A system and method for simultaneous detection of data by multiple experimental techniques

By using a system that combines multiple experimental techniques to simultaneously detect data, the system achieves synchronous triggering and data acquisition of various detection techniques, solving the problem of simultaneous detection in existing technologies and improving temporal resolution and data analysis capabilities.

CN116593506BActive Publication Date: 2026-04-21INST OF HIGH ENERGY PHYSICS CHINESE ACAD OF SCI
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
INST OF HIGH ENERGY PHYSICS CHINESE ACAD OF SCI
Filing Date
2023-05-05
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Existing technologies cannot achieve true simultaneous detection of multiple detection techniques, resulting in low temporal resolution and failing to meet the needs of efficient material structure research.

Method used

A system for simultaneously detecting data using multiple experimental techniques, including a gas ionization chamber, photodiodes, electronic systems, multiple different types of detectors, and a host computer, enables synchronous triggering and data acquisition of multiple detectors. Combined with a monochromator encoder and motor driver, it achieves simultaneous detection using multiple detection techniques.

Benefits of technology

It enables simultaneous detection using multiple detection technologies, improves temporal resolution, meets the needs of efficient material structure research, and provides more accurate data analysis capabilities.

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Abstract

The application discloses a system and method for simultaneously detecting data by combining multiple experimental technologies, which comprises a gas ionization chamber, a first amplifier, a photodiode, a second amplifier, an electronic system, a first host computer, multiple different detectors and multiple second host computers; a sample is arranged between the gas ionization chamber and the photodiode; the gas ionization chamber collects the intensity of incident X-rays before the sample; the photodiode collects the intensity of emitted X-rays after the sample; the incident X-rays are input to the electronic system through the first amplifier; the emitted X-rays are input to the electronic system through the second amplifier; the first host computer is connected with the electronic system through a network port and reads back the intensity data of the incident and emitted X-rays; the electronic system is connected with the multiple different detectors and triggers the multiple different detectors to simultaneously measure; each detector is connected with a second host computer; the application has the advantages that multiple detection technologies are combined to simultaneously detect.
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Description

Technical Field

[0001] This invention relates to the field of detecting the microstructure of matter using X-ray synchrotron radiation technology, and more specifically to a system and method for simultaneously detecting data using multiple experimental techniques. Background Technology

[0002] Synchrotron radiation technology is an effective means of probing and characterizing the microstructure of matter. Traditional synchrotron radiation detection techniques mostly employ a single experimental technique, such as small-angle X-ray scattering (SAXS), wide-angle X-ray scattering (WAXS), X-ray diffraction (XRD), and X-ray absorption fine structure (XAFS). With advancements in synchrotron radiation technology, research combining multiple experimental techniques to simultaneously probe the structure of matter has gradually developed. While research combining SAXS, WAXS, and XAFS exists internationally, truly simultaneous measurements have not yet been achieved. Therefore, combining more experimental methods for simultaneous detection has become an important direction for the study of material structure.

[0003] Chinese Patent Publication No. CN109490340A discloses a method for processing test data using a combined technology, involving the combined use of three detection technologies: XAS, XRD, and SAXS. There are two main challenges in combining XAFS, XRD, and SAXS technologies: First, in transmission mode, the XAFS detector blocks the SAXS signal, making it impossible to simultaneously acquire SAXS information, reducing the temporal resolution of the combined technology, and preventing true simultaneous measurement; only quasi-simultaneous measurement is possible. Second, the energy changes during XAFS spectrum acquisition, and simultaneously acquiring XRD and SAXS signals during this energy change becomes problematic. Failure to acquire these signals also reduces the temporal resolution of the combined technology, preventing true combined and simultaneous measurement. If XRD and SAXS signals are acquired, analyzing the scattering information acquired during the energy change process becomes a challenge.

