CN113447507B - Method, system, equipment and storage medium for collecting X-ray diffraction signals - Google Patents
Method, system, equipment and storage medium for collecting X-ray diffraction signals Download PDFInfo
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Abstract
The embodiment of the invention provides a method, a system and equipment for collecting an X-ray diffraction signal and a storage medium. The method comprises the following steps: the method comprises the steps of emitting X rays through an X-ray source to irradiate a sample, using a two-dimensional plane detector to carry out continuous scanning, controlling the sample to rotate 360 degrees along a psi circle, and determining whether a target reciprocal space Q under current 2 theta and omega values is taken z And after the positive part is scanned, if not, controlling the chi to change by delta chi, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle. If yes, whether the target reciprocal space is scanned completely is judged. And if the target reciprocal space is not scanned completely, controlling 2 theta to change delta 2 theta, controlling omega to change delta omega, and returning to the step to control the sample to rotate 360 degrees along the psi circle. And if the target reciprocal space is scanned completely, ending the processing and obtaining first diffraction data in the target reciprocal space. The invention realizes the rapid and efficient acquisition of most diffraction signals in the wide-area reciprocal space.
Description
Technical Field
The invention relates to the field of X-ray structural analysis, in particular to a method, a system, equipment and a storage medium for collecting X-ray diffraction signals.
Background
Currently, the crystal structure of a material is analyzed by X-ray diffraction, that is, the crystal structure information of the material is analyzed by collecting the distribution of diffraction signals generated by the diffraction of X-rays by the crystal structure in a reciprocal space.
At present, a local three-dimensional diffraction technology is adopted to represent the crystal structure of the material, and although the precision of data acquired by the local three-dimensional diffraction technology is high, the analysis efficiency of the crystal structure is reduced because only diffraction signals in a local space can be acquired, most information can be leaked, so that how to quickly and efficiently acquire most diffraction signals in a wide-area reciprocal space is a problem which needs to be urgently solved by technical personnel in related fields.
Disclosure of Invention
The embodiment of the invention aims to provide a method, a system, equipment and a storage medium for acquiring X-ray diffraction signals, so as to quickly and efficiently acquire most diffraction signals in a wide reciprocal space. The specific technical scheme is as follows:
a method of acquiring X-ray diffraction signals, the method comprising:
the sample is irradiated with X-rays emitted by an X-ray source.
And performing annular symmetrical reciprocal space scanning on the target reciprocal space of the sample by using a two-dimensional plane detector to obtain first diffraction data in the target reciprocal space.
The circular symmetric reciprocal space scanning specifically includes.
Using the two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to be 0, wherein omega is the angle of the sample rotating around a preset X axis, chi is the angle of the sample rotating around a preset Y axis, psi is the angle of the sample rotating around a preset Z axis, and 2 theta is the angle of the two-dimensional detector rotating around the preset X axis.
The sample was controlled to rotate 360 degrees along the psi circle.
Judging whether scanning of the part with the target reciprocal space Qz under the current 2 theta and omega values being positive is finished, if not, controlling the x change delta x, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle; if so, judging whether the target reciprocal space is scanned completely, if not, controlling 2 theta to change by delta 2 theta and controlling omega to change by delta omega, wherein 2 delta omega = delta 2 theta, and returning to the step to control the sample to rotate by 360 degrees along the psi circle; and if the target reciprocal space is scanned completely, ending the processing.
And the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
Optionally, the method further includes:
and converting the first diffraction data into reciprocal space coordinates from angle coordinates by using diffraction fillet values corresponding to irradiation positions of straight-through light on the two-dimensional surface detector, wherein the straight-through light is the ray emitted by the X-ray source after passing through the sample.
Optionally, the transforming, by using each diffraction fillet value corresponding to the irradiation position of the through light on the two-dimensional detector, the angle coordinate of the first diffraction data into a reciprocal space coordinate specifically includes:
the method comprises the steps of calculating all diffraction fillet values corresponding to irradiation positions of direct light on a two-dimensional detector, calculating all diffraction fillet values of pixel points at other positions on the two-dimensional detector except the irradiation positions, and calculating emergent light wave vectors corresponding to the pixel points at other positions according to the calculated all diffraction fillet values of the pixel points at other positions, so that the first diffraction data are converted into reciprocal space coordinates from angle coordinates.
