An XRD automatic testing system

By combining industrial robots with XRD testing equipment, automated sample loading and batch data analysis are achieved, solving the problems of insufficient continuous testing and data analysis capabilities of existing XRD instruments, and realizing efficient and accurate multi-sample testing and data processing.

CN119395060BActive Publication Date: 2025-12-05INSTITUTE OF PHYSICS CHINESE ACADEMY OF SCIENCES
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Patent Information

Application Number
CN202411540052.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-31
Publication Date
2025-12-05
Estimated Expiration
2044-10-31

AI Technical Summary

Technical Problem

Existing XRD instruments cannot perform continuous testing of multiple samples, are subject to human error in sample loading, and have insufficient data analysis capabilities, failing to meet the needs of independent experiments and big data processing.

Method used

By combining industrial robots with XRD testing equipment, automated sample loading and batch data analysis are achieved. Through wireless communication and automatic control of the hatch, combined with sample trays and tray clamps, rapid sample replacement and positioning are realized. A batch phase analysis method is designed for rapid screening and classification.

Benefits of technology

It enables efficient and accurate testing and data analysis of multiple samples, reduces human error, improves sample processing efficiency and data processing capabilities, and is suitable for the fully automated transformation of existing XRD equipment and the construction of smart laboratories.

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Abstract

The application provides an XRD automatic testing system, comprising an XRD testing device and an industrial robot, wherein the industrial robot is configured to: sample a current sample to be tested; send an opening cabin signal to the XRD testing device to trigger the XRD testing device to open a cabin door; place the current sample to be tested into the XRD testing device through a mechanical arm of the industrial robot and send a sample placing completion signal to the XRD testing device to trigger the XRD testing device to close the cabin door; send a test start instruction to the XRD testing device to trigger the XRD testing device to start testing after identifying that the XRD testing device closes the cabin door; and send a test completion signal to the XRD testing device after the industrial robot executes all test instructions. The XRD testing device is configured to: open the cabin door in response to the opening cabin signal; close the cabin door in response to the sample placing completion signal; test the sample in response to the test start instruction to obtain an XRD spectrum corresponding to the sample; and batch process a plurality of XRD spectra in response to the test completion signal to obtain a test report.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of metal material analysis and characterization, in particular to metal material automatic analysis technology, and more particularly to an XRD automatic testing system. BACKGROUND

[0002] The research and development of metal materials are crucial to the development of modern industry and technology, supporting the development of multiple key fields such as construction, aerospace, automobiles, energy, electronics and electrical appliances, medical treatment, environment, and national defense. Among them, the key to developing alloys is to understand the relationship between alloy chemical composition, structure, and performance, and the characterization and analysis of alloy structure are essential links. As a widely used non-destructive testing method, X-ray diffraction (XRD) can provide important information such as material crystal structure, phase composition, and grain size, and is an important means of characterizing alloy structure.

[0003] Current XRD instruments mainly use manual sample loading and single spectrum analysis mode, which can meet the characterization and analysis of small batches of samples. However, with the development of data-driven artificial intelligence research paradigm, people expect to use artificial intelligence for autonomous experiments and verification, which poses a challenge to the continuous testing and batch data analysis capabilities of XRD instruments.

[0004] In order to integrate XRD into an autonomous experiment platform, the existing XRD needs to be automated. In terms of automated characterization, XRD can be equipped with an electrically controlled displacement table inside, which can independently complete multi-point automated collection. However, there are still many problems: first, it cannot be tested continuously. The existing XRD device needs to be manually replaced by the experimenter after a sample test is completed, which cannot realize continuous testing of multiple samples, hindering the autonomous experiment, and is also prone to human error in sample loading. On the other hand, the data analysis capability is insufficient. The existing XRD instrument is only responsible for data collection and saving, and has no data analysis capability. The traditional method is for the experimenter to take the data and use professional analysis software to process and judge the data one by one, but when the data generation efficiency increases and the data volume increases, the speed of manual processing cannot keep up with the 24-hour automatic production of data. Therefore, in order to realize the automation of XRD autonomous experiment, the real-time data analysis capability is crucial. The current XRD manufacturers do not provide corresponding automation solutions, and the customization cost is very high, which is not conducive to the modification of existing equipment.

