Method for identifying microcrystalline particles and method for collecting microcrystalline electron diffraction data and related products

Abstract

The present application relates to a method for identifying microcrystalline particles and a method for collecting microcrystalline electron diffraction data and related products. The method for identifying microcrystalline particles includes: controlling a transmission electron microscope to collect a grid map image of a grid in a first shooting mode; identifying target microcrystalline particles in the grid map image, and obtaining the initial coordinates of the target microcrystalline particles; based on the initial coordinates of the target microcrystalline particles, controlling the transmission electron microscope to collect a particle morphology image of the target microcrystalline particles in a third shooting mode, and determining the precise coordinates of the target microcrystalline particles based on the particle morphology image. The solution provided by the present application can reduce labor costs and time costs, and can improve the reproducibility of the experiment.

Description

Technical Field

[0001] The present application relates to the field of microcrystalline electron diffraction technology, and in particular to a method for identifying microcrystalline particles and a method for collecting microcrystalline electron diffraction data and related products. Background Art

[0002] Microcrystal electron diffraction (MicroED) is a crystal structure determination technology based on the electron diffraction method of transmission electron microscope (TEM). It uses electrons as the incident light beam, transmits the electron beam through microcrystalline particles with a three-dimensional periodic structure, and rotates the microcrystalline particles at the same time. A series of electron diffraction images of the rotating microcrystalline particles are collected through the TEM detector. By processing and analyzing these diffraction images, the three-dimensional crystal structure of the microcrystalline particles can be determined quickly and with high resolution.

[0003] Among them, the premise of collecting diffraction images is to locate the target microcrystalline particles in the map image of the entire carrier network. However, the relevant technology requires manual search and selection of target microcrystalline particles in the map image, which requires a lot of manpower and time, increases labor costs and time costs, and the subsequent collected diffraction images are easily affected by the tendency of human selection, reducing the reproducibility of the experiment. Summary of the invention

[0004] In order to solve or partially solve the problems existing in the related art, the present application provides a method for identifying microcrystalline particles and a method for collecting microcrystalline electron diffraction data and related products, which can reduce labor costs and time costs and improve the reproducibility of experiments.

[0005] The first aspect of the present application provides a method for identifying microcrystalline particles, comprising:

[0006] Control the transmission electron microscope to collect a grid map image of a grid in a first shooting mode, wherein a plurality of microcrystalline particles are distributed on the grid;

[0007] Identify the target microcrystalline particles in the grid map image, and obtain the initial coordinates of the target microcrystalline particles;

[0008] Based on the initial coordinates of the target microcrystalline particles, the transmission electron microscope is controlled to collect a particle morphology picture of the target microcrystalline particles in a third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology picture.

[0009] In one embodiment, the grid is placed on a movable sample stage, and the grid includes a plurality of regions; and the step of identifying target microcrystalline particles in the grid map image includes:

[0010] Identify at least one of the areas from the network map image, and obtain the coordinates of the center point of the identified area;

[0011] Adjusting the transmission electron microscope to a second shooting mode required for the shooting area;

[0012] Control the sample stage to move to the center point coordinates of at least one of the areas, and control the transmission electron microscope to collect a regional morphology image of the corresponding area under the second shooting mode, and identify at least one target microcrystalline particle in the regional morphology image; wherein the target microcrystalline particle is a microcrystalline particle among the multiple microcrystalline particles that meets a preset size range.

[0013] In one embodiment, controlling the transmission electron microscope to collect a grid map image of the grid in the first shooting mode includes:

[0014] The transmission electron microscope is adjusted to a first shooting mode required for shooting the grid;

[0015] The sample stage is controlled to move to different positions in sequence, and the transmission electron microscope is controlled to collect grid map images when the grid is located at the different positions in the first shooting mode.

[0016] In one embodiment, identifying at least one of the regions from the network map image and obtaining the coordinates of the center point of the identified region includes:

[0017] Identify a plurality of the regions from each of the network map images, and obtain the coordinates of the center point of each of the identified regions;

[0018] The step of controlling the sample stage to move to the center point coordinates of at least one of the regions, controlling the transmission electron microscope to collect a regional morphology image of the corresponding region in the second shooting mode, and identifying at least one target microcrystalline particle in the regional morphology image comprises:

[0019] Select at least some of the identified regions as target regions, and record the coordinates of the center point of each target region in a target region list;

[0020] Controlling the sample stage to move to any of the center point coordinates in the target area list, and controlling the transmission electron microscope to collect a regional morphology image of the current target area in the second shooting mode;

[0021] Identify at least one target microcrystalline particle in the current regional morphology image;

[0022] Each center point coordinate in the target area list is traversed until the target microcrystalline particles in all the target areas are identified.

[0023] In one embodiment, the identifying at least one target microcrystalline particle in the regional topography image comprises:

[0024] Identifying a plurality of microcrystalline particles contained in the regional topography image according to a difference in grayscale values ​​of pixels in the regional topography image;

[0025] Microcrystalline particles that meet a preset size range are determined from the plurality of microcrystalline particles, and the microcrystalline particles that meet the preset size range are used as target microcrystalline particles.

[0026] In one embodiment, the grid is placed on a movable sample stage, and the grid includes a plurality of regions; based on the initial coordinates of the target microcrystalline particles, the transmission electron microscope is controlled to collect a particle morphology image of the target microcrystalline particles in a third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology image, including:

[0027] Adjusting the transmission electron microscope to a third shooting mode required for shooting microcrystalline particles;

[0028] Determine the concentric height of the target area where the target microcrystalline particles are located, and control the height of the sample stage to be adjusted to the concentric height;

[0029] According to the initial coordinates of the target microcrystalline particles and the concentric height, the transmission electron microscope is controlled to collect a particle morphology image of the target microcrystalline particles in the third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology image.

[0030] In one embodiment, determining the concentric height of the target region where the target microcrystalline particles are located includes:

[0031] determining reference target microcrystalline particles in the target area;

[0032] Controlling the sample stage to move to the initial coordinates of the reference target microcrystalline particles, and controlling the transmission electron microscope to collect a particle morphology picture of the reference target microcrystalline particles in the third shooting mode, and determining the reference coordinates of the reference target microcrystalline particles based on the particle morphology picture;

[0033] Based on the reference coordinates of the reference target microcrystalline particles, the concentric height of the target area is determined.

[0034] In one embodiment, determining the reference target microcrystalline particles in the target area includes:

[0035] If there is only one target microcrystalline particle in the target area, the target microcrystalline particle is used as a reference target microcrystalline particle;

[0036] If there are a plurality of target microcrystalline particles in the target region, a target microcrystalline particle with the smallest coordinate distance from the center point of the target region is selected as a reference target microcrystalline particle.

[0037] In one embodiment, adjusting the photographing mode of the transmission electron microscope includes:

[0038] Adjust the shooting parameters of the transmission electron microscope to obtain a corresponding shooting mode; wherein the shooting parameters include at least one of magnification, C2 aperture model, spotsize value, intensity value, exposure time, and working mode.

[0039] The second aspect of the present application provides a method for collecting microcrystal electron diffraction data, comprising:

[0040] Obtaining precise coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method as described in any one of the above items;

[0041] According to the precise coordinates of each target microcrystalline particle, the transmission electron microscope is controlled to collect corresponding diffraction data.

[0042] The third aspect of the present application provides a device for identifying microcrystalline particles, comprising:

[0043] A grid map image acquisition module, used to control the transmission electron microscope to acquire a grid map image of a grid in a first shooting mode, wherein a plurality of microcrystalline particles are distributed on the grid;

[0044] A target microcrystalline particle identification module is used to identify the target microcrystalline particles in the grid map image and obtain the initial coordinates of the target microcrystalline particles;

[0045] The precise coordinate determination module is used to control the transmission electron microscope to collect a particle morphology image of the target microcrystalline particle in a third shooting mode based on the initial coordinates of the target microcrystalline particle, and determine the precise coordinates of the target microcrystalline particle based on the particle morphology image.

[0046] A fourth aspect of the present application provides a device for collecting microcrystal electron diffraction data, comprising:

[0047] An accurate coordinate acquisition module, used for obtaining accurate coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method as described in any one of the above items;

[0048] The diffraction data acquisition module is used to control the transmission electron microscope to collect corresponding diffraction data according to the precise coordinates of each target microcrystalline particle.

[0049] A fifth aspect of the present application provides an electronic device, including:

[0050] Processor; and

[0051] A memory having executable codes stored thereon, which, when executed by the processor, causes the processor to execute the method for identifying microcrystalline particles as described in any one of the above items or the method for collecting microcrystalline electron diffraction data as described above.

[0052] The sixth aspect of the present application provides a computer-readable storage medium having executable code stored thereon. When the executable code is executed by a processor of an electronic device, the processor executes the method for identifying microcrystalline particles as described in any one of the above items or the method for collecting microcrystalline electron diffraction data as described above.

[0053] The technical solution provided by this application may have the following beneficial effects:

[0054] The solution provided by the present application controls the transmission electron microscope to collect a grid map image of the grid in the first shooting mode; identifies the target microcrystalline particles in the grid map image, and obtains the initial coordinates of the target microcrystalline particles; based on the initial coordinates of the target microcrystalline particles, controls the transmission electron microscope to collect the particle morphology image of the target microcrystalline particles in the third shooting mode, and determines the precise coordinates of the target microcrystalline particles based on the particle morphology image. The present application can automatically identify the target microcrystalline particles on the grid without human intervention, thereby reducing labor costs and time costs, and reducing the influence of human selection tendency, thereby improving the reproducibility of the experiment.