[0004] Taking the combined use of three technologies on the BM26A beamline of the European Synchrotron Radiation Facility (ESRFF) as an example, the XAFS detector (photodiode) is placed directly behind the sample, and its position is controlled by a motor. Within one acquisition cycle, initially, the photodiode is below the optical path, and the monochromator is at the initial energy position, first acquiring SAXS / WAXS signals. Then, the photodiode is raised to the optical path position to begin acquiring the XAFS spectrum. The monochromator, driven by the motor, begins to rotate, acquiring intensities at different energy points until the entire XAFS spectrum is acquired (the time required varies depending on the energy range to be acquired, typically taking several minutes). Afterward, the monochromator is rotated back to its original position (approximately 10 seconds), and the photodiode position is lowered, starting a new acquisition cycle. It can be seen that in this combined technology mode, the signals from the three technologies are not truly acquired simultaneously, and the time resolution is only a few minutes. Subsequently, the experimental station staff upgraded this combined technique, changing the ordinary XAFS to a fast scanning mode, namely QEXAFS. Compared to before, the motor no longer stops during the XAFS scanning process but continues to rotate while scanning the spectrum. This greatly shortens the XAFS spectrum acquisition time (10-60 seconds, depending on the energy range acquired) and improves the temporal resolution of this combined technique. Although the application of QEXAFS improves the temporal resolution of this combined technique, the signals from the three techniques are still not acquired simultaneously. As before, the SAXS / WAXS signals are acquired at the initial energy point, and then the XAFS spectrum is acquired separately. Therefore, it is evident that developing truly meaningful multi-technology combined techniques is not only a trend in the development of experimental detection techniques for material structure but also an urgent research need. Summary of the Invention

[0005] The technical problem to be solved by the present invention is that the existing technology cannot achieve simultaneous detection when multiple detection technologies are used in combination.

[0006] This invention solves the above-mentioned technical problems through the following technical means: a system for simultaneously detecting data using multiple experimental techniques, including a gas ionization chamber, a first amplifier, a photodiode, a second amplifier, an electronics system, a first host computer, multiple detectors of different types, and multiple second host computers. The sample is placed between the gas ionization chamber and the photodiode. The gas ionization chamber collects the intensity of incident X-rays before the sample, and the photodiode collects the intensity of emitted X-rays after the sample. The incident X-rays are input to the electronics system via the first amplifier, and the emitted X-rays are input to the electronics system via the second amplifier. The first host computer is connected to the electronics system via a network port and reads back the incident and emitted X-ray intensity data. The electronics system is connected to multiple detectors of different types, triggering simultaneous measurements by the detectors of different types. Each detector is connected to a corresponding second host computer.

[0007] Beneficial effects: The electronic system of this invention is connected to multiple detectors of different types, and sends trigger signals to each detector to enable simultaneous detection by multiple detectors, thereby synchronously collecting signals under different detection technologies and realizing simultaneous detection by using multiple detection technologies in combination.

[0008] Furthermore, the system for simultaneously detecting data using multiple experimental techniques also includes a monochromator, which emits X-rays into a gas ionization chamber. The encoder of the monochromator is connected to a first host computer via a serial port, and the first host computer is connected to the electronics system via a network port.

[0009] Furthermore, the system for simultaneously detecting data using multiple experimental techniques also includes a motor driver and a motor, and the pulse transmission port of the electronic system is connected to the motor through the motor driver.

[0010] This invention also provides a method for a system that uses multiple experimental techniques to simultaneously detect data. The intensity of the incident X-ray and the emitted X-ray are amplified by a first amplifier and a second amplifier, respectively, and then input into an electronic system. The electronic system simultaneously sends the amplified incident and emitted light to a first host computer. The first host computer sends trigger signals to each detector through the electronic system, simultaneously triggering multiple detectors of different types to perform detection. The detection result data is uploaded to the corresponding second host computer, which processes and stores the detected data.

[0011] Furthermore, the monochromator emits X-rays into the gas ionization chamber. The monochromator's parameter settings and operating process are as follows:

[0012] The monochromator motor's operating speed parameters are set, including a starting speed (low speed), a constant speed (high speed), and an acceleration (acceleration). Within one scan cycle, the monochromator completes scans in both low-energy and high-energy directions according to a trapezoidal speed curve pattern of acceleration-constant speed-deceleration. Simultaneously, analog signals from the gas ionization chamber and photodiode are sampled at a frequency of 1MHz. The analog signals are converted into digital signals by an ADC and then uploaded to the first host computer. The monochromator's energy scan is defined as an XAFS scan.

