ray detector through a converter, and the infrared detector and the X ray detector are both in communication connection with a control device.
Furthermore, an infrared light exit window is arranged on the infrared equipment.
Preferably, the infrared light exit window is made of calcium fluoride.
Further, the first optical assembly comprises a plane reflector and a first off-axis parabolic reflector which are oppositely arranged, the plane reflector is fixed on the right-angle optical adjusting frame through an optical extension rod, the first off-axis parabolic reflector is fixed on the first optical rotary adjusting frame, and the first optical rotary adjusting frame is fixed on the first displacement table.
Further, the second optical assembly comprises a second off-axis parabolic reflector and a third off-axis parabolic reflector which are oppositely arranged, the second off-axis parabolic reflector is fixed on a second optical rotary adjusting frame, the second optical rotary adjusting frame is fixed on a second displacement table, the third off-axis parabolic reflector is fixed on a third optical rotary adjusting frame, and the third optical rotary adjusting frame is fixed on a third displacement table.
Further, the sample cell is located between the first off-axis parabolic mirror and the second off-axis parabolic mirror, and the first off-axis parabolic mirror, the sample cell and the second off-axis parabolic mirror are located in the same horizontal straight line.
Preferably, the first displacement table, the second displacement table and the third displacement table are all three-dimensional displacement tables.
Preferably, the sample cell is configured to hold a film material or a sample that is a liquid.
Further, the sample cell is provided with a first incident window and a first emergent window for incidence and emergence of X rays, and a second incident window and a second emergent window for incidence and emergence of infrared light.
Preferably, the material of the first incident window and the first exit window is single crystal diamond, and the material of the second incident window and the second exit window is calcium fluoride.
The measuring device can synchronously irradiate the synchronous radiation X-ray and the infrared light to the sample through one-time triggering, thereby realizing the synchronous radiation SAXS detection and the infrared spectrum detection of the sample under the same external field condition. In addition, the infrared light path and the infrared detector are arranged outside the infrared device, so that the intensity of infrared light can be ensured by adjusting each optical device while the X-ray light path and the infrared light path can jointly act on a sample, and the reliability of an experiment is improved.
Drawings
Fig. 1 is a schematic structural diagram of a measuring apparatus for simultaneous use of synchrotron radiation X-rays and asynchronous infrared light according to a preferred embodiment of the present invention.
Fig. 2 is a schematic view of the working principle of the measuring device of fig. 1.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
As shown in fig. 1, the measuring apparatus for simultaneous irradiation of X-ray and asynchronous infrared light according to a preferred embodiment of the present invention is directed to a thin film material or a liquid sample. The device is placed on a roughly rectangular operating platform and comprises an infrared device 1, wherein the infrared device 1 emits infrared light, and a first optical assembly 2, a sample cell 3, a second optical assembly 4 and an infrared detector 5 are sequentially arranged along the path of the emitted infrared light. The infrared device 1 is connected to an external trigger line 6, which external trigger line 6 is connected to an X-ray detector 8 via a BNC converter 7. Furthermore, the infrared detector 5 and the X-ray detector 8 are both connected in communication with a control device 9.
The infrared device 1 is provided with an infrared light exit window 11, and according to the wavelength and the tolerance required by the experiment, the infrared light exit window 11 can be made of materials such as calcium fluoride, zinc selenide, zinc sulfide, magnesium fluoride, lithium fluoride, gallium arsenide, monocrystalline germanium or monocrystalline silicon. In this embodiment, calcium fluoride which absorbs less infrared light is adopted in the infrared light exit window 11 to improve the accuracy of the experiment.
The first optical assembly 2 comprises a planar mirror 21 and a first off-axis parabolic mirror 22, which are oppositely disposed. The plane mirror 21 is fixed on an angle optical adjustment frame 24 through an optical extension rod 23, so that the plane mirror 21 forms an angle of 45 degrees with the infrared light path. The plane mirror 21 serves to change the direction of the infrared light path and focus the infrared light to ensure the intensity of the infrared light to the maximum extent. The first off-axis parabolic reflector 22 is fixed on the first optical rotary adjusting frame 25, and the first optical rotary adjusting frame 25 is fixed on the first displacement table 26, so that the first optical rotary adjusting frame 25 can finely adjust the angle of the first off-axis parabolic reflector 22 in a vertical plane, and finely adjust the position of the first off-axis parabolic reflector 22 by moving the first displacement table 26, so that the infrared light path can be quickly adjusted, the intensity of infrared light is ensured to be maximum, and the reliability of an experiment is improved.
The second optical assembly 4 includes a second off-axis parabolic mirror 41 and a third off-axis parabolic mirror 42, which are oppositely disposed, the second off-axis parabolic mirror 41 is fixed on a second optical rotation adjusting frame 43, the second optical rotation adjusting frame 43 is fixed on a second displacement table 44, the third off-axis parabolic mirror 42 is fixed on a third optical rotation adjusting frame 45, and the third optical rotation adjusting frame 45 is fixed on a third displacement table 46. The functions of the optical rotary adjusting frames 43 and 45 and the displacement platforms 44 and 46 are the same as those of the optical rotary adjusting frame 25 and the displacement table 26, and will not be described again. The displacement tables 26, 44, and 46 are three-dimensional displacement tables, and can move up and down, left and right, and back and forth.
