CN110907483A - Three-dimensional confocal microbeam X-ray diffractometer - Google Patents
Three-dimensional confocal microbeam X-ray diffractometer Download PDFInfo
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- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
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Abstract
The invention relates to a three-dimensional confocal microbeam X-ray diffractometer, which comprises: the X-ray source system, the X-ray filter, the capillary tube converging X-ray lens, the capillary tube X-ray semi-transparent lens or the parallel beam lens, the goniometer, the three-dimensional sample stage, the X-ray energy spectrum detector, the control system and the computer; wherein, the sample is placed on a sample table; the X-ray source system, the X-ray filter and the capillary tube converging X-ray lens are positioned on the same straight line and are arranged on one side of the goniometer; the capillary tube semi-transparent lens or the parallel beam lens and the X-ray energy spectrum detector are positioned on the same straight line and are arranged on the other side of the goniometer; the X-ray energy spectrum detector is electrically connected with the computer; the control system is electrically connected with the three-dimensional sample stage, the goniometer and the computer. The three-dimensional confocal micro-beam X-ray diffraction and micro-beam energy dispersion X-ray fluorescence analysis device has two analysis modes, and can realize element and phase analysis of a small sample or a micro area on the surface of the sample or a certain depth inside the sample.
Description
Technical Field
The invention relates to an X-ray diffraction technology, in particular to a three-dimensional confocal microbeam X-ray diffractometer based on a capillary X-ray lens.
Background
Confocal X-ray spectroscopic analysis was an X-ray spectroscopic analysis technique proposed by russian scientists Gibson and Kumakhov in 1993 that enables three-dimensional non-destructive analysis of a sample. Confocal X-ray spectroscopy devices typically employ a combination of a capillary X-ray converging lens and a capillary X-ray semitransparent or parallel beam lens. The capillary X-ray converging lens is provided with a front focus and a rear focus and is used for converging an X-ray beam emitted by an X-ray source (an X-ray tube and the like) at the front focus into a micro focal spot with the size of dozens of microns to hundreds of microns; the capillary X-ray semi-transparent mirror or the parallel beam lens is combined with the X-ray detector for use, so that X-rays detected from the detection micro-elements are changed into quasi-parallel X-ray beams and then enter the X-ray detector. In the process, only the sample point to be measured in the area of the detection infinitesimal can be analyzed. Based on this feature of confocal X-ray spectroscopy, the technique can be applied to three-dimensional non-destructive X-ray diffraction analysis.
X-ray diffraction analysis is a method for performing nondestructive structural analysis of a substance by using the diffraction effect of X-rays in a crystalline substance. The principle is that when X-rays emitted from an X-ray source (such as an X-ray tube) are monochromatized and then incident on a surface of a sample with a certain interplanar spacing d, an X-ray detector receives the X-rays diffracted from the sample under the condition of meeting the bragg equation 2dsin theta-n lambda, and the interplanar spacing d is calculated according to the value of the diffraction angle theta, so that phase information of the crystal is obtained.
The conventional X-ray diffraction experimental apparatus is shown in fig. 1, and comprises an X-ray source system 1, a monochromator 2, X-ray collimation systems 3 and 4, a goniometer and sample holder 5, an X-ray detector 6, an electronics system 7, a computer 8, and the like. The X-ray source system 1 generally comprises an X-ray tube with power not lower than 2000W and a circulating water cooling system; most diffractometers are equipped with graphite curved crystals as monochromators 2; the X-ray collimation systems 3 and 4 generally comprise slit collimators with the width of 0.1-1 mm and the length of 5-30 mm; the goniometer and the sample holder 5 are structurally integrated, and a sample is fixed on the sample holder; the space size between the X-ray source system 1 and the sample and between the sample and the X-ray detector 6 are all larger than 200 mm; the X-ray detector 6 typically employs a NaI crystal detector.
The conventional X-ray diffraction experimental device at present has the following defects: (1) x-ray diffraction analysis and two-dimensional continuous scanning of micro-areas cannot be realized; (2) the chemical composition information and element depth distribution of the sample cannot be detected; (3) analysis of the depth distribution of the phase structure inside the sample cannot be performed.
Disclosure of Invention
Based on the characteristics of the prior art, the invention combines the X-ray diffraction technology and the capillary X-ray lens technology to develop an instrument which has two analysis modes of three-dimensional confocal microbeam X-ray diffraction analysis and three-dimensional confocal microbeam energy dispersion X-ray fluorescence analysis and can adapt to the analysis of the surface micro-area of a sample or the depth distribution of the phase structure and the chemical composition in the sample.