[0013] Furthermore, the XAFS scanning process acquires the XAFS spectrum, and the energy coordinates of the XAFS spectrum are determined by calculating the initial energy using the Bragg formula 2dsin(theta) = 12398.42 / E, where d is the interplanar spacing, theta is the Bragg angle, and E is the current energy point.

[0014] Furthermore, the different types of detectors include SDD silicon drift detectors, Mythen12K detectors, and Pilatus two-dimensional surface detectors. The SDD silicon drift detectors, Mythen12K detectors, and Pilatus two-dimensional surface detectors correspond to the F-XAFS detection system, the WAXS detection system, and the SAXS detection system, respectively, and respectively acquire F-XAFS signals, WAXS signals, and SAXS signals.

[0015] Furthermore, the simultaneous sampling of analog signals from the gas ionization chamber and photodiode during energy scanning includes:

[0016] The WAXS detection system begins detection at the start of each XAFS scan cycle according to its preset parameters. The SAXS and F-XAFS detection systems require setting the single exposure time, single exposure delay time, and number of exposures within an XAFS scan cycle. Detection then begins based on these settings. The SAXS detection system uses the Pilatus delt energy resolution value, calculated as: one scan cycle time / (energy range / Pilatus delt) to determine the single exposure time (PilatusTimes). The single exposure delay time (PilatusDelay) is a preset value for the SAXS detection system, calculated as: one scan cycle time / (PilatusTimes + PilatusDelay) to determine the number of exposures (PilatusTriggers). The calculation methods for the single exposure time, single exposure delay time, and number of exposures in the F-XAFS detection system are the same as those in the SAXS detection system.

[0017] Furthermore, the second host computer corresponding to the F-XAFS detection system performs offline processing on the detected data. The processing includes:

[0018] The data acquired online by the SDD silicon drift detector is a series of fluorescence intensity data I that varies with energy, but there is no corresponding energy axis coordinate data E. The time, energy, and incident light intensity data columns are extracted from the SDD data file. The corresponding energy range and incident light intensity range are obtained according to the exposure time and delay time. The energy range and incident light intensity range are averaged to obtain the energy axis coordinate data E and the incident light intensity I0. The fluorescence intensity data I is normalized by the formula Is=I / I0 to obtain the E and Is data. The E and Is data are divided into five segments according to the energy resolution, and each segment is integrally averaged according to its own energy step size.

[0019] Furthermore, the second host computer corresponding to the SAXS detection system performs offline processing on the detected data. The processing includes:

[0020] Before sample testing, an empty energy scan is performed in both directions to obtain a background image G. After the sample is placed in the sample for testing, time, energy, and emitted light intensity data columns are extracted from the pilatus data file. The corresponding energy range and emitted light intensity range are obtained according to the exposure time and delay time. The energy range and emitted light intensity range are averaged to obtain the energy coordinates E' and emitted light intensity I0'. The image G is normalized according to Bragg's formula. The sum and average of all images within one period after normalization are obtained to obtain image G0. The SAXS two-dimensional image S obtained from the energy coordinates E' and emitted light intensity I0' is also normalized to obtain image S0. S0-G0 is then used to obtain the SAXS image after removing the background.

[0021] The advantages of this invention are:

[0022] (1) The electronic system of the present invention is connected to multiple detectors of different types. The electronic system simultaneously sends trigger signals to each detector, enabling multiple detectors to detect simultaneously, thereby synchronously collecting signals under different detection technologies, and realizing simultaneous detection while using multiple detection technologies.

[0023] (2) The WAXS detection system of the present invention starts detection according to its preset parameters at the beginning of each XAFS scan cycle. The SAXS detection system and the F-XAFS detection system need to set the single exposure time, single exposure delay time and exposure number within an XAFS scan cycle, and then start detection according to the set single exposure time, single exposure delay time and exposure number. Thus, the three detection systems are triggered at the same time and obtain the corresponding data simultaneously when the detection requirements are met.