[0005] Therefore, there is an urgent need for a simple and practical automation modification method.

[0006] It should be noted that the background art is only used to introduce the related information of the present application, so as to help understand the technical solutions of the present application, but does not mean that the related information must be prior art. In the absence of evidence that the related information has been disclosed before the filing date of the present application, the related information should not be regarded as prior art. SUMMARY

[0007] Therefore, the purpose of the present application is to overcome the defects of the prior art, and to provide a new XRD automatic testing system.

[0008] The XRD automatic testing system provided by the present application comprises an XRD testing device and an industrial robot, the XRD testing device and the industrial robot are in wireless communication, the XRD testing device is configured with an automatically controlled cabin door, and the industrial robot is configured with a mechanical arm, wherein the industrial robot is configured to respond to a plurality of sample testing instructions one by one and perform the following steps when responding to each testing instruction: sampling the current sample to be tested; sending an opening cabin signal to the XRD testing device to trigger the XRD testing device to open the cabin door; placing the current sample to be tested into the XRD testing device through the mechanical arm and sending a sample placing completion signal to the XRD testing device to trigger the XRD testing device to close the cabin door; sending a testing start instruction to the XRD testing device to trigger the XRD to start testing after identifying that the XRD testing device has closed the cabin door; and sending a testing completion signal to the XRD testing device after the industrial robot has executed all the testing instructions. The XRD testing device is configured to: open the cabin door in response to the opening cabin signal; close the cabin door in response to the sample placing completion signal; test the sample in response to the testing start instruction to obtain the XRD pattern corresponding to the sample; and batch process a plurality of XRD patterns in response to the testing completion signal to obtain a testing report.

[0009] Preferably, the automatically controlled cabin door is a double-door, wherein a cylinder is arranged on each door, and the cylinders on the two doors are configured to be connected or disconnected through extension and retraction under the control of a remote signal to realize the opening and closing actions of the doors, wherein under the control of the opening cabin signal, the cylinders connected to the two doors are retracted to realize the disconnection operation to achieve the opening action, and under the control of the sample placing completion signal, the cylinders connected to the two doors are extended to realize the connection operation to achieve the closing action.

[0010] Preferably, the system is further configured with a sample tray, which is a circular tray, used for placing the sample to be tested so that the mechanical arm can clamp and place it into the XRD testing device.

[0011] Preferably, the sample to be tested is in the form of a film or a block; the front of the sample tray is provided with a recess for loading the sample to be tested, and the inner side of the recess is provided with a positioning notch for indicating the direction of the sample to be tested placed in the recess; the edges of the tray are symmetrically provided with two open notches for being gripped by a mechanical arm; and the back of the tray is provided with a triangular protrusion for positioning the sample tray.

[0012] Preferably, the XRD testing device is provided with a tray clamp, which is circular and used for fixing the sample tray, and the front of the tray clamp is provided with a triangular recess coupled with the triangular protrusion on the back of the sample tray.

[0013] Preferably, the sample tray is made of acrylic, and the tray clamp is a metal disc provided with threaded holes around the periphery and fixed in the XRD testing device by bolts.

[0014] Preferably, the XRD testing device is configured to batch process a plurality of XRD patterns in the following manner: performing a background removal operation on the plurality of XRD pattern data to obtain XRD signals after background removal; performing a peak searching operation on the XRD signals after background removal to obtain a plurality of peak values; performing a fitting operation on the obtained peak types to obtain peak position information; performing a phase clustering analysis using the peak position information obtained by fitting; and associating the phase clustering analysis result with a composition to obtain an analysis result.

[0015] Preferably, the XRD testing device is configured to perform a background removal operation on XRD pattern data in the following manner: dividing the XRD pattern data into 30 equal parts, calculating the average value of each equal part of data and taking the average value as an anchor point of the part; and converting each anchor point into a background index point in the following manner :

[0016]

[0017] wherein, is the abscissa of the i-th anchor point, is the ordinate of the i-th anchor point, and

[0018]

[0019] performing a linear interpolation based on all the background index points to obtain a background signal, and performing a background signal subtraction on the XRD pattern data based on the obtained background signal to obtain XRD signals after background removal.