The invention is realized by the following technical scheme:
a three-dimensional confocal microbeam X-ray diffractometer comprising: the X-ray detector comprises an X-ray source system, an X-ray filter, a capillary X-ray converging lens, a capillary X-ray semi-transparent lens or a parallel beam lens, an X-ray energy spectrum detector, an angle gauge, a three-dimensional sample stage, a control system and a computer; wherein, a sample to be detected is placed on the three-dimensional sample table; the X-ray filter is arranged between the X-ray source system and the capillary X-ray converging lens; the X-ray source system and the capillary X-ray converging lens are arranged on one side of the goniometer, the capillary X-ray converging lens converges X-rays from the X-ray source system into micro-beam X-rays, and the included angle between the central line of the micro-beam X-rays and the surface of the three-dimensional sample stage is theta1(ii) a The X-ray energy spectrum detector and the capillary X-ray semi-transparent mirror or the parallel beam lens are arranged at the other side of the goniometer, and the X-ray energy spectrum detector and the capillary X-ray semi-transparent mirror or the parallel beam lens are arranged at the other side of the goniometerThe central line of the energy spectrum detector is superposed with the axis of the capillary X-ray semi-transparent mirror or the parallel beam lens and forms an included angle theta with the surface of the three-dimensional sample stage2(ii) a The rear focus of the capillary X-ray converging lens is superposed with the front focus of the capillary X-ray semi-transparent lens or the parallel beam lens to form a detection infinitesimal, the detection infinitesimal is positioned on the circle center of the goniometer, and the detection infinitesimal is also positioned at the point to be detected of the sample; the X-ray energy spectrum detector is electrically connected with the computer; the control system is respectively electrically connected with the goniometer, the three-dimensional sample stage and the computer.
Furthermore, the X-ray source system comprises a micro-focal spot X-ray tube with a focal spot diameter of 30-100 mu m and power of 30-50W, a temperature control device and a cooling fan or a point light source X-ray tube with a focal spot diameter of 1mm and power of 0.8-3 kW, and a circulating water cooling system.
Further, the X-ray energy spectrum detector is an SDD high-count X-ray energy spectrum detector or a 2D X ray surface detector.
Furthermore, the goniometer adopts a theta-theta structure and is controlled by a high-precision servo motor or a stepping motor.
Further, an encoder is mounted on the goniometer shaft to form a closed loop feedback system.
Furthermore, the diameter of an X-ray beam spot irradiated on the sample after the X-ray is converged by the capillary X-ray converging lens is 0.05-0.8 mm, and the distance from a point to be measured of the sample to the capillary X-ray converging lens is the back focal length of the capillary X-ray converging lens.
Furthermore, divergent X-rays emitted from the point to be measured of the sample enter the X-ray energy spectrum detector after being converged by the capillary X-ray semi-transparent mirror or the parallel beam lens, and the distance from the point to be measured of the sample to the capillary X-ray semi-transparent mirror or the parallel beam lens is the front focal length of the capillary X-ray semi-transparent mirror or the parallel beam lens.
Furthermore, the three-dimensional confocal microbeam X-ray diffractometer has two analysis modes of three-dimensional confocal micro-area X-ray diffraction analysis and three-dimensional confocal micro-area energy dispersion X-ray fluorescence analysis.
The technical scheme provided by the invention has the beneficial effects that:
1. the X-ray intensity of the point to be measured of the irradiated sample is improved by using a capillary X-ray converging lens;
2. the intensity of an X-ray diffraction peak is improved by utilizing parallel beam X-rays with high transmission efficiency at the center of a capillary X-ray converging lens;
3. realizing the scanning analysis of the two-dimensional element distribution and phase structure on the surface of the sample or the analysis of the depth distribution of the element and phase structure in the sample or the 3D analysis of the sample
4. The three-dimensional confocal micro-area energy dispersion X-ray fluorescence analysis mode provides reference information of element types for the identification process of the phase structure of the sample on the surface and depth distribution of the sample.
Drawings
Fig. 1 is an X-ray diffraction experimental apparatus in the prior art.
Fig. 2 is a schematic diagram of the present invention.