[0024] (3) The data obtained after the three detection systems of the present invention are triggered and detected simultaneously cannot simultaneously meet the requirements of data analysis. Therefore, the data obtained by detection is processed offline, so as to achieve the data that can be used for data analysis while meeting the requirements of simultaneous detection. Thus, the three detection technologies are combined by synchronous detection and data processing methods. Attached Figure Description

[0025] Figure 1 This is a schematic diagram of a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0026] Figure 2 This is a software flowchart of the XAFS system in a system for simultaneously probing data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0027] Figure 3 This is a schematic diagram of the XAFS data acquisition software interface in a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0028] Figure 4 This is a diagram of the F-XAFS data acquisition software interface in a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0029] Figure 5 This is a diagram of the WAXS data acquisition software interface in a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0030] Figure 6 This is a diagram of the F-XAFS fluorescence data processing interface in a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention.

[0031] Figure 7 This is a diagram of the SAXS data processing interface in a system for simultaneously detecting data using multiple experimental techniques, as disclosed in an embodiment of the present invention. Detailed Implementation

[0032] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0033] like Figure 1As shown, a system for simultaneously detecting data using multiple experimental techniques includes a gas ionization chamber, a first amplifier, a photodiode, a second amplifier, an electronics system, multiple detectors of different types, a first host computer, a monochromator, multiple second host computers, a motor driver, and a motor. The sample is placed between the gas ionization chamber and the photodiode. X-rays emitted from the monochromator are fed into the gas ionization chamber. The gas ionization chamber collects the intensity of the incident X-rays before the sample is collected, and the photodiode collects the intensity of the emitted X-rays after the sample is collected. The incident X-rays are input to the electronics system via the first amplifier, and the emitted X-rays are input to the electronics system via the second amplifier. The electronics system is connected to multiple detectors of different types, and each detector is connected to a corresponding second host computer. The encoder of the monochromator is connected to the first host computer via a serial port, and the first host computer is connected to the electronics system via a network port. The pulse transmission port of the electronics system is connected to the motor via the motor driver. The movement of the monochromator is controlled by the motor. The first host computer can detect the energy value corresponding to each energy point during the monochromator's energy scanning process through the monochromator encoder.

[0034] The intensity of the incident X-ray and the intensity of the emitted X-ray are amplified by the first amplifier and the second amplifier, respectively, and then input into the electronic system. The first host computer is connected to the electronic system through the network port and reads back the incident and emitted X-ray intensity data. The electronic system sends trigger signals to different types of detectors, triggering multiple different types of detectors to perform detection. The detection result data is uploaded to the corresponding second host computer, which processes the detection data. Figure 1 In this embodiment, computer 1 is the first host computer, and computers 2, 3, and 4 are the second host computers. The rapid electronics system is the electronics system in this embodiment, and both the first and second amplifiers are SR570 amplifiers. The environmental system is the test environment system for the sample, which is not involved in this embodiment.

[0035] In this embodiment, the different types of detectors include SDD silicon drift detectors, Mythen12K detectors, and Pilatus two-dimensional surface detectors. These detectors correspond to the F-XAFS detection system, WAXS detection system, and SAXS detection system, respectively, and acquire F-XAFS, WAXS, and SAXS signals. The energy scan of the monochromator is defined as an XAFS scan. The following details the energy scan process of the monochromator, and the data acquisition and processing processes of the F-XAFS, WAXS, and SAXS detection systems.

[0036] 1. XAFS scanning and XAFS signal acquisition process

[0037] Traditional XAFS signal acquisition typically employs a step-scan method. For example, after the computer sends a motion command A1 to the monochromator controller, the monochromator moves from the current energy point E0 to the next energy point E1. Upon reaching E1, the computer sends a data acquisition command B1 to the detector counter. The counter accumulates data according to a pre-set acquisition time t1. After acquisition, the computer sends a motion command A2 to the monochromator controller, and the monochromator moves to the next energy point E2. Upon reaching E2, the computer sends a data acquisition command B2 to the detector counter to acquire data, and so on until all energy points are acquired. The disadvantages of the traditional step-scan method are: firstly, data acquisition at each energy point consumes computer command time; secondly, the entire energy scan process follows a monochromator movement-stop-acquisition sequence, significantly consuming the overall scan time; and thirdly, the scan direction is always fixed in a single direction from low energy to high energy, lacking a direction from high energy to low energy, which also wastes scan time. Acquiring an XAFS spectrum using traditional step-scan takes approximately ten minutes, which is unsuitable for testing sample environment systems with time resolution on the order of seconds.