[0020] Preferably, the XRD testing device is configured to perform a peak searching operation on the XRD signals after background removal according to a preset crystal peak signal criterion, wherein the preset crystal peak signal criterion is:

[0021]

[0022] in,

[0023]

[0024] , , All values ​​are preset parameters, among which, The range of values ​​for signal smoothing processing. To find the signal range with a local maximum value, The threshold should be determined.

[0025] Preferably, y=5, W=50, and T=6σ, where σ is the standard deviation of the signal-noise component.

[0026] Preferably, the XRD testing apparatus is configured to perform peak shape fitting using the Gaussian-Lorentzian method.

[0027] Compared with existing technologies, the advantages of this invention are as follows: The method of this invention has strong universality, low cost, and can be used to fully automate the transformation of existing XRD equipment, as well as for building new intelligent laboratories; the overall method of this invention is applicable to existing commercial XRD equipment, without affecting the original equipment structure and function, and does not rely on the communication interface services opened by instrument manufacturers; the sample tray and fixture designed in this invention can adapt to different types of samples, such as block and film samples, eliminating the cumbersome sample loading and height correction process; the data batch processing method of this invention can process the data collected by the instrument in real time and perform phase classification, accelerating data flow and processing efficiency. Compared with existing XRD processing software, this method has stronger batch processing capabilities and good adaptability, and can automatically read data generated by different XRD models; the automation solution provided by this invention can feed the test results back to the artificial intelligence model without human intervention. Attached Figure Description

[0028] The embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein:

[0029] Figure 1 This is a schematic diagram of the components of an XRD automated testing system according to an embodiment of the present invention;

[0030] Figure 2 This is a schematic diagram of the automatic door closing of an XRD testing device according to an embodiment of the present invention;

[0031] Figure 3 This is a schematic diagram of the automatic door opening of an XRD testing device according to an embodiment of the present invention;

[0032] Figure 4Front view of sample tray according to embodiments of the present application;

[0033] Figure 5 Back view of sample tray according to embodiments of the present application;

[0034] Figure 6 Industrial robot picking up sample tray according to embodiments of the present application;

[0035] Figure 7 Tray gripper according to embodiments of the present application;

[0036] Figure 8 Flowchart of system for testing according to embodiments of the present application;

[0037] Figure 9 XRD pattern array scanning result according to embodiments of the present application;

[0038] Figure 10 Phase classification result according to embodiments of the present application;

[0039] Figure 11 XRD pattern according to embodiments of the present application. DETAILED DESCRIPTION

[0040] In order to make the objects, technical solutions and advantages of the present application clearer, the present application will be further described in detail below with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not to limit the present application.

[0041] As described in the background, the XRD instrument in the prior art cannot be continuously tested, is easy to introduce artificial sample loading errors, and does not have sufficient data analysis capabilities. In order to solve these problems, the present application proposes a new XRD automatic testing system capable of automatic sample loading and data analysis. In the scheme of the present application, an industrial robot is used to automatically load samples, and a phase batch analysis method is designed to quickly analyze multiple samples. Thus, the system of the present application can efficiently and accurately process multiple samples while reducing the influence of human operation on the analysis results. Through the automatic sample loading technology, the rapid replacement and positioning of different samples can be realized, and the efficiency and accuracy of sample processing are improved. In addition, the phase batch analysis method can quickly screen and classify multiple samples, providing a guarantee for the rapid identification of metal materials and data quality control.

[0042] In order to better understand the present application, the present application will be described in detail below from the aspects of system structure, working mode, etc. in combination with the drawings and embodiments.

[0043] I. System structure

[0044] In general, as shown in Figure 1 The XRD automatic testing system of the present application comprises two parts, an XRD testing device 1 and an industrial robot 2, and the XRD testing device and the industrial robot perform wireless communication, the XRD testing device is configured with an automatic control cabin door, and the industrial robot is configured with a mechanical arm. The industrial robot, under the control of sample testing instructions, performs the following actions: sampling on the current sample to be tested; sending an opening cabin signal to the XRD testing device to trigger the XRD testing device to open the cabin door; placing the current sample to be tested into the XRD testing device through the mechanical arm and sending a sample placement completion signal to trigger the XRD testing device to close the cabin door; sending a test start instruction to the XRD testing device to trigger the XRD to start testing after identifying that the XRD testing device closes the cabin door; wherein the industrial robot sends a test completion signal to the XRD testing device after executing all the test instructions. The XRD testing device is configured to: open the cabin door in response to the opening cabin signal; close the cabin door in response to the sample placement completion signal; test the sample in response to the test start instruction to obtain the XRD pattern corresponding to the sample; and batch process a plurality of XRD patterns in response to the test completion signal to obtain a test report. Wherein the industrial robot can continuously repeat the test instructions until the sample testing is completed.