Description of the main reference numerals:
1, an X-ray source system; 2, a monochromator; 3. 4, an X-ray collimation system; 5, an angle gauge and a sample holder; 6, an X-ray detector; 7, an electronics system; 8, a computer; 9, an X-ray filter plate; 10, a capillary X-ray converging lens; 11, a capillary X-ray semi-transparent mirror or a parallel beam lens; 12, an X-ray energy spectrum detector; 13, an angle measuring instrument; 14, a three-dimensional sample stage; and 15, controlling the system.
Detailed Description
Referring to fig. 2, the present invention provides a three-dimensional confocal microbeam X-ray diffractometer, which comprises an X-ray source system 1, an X-ray filter 9, a capillary X-ray converging lens 10, a capillary X-ray semi-transparent lens or parallel beam lens 11, an X-ray energy spectrum detector 12, an angle measuring instrument 13, a three-dimensional sample stage 14, a control system 15 and a computer 8; the X-ray source system 1 comprises a micro focal spot X-ray tube with a focal spot diameter of 30-100 mm and power of 30-50W, a temperature control device and a heat dissipation fan or a point light source X-ray tube with a focal spot diameter of 1mm and power of 0.8-3 kW, and a circulating water cooling system; x-rayThe diameter of an X-ray beam spot irradiated on a sample by a capillary X-ray converging lens 10 is 0.05-0.8 mm, and the distance from a point to be measured of the sample to the capillary X-ray converging lens is 10-100 mm; the distance from the point to be measured of the sample to the capillary X-ray semi-transparent mirror or the parallel beam lens 11 is 10-100 mm; the goniometer 13 controlled by a high-precision servo motor or a stepping motor adopts a theta-theta structure1And theta2Can rotate independently and can also be linked in a certain angle relationship; the X-ray spectral detector 12 employs an SDD X-ray spectral detector or a 2D X ray-plane detector, into which electronics are integrated.
The invention adopts the solution shown in figure 2, and has two analysis modes of three-dimensional confocal micro-area X-ray diffraction analysis and three-dimensional confocal micro-area energy dispersion X-ray fluorescence analysis: the difference between the two modes is that when the X-ray source system 1 is in a three-dimensional confocal micro-area X-ray diffraction analysis mode, the target material is a copper target, X-rays firstly penetrate through an X-ray filter 9 and then are converged into micro-beam X-rays through a capillary X-ray converging lens 10, and a single-channel pulse analyzer in an X-ray energy spectrum detector 12 works; when the X-ray source system is in a three-dimensional confocal microbeam energy dispersive X-ray fluorescence analysis mode, the X-ray source system 1 is provided with a target material and is switched into a molybdenum target, X-rays are directly converged into microbeam X-rays through a capillary X-ray converging lens 10, and a multichannel pulse analyzer in an X-ray energy spectrum detector 12 works; the two modes are the same, a sample to be detected is placed on a three-dimensional sample table 12, X-rays emitted by an X-ray source system 1 are converged into micro-beam X-rays by a capillary X-ray converging lens 10 and then irradiate the micro-beam X-rays on the sample, the X-rays diffracted or excited from the sample are collected into an X-ray energy spectrum detector 12 through a capillary semi-transparent lens or parallel beam lens 11, a back focal point of the capillary X-ray converging lens 10 and a front focal point of the capillary semi-transparent lens or parallel beam lens 11 are overlapped at an X-ray focal spot to form a detection infinitesimal, only a point to be detected at the position of the detection infinitesimal on the surface or inside of the sample can be detected, and a detected signal is processed by an electronic system integrated with the X-ray energy spectrum detector and then displayed and stored in a computer. Can be controlled by a computer 8 according to requirements, and is mainly composed of a PLC, a servo motor or a stepping motor, a driver and the likeA control system 15 is prepared for controlling XYZ axes of the three-dimensional sample stage 14 and adjusting a point to be measured (a micro-area on the surface of the sample or a certain depth inside the sample) of the sample to be measured to be located at a detection micro-element; the goniometer 13 controlled by the servo motor is controlled to rotate, so as to change the included angle theta between the central line of the microbeam X-ray irradiating the sample and the surface of the three-dimensional sample table 141And an included angle theta between the central line of the X-ray energy spectrum detector 12 and the surface of the three-dimensional sample table 142And the measurement on different angles of the sample is realized.
While the foregoing is directed to the preferred embodiment of the present invention, the scope of the present invention is not limited thereto, and it will be appreciated by those skilled in the art that changes and modifications may be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents, and that such changes and modifications are to be considered as within the scope of the invention.