[0055] It should be understood that the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the present application. BRIEF DESCRIPTION OF THE DRAWINGS

[0056] The above and other objects, features and advantages of the present application will become more apparent by describing in more detail the exemplary embodiments of the present application in conjunction with the accompanying drawings, wherein the same reference numerals generally represent the same components in the exemplary embodiments of the present application.

[0057] Figure 1 is a schematic flow chart of a method for identifying microcrystalline particles shown in an embodiment of the present application;

[0058] Figure 2 is another schematic flow chart of a method for identifying microcrystalline particles shown in an embodiment of the present application;

[0059] Figure 3It is a schematic flow chart of a method for collecting microcrystal electron diffraction data shown in an embodiment of the present application;

[0060] Figure 4 is a schematic diagram of identifying an area in a network map image shown in an embodiment of the present application;

[0061] Figure 5 is a schematic diagram of identifying target microcrystalline particles in a regional morphology image according to an embodiment of the present application;

[0062] Figure 6 is a schematic diagram of a particle morphology picture of a target microcrystalline particle shown in an embodiment of the present application;

[0063] Figure 7 is a schematic structural diagram of a device for identifying microcrystalline particles shown in an embodiment of the present application;

[0064] Figure 8 is a schematic structural diagram of a device for collecting microcrystal electron diffraction data shown in an embodiment of the present application;

[0065] Fig. 9 It is a schematic diagram of the structure of an electronic device shown in an embodiment of the present application. DETAILED DESCRIPTION

[0066] The embodiments of the present application will be described in more detail below with reference to the accompanying drawings. Although the embodiments of the present application are shown in the accompanying drawings, it should be understood that the present application can be implemented in various forms and should not be limited by the embodiments described herein. On the contrary, these embodiments are provided to make the present application more thorough and complete, and to fully convey the scope of the present application to those skilled in the art.

[0067] The terms used in this application are for the purpose of describing specific embodiments only and are not intended to limit this application. The singular forms of "a", "said" and "the" used in this application and the appended claims are also intended to include plural forms unless the context clearly indicates other meanings. It should also be understood that the term "and / or" used herein refers to and includes any or all possible combinations of one or more associated listed items.

[0068] It should be understood that although the terms "first", "second", "third", etc. may be used in this application to describe various information, this information should not be limited to these terms. These terms are only used to distinguish the same type of information from each other. For example, without departing from the scope of this application, the first information may also be referred to as the second information, and similarly, the second information may also be referred to as the first information. Thus, the features defined as "first" and "second" may explicitly or implicitly include one or more of the features. In the description of this application, the meaning of "multiple" is two or more, unless otherwise clearly and specifically defined.

[0069] In the related technology, it is necessary to manually search and select the target microcrystalline particles in the map image, which requires a lot of manpower and time, increases labor costs and time costs, and the diffraction images collected subsequently are easily affected by the tendency of human selection, reducing the reproducibility of the experiment.

[0070] In response to the above problems, an embodiment of the present application provides a method for identifying microcrystalline particles, which can automatically identify target microcrystalline particles on a carrier grid without human intervention, thereby reducing labor costs and time costs, and reducing the impact of human selection tendencies, thereby improving the reproducibility of the experiment.

[0071] The technical solution of the embodiments of the present application is described in detail below with reference to the accompanying drawings.

[0072] Figure 1 It is a schematic flow chart of the method for identifying microcrystalline particles shown in an embodiment of the present application.

[0073] See also Figure 1 The method for identifying microcrystalline particles of the present application comprises:

[0074] S110, controlling the transmission electron microscope to collect a grid map image of the grid in a first shooting mode, where a plurality of microcrystalline particles are distributed on the grid.

[0075] In the embodiment of the present application, it can be applied to the microcrystalline electron diffraction collection system. The embodiment of the present application can use the TEM control interface and modify the open source script of the Instamatic software (Instamatic software is a software that controls TEM to collect MicroED data), so as to configure the automatic execution script in the microcrystalline electron diffraction collection system. Among them, the automatic execution script is a computer program, which consists of a series of instructions and can be used to automatically perform a series of operations in the MicroED experimental environment, including but not limited to: adjusting the shooting mode, identifying the area on the carrier, identifying the target microcrystalline particles on the area, collecting MicroED data, etc.

[0076] In a specific implementation, after receiving the "start" command, the microcrystalline electron diffraction collection system can trigger an automated script execution, so that the TEM can be controlled by the automated script execution to collect the grid map image of the grid, and the grid map image can include at least one. Among them, the grid is a substrate for carrying microcrystalline powder samples, which can be composed of a circular metal grid hollow sheet with a diameter of 3.05mm and a carbon film covered thereon. Copper or gold is commonly used as the metal material, and other new alloys such as molybdenum can also be used as the metal material. The microcrystalline powder sample is attached to the carbon film. Among them, the microcrystalline powder sample is composed of multiple microcrystalline particles.

[0077] S120, identifying target microcrystalline particles in the grid map image, and obtaining initial coordinates of the target microcrystalline particles.

[0078] There are multiple microcrystalline particles attached to the grid. The automated execution script can identify multiple microcrystalline particles in the grid map image. Since microcrystalline particles that are too large or too small are not suitable for subsequent MicroED experiments, the automated execution script can screen out target microcrystalline particles that meet the preset size range from the multiple identified microcrystalline particles.

[0079] S130, based on the initial coordinates of the target microcrystalline particles, controlling the transmission electron microscope to collect a particle morphology image of the target microcrystalline particles in a third shooting mode, and determining the precise coordinates of the target microcrystalline particles based on the particle morphology image.

[0080] The size of the microcrystalline particles is much smaller than that of the grid. In order to optimize the imaging effect of TEM, the automated execution script can adjust the TEM to the third shooting mode required for shooting microcrystalline particles, and then control the TEM to collect the particle morphology image of the target microcrystalline particles in the third shooting mode based on the initial coordinates of the target microcrystalline particles, so as to determine the precise coordinates of the target microcrystalline particles based on the particle morphology image. In this way, in the subsequent MicroED data collection process, the target microcrystalline particles can be accurately located through the precise coordinates of the target microcrystalline particles.

[0081] As can be seen from this example, the solution provided by the present application controls the transmission electron microscope to collect the grid map image of the grid in the first shooting mode; identifies the target microcrystalline particles in the grid map image, and obtains the initial coordinates of the target microcrystalline particles; based on the initial coordinates of the target microcrystalline particles, controls the transmission electron microscope to collect the particle morphology image of the target microcrystalline particles in the third shooting mode, and determines the precise coordinates of the target microcrystalline particles based on the particle morphology image. The present application automatically identifies the target microcrystalline particles on the grid by calling a program without human intervention, thereby reducing labor costs and time costs, and reducing the influence of human selection tendencies, thereby improving the reproducibility of the experiment.

[0082] Figure 2 It is another schematic flow chart of the method for identifying microcrystalline particles shown in the embodiment of the present application.

[0083] See also Figure 2 The method for identifying microcrystalline particles of the present application comprises:

[0084] S210, controlling the transmission electron microscope to collect a grid map image of the grid in a first shooting mode, wherein the grid is placed on a movable sample stage, and the grid includes a plurality of regions and has a plurality of microcrystalline particles distributed thereon.

[0085] It should be noted that the model of TEM used in the related art is JEOL JEM-2100 electron microscope, so some modules in the related art are not applicable to Glacios electron microscope (cryo transmission electron microscope). For this, the embodiment of the present application can use the TEM control interface and modify the open source script of Instamatic software, so as to configure the microcrystalline electron diffraction collection system to obtain an automated execution script suitable for Glacios electron microscope, so the type of TEM used in the embodiment of the present application can be Glacios electron microscope. In addition, the type of TEM used in the embodiment of the present application can also be a transmission electron microscope at room temperature, and the embodiment of the present application does not limit this.

[0086] Before taking different types of images (such as grid map images, regional morphology images, and particle morphology images), the automated execution script can control the TEM (such as the Glacios electron microscope) to adjust the TEM's shooting mode according to the set program to meet the shooting requirements of the current type of image.

[0087] In one embodiment, adjusting the photographing mode of the transmission electron microscope may include:

[0088] Adjust the shooting parameters of the transmission electron microscope to obtain a corresponding shooting mode; wherein the shooting parameters may include but are not limited to at least one of magnification, C2 aperture model, spotsize value, intensity value, exposure time, working mode, etc.

[0089] The working mode may include a microprobe mode or a nanoprobe mode. The microprobe mode and the nanoprobe mode correspond to two different sizes of electron beam irradiation areas. The microprobe mode and the nanoprobe mode can exist in both the shooting mode and the diffraction mode. The shooting mode refers to the mode of shooting the grid map picture, the regional morphology picture, and the particle morphology picture. The diffraction mode refers to the mode of collecting MicroED data. For example, the microprobe mode can be selected in the shooting mode, and the nanoprobe mode can be selected in the diffraction mode. The embodiment of the present application does not limit this.

[0090] In one embodiment, controlling the transmission electron microscope to collect a grid map image of the grid in the first shooting mode may include:

[0091] The transmission electron microscope is adjusted to a first shooting mode required for shooting the grid; the sample stage is controlled to move to different positions in sequence, and the transmission electron microscope is controlled to collect grid map images when the grid is located at different positions under the first shooting mode.