[0045] According to one embodiment of the present application, the automatic control cabin door of the XRD testing device is realized by installing a power mechanism on the basis of the existing double-door cabin door without any destructive modification to the equipment, as shown in Figure 2 A cylinder-controlled pull rod is additionally installed outside the XRD door lock, and the cylinder can be controlled by a remote signal to simulate the human opening and closing door behavior. When the XRD testing device receives the opening cabin signal sent by the industrial robot, the cylinder sends a sample taking and placing signal, and the electronic door lock of the instrument will automatically open; after the waiting indicator light is turned on, as shown in Figure 3 The two side cylinders are retracted to pull the two side doors to automatically open; when the industrial robot completes sample placement and sends a sample placement completion signal to the XRD, the two side cylinders automatically extend to close the door.

[0046] According to one embodiment of the present application, in order to facilitate the sample taking and placing of the industrial robot, a professional sample tray is designed in the present application to facilitate the robot to place the sample to be tested. Generally, the sample to be tested is in a thin film or block shape, and in order to facilitate the industrial robot to place the sample, as shown in Figure 4 The present application is provided with a recess for loading the sample to be tested on the front surface of the sample tray, a positioning notch is arranged on the inner side of the recess to indicate the direction of placing the sample to be tested in the recess, and two open notches for the mechanical arm to clamp are symmetrically arranged on the edges of the tray, as shown in Figure 5As shown, the back of the sample tray is provided with a triangular protrusion for sample tray positioning. For example, for a sample tray for a 4-inch film, the upper surface can be provided with a 100-mm circular groove with a closed gap (positioning gap) for film direction positioning, and the two sides of the groove can be provided with open gaps for facilitating placement of the film sample by the mechanical arm gripper. Such a sample tray can also be used for a sample tray for bulk metal after appropriate modification.

[0047] According to one embodiment of the present application, still referring to Figure 1 In the present application, the industrial robot for sample picking and placing is fixed in front of the XRD testing device, and the mechanical arm thereof can be flexibly swung. When the system receives a sample testing instruction, the industrial robot places the sample tray with the sample on the designated XRD tooling fixture. The industrial robot for sample picking and placing does not touch the internal mechanism of the XRD, simulates manual sample picking, and places the sample according to positioning.

[0048] According to one embodiment of the present application, in order to facilitate positioning of the sample tray by the industrial robot, the XRD testing device is provided with a tray fixture matched with the sample tray, as shown in Figure 6 The tray fixture is circular, and the front surface thereof is provided with a triangular groove coupled with the triangular protrusion on the back of the sample tray. According to one embodiment of the present application, in order to avoid signal interference, the sample tray is made of acrylic plate, and the tray fixture is a metal disc provided with threaded holes around the periphery and fixed in the XRD testing device by bolts.

[0049] Figure 8 The working flow of the system of the present application is intuitively shown. When the system of the present application is used for automatic sample testing, the following steps are mainly included:

[0050] Sending instruction: the user sends a testing instruction to the automatic system;

[0051] Picking sample: the industrial robot goes to a designated position, places the sample in a special sample tray, and transports to the front of the XRD instrument;

[0052] Opening hatch: the industrial robot communicates with the XRD equipment or simulates manual operation, triggers the hatch opening button, and opens the hatch;

[0053] Placing sample: the industrial robot places the special sample tray on the pre-designed XRD fixture, withdraws the mechanical arm, and triggers the XRD testing device to close the hatch;

[0054] Starting testing: the industrial robot sends a testing instruction to the automatic system after identifying the hatch closed signal light by the vision sensor;

[0055] Data collection: The automated system monitors that the test is completed, transfers the path file to the database for categorization, and waits for analysis;

[0056] Data analysis: The automated system performs background removal, peak finding, and peak shape fitting on the XRD pattern, and performs cluster analysis of the alloy phases according to the peak position and peak width;

[0057] Test completion and report formation: The phase structure classification and experimental data corresponding to the alloy are formed into a test report and stored in the database;

[0058] New round of testing: The automated system starts a new round of testing according to new instructions.