[0038] In this embodiment, the electronics system integrates a pulse generator and a 1MHz high-frequency data acquisition module, enabling second-level time-resolved XAFS spectrum data acquisition. XAFS signal acquisition utilizes a gas ionization chamber and a photodiode. During XAFS signal acquisition, the electronics system can send trigger acquisition signals to the WAXS, SAXS, and F-XAFS detection systems respectively, simultaneously acquiring data from the WAXS, SAXS, and F-XAFS systems to achieve simultaneous measurement using the three experimental methods. The gas ionization chamber is used to acquire the intensity of incident X-rays before the sample, and the photodiode is used to acquire the intensity of emitted X-rays after the sample. Simultaneously, an SR570 low-current amplifier amplifies the incident and emitted light intensity signals. Figure 3 The diagram shows the XAFS data acquisition software interface. The process of XAFS data acquisition and sending trigger signals to the outside is as follows:

[0039] (1) First, set the XAFS system energy scanning parameters. Select the absorption edge energy value (Energy) of the feature element (e.g., Cu), set the initial energy value (Pre) and the final energy value (Post) of the feature element, and set the XAFS scanning cycle number (Cycles). Second, set the speed parameters of the monochromator motor, including the initial speed value (low speed), the constant speed value (high speed), and the acceleration value (acceleration). Within one scanning cycle, the monochromator completes scanning in both low-energy and high-energy directions according to a trapezoidal speed curve pattern of acceleration-constant speed-deceleration. Simultaneously, the detector analog signal is sampled at a sampling frequency of 1MHz. The analog signal is converted into a digital signal by the ADC and then uploaded to the first host computer. The energy scanning of the monochromator is defined as XAFS scanning. Figure 2 The diagram shown is a software flowchart of the XAFS system. Figure 2 QXAFS refers to Fast XAFS, which is equivalent to the meaning of XAFS in this embodiment.

[0040] (2) Determination of energy axis coordinates. The XAFS spectrum is obtained during the XAFS scanning process. The energy coordinates of the XAFS spectrum are determined by calculating the initial energy using the Bragg formula 2dsin(theta) = 12398.42 / E, where d is the interplanar spacing, theta is the Bragg angle, and E is the current energy point. For example, given the initial energy E0 (eV) and the monochromator angular resolution delttheta (degree / pulse), theta0 can be obtained using the formula sin(theta0) = 1977.1 / E0, E1 can be obtained using the formula E1 = 1977.1 / sin(theta0 + delttheta0), and E2 can be obtained using the formula E2 = 1977.1 / sin(theta0 + 2dsin(theta0 + 2dsin(theta0 + 2dsin(theta0) ... E2 can be obtained by delttheta0, and so on, all energy coordinate values ​​can be obtained. Since there is a gap between the gears of the monochromator motor, the backflip difference must also be determined. The backflip difference can be accurately determined by calculating the pulse offset between the two measured standard spectra. The backflip difference is used to correct the energy axis coordinates.

[0041] (3) Online processing and storage of XAFS data. XAFS data has four storage methods: raw, xafs, sdd, and pilatus, which correspond to four types of data files.

[0042] 1) Raw data file. The raw file stores the original XAFS data, stored in a five-column format: pulse, energy, front detector (I0), back detector (I1), ln(I0 / I1) or (I1 / I0). The storage strategy is to store the data after each cycle of data acquisition, rather than storing it immediately after each pulse of data acquisition. This avoids TCP port data congestion and improves data acquisition efficiency.

[0043] 2) XAFS data files. XAFS files are XAFS data with a higher signal-to-noise ratio obtained after online processing of the raw data, and are used for XAFS data analysis. The specific processing method is to divide the raw XAFS data into five segments, set different energy step sizes for each segment according to the energy resolution, and merge the corresponding data by integration, which reduces the amount of data and improves the signal-to-noise ratio of the XAFS spectrum.