[0092] The automated execution script can adjust the TEM to the shooting parameters required for shooting the grid, for example, the magnification of the TEM can be adjusted to the first magnification. For example, the first magnification can be set to 155X (times), so that the TEM (such as a Glacios electron microscope) can be adjusted to the first shooting mode with a magnification of 155X.

[0093] In addition, the automated execution script can also adjust the C2 aperture model, spotsize value, intensity value, exposure time and working mode of the TEM. For example, the C2 aperture model of the TEM can be adjusted to 150, the spotsize value can be adjusted to 8, the intensity value can be adjusted to 1.024, the exposure time can be adjusted to 1s (second), and the microprobe mode can be selected to obtain the first shooting mode, so that the TEM can collect the grid map image of the grid in the first shooting mode.

[0094] In order to collect complete information of the entire grid as much as possible, the automated execution script can control the sample stage to move to different positions in sequence, so as to control the TEM to collect grid map images when the grid is located at different positions in the first shooting mode, thereby obtaining multiple grid map images, each of which can contain a part of the characteristics of the grid. Among them, the moving position and trajectory of the sample stage can be set in advance, so as to be able to capture the entire grid as much as possible, and this application does not limit this.

[0095] In the process of collecting grid map images, the optical path position of TEM can remain unchanged. It is only necessary to control the sample stage to move to different positions, so that TEM can collect grid map images at different positions.

[0096] It should be noted that, for the convenience of display, the embodiment of the present application can splice multiple network map images to obtain a total network map image with a larger data area. Of course, splicing is also possible, and the embodiment of the present application does not limit this.

[0097] S220, identifying at least one area from the network map image, and obtaining the coordinates of the center point of the identified area.

[0098] In one embodiment, when multiple network map images are collected during step S210, step S220 may specifically include: identifying multiple areas from each network map image, and obtaining the coordinates of the center point of each identified area.

[0099] The carrier grid may include multiple squares (areas), and a square may be regarded as an area enclosed by a metal grid on the carrier grid.

[0100] The automated execution script can perform target shape edge recognition on each grid map image based on the skimage morphology library, thereby obtaining multiple squares contained in each grid map image. Among them, the skimagemorphology library is mainly used for morphological image processing. In the specific implementation, the automated execution script can identify the grayscale value of each pixel in each grid map image, and then calculate the grayscale value difference of each pixel in each grid map image, so as to find the boundary with the largest grayscale value difference from each grid map image. The boundary found in the grid map image is the edge of the square, thereby obtaining multiple squares contained in each grid map image, and then obtaining the coordinates of the center point of each identified square.

[0101] S230, adjusting the transmission electron microscope to a second shooting mode required for the shooting area.

[0102] The size of the square is much smaller than that of the grid. In order to optimize the imaging effect of the TEM, the automated execution script can adjust the TEM to the second shooting mode required for the shooting area, for example, by adjusting the magnification of the TEM to the second magnification. The second magnification is greater than the first magnification, for example, the second magnification can be set to 700X, so that the TEM (such as the Glacios electron microscope) can be adjusted to the second shooting mode with a magnification of 700X.

[0103] In addition, the automated execution script can also adjust the C2 aperture model, spotsize value, intensity value, exposure time and working mode of the TEM. For example, the C2 aperture model of the TEM can be adjusted to 50, the spotsize value can be adjusted to 8, the intensity value can be adjusted to 0.898, the exposure time can be adjusted to 1s, and the microprobe mode can be selected to obtain the second shooting mode, so that the TEM can collect regional morphology images of the square in the second shooting mode.

[0104] S240, controlling the sample stage to move to the center point coordinates of at least one area, and controlling the transmission electron microscope to collect a regional morphology image of the corresponding area in a second shooting mode, and identifying at least one target microcrystalline particle in the regional morphology image; wherein the target microcrystalline particle is a microcrystalline particle in a plurality of microcrystalline particles that meets a preset size range.

[0105] The entire metal grid of the carrier grid is covered with a carbon film, and a plurality of microcrystalline particles are distributed on the carbon film, so a plurality of squares are distributed with a plurality of microcrystalline particles.

[0106] In a specific implementation, the automated execution script can control the sample stage to move to the sample stage coordinates corresponding to the center point coordinates of each square in turn. Whenever the sample stage reaches the sample stage coordinates corresponding to a center point coordinate, the automated execution script can control the TEM to collect the regional morphology image of the square at the current position in the second shooting mode, and then identify the multiple microcrystalline particles contained in the square from the current regional morphology image. Since microcrystalline particles that are too large and too small are not suitable for subsequent MicroED experiments, the automated execution script can screen out at least one target microcrystalline particle that meets the preset size range from the multiple microcrystalline particles currently identified.

[0107] In this way, each center point coordinate is traversed to obtain the regional morphology image of each square in turn, and then multiple microcrystalline particles in each regional morphology image are identified in turn, and then at least one target microcrystalline particle that meets the preset size range is screened out from the identified multiple microcrystalline particles in turn.

[0108] In one embodiment, step S240 controls the sample stage to move to the center point coordinates of at least one region, controls the transmission electron microscope to collect a regional morphology image of the corresponding region in the second shooting mode, and identifies at least one target microcrystalline particle in the regional morphology image, which may include:

[0109] At least part of the identified multiple areas are selected as target areas, and the center point coordinates of each target area are recorded in the target area list; the sample stage is controlled to move to any center point coordinate in the target area list, and the transmission electron microscope is controlled to collect a regional morphology image of the current target area in the second shooting mode; at least one target microcrystalline particle in the current regional morphology image is identified; each center point coordinate in the target area list is traversed until the target microcrystalline particles in all target areas are identified.

[0110] In one example, in order to improve the efficiency and quality of data collection, the automated execution script can randomly select some squares from the identified squares as target squares, or select squares with N (N is a positive integer greater than or equal to 1) or more target microcrystalline particles from the identified squares as target squares, or select squares located near the middle of the corresponding grid map image (such as within a preset radius of the center point coordinates of the corresponding grid map image) from the identified squares as target squares, or select squares with complete area edges from the identified squares as target squares, etc. Then the center point coordinates of each target square are recorded in the target square list.

[0111] In another example, in order to cover all target microcrystalline particles, the automated execution script may also select all squares from the identified squares as target squares, and then record the coordinates of the center point of each target square into the target square list.

[0112] The target square list may be referred to as a square list to be tested, that is, the automated execution script needs to perform particle recognition processing on each target square in the target square list.

[0113] After forming the target square list, the automated execution script can control the sample stage to move to the center point coordinates of any target square in the target square list. In a specific implementation, the automated execution script can first select the center point coordinates of any target square from the target square list, and then control the sample stage to move from the current coordinates to the center point coordinates of the target square, so that the target square can be within the field of view of the TEM. At this time, the automated execution script can control the TEM to collect the regional morphology image of the target square at the current position in the second shooting mode, and then identify the multiple microcrystalline particles contained in the target square from the current regional morphology image through the particle recognition algorithm, and then screen out at least one target microcrystalline particle that meets the preset size range based on the size of each microcrystalline particle.

[0114] In this way, the center point coordinates of each target square in the target square list are traversed to obtain the regional morphology images of each target square in turn, and then the multiple microcrystalline particles in each regional morphology image are identified in turn, and then at least one target microcrystalline particle that meets the preset size range is screened out from the identified multiple microcrystalline particles in turn, until the target microcrystalline particles in all target squares are identified.

[0115] In one embodiment, identifying at least one target microcrystalline particle in a regional topography image may include:

[0116] According to the gray value difference of each pixel in the regional morphology image, multiple microcrystalline particles contained in the regional morphology image are identified; microcrystalline particles that meet a preset size range are determined from the multiple microcrystalline particles, and the microcrystalline particles that meet the preset size range are used as target microcrystalline particles.

[0117] The automated execution script can perform target shape edge recognition on the current region morphology image based on the skimage morphology library, thereby obtaining multiple microcrystalline particles contained in the current region morphology image. In a specific implementation, the automated execution script can identify the gray value of each pixel in the current region morphology image, and then calculate the gray value difference of each pixel in the current region morphology image, so as to find the boundary with the largest gray value difference from the current region morphology image. The boundary found in the current region morphology image is the edge of the microcrystalline particle, thereby obtaining multiple microcrystalline particles contained in the current region morphology image.

[0118] Since microcrystalline particles that are too large or too small are not suitable for subsequent MicroED experiments, the automated execution script can identify the size of each microcrystalline particle and then determine whether the size of each microcrystalline particle meets the preset size range. If the size of a microcrystalline particle does not meet the preset size range, the microcrystalline particle will not be processed subsequently; if the size of a microcrystalline particle meets the preset size range, the microcrystalline particle will be screened as a target microcrystalline particle so that the target microcrystalline particle can be processed subsequently.

[0119] S250, obtaining the initial coordinates of each target microcrystalline particle.

[0120] In one embodiment, the method may further include:

[0121] The initial coordinates of each target microcrystal particle are recorded in the target microcrystal particle list.

[0122] Whenever at least one target microcrystalline particle is identified in the current area morphology image, the automated execution script can obtain the initial coordinates of each target microcrystalline particle, and then record the currently obtained initial coordinates into the target microcrystalline particle list until the initial coordinates of all target microcrystalline particles have been recorded in the target microcrystalline particle list.

[0123] Since the initial coordinates are obtained based on the second photographing mode, the initial coordinates can be considered as rough coordinates, and thus the target microcrystalline particle list can be called a rough particle coordinate list.