[0059] According to one embodiment of the present application, the system of the present application uses a batch processing method to process XRD patterns to avoid the low efficiency problem caused by manual analysis. According to one embodiment of the present application, the XRD testing device of the present application is configured to perform the following steps to realize batch processing of XRD patterns:

[0060] (1) Background removal operation: Assuming that the XRD data contains N data points , where is the horizontal axis (wave vector) of the XRD data, is the vertical axis (intensity) of the XRD data. These data are divided into 30 equal parts, and the average value of each part of data is calculated to convert into 30 anchor points , where, is the horizontal coordinate of the i-th anchor point, is the vertical coordinate of the i-th anchor point, where:

[0061]

[0062] , where, is an integer in , ,

[0063] represents the average value. On this basis, the anchor points are converted into background index points according to the following formula , which is expressed as:

[0064]

[0065] and,

[0066]

[0067] The data obtained by linear interpolation based on these background index points are used as background signals for background signal subtraction of the XRD pattern. In this way, the original XRD signal is converted into the signal after background removal .

[0068] (2) Peak searching: According to an embodiment of the present application, the signal criterion of defining a crystal peak is defined as: there is a local maximum value in a continuous signal, and the difference between the local maximum value and the local average value is greater than a threshold value , which is expressed by the formula as:

[0069]

[0070] wherein,

[0071]

[0072] , , The values are all preset parameters, wherein, is the value range of signal smoothing processing, is the signal range for searching the local maximum value, is the judgment threshold value. According to the data condition, the appropriate , , value can be selected to realize effective crystal peak labeling.

[0073] According to an embodiment of the present application, = 5, W = 50, and T = 6σ, wherein σ is the data standard deviation of the signal noise part.

[0074] (3) Peak shape fitting: Gaussian-Lorentzian is used for fitting, and the formula is expressed as:

[0075]

[0076] wherein , , , , are all fitting parameters, is related to the peak intensity, is related to the peak position, and is related to the peak shape

[0077] (4) Phase clustering analysis: the proportion of the arrangement of each peak position is counted by using the peak position information obtained by fitting. According to the clustering algorithm, the similar arrangement proportion of the atlas is classified into a class. The results after clustering are matched with the phases by referring to the peak position proportion of the common crystal structures such as BCC, FCC, HCP, etc.

[0078] ​(5) Data display: The processed data is plotted and associated with the components to generate a test report. The data results can be used for the iteration of the artificial intelligence model.

[0079] Compared with existing technologies, the batch processing method designed in this invention has two advantages. First, this method can automatically execute the analysis steps of background removal, peak finding, fitting, and phase analysis sequentially, eliminating the need for manual clicking in commercial software, thus enabling rapid processing of large amounts of data. Second, this method uses Gaussian-Lorentzian fitting for peak shape fitting, which is very helpful for the structural analysis of amorphous materials, because the XRD diffraction peaks of amorphous materials are relatively broad, dome-shaped peaks, which are significantly different from those of crystalline materials. The four parameters provided by Gaussian-Lorentzian fitting can effectively capture the detailed changes in the amorphous diffraction peaks, thereby obtaining more quantifiable structural information. Commercial software lacks these functions.

[0080] To better understand the solution of this invention, two specific examples are provided below for brief explanation.

[0081] Example 1: Continuous testing of 3 thin film samples

[0082] The automated system issues an instruction to test three thin film samples using XRD. The testing mode is slightly incident, with a scanning angle of 20-135 degrees, a scanning speed of 20 degrees per minute, and a 19x19 array area scan. Upon receiving the system instruction, the industrial robot's arm moves to the area where the thin film samples are placed, picks up the samples, and places them into the sample tray. The robot sends an instruction to the system, disengaging the XRD chamber door control, and a pneumatic device on the outside of the door opens it. The robotic arm, holding the sample tray, transfers the tray and the thin film samples together into the XRD instrument. Following a designated path, it slowly moves the tray above the internal XRD fixture. The robotic arm then descends vertically, embedding the tray into the XRD fixture, and slowly retracts. The pneumatic device on the outside of the door closes the door, completing the automatic sample placement.