A thin film material or a sample of liquid is placed in the sample cell 3, and the sample is irradiated with the synchrotron radiation X-rays emitted from an external device (not shown) and the infrared light from the infrared device 1. In order to make the infrared light energy and the X-rays simultaneously irradiate the same sample and weaken the influence of the infrared light attenuation as much as possible, the sample cell 3 is arranged between the first off-axis parabolic reflector 22 and the second off-axis parabolic reflector 41, and the first off-axis parabolic reflector 22, the sample cell 3 and the second off-axis parabolic reflector 41 are approximately in the same horizontal straight line. The sample cell 3 has a first entrance window 31, a first exit window 32, a second entrance window 33, and a second exit window 34, the first entrance window 31 and the first exit window 32 are used for entrance and exit of X-rays, and the second entrance window 33 and the second exit window 34 are used for entrance and exit of infrared light. In the present embodiment, the material of the first incident window 31 and the first exit window 32 is single crystal diamond, which can ensure that the X-ray transmittance is higher than 0.65 and there is no interference of scattered signals on the premise of ensuring the mechanical strength. The material of the second entrance window 33 and the second exit window 34 uses calcium fluoride to reduce absorption of infrared light. In this embodiment, the material of the main body of the cuvette 3 (excluding the four windows) is stainless steel which is low cost, high strength and easy to process.
The X-ray light path inside the sample cell 3 is always a transmission type light path, and the infrared light path is a transmission or reflection type light path, and can be selected according to actual needs. In addition, two optical paths can be designed by adjusting the positions of the four windows. For example, when the infrared optical path is selected as a transmission optical path, two optical paths may be designed to meet at the same sample point; when the infrared light path is selected as a reflection light path, the two light paths can be designed at different positions at the same height (excluding the effect of gravity), and a uniform homogeneous sample can be tested at the moment.
The infrared detector 5 is configured to receive the infrared signal reflected from the third off-axis parabolic mirror 42 and transmit the received infrared signal to the control device 9, which is, for example, a computer. The control device 9 monitors the infrared signal in real time through the built-in software ominic, and adjusts the displacement tables 26, 44, 46 up and down, left and right, and front and back, so that the voltage on the software reaches the saturation voltage, and the intensity of the infrared light is maximum at this time. In order to be able to receive the infrared signal, the infrared detector 5 is mounted on the fourth moving platform 51 such that the height of the infrared detector 5 can be adjusted.
The external trigger line 6 enables the X-ray detector 8 to trigger the infrared device 1 to start operating when it receives the X-ray scatter signal. Because the scattering signal received by the X-ray detector 8 is a rising edge signal, and an external falling edge signal is required to trigger the infrared device 1 to operate, a BNC converter 7 is arranged between the infrared device 1 and the X-ray detector 8 to convert the rising edge signal of the X-ray detector 8 into a falling edge signal capable of triggering the infrared device 1 to operate, thereby achieving the purpose of synchronous triggering.
The operation of the measuring device of the present invention will be described with reference to fig. 2.
First, synchrotron radiation X-rays are generated by an external device, the X-rays are incident on the surface of the experimental sample from the first incident window 31 of the sample cell 3 at a small angle, and the X-rays interact with electrons in the sample and are scattered. The scattered X-rays pass through the first exit window 32 and reach the X-ray detector 8, and after the X-ray detector 8 receives the scattered signals, the scattered signals can be analyzed to obtain the microstructure of the sample. At the same time, the X-ray detector 8 receiving the scatter signal triggers the infrared device 1 to emit infrared light via the BNC converter 7. After being emitted from the infrared light emitting window 11 of the infrared device 1, the infrared light sequentially passes through the plane reflector 21 and the first off-axis parabolic reflector 22, and then irradiates the surface of the sample from the second incident window 33 of the sample cell 3, so that the infrared light resonates with some groups of the sample. The generated infrared light passes through the second exit window 34, sequentially passes through the second off-axis parabolic mirror 41 and the third off-axis parabolic mirror 42, and then enters the infrared detector 5. The infrared detector 5 analyzes the received infrared signal to complete the infrared spectrum detection of the sample, thereby completing the combined experiment of the synchronous radiation SAXS and the infrared spectrum of the sample.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (10)
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| CN202110112178.5A CN112924480B (en) | 2021-01-27 | 2021-01-27 | Measuring device for synchronous radiation X-ray and asynchronous infrared light combined use |
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| CN202110112178.5A CN112924480B (en) | 2021-01-27 | 2021-01-27 | Measuring device for synchronous radiation X-ray and asynchronous infrared light combined use |
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| CN112924480B CN112924480B (en) | 2023-04-07 |
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| CN112924480B (en) | 2023-04-07 |
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