[0124] S260, based on the initial coordinates of the target microcrystalline particles, controlling the transmission electron microscope to collect a particle morphology image of the target microcrystalline particles in a third shooting mode, and determining the precise coordinates of the target microcrystalline particles based on the particle morphology image.

[0125] This step may specifically include: adjusting the transmission electron microscope to the third shooting mode required for photographing microcrystalline particles; determining the concentric height of the target area where the target microcrystalline particles are located, and controlling the height of the sample stage to be adjusted to the concentric height; according to the initial coordinates and concentric height of the target microcrystalline particles, controlling the transmission electron microscope to collect particle morphology images of the target microcrystalline particles in the third shooting mode, and determining the precise coordinates of the target microcrystalline particles based on the particle morphology images.

[0126] The size of the microcrystalline particles is much smaller than the size of the square. In order to optimize the imaging effect of the TEM, the automated execution script can adjust the TEM to the third shooting mode required for shooting the microcrystalline particles, for example, by adjusting the magnification of the TEM to the third magnification. The third magnification is respectively greater than the first magnification and the second magnification, for example, the third magnification can be set to 4300X, so that the TEM (such as the Glacios electron microscope) can be adjusted to the third shooting mode with a magnification of 4300X.

[0127] In addition, the automated execution script can also adjust the C2 aperture model, spotsize value, intensity value, exposure time and working mode of the TEM. For example, the C2 aperture model of the TEM can be adjusted to 100, the spotsize value can be adjusted to 8, the intensity value can be adjusted to 0.617, the exposure time can be adjusted to 1s, and the microprobe mode can be selected to obtain a third shooting mode, so that the TEM can collect particle morphology images of the target microcrystalline particles in the third shooting mode.

[0128] Since the subsequent MicroED data collection is completed during the rotation of the target microcrystal particles, that is, the sample stage drives the target microcrystal particles to rotate, the position of the target microcrystal particles is required not to change during this process. Generally, if the height of the target microcrystal particles is not on the rotation axis, the horizontal position of the target microcrystal particles in the field of view of the fluorescent screen will change during the rotation of the target microcrystal particles driven by the sample stage. Therefore, the automated execution script can first determine the concentric height of the target area where the target microcrystal particles are located, and then control the vertical height of the sample stage (i.e., the Z-axis coordinate) to be adjusted to the currently determined concentric height.

[0129] The concentric height is the vertical coordinate required to keep the target microcrystalline particles from shifting left and right in the field of view of the fluorescent screen during the rotation of the sample stage. Generally, the surface of the grid in the same target square is roughly flat, so it can be assumed that the Z-axis coordinates of all target microcrystalline particles in the same target square are the same. Therefore, for all target microcrystalline particles in the same target square, it is only necessary to adjust the concentric height once.

[0130] After controlling the vertical height of the sample stage to be adjusted to the currently determined concentric height, the Z-axis coordinates of all target microcrystalline particles in the current target square are accurate. However, since the X-axis coordinates and Y-axis coordinates are obtained based on the second shooting mode, the X-axis coordinates and Y-axis coordinates of all target microcrystalline particles in the current target square are rough. Therefore, the automated execution script can adjust the X-axis coordinates and Y-axis coordinates of all target microcrystalline particles in the current target square. In a specific implementation, after controlling the vertical height of the sample stage to be adjusted to the currently determined concentric height Z', the automated execution script can first select (X0, Y0) from the target microcrystal particle list of any target microcrystal particle belonging to the current target square; control the sample stage to move to the coordinates (X0, Y0, Z') so that the target microcrystal particle can be within the field of view of the TEM; the automated execution script can control the TEM to collect a particle morphology image of the current target microcrystal particle under the third shooting mode, so as to determine the precise coordinates (X', Y', Z') of the current target microcrystal particle based on the particle morphology image. Compared with the initial coordinates (X0, Y0, Z0) obtained under the second shooting mode, the precise coordinates (X', Y', Z') currently obtained under the third shooting mode are more accurate.

[0131] In this way, the initial coordinates of each target microcrystalline particle in the current target square are traversed to obtain the precise coordinates of each target microcrystalline particle in the current target square in turn, until the precise coordinates of all target microcrystalline particles in the current target square are obtained.

[0132] In the above manner, the initial coordinates of each target microcrystalline particle in each target square are traversed to obtain the precise coordinates of each target microcrystalline particle in each target square in turn, until the precise coordinates of all target microcrystalline particles in all target squares are obtained.

[0133] In one example, assuming that the target square list includes target square1 and target square2, where target square1 includes two target microcrystalline particles (particle A and particle B), and target square2 includes three target microcrystalline particles (particles C to E), the automated execution script can start the traversal of target square1: the automated execution script can determine the concentric height of target square1, assuming that the concentric height of target square1 is Z1', the automated execution script can control the vertical height of the sample stage to be adjusted to the concentric height Z1'; then obtain the initial coordinates of particle A (X A0 ,Y A0 ), and then control the sample stage to move from the current coordinate to the coordinate (X A0 ,YA0 , Z1'), so that the particle A can be within the field of view of the TEM; the automated execution script can control the TEM to collect the particle morphology image ImageA of the particle A in the third shooting mode of 4300X, so as to determine the precise coordinates (X) of the particle A based on the particle morphology image ImageA. A ',Y A ',Z1'); Then, the automated execution script can obtain the initial coordinates of particle B (X B0 ,Y B0 ), and then control the sample stage to move from the current coordinate to the coordinate (X B0 ,Y B0 , Z1'), so that the particle B can be within the field of view of the TEM; the automated execution script can control the TEM to collect the particle morphology image ImageB of the particle B in the third shooting mode of 4300X, so as to determine the precise coordinates (X) of the particle B based on the particle morphology image ImageB. B ',Y B ', Z1'). The traversal of target square 1 ends, and the traversal of target square 2 begins. The traversal process of target square 2 is the same as that of target square 1, and will not be repeated here.

[0134] In one embodiment, determining the concentric height of the target region where the target microcrystalline particles are located may include:

[0135] Determine the reference target microcrystalline particles in the target area; control the sample stage to move to the initial coordinates of the reference target microcrystalline particles, and control the transmission electron microscope to collect particle morphology images of the reference target microcrystalline particles in a third shooting mode, and determine the reference coordinates of the reference target microcrystalline particles based on the particle morphology images; determine the concentric height of the target area based on the reference coordinates of the reference target microcrystalline particles.

[0136] In one embodiment, determining a reference target microcrystalline particle in a target area may include:

[0137] If there is only one target microcrystalline particle in the target area, the target microcrystalline particle is used as the reference target microcrystalline particle; if there are multiple target microcrystalline particles in the target area, the target microcrystalline particle with the smallest coordinate distance from the center point of the target area is selected as the reference target microcrystalline particle.

[0138] If the target square includes only one target microcrystalline particle, the automated execution script can directly use the target microcrystalline particle as the reference target microcrystalline particle. The determination of the precise coordinates of the reference target microcrystalline particle can be based on the aforementioned step of "according to the initial coordinates and concentric height of the target microcrystalline particle (here, the reference target microcrystalline particle), controlling the transmission electron microscope to collect the particle morphology picture of the target microcrystalline particle in the third shooting mode, and determining the precise coordinates of the target microcrystalline particle based on the particle morphology picture"; it can also be obtained based on the reference coordinates and concentric height of the reference target microcrystalline particle, for example, replacing the Z coordinate in the reference coordinates with the concentric height to obtain the precise coordinates, or, according to the reference coordinates and concentric height of the reference target microcrystalline particle, controlling the transmission electron microscope to collect the particle morphology picture of the target microcrystalline particle in the third shooting mode, and determining the precise coordinates of the target microcrystalline particle based on the particle morphology picture.

[0139] If the target square includes multiple target microcrystalline particles, since the surface of the carrier grid in the same target square is not as flat as in the ideal situation, the concentric heights of the target microcrystalline particles at different positions in the same target square may not be completely consistent. In this regard, the embodiment of the present application can use the target microcrystalline particles located near the center of the target square as the reference target microcrystalline particles, and then use the concentric height of the reference target microcrystalline particles as the concentric height of the target square, so that the error can be minimized. There are two main reasons for this: first, the target microcrystalline particles located near the center of the target square will not run out of the field of view of the fluorescent screen during small-angle rotation; second, the distance between the target microcrystalline particles located near the center of the target square and the target microcrystalline particles at other positions in the target square is relatively average.

[0140] In a specific implementation, the automated execution script can calculate the distances between the center point coordinates of the current target square and the initial coordinates of each target microcrystalline particle belonging to the current target square, and then use the target microcrystalline particle with the smallest distance as the reference target microcrystalline particle of the current target square, and then determine the concentric height of the reference target microcrystalline particle that remains unchanged during the rotation process, so that the concentric height of the reference target microcrystalline particle is used as the concentric height of the current target square. For example, assuming that the target square 1 contains 2 target microcrystalline particles (particle A and particle B), the automated execution script can calculate the distance D between the center point coordinates of the target square 1 and the initial coordinates of particle A. A , and the distance D between the center point coordinates of the target square 1 and the initial coordinates of particle B can be calculated B , if the distance D A Less than distance D B, it can be determined that particle A is a target microcrystalline particle located near the center of target square 1, so particle A can be used as the reference target microcrystalline particle of target square 1, and then the concentric height of particle A that keeps its position unchanged during rotation is determined. Assume that the concentric height of particle A is Z A ', then the concentric height Z of particle A can be A 'Z1' is the concentric height of the target square1.