[0083] The industrial robot's vision system opens, detecting the door closing indicator light and sending a test command to the automation system. The automation system then sends the command to the XRD testing software, which automatically initiates optical path correction and array scanning. After several hours of array scanning, the XRD system completes the test, and the high-voltage indicator light goes out. The automation system recognizes the test completion and uploads the test data to the internal server via the local area network, initiating a batch processing program to analyze the data. The program performs background removal, peak finding, and peak shape fitting on the XRD patterns. Figure 9XRD pattern array scan results are shown, each square represents a region of the test results, where the green line is the XRD spectrum, and the red line is the automatic peak search annotation line. The system will perform Gaussian-Lorentz fitting on each diffraction peak to obtain the peak position and peak width. According to the peak position and peak width, the program performs cluster analysis on the alloy phase to obtain the phase classification of each component point, as shown in Figure 10 BCC represents body-centered cubic, HCP represents hexagonal close-packed, MG represents amorphous structure, BCC+HCP represents both body-centered cubic and hexagonal close-packed, and unconfirmed represents that the program cannot classify temporarily. Note that this classification result is based on the analysis of the test results, and the true phase of the material may be affected by texture, test method, etc., which is not within the scope of the present invention. The system generates a test report and stores it in the database, and the test is completed. The system automatically enters a new round of testing, and repeats the above steps to open the hatch and replace the film sample.

[0084] Example 2: Continuous testing of 10 film samples

[0085] The instruction to test 10 block samples by XRD is given in the automated system, the test mode is theta-theta mode, the scan angle is 20-80 degrees, the scan speed is 5 degrees per minute, and the scan mode is single-point scanning. The industrial robot receives the system instruction, and the robot arm goes to the area where the block samples are placed, and clamps the block samples into the block sample tray. The mechanical arm simulates human hand, touches the XRD hatch switch to release the hatch control, and the pneumatic device outside the hatch pushes the hatch open. The mechanical arm clamps the sample tray and transfers the tray and block sample to the inside of the XRD instrument. According to the specified travel route, it is slowly sent to the top of the XRD clamp. Then the mechanical arm descends vertically, embeds the tray into the XRD clamp, and the mechanical arm slowly exits. The pneumatic device outside the hatch pushes the hatch to close, and the automatic sample loading is completed.

[0086] The industrial robot vision recognition is turned on, recognizes that the hatch close indicator light is on, and sends a test instruction to the automated system. The automated system sends a test instruction to the XRD test software, and the XRD system automatically opens the light path correction and performs a single scan. After 20 minutes of array scan, the XRD system completes the test, and the high-voltage indicator light is turned off. The automated system recognizes that the test is completed, uploads the test data to the internal server through the local area network, and calls the phase batch processing program to start data analysis. The program performs background removal, peak search and peak shape fitting on the XRD pattern, as shown in Figure 11 The XRD single scan result is shown. The system generates a test report and stores it in the database, and the test is completed.

[0087] Compared with the prior art, the method has the advantages of strong universality, low cost, full automation of existing XRD equipment, and application to new intelligent laboratories; the overall method is suitable for existing commercial XRD equipment, does not affect the original equipment structure and function, and does not depend on the communication interface service opened by the instrument manufacturer; the sample tray and clamp designed by the application can adapt to different types of samples, such as blocks and films, and the cumbersome sample loading and height correction process is saved; the data batch processing method can process the data collected by the instrument in real time, classify the phases, and speed up the data flow and processing efficiency. Compared with the existing XRD processing software, the batch processing capability of the method is stronger, and it has good adaptability and can automatically read the data generated by different XRD models; the automatic scheme provided by the application can feed back the test results to the artificial intelligence model without human intervention.

[0088] The above has described various embodiments of the application, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles, practical applications or technical improvements in the market of the embodiments, or to enable other ordinary skilled persons in the art to understand the embodiments disclosed herein.