Optionally, the method further includes:
and carrying out interpolation reconstruction on the reciprocal space coordinates by utilizing a parallel interpolation algorithm to obtain a diffraction intensity value on an interpolation point in the target reciprocal space.
Optionally, the performing interpolation reconstruction on the reciprocal space coordinate by using a parallel interpolation algorithm to obtain a diffraction intensity value on an interpolation point in the target reciprocal space specifically includes:
and determining a regular three-dimensional grid according to the space range to be interpolated and the interpolation step length, wherein the diffraction intensity value of each grid point to be interpolated is equal to the average diffraction intensity value of all original data points, the original data points are positioned in a square range taking the grid point to be interpolated as the center and the interpolation step length as the side length, and the original data points are points corresponding to the reciprocal space coordinates.
And adding the intensity of each original data point in the same cube range to the grid point to be interpolated in the center of the cube.
And determining an arithmetic mean value of the intensity added to each grid point to be interpolated respectively, and determining the arithmetic mean value as a diffraction intensity value on the interpolation point in the target reciprocal space.
Optionally, the spatial range to be interpolated is determined according to the range of the target reciprocal space.
The interpolation step is not greater than a resolution of the reciprocal space coordinate in the target reciprocal space.
Optionally, the two-dimensional detector is located on a diffractometer, and the diffractometer is not less than four diffraction circles.
An acquisition system for X-ray diffraction signals, comprising:
and the light source module is used for emitting X rays to irradiate the sample through the X-ray source.
And the acquisition module is used for performing annular symmetrical reciprocal space scanning on the target reciprocal space of the sample through a two-dimensional detector to obtain first diffraction data in the target reciprocal space.
The acquisition module carries out annular symmetrical reciprocal space scanning and specifically sets as:
using the two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to 0, wherein omega is the angle of the sample rotating around a preset X axis, chi is the angle of the sample rotating around a preset Y axis, psi is the angle of the sample rotating around a preset Z axis, and 2 theta is the angle of the two-dimensional plane detector rotating around the preset X axis.
The sample was controlled to rotate 360 degrees around the psi circle.
Determining whether scanning of the part with the target reciprocal space Qz under the current 2 theta and omega values being positive is finished, if not, controlling the x change delta x, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle; if so, judging that the target reciprocal space is scanned completely, if not, controlling 2 theta to change by delta 2 theta, controlling omega to change by delta omega, wherein 2 delta omega = delta 2 theta, and returning to the step to control the sample to rotate by 360 degrees along a psi circle; and if the target reciprocal space is scanned completely, ending the processing.
And the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
Optionally, the system further includes:
and the coordinate conversion module converts the first diffraction data into reciprocal space coordinates from angle coordinates by utilizing all diffraction fillet values corresponding to the irradiation positions of the direct light on the two-dimensional detector, wherein the direct light is the rays emitted by the X-ray source after passing through the sample.
Optionally, the coordinate transformation module may be specifically configured to:
the method comprises the steps of calculating all diffraction fillet values corresponding to irradiation positions of direct light on a two-dimensional detector, calculating all diffraction fillet values of pixel points at other positions on the current two-dimensional detector except the irradiation positions, and calculating emergent light wave vectors corresponding to the pixel points at other positions according to the calculated all diffraction fillet values of the pixel points at other positions, so that first diffraction data are converted into reciprocal space coordinates from angle coordinates.
Optionally, the system further includes:
and the interpolation reconstruction module is used for carrying out interpolation reconstruction on the reciprocal space coordinates by using a parallel interpolation algorithm to obtain the diffraction intensity value on the interpolation point in the target reciprocal space.
Optionally, the interpolation reconstruction module may be specifically configured to:
and determining a regular three-dimensional grid according to the space range to be interpolated and the interpolation step length, wherein the diffraction intensity value of each grid point to be interpolated is equal to the average diffraction intensity value of all original data points, the original data points are positioned in a cube range taking the grid point to be interpolated as the center and the interpolation step length as the side length, and the original data points are points corresponding to reciprocal space coordinates.