[0044] 3) SDD data file. The SDD file is stored in six columns: time, energy, detector, exposure time, delay time, and number of exposures in one cycle. It is mainly used for offline F-XAFS (fluorescence) data processing.

[0045] 4) Pilatus data file. The pilatus file is stored in six columns: time, energy, detector, exposure time, delay time, and number of exposures in one cycle. It is mainly used for offline SAXS data processing.

[0046] (4) The simultaneous sampling of detector signals during energy scanning includes:

[0047] The WAXS detection system begins detection at the start of each XAFS scan cycle according to its preset parameters. The SAXS and F-XAFS detection systems require setting the single exposure time, single exposure delay time, and number of exposures within an XAFS scan cycle. Detection then begins based on these settings. The SAXS detection system uses the Pilatus delt energy resolution value, calculated as: one scan cycle time / (energy range / Pilatus delt) to determine the single exposure time (PilatusTimes). The single exposure delay time (PilatusDelay) is a preset value for the SAXS detection system, calculated as: one scan cycle time / (PilatusTimes + PilatusDelay) to determine the number of exposures (PilatusTriggers). The calculation methods for the single exposure time, single exposure delay time, and number of exposures in the F-XAFS detection system are the same as those in the SAXS detection system.

[0048] The XAFS energy scanning, data acquisition, and trigger signal transmission to each detector are all accomplished by a combination of pre-configured uplink and downlink command codes. The uplink command code is responsible for the monochromator's forward and reverse movement and for sending trigger signals externally, while the downlink command code is responsible for XAFS data acquisition. The electronics system sends pulse signals to the monochromator motor according to the specific uplink command. As the motor rotates continuously upon receiving the pulse signals, the electronics system continuously acquires data from the gas ionization chamber and photodiode signals. Simultaneously, the electronics system sends data to the TCP port, and the first host computer receives the port data via the TCP communication protocol. Each 10-second interval constitutes one XAFS data acquisition cycle.

[0049] 2. Acquisition of F-XAFS, WAXS, and SAXS signals

[0050] Figure 4 This is the interface diagram of the F-XAFS (fluorescence) data acquisition software. The F-XAFS (fluorescence) signal acquisition uses the SDD silicon drift detector. Before the XAFS data acquisition begins, the SDD detector system must set the SDD exposure time, delay time, number of exposures, exposure cycle, and other parameters according to the XAFS system interface parameters. For the specific setting process, please refer to the description in point 1, section (4) above. When the acquisition begins, the electronics system sends a trigger signal to the SDD detector according to the pre-set trigger parameters. After receiving the trigger signal, the SDD detector begins data acquisition. The F-XAFS data acquisition software displays the real-time data spectrum and stores the data once per cycle.

[0051] Figure 5 This is an interface diagram of the WAXS data acquisition software. WAXS data acquisition uses the Mythen12K detector, which consists of a one-dimensional arc detector system composed of 12 detector modules, with a frame rate of 1000Hz and a pixel size of 50µm. The electronics system only sends a trigger signal to the Mythen detector at the beginning of each XAFS data acquisition cycle. After receiving the trigger signal, the detector begins to acquire data in an exposure manner. The WAXS data acquisition parameters, such as exposure time, delay time, number of exposures, and exposure cycle, are preset by the WAXS signal acquisition software according to the actual situation and are displayed and stored in real time.

[0052] SAXS signal acquisition uses a Pilatus two-dimensional surface detector with a frame rate of 25Hz and a pixel size of 172µm. Similar to F-XAFS signal data acquisition, before acquisition begins, the Pilatus detector system is configured with parameters such as exposure time, delay time, number of exposures, and exposure period according to the XAFS software interface. At the start of acquisition, the electronics system sends a trigger signal to the Pilatus detector based on the pre-set trigger parameters. Upon receiving the trigger signal, the Pilatus detector begins data acquisition.