Claims (8)
1. A three-dimensional confocal microbeam X-ray diffractometer, the diffractometer comprising: the X-ray detector comprises an X-ray source system (1), an X-ray filter (9), a capillary X-ray converging lens (10), a capillary X-ray semi-transparent lens or parallel beam lens (11), an X-ray energy spectrum detector (12), an angle measuring instrument (13), a three-dimensional sample table (14), a control system (15) and a computer (8); wherein, a sample to be measured is placed on the three-dimensional sample table (14); the X-ray filter (9) is arranged between the X-ray source system (1) and the capillary X-ray converging lens (10); the X-ray source system (1) and the capillary X-ray converging lens (10) are installed on one side of the goniometer (13), the capillary X-ray converging lens (10) converges X-rays from the X-ray source system (1) into micro-beam X-rays, and the included angle between the central line of the micro-beam X-rays and the surface of the three-dimensional sample table (14) is theta1(ii) a The X-ray energy spectrum detector (12) and the capillary X-ray semi-transparent mirror or the parallel beam lens (11) are installed on the other side of the goniometer (13), the central line of the X-ray energy spectrum detector (12) is overlapped with the axis of the capillary X-ray semi-transparent mirror or the parallel beam lens (11) and forms an included angle theta with the surface of the three-dimensional sample table (14)2(ii) a The back focus of the capillary X-ray converging lens (10) andthe front focuses of the capillary X-ray semi-transparent mirror or the parallel beam lens (11) are overlapped to form a detection infinitesimal, the detection infinitesimal is positioned on the circle center of the goniometer (13), and a point to be measured of the sample is also positioned at the detection infinitesimal; the X-ray energy spectrum detector (12) is electrically connected with the computer (8); the control system (15) is respectively electrically connected with the goniometer (13), the three-dimensional sample table (14) and the computer (8).
2. The three-dimensional confocal microbeam X-ray diffractometer according to claim 1, wherein the X-ray source system (1) comprises a micro focal spot X-ray tube with a focal spot diameter of 30-100 μm and power of 30-50W, a temperature control device and a heat dissipation fan or a point light source X-ray tube with a focal spot diameter of 1mm and power of 0.8-3 kW, and a circulating water cooling system.
3. The three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, wherein the X-ray spectrum detector (12) is selected from the group consisting of an SDD high count X-ray spectrum detector and a 2D X ray plane detector.
4. A three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, characterized in that said goniometer (13) adopts a theta-theta configuration, controlled by high precision servomotors or stepper motors.
5. A three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, characterized in that said goniometer (13) is equipped with encoders on its axis to form a closed-loop feedback system.
6. The three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, wherein the diameter of the X-ray beam spot irradiated by the X-ray on the sample through the capillary X-ray converging lens (10) is 0.05-0.8 mm, and the distance from the point to be measured of the sample to the capillary X-ray converging lens (10) is the back focal length of the capillary X-ray converging lens (10).
7. The three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, wherein the divergent X-rays emitted from the point to be measured of the sample enter the X-ray energy spectrum detector (12) after being converged by the capillary X-ray semitransparent mirror or parallel beam lens (11), and the distance from the point to be measured of the sample to the capillary X-ray semitransparent mirror or parallel beam lens (11) is the front focal length of the capillary X-ray semitransparent mirror or parallel beam lens (11).
8. The three-dimensional confocal microbeam X-ray diffractometer as claimed in claim 1, wherein there are two analysis modes of three-dimensional confocal micro-area X-ray diffraction analysis and three-dimensional confocal micro-area energy dispersive X-ray fluorescence analysis.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111537537A (en) * | 2020-05-19 | 2020-08-14 | 北京市辐射中心 | Monochromatic confocal X-ray fluorescence spectrum analysis device based on laboratory X-ray source |
| CN112033988A (en) * | 2020-09-15 | 2020-12-04 | 北京师范大学 | Self-adaptive beam spot X-ray diffractometer |
| CN114720496A (en) * | 2022-06-08 | 2022-07-08 | 四川大学 | Full-field X-ray fluorescence imaging analysis or X-ray diffraction analysis device and method |
Citations (8)
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| CN112033988B (en) * | 2020-09-15 | 2022-04-12 | 北京师范大学 | Self-adaptive beam spot X-ray diffractometer |
| CN114720496A (en) * | 2022-06-08 | 2022-07-08 | 四川大学 | Full-field X-ray fluorescence imaging analysis or X-ray diffraction analysis device and method |
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