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CN-121994839-A - XAFS automatic sample changing device integrating light intensity management and operation method

CN121994839ACN 121994839 ACN121994839 ACN 121994839ACN-121994839-A

Abstract

The invention relates to the technical field of synchrotron radiation experiments, in particular to an XAFS automatic sample changing device integrating light intensity management and an operation method thereof, comprising a filter wheel, a sample table and a control component, wherein the filter wheel and the sample table form an integrated structure for the XAFS experiment, so that a sample switching process and an incident X-ray light intensity adjusting process are mutually matched, and the light intensity management is realized in the automatic sample changing process; by introducing an automatically switchable filter wheel, a sample table capable of being positioned accurately and a temperature monitoring and remote control system which is cooperated with the filter wheel and the sample table in a synchronous radiation X-ray light path, photon flux incident on a sample can be optimized in real time according to the signal state of a detector and the thermal load of the filter, and the stability, the repeatability and the safety of an XAFS experiment are obviously improved while signal saturation and equipment overheating are avoided, so that manual intervention is reduced, debugging time is shortened, and the operation efficiency of the whole beam line is improved.

Inventors

  • CHEN JINGSHUAI
  • Qian Baohao
  • SUN SONG
  • WEI YUXUE
  • CAI MENGDIE

Assignees

  • 安徽大学

Dates

Publication Date
20260508
Application Date
20260228

Claims (10)

  1. 1. The XAFS automatic sample changing device integrated with light intensity management is characterized by comprising a light filter wheel (1), a sample table (2) and a control component, wherein the light filter wheel (1) is arranged on a synchronous radiation X-ray transmission path and is used for selectively attenuating passing X-rays, the sample table (2) is used for carrying a plurality of samples (12) and realizing that different samples (12) sequentially enter an X-ray irradiation area through position switching, the control component is respectively and electrically connected with the light filter wheel (1) and the sample table (2) and is used for coordinating and controlling the working states of the light filter wheel (1) and the sample table (2), and the light filter wheel (1) and the sample table (2) form an integrated structure for XAFS experiments, so that the sample switching process and the incident X-ray light intensity adjusting process are mutually matched, and light intensity management is realized in the automatic sample changing process.
  2. 2. The XAFS automatic sample changing device for integrated light intensity management according to claim 1, wherein a plurality of sample mounting holes (3) are provided on the sample stage (2), each sample mounting hole (3) is used for mounting one sample (12), and the sample stage (2) rotates to enable different sample mounting holes (3) to sequentially enter the X-ray irradiation position.
  3. 3. The XAFS automatic sample exchange device integrated with light intensity management according to claim 2, wherein the sample stage (2) is a turntable structure rotating around a fixed axis, and a plurality of sample mounting holes (3) are distributed along the circumference of the sample stage (2).
  4. 4. The XAFS automatic sample exchange device integrated with light intensity management according to claim 1, wherein a plurality of filter clamping grooves (4) are provided on the filter wheel (1), and the filter clamping grooves (4) are used for installing filters or light barriers (13) to form different X-ray attenuation states.
  5. 5. The XAFS automatic sample exchange device integrated with light intensity management according to claim 4, wherein the filter card slots (4) are detachable structures, so that different filter card slots (4) can be replaced according to experimental requirements.
  6. 6. The XAFS automatic sample exchange device integrated with light intensity management according to claim 4, wherein a thermocouple (5) is provided on at least one filter card slot (4), and the thermocouple (5) is used for detecting the temperature of the filter during X-ray irradiation.
  7. 7. The XAFS automatic sample device integrated with light intensity management according to claim 6, wherein the filter wheel (1) is provided with a condensed water interface (6) for introducing a cooling medium for cooling the filters.
  8. 8. The XAFS automatic sample exchange device integrated with light intensity management according to claim 1, characterized in that the device is provided with a zeroing control key (8) for returning the filter wheel (1) and/or the sample stage (2) to a preset reference position.
  9. 9. The XAFS automatic sample-changing device for integrated light intensity management according to claim 1, characterized in that the device is adapted to be arranged on an X-ray path after a synchrotron radiation light source (16) via a bicrystal monochromator (15), the sample (12) being located between a front ionization chamber (14) and a rear ionization chamber (11).
  10. 10. A method of operation using the light intensity management integrated XAFS automatic sample exchange device of any one of claims 1-9, comprising the steps of: S1, setting a filter wheel (1) and a sample stage (2) in an X-ray light path formed by a synchrotron radiation light source (16) through a bicrystal monochromator (15), wherein the filter wheel (1) is used for adjusting the light intensity of incident X-rays, and the sample stage (2) is used for bearing a plurality of samples (12); S2, controlling the sample table (2) to rotate through the control assembly, so that samples (12) installed in different sample installation holes (3) sequentially enter the X-ray irradiation position, and realizing automatic switching of the samples; S3, in the sample switching process, the control component controls the filter wheel (1) to switch different filter clamping grooves (4) so as to change the state of the filter or the light barrier (13) in an X-ray light path, thereby adjusting the intensity of the X-ray incident to the sample (12); s4, in the X-ray irradiation process, utilizing a thermocouple (5) arranged on the optical filter clamping groove (4) to acquire temperature information of the optical filter, and cooling the optical filter through a condensed water interface (6) when the temperature reaches a preset threshold value; S5, the sample switching step and the light intensity adjusting step are cooperatively carried out in the same experimental flow, so that the testing efficiency and the safety of the sample and the optical filter are considered in the continuous XAFS testing process.