[0053] 3. Offline data processing

[0054] (1) Offline F-XAFS data processing

[0055] Figure 6 This is a diagram of the F-XAFS fluorescence data processing interface. The data acquired online by the SDD detector is a series of fluorescence intensity data I that varies with energy. There is no corresponding energy axis coordinate data E, nor is there incident light intensity data I0 after intensity normalization. The signal-to-noise ratio is relatively poor, and further data analysis is not yet possible; curve smoothing is required. Specifically, the second host computer corresponding to the F-XAFS detection system performs offline processing on the detected data. The processing includes:

[0056] The data acquired online by the SDD silicon drift detector is a series of fluorescence intensity data I that varies with energy, but there is no corresponding energy axis coordinate data E. The time, energy, and incident light intensity data columns are extracted from the SDD data file. The corresponding energy range and incident light intensity range are obtained according to the exposure time and delay time. The energy range and incident light intensity range are averaged to obtain the energy axis coordinate data E and incident light intensity I0. The fluorescence intensity data I is normalized by the formula Is=I / I0 to obtain E and Is data. The E and Is data are divided into five segments according to the energy resolution. Each segment is integrally averaged according to its own energy step size to obtain fluorescence data that can be used for data analysis.

[0057] (2) Offline SAXS data processing

[0058] Figure 7 This is a diagram of the SAXS data preprocessing interface. The SAXS two-dimensional image S acquired online by the Pilatus detector represents images corresponding to different energy points. Background subtraction and energy normalization are required for image S. Specifically, the second host computer corresponding to the SAXS detection system performs offline processing on the detected data. The processing includes:

[0059] Before sample testing, an empty energy scan is performed in both directions to obtain a background image G. After the sample is placed in the sample for testing, time, energy, and emitted light intensity data columns are extracted from the Pilatus data file. The corresponding energy range and emitted light intensity range are obtained according to the exposure time and delay time. The energy range and emitted light intensity range are averaged to obtain the energy coordinates E' and emitted light intensity I0'. The image G is normalized according to Bragg's formula 2dsin(theta) = lambda. The average of all images within one period after normalization is obtained to obtain image G0. The SAXS two-dimensional image S obtained from the energy coordinates E' and emitted light intensity I0' is also normalized to obtain image S0. S0-G0 is then used to obtain the SAXS image after removing the background. The SAXS image can be used for data analysis.

[0060] Through the above technical solutions, the electronic system of this invention is connected to multiple detectors of different types, and trigger signals are transmitted to different detectors at the same time, so as to realize the simultaneous detection of multiple detectors, thereby synchronously collecting signals under different detection technologies, and realizing the simultaneous detection of multiple detection technologies in combination.

[0061] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for simultaneously detecting data using multiple experimental techniques in combination, characterized in that, The system for simultaneously detecting data using multiple experimental techniques combined to implement the described method includes a gas ionization chamber, a first amplifier, a photodiode, a second amplifier, an electronics system, a first host computer, multiple detectors of different types, and multiple second host computers. The sample is placed between the gas ionization chamber and the photodiode. The gas ionization chamber collects the intensity of the incident X-ray before the sample is collected, and the photodiode collects the intensity of the emitted X-ray after the sample is collected. The incident X-ray is input to the electronics system via the first amplifier, and the emitted X-ray is input to the electronics system via the second amplifier. The first host computer is connected to the electronics system via a network port and reads back the intensity of the incident and emitted X-rays. The system connects to multiple detectors of different types, triggering them to measure simultaneously. Each detector is connected to a corresponding second host computer. The intensity of the incident X-ray and the emitted X-ray are amplified by a first amplifier and a second amplifier, respectively, and then input to the electronic system. The electronic system simultaneously sends the amplified incident and emitted X-rays to the first host computer. The first host computer sends trigger signals to each detector through the electronic system, simultaneously triggering multiple detectors of different types to perform detection. The detection result data is uploaded to the corresponding second host computer, which processes the detection data. The system, which combines multiple experimental techniques to simultaneously detect data, simultaneously samples analog signals from the gas ionization chamber and photodiode while performing energy scanning, including: The WAXS detection system starts detection at the beginning of each XAFS scan cycle according to its preset parameters. The SAXS detection system and the F-XAFS detection system need to set the single exposure time, single exposure delay time and number of exposures within an XAFS scan cycle, and then start detection according to the set single exposure time, single exposure delay time and number of exposures. The energy resolution value of the SAXS detection system is Pilatus delt, according to the formula: The single exposure time (PilatusTimes) is calculated, and the single exposure delay time (PilatusDelay) is a preset value for the SAXS detection system, based on the formula: Calculate the number of exposures using PilatusTriggers; The calculation methods for single exposure time, single exposure delay time, and number of exposures in the F-XAFS detection system are the same as those in the SAXS detection system.