[0141] It should be noted that after the height of the sample stage is controlled to be adjusted to the currently determined concentric height, the reference target microcrystalline particle can participate in the subsequent step of "traversing the initial coordinates of each target microcrystalline particle in the current target square" to determine the precise coordinates of the reference target microcrystalline particle. The reference target microcrystalline particle may not participate in the subsequent traversal step, and the precise coordinates may be determined directly based on the reference coordinates and the concentric height. For example, the reference coordinates of the reference target microcrystalline particle are (X M ,Y M ,Z M ), the concentric height is Z1', then the precise coordinates of the reference target microcrystalline particles are (X M ,Y M ,Z1').

[0142] In one embodiment, determining the concentric height of the target region based on the reference coordinates of the reference target microcrystalline particles may include:

[0143] Control the sample stage to move to the reference coordinates of the reference target microcrystalline particles; control the height of the sample stage to adjust according to a preset step size, and control the sample stage to rotate by preset angles in both positive and negative directions each time the height of the sample stage is adjusted once; calculate the position offset of the reference target microcrystalline particles rotated by the same preset angles in both positive and negative directions at the current height to obtain multiple position offsets; perform linear regression calculation on the multiple position offsets and their corresponding sample stage heights (Z-axis coordinates) to obtain the concentric height of the reference target microcrystalline particles that keep their positions unchanged during rotation (i.e., the position offset is 0), and determine the concentric height of the reference target microcrystalline particles as the concentric height of the target area.

[0144] After determining the reference target microcrystalline particles of the current target square, the automated execution script can obtain the initial coordinates (X0, Y0, Z0) of the reference target microcrystalline particles, and then control the sample stage to move to the initial coordinates (X0, Y0, Z0). At this time, the automated execution script can control the TEM to collect particle morphology images of the reference target microcrystalline particles in the third shooting mode, so as to determine the reference coordinates (X', Y', Z') of the reference target microcrystalline particles based on the particle morphology images. Among them, since (X', Y', Z') is obtained based on the third shooting mode, (X', Y', Z') is accurate, so the automated execution script can control the sample stage to move to the reference coordinate (X', Y', Z'). At this time, the automated execution script can control the vertical height of the sample stage to move up or down in sequence based on Z' according to a preset step size (such as 5μm, 10μm, 15μm, 20μm, 30μm, etc.). Assuming the preset step size is 10μm (micrometer), the new Z-axis coordinates that can be obtained after the sample stage moves are Z'-30, Z'-20, Z'-10, Z'+10, Z'+20, Z'+30, etc. Whenever the vertical height of the sample stage is adjusted to a new height, the automated execution script can control the sample stage to rotate by preset angles (such as 5 degrees, 10 degrees, 15 degrees, 20 degrees, etc.) in both the positive and negative directions. Assuming that the sample stage is controlled to rotate 10 degrees clockwise and 10 degrees counterclockwise, the position offset between the reference target microcrystalline particles rotating by the preset angle in the positive direction and the preset angle in the negative direction at the current new height is calculated, thereby obtaining the position offset corresponding to the current new height. Repeating the above operation, the position offset corresponding to the reference target microcrystalline particles at each new height can be obtained. Since the position offset has a linear relationship with the sample stage height, the automated execution script can perform linear regression calculations on multiple position offsets and their corresponding sample stage heights to obtain the target height when the position offset is zero. The automated execution script can determine the target height as the concentric height at which the reference target microcrystalline particles remain unchanged during rotation.

[0145] In one example, assuming that particle A is used as the reference target microcrystalline particle of target square 1, the automated execution script can control the sample stage to move to the initial coordinate (X A0 ,Y A0 ,Z A0 ), the automated execution script can control the TEM to collect the particle morphology image Image0 of particle A in the third shooting mode of 4300X, so as to determine the reference coordinates (X) of particle A based on the particle morphology image Image0. A ',Y A ',Z A '). Then, the automated execution script can control the sample stage to move to the reference coordinate (XA ',Y A ',Z A '), and then control the vertical height of the sample stage to adjust to Z A '+10 (assuming the preset step size is 10μm), then at the new height Z A '+10, the automated script can control the sample stage to rotate 10° in the positive direction (assuming the preset angle is 10°). A '+10 and the rotation angle (+10°), the automated execution script can control the TEM to collect the particle morphology image Image1 of particle A in the third shooting mode of 4300X, so as to determine the first test coordinate (X) of particle A based on the particle morphology image Image1. A1 ',Y A1 ',Z A '+10); also at this new height Z A '+10, the automated script can control the sample stage to rotate 10° in the negative direction, and at this new height Z A '+10 and the rotation angle (-10°), the automated execution script can control the TEM to collect the particle morphology image Image2 of particle A in the third shooting mode of 4300X, so as to determine the second test coordinate (X A2 ',Y A2 ',Z A '+10). The automated execution script can be used (X A1 ',Y A1 ') and (X A2 ',Y A2 '), calculate the particle A at the new height Z A 'The position offset offset1 between the two rotation angles (+10° and -10°) under +10.

[0146] In this way, the new height Z is calculated in sequence A '+20, Z A '+30, Z A '-10, Z A '-20, Z A '-30, ... the corresponding position offset, thereby obtaining the position offset offset1 to the position offset offset n Since each position offset has a linear relationship with the corresponding height, for example, position offset offset1 is related to height Z A '+10 has a linear relationship, so the automation script can perform position offset offset1 to position offset offset nA linear regression calculation is performed on the corresponding n height values ​​to obtain the target height when the position offset is zero. The automated execution script can determine the target height as the concentric height at which particle A keeps its position unchanged during the rotation process.

[0147] It should be noted that the various coordinates involved in the embodiments of the present application (such as the initial coordinates of the microcrystalline particles, reference coordinates, precise coordinates, center point coordinates of the region, etc.) can be regarded as physical coordinates based on the sample stage. In specific applications, the coordinates of the target object in the picture (such as pixel coordinates) can be obtained based on the position of the target object (such as microcrystalline particles, square, etc.) in the picture, and then based on the coordinate conversion matrix, the coordinates of the target object in the picture are converted into corresponding sample stage coordinates. Among them, the coordinate conversion matrix can be determined based on the magnification in the shooting mode of TEM, and the coordinate conversion matrices corresponding to different magnifications are different. These coordinate conversion matrices can be obtained from the output file of the EPU-D software (EPU-D software is a MicroED data acquisition software), or they can be obtained through actual testing.

[0148] As can be seen from this example, the solution provided in this application automatically identifies the target microcrystalline particles on the carrier grid by calling the program without human intervention, thereby reducing labor costs and time costs, and reducing the impact of human selection tendencies, thereby improving the reproducibility of the experiment.

[0149] Furthermore, the solution provided by the present application can select some squares from the identified squares as target squares, and then record the coordinates of the center point of each target square into the target square list, thereby improving data collection efficiency. In addition, all squares can be selected from the identified squares as target squares, and then the coordinates of the center point of each target square can be recorded into the target square list, so that all target microcrystalline particles can be covered.

[0150] Furthermore, the solution provided in the present application collects a network map image in a first shooting mode, collects a regional morphology image in a second shooting mode, and collects a particle morphology image in a third shooting mode, wherein the first magnification of the first shooting mode is less than the second magnification of the second shooting mode and less than the third magnification of the third shooting mode, so that the precise coordinates finally obtained can be more accurate.

[0151] Furthermore, the solution provided in the present application uses a target microcrystalline particle located near the center of a target square as a reference target microcrystalline particle, and then uses the concentric height of the reference target microcrystalline particle as the concentric height of the target square, thereby minimizing the error.

[0152] Figure 3 It is a flow chart of the method for collecting microcrystal electron diffraction data shown in the embodiment of the present application.

[0153] See also Figure 3 , the method for collecting microcrystal electron diffraction data of the present application comprises:

[0154] S310, obtaining precise coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method as described above;

[0155] S320, controlling the transmission electron microscope to collect corresponding diffraction data according to the precise coordinates of each target microcrystalline particle.

[0156] In one embodiment, after obtaining the precise coordinates of the current target microcrystalline particles based on the above-mentioned identification method of microcrystalline particles, the method may further include:

[0157] Control the sample stage to move to the precise coordinates of the current target microcrystalline particles to import the precise coordinates of the current target microcrystalline particles into the first data collection list of the batch mode of the EPU-D software until the precise coordinates of all target microcrystalline particles have been imported into the first data collection list; or, write the precise coordinates of the current target microcrystalline particles into the input file of the EPU-D software until the precise coordinates of all target microcrystalline particles have been written into the input file, and then use the input file to establish a second data collection list.

[0158] In one example, after obtaining the precise coordinates (X', Y', Z') of the current target microcrystalline particles based on the identification method of the microcrystalline particles as described above, the automated execution script can control the sample stage to move to the precise coordinates (X', Y', Z') of the current target microcrystalline particles, so that the precise coordinates (X', Y', Z') of the current target microcrystalline particles can be imported into the first data collection list of the batch mode of the EPU-D software. According to the above method, until the precise coordinates (X', Y', Z') of all target microcrystalline particles have been imported into the first data collection list.

[0159] In another example, after obtaining the precise coordinates (X', Y', Z') of the current target microcrystalline particles based on the identification method of the microcrystalline particles as described above, the automated execution script can write the precise coordinates (X', Y', Z') of the current target microcrystalline particles into the input file of the EPU-D software. According to the above method, until the precise coordinates (X', Y', Z') of all target microcrystalline particles have been written into the input file, the automated execution script can control the EPU-D software to open the input file, and the second data collection list can be automatically established.