Claims

1. An XRD automated testing system, characterized in that, The system comprises an XRD testing device and an industrial robot, the XRD testing device and the industrial robot are in wireless communication, the XRD testing device is configured with an automatically controlled cabin door, and the industrial robot is configured with a mechanical arm, wherein: The industrial robot is configured to respond to a plurality of sample testing instructions one by one and perform the following steps when responding to each testing instruction: Sampling the current sample to be tested; Sending an opening cabin signal to the XRD testing device to trigger the XRD testing device to open the cabin door; Placing the current sample to be tested into the XRD testing device through the mechanical arm and sending a sample placement completion signal to trigger the XRD testing device to close the cabin door; After identifying that the XRD testing device closes the cabin door, sending a testing start instruction to the XRD testing device to trigger the XRD to start testing; After the industrial robot executes all the testing instructions, sending a testing completion signal to the XRD testing device; The XRD testing device is configured to: Open the cabin door in response to the opening cabin signal; Close the cabin door in response to the sample placement completion signal; Test the sample in response to the testing start instruction to obtain the XRD pattern corresponding to the sample; In response to the testing completion signal, batch process a plurality of XRD patterns to obtain a test report.

2. The system of claim 1, wherein, The automatically controlled cabin door is a double-door, each door is configured with a cylinder, and the cylinders on the two doors are configured to be connected or disconnected through extension and retraction under the control of a remote signal to realize the actions of opening and closing the door, wherein under the control of the opening cabin signal, the connected cylinders on the two doors retract to disconnect to realize the opening action, and under the control of the sample placement completion signal, the connected cylinders on the two doors extend to connect to realize the closing action.

3. The system of claim 1, wherein, The system is also configured with: A sample tray, which is a circular tray, is used to place the sample to be tested so that the mechanical arm can clamp and place it into the XRD testing device.

4. The system of claim 3, wherein, The sample to be tested is in the form of a film or a block; The front of the sample tray is provided with a recess for loading the sample to be tested, the inner side of the recess is provided with a positioning notch for indicating the direction of placing the sample to be tested in the recess, and the edges of the tray are symmetrically provided with two open notches for clamping by the mechanical arm; The back of the sample tray is provided with a triangular protrusion for positioning the sample tray.

5. The system of claim 4, wherein, The XRD testing device is provided with: A tray clamp, which is circular, is used to fix the sample tray, and the front of the tray clamp is provided with a triangular recess coupled with the triangular protrusion on the back of the sample tray.

6. The system according to claim 5, wherein: The sample tray is a Perspex plate; The tray clamp is a metal disc provided with threaded holes around the periphery and fixed in the XRD testing device by bolts.

7. The system of claim 1, wherein, The XRD testing device is configured to batch process a plurality of XRD patterns in the following manner: Perform background removal operation on a plurality of XRD pattern data to obtain XRD signals after background removal; Perform peak searching operation on the XRD signals after background removal to obtain a plurality of peak values; Perform fitting operation on the obtained peak types to obtain peak position information; Perform phase clustering analysis using the fitted peak position information; Correlate the phase clustering analysis result with the composition to obtain an analysis result.

8. The system of claim 1, wherein, The XRD testing device is configured to perform background removal on the XRD pattern data in the following manner: divide the XRD pattern data into 30 equal parts, average the data of each equal part and take the average as an anchor point of the part; Each anchor point is converted to a background index point by : wherein is the x-coordinate of the i-th anchor point, is the y-coordinate of the i-th anchor point, and perform linear interpolation based on all the background anchor points to obtain a background signal, and perform background signal deduction on the XRD pattern data based on the obtained background signal to obtain the XRD signal after background removal.

9. The system of claim 8, wherein, The XRD testing device is configured to perform peak searching on the XRD signal after background removal according to a preset crystal peak signal criterion, wherein the preset crystal peak signal criterion is: wherein, , , The values are all preset parameters, wherein, is a signal smoothing processing value range, is a signal range for finding a local maximum value, is a determination threshold value.

10. The system of claim 9, wherein, y=5, W=50, and T=6σ, wherein σ is the data standard deviation of the signal noise part.

11. The system of claim 10, wherein, The XRD testing device is configured to perform fitting on the peak type by using a Gaussian-Lorentzian method.

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