Description

XAFS automatic sample changing device integrating light intensity management and operation method Technical Field The invention relates to the technical field of synchrotron radiation experiments, in particular to an XAFS automatic sample changing device integrating light intensity management and an operation method. Background The synchronous radiation is electromagnetic wave with high intensity and wide frequency spectrum released along tangential direction when electrons moving in the energy storage ring at near light speed deflect in the magnetic field. The light source has excellent characteristics of high brightness, high collimation, wide frequency spectrum, polarization, pulse time structure and the like, becomes an indispensable tool for basic leading edge scientific research, and promotes the breakthrough development of a plurality of subjects such as material science, chemistry, physics, life science, environmental science and the like. Among the numerous experimental methods of synchrotron radiation, X-ray absorption fine structure spectroscopy is a unique structural characterization technique. The XAFS technique is independent of long range order structure, and can accurately detect local atomic structure information around the absorbed atoms, including the kind, number, distance, disorder, etc. of the coordinated atoms. The XAFS plays a vital role in the fields of research on amorphous materials, catalyst active centers, ionic species in solution, charge and discharge processes of battery electrode materials, migration and conversion of environmental pollutants and the like. The study objects in these fields often lack perfect crystal structures, while XAFS technology provides just a strong ability to resolve its "chemical environment" on an atomic scale. In the existing synchronous radiation XAFS experiment, the dynamic range mismatch is easy to occur due to the fact that the incident light intensity is scanned along with energy and the beam current fluctuates, the problems of saturation, linear distortion or insufficient signal to noise ratio of detection signals are often caused by untimely manual filter replacement or inaccurate adjustment, and further deviation and repeatability of absorption spectrum data are reduced, meanwhile, the temperature rise of an optical filter is accumulated due to high-flux irradiation, thermal drift, deformation and even failure are easy to occur when effective monitoring and cooling are lacking, the light path is unstable, the experiment is interrupted, and the maintenance cost is increased. Disclosure of Invention Aiming at the defects existing in the prior art, the invention provides an integrated light intensity management XAFS automatic sample changing device and an operation method, and by introducing an automatically switchable filter wheel, a sample table capable of being precisely positioned and a temperature monitoring and remote control system which is cooperated with the filter wheel and the sample table in a synchronous radiation X-ray light path, photon flux incident on a sample can be optimized in real time according to the signal state of a detector and the heat load of the filter, and the stability, the repeatability and the safety of an XAFS experiment are obviously improved while signal saturation and equipment overheating are avoided, so that the manual intervention is reduced, the debugging time is shortened, and the operation efficiency of the whole beam line is improved. In order to achieve the above purpose, the present invention adopts the following technical scheme: The XAFS automatic sample changing device integrating light intensity management comprises a light filter wheel, a sample table and a control component, wherein the light filter wheel is arranged on a synchronous radiation X-ray transmission path and used for selectively attenuating passing X-rays, the sample table is used for carrying a plurality of samples and enabling different samples to sequentially enter an X-ray irradiation area through position switching, the control component is respectively and electrically connected with the light filter wheel and the sample table and used for coordinately controlling working states of the light filter wheel and the sample table, the light filter wheel and the sample table form an integrated structure used for XAFS experiments, and a sample switching process and an incident X-ray light intensity adjusting process are mutually matched, so that light intensity management is realized in an automatic sample changing process. Preferably, the sample stage is provided with a plurality of sample mounting holes, each sample mounting hole is used for mounting a sample, and the sample stage rotates to enable different sample mounting holes to sequentially enter the X-ray irradiation position. Preferably, the sample stage is a turntable structure rotating around a fixed axis, and the plurality of sample mounting holes are distributed along