[0160] In one embodiment, controlling the transmission electron microscope to collect corresponding diffraction data for the precise coordinates of each target microcrystalline particle may include:

[0161] After obtaining the first data collection list or the second data collection list, trigger the EPU-D software to control the sample stage to move to any precise coordinate in the first data collection list or the second data collection list through the EPU-D software; control the transmission electron microscope to switch to the diffraction mode through the EPU-D software, and control the transmission electron microscope to collect the diffraction image of the current target microcrystalline particles in the rotation process in the diffraction mode, and save the currently collected diffraction image; traverse each precise coordinate in the first data collection list or the second data collection list until the diffraction images of all target microcrystalline particles are collected and saved.

[0162] After obtaining the first data collection list or the second data collection list, the first data collection list or the second data collection list now covers the precise coordinates (X', Y', Z') of all target microcrystalline particles, so the automated execution script can trigger the EPU-D software to collect MicroED data using the EPU-D software.

[0163] In the specific implementation, after the automatic execution script triggers the EPU-D software, the EPU-D software can control the sample stage to move to the precise coordinates (X', Y', Z') of any target microcrystalline particle in the first data collection list or the second data collection list, and then control the TEM to switch to the diffraction mode. Under the precise coordinates (X', Y', Z'), the EPU-D software can control the TEM to collect the diffraction image of the current target microcrystalline particle in the diffraction mode during the rotation process.

[0164] In this way, the precise coordinates (X', Y', Z') of each target microcrystalline particle in the first data collection list or the second data collection list are traversed to collect and save the diffraction image of each target microcrystalline particle in turn. The diffraction image is the diffraction data (microcrystalline electron diffraction data).

[0165] The EPU-D software collects the diffraction images uniformly after obtaining the precise coordinates (X', Y', Z') of all target microcrystalline particles. In addition, the embodiments of the present application may not use the EPU-D software, but instead collect the diffraction images of the target microcrystalline particles in real time through the automated execution of scripts.

[0166] In another embodiment, controlling the transmission electron microscope to collect corresponding diffraction data for the precise coordinates of each target microcrystalline particle may include:

[0167] After obtaining the precise coordinates of the current target microcrystalline particles based on the identification method of the microcrystalline particles as described above, the script is automatically executed to control the transmission electron microscope to switch to the diffraction mode; the sample stage is controlled to move to the precise coordinates of the current target microcrystalline particles, and the transmission electron microscope is controlled to collect the diffraction image of the current target microcrystalline particles during the rotation process in the diffraction mode, and the currently collected diffraction image is saved until the diffraction images of all target microcrystalline particles are collected and saved.

[0168] In a specific implementation, after obtaining the precise coordinates (X', Y', Z') of the current target microcrystalline particles based on the identification method of the microcrystalline particles as described above, the automated execution script can control the sample stage to move to the precise coordinates (X', Y', Z') of the current target microcrystalline particles. Under the precise coordinates (X', Y', Z'), the automated execution script can control the TEM to collect the diffraction image of the current target microcrystalline particles during the rotation process in the diffraction mode, and can save the diffraction image of the current target microcrystalline particles at the same time, until the diffraction images of all target microcrystalline particles are collected and saved.

[0169] It should be noted that after the MicroED data is collected, the embodiment of the present application can process and analyze the MicroED data, so as to quickly and with high resolution determine the crystal structure of the microcrystalline powder sample.

[0170] In the specific implementation, XDS (X-ray Detector Software), SHELXT, SHELXD and XSCALE can be used, and the appropriate software can be selected according to the target molecular size. Among them, XDS software is a software for processing crystal X-ray diffraction data, SHELXT or SHELXD software is a program package for crystal structure analysis, including SHELXL (structure refinement) module, etc., XSCALE is an embedded processor, and the embodiment of the present application can use XDS software to index and integrate each set of diffraction data (i.e., the diffraction image of each target microcrystalline particle) to obtain the unit cell parameters of each set of diffraction data, and then use XSCALE to merge the best quality multiple sets of diffraction data to obtain HKL files (H, K, L represent the direction of atomic or molecular arrangement in the crystal), and then use SHELXT or SHELXD software to analyze and obtain the crystal structure, and finally use the SHELXL module to complete the structure refinement.

[0171] As can be seen from this example, the solution provided by the present application can not only import the precise coordinates into the first data collection list of the batch mode of the EPU-D software, but also write the precise coordinates into the input file of the EPU-D software, and then use the input file to automatically create a second data collection list, thereby expanding the recording method of the precise coordinates.

[0172] Furthermore, the solution provided in the present application can not only use EPU-D software to perform unified automatic collection of diffraction images, but also use automated execution scripts to perform real-time automatic collection of diffraction images, thereby broadening the automatic collection method of diffraction images.

[0173] In order to enable those skilled in the art to better understand the embodiments of the present application, the embodiments of the present application are described below through the following examples.

[0174] The embodiment of the present application adopts the above-mentioned method for identifying microcrystalline particles and the method for collecting microcrystalline electron diffraction data to automatically collect 12 sets of diffraction data (i.e., diffraction images of 12 target microcrystalline particles) of ibuprofen bulk drug samples. The specific process of automatic MicroED data collection is as follows:

[0175] (1) The TEM is adjusted to a first shooting mode required for shooting a grid; wherein the first magnification of the first shooting mode can be set to 155X; wherein the grid is placed on a movable sample stage, and an ibuprofen raw material drug sample is attached to the carbon film of the grid.

[0176] (2) Control the sample stage to move to different positions in sequence, and control the TEM to collect grid map images when the grid is at different positions in the first shooting mode of 155X, and obtain 4 grid map images. For the convenience of display, the 4 grid map images can be spliced ​​to obtain a total grid map image with a larger data area. Figure 4 As shown, Figure 4 It is the total load network map image obtained by stitching together 4 load network map images.

[0177] (3) Identify multiple squares from each network map image and obtain the coordinates of the center point of each identified square. Figure 4 As shown, Figure 4 The multiple numbers in are the multiple squares that have been identified.

[0178] (4) Adjust the TEM to the second shooting mode required for shooting the square; wherein the second magnification of the second shooting mode can be set to 700X.

[0179] (5) Select two squares from the identified multiple squares as target squares, and record the coordinates of the center point of each target square into the list of squares to be tested.

[0180] (6) Control the sample stage to move to any center point coordinate in the list of squares to be tested. Under the center point coordinate, control the TEM to collect the regional morphology image of the current target square in the second shooting mode of 700X. Figure 5 As shown, Figure 5 It is the regional morphology image of the current target square.

[0181] (7) Identify at least one target microcrystalline particle in the current region morphology image; wherein the target microcrystalline particle is a microcrystalline particle that meets a preset size range among the multiple microcrystalline particles. Figure 5 As shown, Figure 5 The multiple numbers in the figure are multiple target microcrystalline particles identified from the current area morphology image and selected by size.

[0182] (8) Obtain the initial coordinates of each target microcrystal particle and record the initial coordinates in the rough particle coordinate list.

[0183] (9) Control TEM to repeatedly execute steps (6) to (8) so as to traverse the coordinates of each center point in the list of squares to be tested until the target microcrystalline particles in all target squares are identified and the initial coordinates of all target microcrystalline particles are recorded in the rough particle coordinate list.

[0184] (10) The TEM is adjusted to a third shooting mode required for shooting microcrystalline particles; wherein the third magnification of the third shooting mode can be set to 4300X.

[0185] (11) If there is only one target microcrystalline particle in the current target square, the target microcrystalline particle is used as the reference target microcrystalline particle; if there are multiple target microcrystalline particles in the current target square, the target microcrystalline particle with the smallest coordinate distance to the center point of the current target square is selected as the reference target microcrystalline particle.

[0186] (12) Control the sample stage to move to the initial coordinates of the reference target microcrystalline particles, and control the TEM to collect particle morphology images of the reference target microcrystalline particles in the third shooting mode of 4300X, and determine the reference coordinates of the reference target microcrystalline particles based on the particle morphology images.

[0187] (13) Control the sample stage to move to the reference coordinates of the reference target microcrystalline particles, and control the height of the sample stage to be adjusted according to a preset step length, and control the sample stage to rotate by a preset angle in both the positive and negative directions each time the height of the sample stage is adjusted.

[0188] (14) Calculate the position offset of the reference target microcrystalline particles at each height when they are rotated along the positive and negative directions by the same preset angle to obtain multiple position offsets.

[0189] (15) A linear regression calculation is performed on multiple position offsets and their corresponding heights to obtain a target height when the position offset is zero, and then the target height is determined as the concentric height of the reference target microcrystalline particle that remains unchanged during the rotation process.

[0190] (16) The concentric height of the reference target microcrystalline particle is used as the concentric height of the current target square, and the height of the sample stage is controlled to be adjusted to the currently determined concentric height.

[0191] (17) According to the initial coordinates and concentric height of the target microcrystalline particles, the TEM is controlled to collect the particle morphology image of the current target microcrystalline particles in the third shooting mode of 4300X, such as Figure 6 As shown, Figure 6 It is a particle morphology picture of the current target microcrystalline particle obtained in the third shooting mode of 4300X. The precise coordinates of the current target microcrystalline particle are determined based on the particle morphology picture.

[0192] (18) Control the sample stage to move to the precise coordinates of the current target microcrystalline particles, so as to import the precise coordinates of the current target microcrystalline particles into the first data collection list of the batch mode of the EPU-D software.