The intensities of all original data points in the same cube range are added to the grid point to be interpolated in the center of the cube.
And determining an arithmetic mean value of the intensity added to each grid point to be interpolated respectively, and determining the arithmetic mean value as a diffraction intensity value on the interpolation point in the target reciprocal space.
Optionally, the spatial range to be interpolated may be determined according to a range of the target reciprocal space.
The interpolation step size is not greater than the resolution of the reciprocal space coordinate in the target reciprocal space.
Optionally, in the system, the two-dimensional plane detector is located on a diffractometer, and the diffractometer is a diffractometer with at least four diffraction circles.
An apparatus for acquiring X-ray diffraction signals, comprising:
a processor.
A memory for storing processor-executable instructions.
Wherein the processor is configured to execute the instructions to implement the method of acquiring X-ray diffraction signals as defined in any one of the above.
A computer readable storage medium, wherein instructions, when executed by a processor of an electronic device, enable the electronic device to perform a method of acquiring X-ray diffraction signals as described in any one of the above.
The embodiment of the invention provides a method, a system, equipment and a storage medium for collecting X-ray diffraction signals. Meanwhile, the method processes the acquired data by utilizing the matrix operation, the matrix transformation and the parallel interpolation algorithm, realizes the rapid processing of the diffraction signal, shortens the processing time of the data, and further plays a role in promoting the acquisition speed of the diffraction signal.
Therefore, the invention realizes the rapid and efficient acquisition of most diffraction signals in the wide-area reciprocal space by adopting the diffractometer with at least four diffraction circles, matching with the two-dimensional surface detector and assisting with the parallel interpolation algorithm and the data coordinate conversion.
Of course, it is not necessary for any product or method to achieve all of the above-described advantages at the same time for practicing the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of a six-circle diffractometer used in an embodiment of the present invention;
fig. 2 is a flowchart of circular symmetric reciprocal space scanning in the method for acquiring X-ray diffraction signals according to the embodiment of the present invention;
FIG. 3 is a schematic diagram of a circular symmetric reciprocal space scan according to an alternative embodiment of the present invention;
FIG. 4- (a) is a schematic diagram of a diffraction geometry for performing three-dimensional diffraction according to an alternative embodiment of the present invention;
FIG. 4- (b) is a schematic diagram of a diffraction geometry for performing three-dimensional diffraction according to an alternative embodiment of the present invention;
FIG. 5 is a schematic diagram of a parallel interpolation algorithm according to an alternative embodiment of the present invention;
FIG. 6 is a block diagram of an X-ray diffraction signal acquisition system according to an embodiment of the present invention;
fig. 7 is a block diagram of an apparatus for acquiring X-ray diffraction signals according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The embodiment of the invention provides a method for acquiring an X-ray diffraction signal, which comprises the following steps:
the sample is irradiated with X-rays emitted by an X-ray source.
Wherein, the X-ray source includes but is not limited to: the specific choice of the X-ray tube and the synchrotron radiation light source lamp is selected by a person skilled in the art according to the actual application scenario, and the invention is not limited herein.
And performing annular symmetrical reciprocal space scanning on the target reciprocal space of the sample by using a two-dimensional plane detector to obtain first diffraction data in the target reciprocal space.
The two-dimensional plane detector is positioned on the diffractometer, and the diffractometer required to be adopted by the invention needs to comprise not less than four diffraction circles (omega, chi, psi and 2 theta). Synchrotron radiation and diffractometers used in the conventional laboratory are typically "4S +2D" six-circle mode and "3S +1D" four-circle mode (S: sample D: detector). Fig. 1 shows a typical six-circle diffractometer structure, wherein the X-ray (X-ray) emission direction is a preset Y-axis direction, the preset X-axis and the preset Z-axis are perpendicular to the preset Z-axis respectively, a spatial coordinate system with the sample center as the center is formed, 4 rotation circles of the sample are μ, ω, χ, ψ, and 2 rotation circles of the detector are 2 θ, ν. If the mu and upsilon circles in the six-circle diffractometer are fixed, the four-circle diffraction mode is changed, and the corresponding four circles are the omega, chi and psi circles of the sample and the 2 theta circle corresponding to the detector respectively. The diffractometer used in the present invention needs to contain not less than four diffraction circles, and the signal collection of the present invention is described below in the "3S +1D" four-circle diffraction mode.