2. The method for simultaneously detecting data using multiple experimental techniques in combination according to claim 1, characterized in that, It also includes a monochromator that emits X-rays into a gas ionization chamber. The encoder of the monochromator is connected to the first host computer via a serial port, and the first host computer is connected to the electronics system via a network port.

3. The method for simultaneously detecting data using multiple experimental techniques according to claim 1, characterized in that, It also includes a motor driver and a motor, and the pulse transmission port of the electronics system is connected to the motor through the motor driver.

4. The method for simultaneously detecting data using multiple experimental techniques in combination according to claim 1, characterized in that, The monochromator emits X-rays into the gas ionization chamber. The monochromator's parameter settings and operating procedure are as follows: The monochromator motor's operating speed parameters are set, including a starting speed (low speed), a constant speed (high speed), and an acceleration (acceleration). Within one scan cycle, the monochromator completes scans in both low-energy and high-energy directions according to a trapezoidal speed curve pattern of acceleration-constant speed-deceleration. Simultaneously, analog signals from the gas ionization chamber and photodiode are sampled at a frequency of 1MHz. The analog signals are converted into digital signals by an ADC and then uploaded to the first host computer. The monochromator's energy scan is defined as an XAFS scan.

5. The method for simultaneously detecting data using multiple experimental techniques in combination according to claim 4, characterized in that, The XAFS scanning process acquires the XAFS spectrum, and the energy coordinates of the XAFS spectrum are determined based on the initial energy using Bragg's formula 2dsin( The formula is calculated as 12398.42 / E, where d is the interplanar spacing. Let E be the Bragg angle and E be the current energy point.

6. The method for simultaneously detecting data using multiple experimental techniques in combination according to claim 5, characterized in that, The different types of detectors include SDD silicon drift detectors, Mythen12K detectors, and Pilatus two-dimensional surface detectors. The SDD silicon drift detectors, Mythen12K detectors, and Pilatus two-dimensional surface detectors correspond to the F-XAFS detection system, the WAXS detection system, and the SAXS detection system, respectively, and respectively acquire F-XAFS signals, WAXS signals, and SAXS signals.

7. The method for simultaneously detecting data using multiple experimental techniques according to claim 1, characterized in that, The second host computer corresponding to the F-XAFS detection system performs offline processing on the detected data. The processing includes: The data acquired online by the SDD silicon drift detector is a series of fluorescence intensity data I that varies with energy, without corresponding energy axis coordinate data E. The time, energy, and incident light intensity data columns are extracted from the SDD data file. The corresponding energy range and incident light intensity range are obtained according to the exposure time and delay time. The energy axis coordinate data E and incident light intensity I0 are obtained by averaging the energy range and incident light intensity range respectively. The fluorescence intensity data I is normalized by the formula Is=I / I0, and Is is the normalized fluorescence intensity data, resulting in E and Is data. The E and Is data are divided into five segments according to the energy resolution, and each segment is integrally averaged according to its own energy step size.

8. The method for simultaneously detecting data using multiple experimental techniques according to claim 1, characterized in that, The second host computer corresponding to the SAXS detection system performs offline processing on the detected data. The processing includes: Before sample testing, an empty energy scan is performed in both directions to obtain a background image G. After the sample is placed in the sample for testing, time, energy, and emitted light intensity data columns are extracted from the pilatus data file. The corresponding energy range and emitted light intensity range are obtained according to the exposure time and delay time. The energy range and emitted light intensity range are averaged to obtain the energy coordinates E' and emitted light intensity I0'. The image G is normalized according to Bragg's formula. The sum and average of all images within one period after normalization are obtained to obtain image G0. The SAXS two-dimensional image S obtained from the energy coordinates E' and emitted light intensity I0' is also normalized to obtain image S0. S0-G0 is then used to obtain the SAXS image after removing the background.

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