[0193] (19) Control TEM to repeatedly execute steps (17) and (18) so as to traverse the initial coordinates of each target microcrystalline particle in the current target square until the precise coordinates of all target microcrystalline particles in the current target square are obtained, and the precise coordinates of all target microcrystalline particles in the current target square have been imported into the first data collection list.

[0194] (20) Control TEM to repeatedly execute steps (11) to (19) so as to traverse the initial coordinates of each target microcrystalline particle in each target square until the precise coordinates of all target microcrystalline particles in all target squares are obtained, and the precise coordinates of all target microcrystalline particles in all target squares have been imported into the first data collection list.

[0195] (21) Trigger the EPU-D software through automated execution scripts.

[0196] (22) The sample stage is controlled to move to any precise coordinate in the first data collection list through the EPU-D software. At the current precise coordinate, the TEM is controlled by the EPU-D software to collect and save the diffraction image of the current target microcrystalline particle during rotation in the diffraction mode.

[0197] (23) Controlling the TEM through the EPU-D software, the TEM is repeatedly executed in step (22) so as to traverse each precise coordinate in the first data collection list until the diffraction images of all target microcrystalline particles are obtained.

[0198] The above process is completed by automated execution scripts without human intervention, which can reduce labor costs and time costs. For example, it can save more than 1 hour of manpower time.

[0199] After collecting 12 sets of diffraction data, each set of diffraction data can be indexed and integrated using the XDS software to obtain the unit cell parameters of each set of diffraction data. Then, the 5 sets of diffraction data with the best quality can be merged using XSCALE to obtain the HKL file. The crystal structure can then be analyzed using the SHELXT software. Finally, the structure can be refined using the SHELXL module.

[0200] After the above crystal structure analysis, the crystal structure of ibuprofen in the sample was obtained. The unit cell parameters of the crystal obtained by analysis are a=14.34(4), b=7.78(2), c=10.49(3), α=90°, β=98.58(14)°, c=90°, the space group is P21 / c(No.14), the R1 value obtained by structure refinement is 0.3073, the goodness of fit value of all diffractions is 1.643, and it is consistent with the unit cell parameters of the published single crystal structure (CSD Entry: IBPRAC19), which shows the correctness of the analysis results and the effectiveness of the automated data acquisition method.

[0201] Among them, the R1 value is the output index of structure refinement, which is a common index for single crystal XRD (X-Ray Diffraction) structure analysis and MicroED structure analysis. Its physical meaning is the residual factor of all diffraction points based on the structure factor, reflecting the matching degree between the refined structure and the diffraction data. The smaller the R1 value, the better. For example, the smaller the R1 value, the more matching the structure and diffraction data. In MicroED, it is generally between 0.1 and 0.5.

[0202] Corresponding to the aforementioned application function realization method embodiment, the present application also provides a device for identifying microcrystalline particles, a device for collecting microcrystalline electron diffraction data, an electronic device, a computer-readable storage medium and corresponding embodiments.

[0203] Figure 7 It is a schematic diagram of the structure of a device for identifying microcrystalline particles shown in an embodiment of the present application.

[0204] See also Figure 7 The present application provides a device for identifying microcrystalline particles, which may include:

[0205] A grid map image acquisition module 710, used to control the transmission electron microscope to acquire a grid map image of a grid in a first shooting mode, where a plurality of microcrystalline particles are distributed;

[0206] The target microcrystalline particle identification module 720 is used to identify the target microcrystalline particles in the grid map image and obtain the initial coordinates of the target microcrystalline particles;

[0207] The precise coordinate determination module 730 is used to control the transmission electron microscope to collect particle morphology images of the target microcrystalline particles in the third shooting mode based on the initial coordinates of the target microcrystalline particles, and determine the precise coordinates of the target microcrystalline particles based on the particle morphology images.

[0208] In one embodiment, the grid is placed on a movable sample stage, and the grid includes multiple areas; the target microcrystalline particle identification module 720 may include:

[0209] The region identification submodule is used to identify at least one region from the network map image and obtain the coordinates of the center point of the identified region;

[0210] A second adjustment submodule, used to adjust the transmission electron microscope to a second shooting mode required by the shooting area;

[0211] The target microcrystalline particle identification submodule is used to control the sample stage to move to the center point coordinates of at least one area, and control the transmission electron microscope to collect a regional morphology image of the corresponding area in the second shooting mode, and identify at least one target microcrystalline particle in the regional morphology image; wherein the target microcrystalline particle is a microcrystalline particle among multiple microcrystalline particles that meets a preset size range.

[0212] In one embodiment, the network map image acquisition module 710 may include:

[0213] A first adjustment submodule, used to adjust the transmission electron microscope to a first shooting mode required for shooting the grid;

[0214] The grid map image acquisition submodule is used to control the sample stage to move to different positions in sequence, and control the transmission electron microscope to acquire grid map images when the grid is located at different positions in the first shooting mode.

[0215] In one embodiment, the region identification submodule may include:

[0216] A region identification unit, used to identify multiple regions from each network map image and obtain the coordinates of the center point of each identified region;

[0217] Target microcrystalline particle identification submodule, including:

[0218] A center point coordinate recording unit, used to select at least part of the identified multiple areas as target areas, and record the center point coordinates of each target area in a target area list;

[0219] A regional morphology image acquisition unit, used to control the sample stage to move to any center point coordinate in the target region list, and control the transmission electron microscope to acquire a regional morphology image of the current target region in the second shooting mode;

[0220] A target microcrystalline particle identification unit, used to identify at least one target microcrystalline particle in the current region morphology picture;

[0221] The center point coordinate traversal unit is used to traverse each center point coordinate in the target area list until the target microcrystalline particles in all the target areas are identified.

[0222] In one embodiment, the target microcrystalline particle identification unit may include:

[0223] A microcrystalline particle identification subunit is used to identify a plurality of microcrystalline particles contained in the regional topography image according to the gray value difference of each pixel in the regional topography image;

[0224] The target microcrystalline particle determination subunit is used to determine microcrystalline particles that meet a preset size range from a plurality of microcrystalline particles, and use the microcrystalline particles that meet the preset size range as target microcrystalline particles.

[0225] In one embodiment, the grid is placed on a movable sample stage, and the grid includes multiple areas; the precise coordinate determination module 730 may include:

[0226] A third adjustment submodule, used to adjust the transmission electron microscope to a third shooting mode required for shooting microcrystalline particles;

[0227] The concentric height determination submodule is used to determine the concentric height of the target area where the target microcrystalline particles are located, and control the height of the sample stage to be adjusted to the concentric height;

[0228] The precise coordinate determination submodule is used to control the transmission electron microscope to collect particle morphology images of the target microcrystalline particles in the third shooting mode according to the initial coordinates and concentric height of the target microcrystalline particles, and determine the precise coordinates of the target microcrystalline particles based on the particle morphology images.

[0229] In one embodiment, the concentric height determination submodule may include:

[0230] A reference target microcrystalline particle determination unit, used to determine reference target microcrystalline particles in a target area;

[0231] A reference coordinate determination subunit, used to control the sample stage to move to the initial coordinates of the reference target microcrystalline particles, and control the transmission electron microscope to collect a particle morphology image of the reference target microcrystalline particles in a third shooting mode, and determine the reference coordinates of the reference target microcrystalline particles based on the particle morphology image;

[0232] The concentric height determination unit is used to determine the concentric height of the target area based on the reference coordinates of the reference target microcrystalline particles.

[0233] In one embodiment, the reference target microcrystalline particle determination unit may include:

[0234] A first determination subunit is used to use the target microcrystalline particle as a reference target microcrystalline particle if there is only one target microcrystalline particle in the target area;

[0235] The second determination subunit is used to select a target microcrystalline particle with the smallest coordinate distance from the center point of the target area as a reference target microcrystalline particle if there are multiple target microcrystalline particles in the target area.

[0236] In one embodiment, the first adjustment submodule, the second adjustment submodule and the third adjustment submodule adjust the shooting mode of the transmission electron microscope through the parameter adjustment unit:

[0237] The parameter adjustment unit is used to adjust the shooting parameters of the transmission electron microscope to obtain a corresponding shooting mode; wherein the shooting parameters include at least one of the magnification, C2 aperture model, spotsize value, intensity value, exposure time, and working mode.

[0238] Control the transmission electron microscope to collect a grid map image of the grid in the first shooting mode; identify the target microcrystalline particles in the grid map image, and obtain the initial coordinates of the target microcrystalline particles; based on the initial coordinates of the target microcrystalline particles, control the transmission electron microscope to collect the particle morphology image of the target microcrystalline particles in the third shooting mode, and determine the precise coordinates of the target microcrystalline particles based on the particle morphology image. The present application automatically identifies the target microcrystalline particles on the grid by calling a program without human intervention, thereby reducing labor costs and time costs, and reducing the influence of human selection tendency, thereby improving the reproducibility of the experiment.

[0239] Figure 8 It is a schematic diagram of the structure of a device for collecting microcrystal electron diffraction data shown in an embodiment of the present application.

[0240] See also Figure 8 , the present application provides a device for collecting microcrystal electron diffraction data, which may include:

[0241] The precise coordinate acquisition module 810 is used to obtain precise coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method described above;

[0242] The diffraction data acquisition module 820 is used to control the transmission electron microscope to collect corresponding diffraction data according to the precise coordinates of each target microcrystalline particle.

[0243] Regarding the device in the above embodiment, the specific manner in which each module performs operations has been described in detail in the embodiment of the method, and will not be elaborated again here.

[0244] Fig. 9 It is a schematic diagram of the structure of an electronic device shown in an embodiment of the present application.

[0245] See also Fig. 9 , the electronic device 900 includes a memory 910 and a processor 920 .

[0246] The processor 920 may be a central processing unit (CPU), or other general-purpose processors, digital signal processors (DSP), application-specific integrated circuits (ASIC), field-programmable gate arrays (FPGA), or other programmable logic devices, discrete gate or transistor logic devices, discrete hardware components, etc. A general-purpose processor may be a microprocessor or the processor may be any conventional processor, etc.

[0247] The memory 910 may include various types of storage units, such as system memory, read-only memory (ROM), and permanent storage devices. Among them, ROM can store static data or instructions required by the processor 920 or other modules of the computer. The permanent storage device may be a readable and writable storage device. The permanent storage device may be a non-volatile storage device that does not lose the stored instructions and data even after the computer is powered off. In some embodiments, the permanent storage device uses a large-capacity storage device (such as a magnetic or optical disk, flash memory) as a permanent storage device. In some other embodiments, the permanent storage device may be a removable storage device (such as a floppy disk, optical drive). The system memory may be a readable and writable storage device or a volatile readable and writable storage device, such as a dynamic random access memory. The system memory may store some or all instructions and data required by the processor at run time. In addition, the memory 910 may include any combination of computer-readable storage media, including various types of semiconductor memory chips (such as DRAM, SRAM, SDRAM, flash memory, programmable read-only memory), and disks and / or optical disks may also be used. In some embodiments, the memory 910 may include a readable and / or writable removable storage device, such as a laser disc (CD), a read-only digital versatile disc (such as a DVD-ROM, a double-layer DVD-ROM), a read-only Blu-ray disc, an ultra-density optical disc, a flash memory card (such as an SD card, a mini SD card, a Micro-SD card, etc.), a magnetic floppy disk, etc. The computer-readable storage medium does not include carrier waves and transient electronic signals transmitted wirelessly or wired.

[0248] The memory 910 stores executable codes, and when the executable codes are processed by the processor 920 , the processor 920 can execute part or all of the methods described above.

[0249] In addition, the method according to the present application may also be implemented as a computer program or a computer program product, which includes computer program code instructions for executing some or all of the steps in the above method of the present application.

[0250] Alternatively, the present application can also be implemented as a computer-readable storage medium (or non-transitory machine-readable storage medium or machine-readable storage medium) on which executable code (or computer program or computer instruction code) is stored. When the executable code (or computer program or computer instruction code) is executed by a processor of an electronic device (or server, etc.), the processor executes part or all of the steps of the above-mentioned method according to the present application.

[0251] The embodiments of the present application have been described above, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes will be apparent to those of ordinary skill 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 of the embodiments, practical applications, or improvements to the technology in the market, or to enable other persons of ordinary skill in the art to understand the embodiments disclosed herein.

Claims

1. A method for identifying microcrystalline particles, characterized in that: include: Control the transmission electron microscope to collect a grid map image of a grid in a first shooting mode, wherein a plurality of microcrystalline particles are distributed on the grid; Identify the target microcrystalline particles in the grid map image, and obtain the initial coordinates of the target microcrystalline particles; Based on the initial coordinates of the target microcrystalline particles, the transmission electron microscope is controlled to collect a particle morphology image of the target microcrystalline particles in a third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology image.

2. The method according to claim 1, characterized in that The grid is placed on a movable sample stage, and the grid includes a plurality of regions; The identifying target microcrystalline particles in the grid map image includes: Identify at least one of the areas from the network map image, and obtain the coordinates of the center point of the identified area; Adjusting the transmission electron microscope to a second shooting mode required for the shooting area; Control the sample stage to move to the center point coordinates of at least one of the areas, and control the transmission electron microscope to collect a regional morphology image of the corresponding area under the second shooting mode, and identify at least one target microcrystalline particle in the regional morphology image; wherein the target microcrystalline particle is a microcrystalline particle among the multiple microcrystalline particles that meets a preset size range.

3. The method according to claim 2, characterized in that The controlling the transmission electron microscope to collect a grid map image of the grid in the first shooting mode comprises: The transmission electron microscope is adjusted to a first shooting mode required for shooting the grid; The sample stage is controlled to move to different positions in sequence, and the transmission electron microscope is controlled to collect grid map images when the grid is located at the different positions in the first shooting mode.

4. The method according to claim 3, characterized in that The step of identifying at least one of the regions from the network map image and obtaining the coordinates of the center point of the identified region includes: Identify a plurality of the regions from each of the network map images, and obtain the coordinates of the center point of each of the identified regions; The step of controlling the sample stage to move to the center point coordinates of at least one of the regions, controlling the transmission electron microscope to collect a regional morphology image of the corresponding region in the second shooting mode, and identifying at least one target microcrystalline particle in the regional morphology image comprises: Select at least some of the identified regions as target regions, and record the coordinates of the center point of each target region in a target region list; Controlling the sample stage to move to any of the center point coordinates in the target area list, and controlling the transmission electron microscope to collect a regional morphology image of the current target area in the second shooting mode; Identify at least one target microcrystalline particle in the current regional morphology image; Each center point coordinate in the target area list is traversed until the target microcrystalline particles in all the target areas are identified.

5. The method according to any one of claims 2 to 4, characterized in that: The identifying at least one target microcrystalline particle in the regional morphology image comprises: Identifying a plurality of microcrystalline particles contained in the regional topography image according to a difference in grayscale values ​​of pixels in the regional topography image; Microcrystalline particles that meet a preset size range are determined from the plurality of microcrystalline particles, and the microcrystalline particles that meet the preset size range are used as target microcrystalline particles.

6. The method according to any one of claims 1 to 5, characterized in that: The grid is placed on a movable sample stage, and the grid includes a plurality of regions; based on the initial coordinates of the target microcrystalline particles, the transmission electron microscope is controlled to collect a particle morphology picture of the target microcrystalline particles in a third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology picture, including: Adjusting the transmission electron microscope to a third shooting mode required for shooting microcrystalline particles; Determine the concentric height of the target area where the target microcrystalline particles are located, and control the height of the sample stage to be adjusted to the concentric height; According to the initial coordinates of the target microcrystalline particles and the concentric height, the transmission electron microscope is controlled to collect a particle morphology image of the target microcrystalline particles in the third shooting mode, and the precise coordinates of the target microcrystalline particles are determined based on the particle morphology image.

7. The method according to claim 6, characterized in that Determining the concentric height of the target area where the target microcrystalline particles are located includes: determining reference target microcrystalline particles in the target area; Controlling the sample stage to move to the initial coordinates of the reference target microcrystalline particles, and controlling the transmission electron microscope to collect a particle morphology picture of the reference target microcrystalline particles in the third shooting mode, and determining the reference coordinates of the reference target microcrystalline particles based on the particle morphology picture; Based on the reference coordinates of the reference target microcrystalline particles, the concentric height of the target area is determined.

8. The method according to claim 7, characterized in that The step of determining the reference target microcrystalline particles in the target area comprises: If there is only one target microcrystalline particle in the target area, the target microcrystalline particle is used as a reference target microcrystalline particle; If there are a plurality of target microcrystalline particles in the target region, a target microcrystalline particle with the smallest coordinate distance from the center point of the target region is selected as a reference target microcrystalline particle.

9. The method according to any one of claims 1 to 8, characterized in that: Adjust the transmission electron microscope acquisition mode, including: Adjust the shooting parameters of the transmission electron microscope to obtain a corresponding shooting mode; wherein the shooting parameters include at least one of magnification, C2 aperture model, spotsize value, intensity value, exposure time, and working mode.

10. A method for collecting microcrystal electron diffraction data, characterized in that: include: Obtaining precise coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method according to any one of claims 1 to 9; According to the precise coordinates of each target microcrystalline particle, the transmission electron microscope is controlled to collect corresponding diffraction data.

11. A device for identifying microcrystalline particles, characterized in that: include: A grid map image acquisition module, used to control the transmission electron microscope to acquire a grid map image of a grid in a first shooting mode, wherein a plurality of microcrystalline particles are distributed on the grid; A target microcrystalline particle identification module is used to identify the target microcrystalline particles in the grid map image and obtain the initial coordinates of the target microcrystalline particles; The precise coordinate determination module is used to control the transmission electron microscope to collect a particle morphology image of the target microcrystalline particle in a third shooting mode based on the initial coordinates of the target microcrystalline particle, and determine the precise coordinates of the target microcrystalline particle based on the particle morphology image.

12. A device for collecting microcrystal electron diffraction data, characterized in that: include: An accurate coordinate acquisition module, used for obtaining accurate coordinates of a plurality of target microcrystalline particles based on the microcrystalline particle identification method according to any one of claims 1 to 9; The diffraction data acquisition module is used to control the transmission electron microscope to collect corresponding diffraction data according to the precise coordinates of each target microcrystalline particle.

13. An electronic device, characterized in that: include: processor; as well as A memory having executable codes stored thereon, which, when executed by the processor, causes the processor to execute the method for identifying microcrystalline particles as described in any one of claims 1 to 9 or the method for collecting microcrystalline electron diffraction data as described in claim 10.

14. A computer-readable storage medium having executable code stored thereon, which, when executed by a processor of an electronic device, enables the processor to execute the method for identifying microcrystalline particles as described in any one of claims 1 to 9 or the method for collecting microcrystalline electron diffraction data as described in claim 10.

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