Compared with a common point detector, the two-dimensional plane detector has the advantages that the result acquired by one-time scanning is three-dimensional, the content of the acquired data is richer, and the later-stage data processing efficiency is more favorably improved.
As shown in fig. 2, the process of circular symmetric reciprocal space scanning may specifically include:
using a two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to be 0, wherein omega is the angle of the sample rotating around the preset X axis, chi is the angle of the sample rotating around the preset Y axis, psi is the angle of the sample rotating around the preset Z axis, and 2 theta is the angle of the two-dimensional detector rotating around the preset X axis.
Step S201, controlling the sample to rotate 360 degrees along the psi circle.
Step S202, determining whether the part of the target reciprocal space Qz under the current 2 θ and ω values is positive, if so, triggering step S204, and if not, triggering step S203.
Step S203, control χ change Δ χ, and return to step S201.
Step S204, determining whether the target reciprocal space has been scanned, if yes, triggering step S206, and if not, triggering step S205.
Step S205, control 2 θ changes by Δ 2 θ, control ω changes by Δ ω where 2 Δ ω = Δ 2 θ, and the process returns to step S201.
And step S206, ending the processing.
And the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
For ease of understanding, an alternative embodiment of the present invention is described herein specifically in connection with FIG. 3:
in fig. 3, the horizontal axis of the coordinate system is h00, and the vertical axis is 00l, where the horizontal axis h00 is the horizontal plane of the sample, and the vertical axis 00l is the coordinate axis of the target reciprocal space along the normal direction of the sample. The box in fig. 3 is the real-time detection range of the two-dimensional area detector.
Where (1) in fig. 3 is a fixed 2 θ, ω, the sample is controlled to rotate 360 degrees along the ψ circle.
In fig. 3, (2) shows the control χ variation Δ χ, and the scanning process of (1) is repeated.
Fig. 3 (3) is a scan process of repeating (2) until the positive portion of the reciprocal space along the coordinate axis normal to the sample is scanned.
Fig. 3 (4) shows the linkage 2 θ, ω, the change 2 Δ ω = Δ 2 θ, and the scanning process of (3) is repeated.
Fig. 3 (5) shows the scanning process of (4) being repeated until the target reciprocal space is scanned.
Optionally, in another alternative embodiment of the present invention, the real-time detection range and the resolution of the two-dimensional area detector may be adjustable, wherein the resolution is determined by the pixels of the two-dimensional area detector, typically 1000 × 1000. If the distance between the two-dimensional plane detector and the sample is reduced, the real-time detection range in the reciprocal space is enlarged, the range corresponding to a single pixel is enlarged, and the resolution is reduced. On the contrary, the distance between the two-dimensional surface detector and the sample is increased, so that the real-time detection range of the two-dimensional surface detector in the reciprocal space is reduced, the range corresponding to a single pixel is reduced, and the resolution ratio is increased.
Optionally, in the scanning process, the specific size of Δ χ and Δ 2 θ may be determined by a person skilled in the art according to the real-time detection range of the two-dimensional detector, which is not limited in the present invention.
Optionally, the actual range of the target reciprocal space of the final scan is determined by the actual ranges of χ and 2 θ, and those skilled in the art can determine the actual ranges according to actual needs.
Optionally, in another optional embodiment of the present invention, in the step S205, ω and 2 θ are linked, and ω = θ is selected in the present invention, and a person skilled in the art may determine the quantitative relationship between ω and θ according to actual needs, without limiting the present invention.
Optionally, as shown in fig. 2, the annular symmetric reciprocal space scanning is performed on a diffractometer with four diffraction circles, and when the diffractometer with six diffraction circles is adopted, only μ needs to be fixed, and θ = 0. In other alternative embodiments of the present invention, those skilled in the art can fix the variables other than ω, χ, ψ, and 2 θ to 0 when using a diffractometer having not less than four diffraction circles according to actual needs, that is, those skilled in the art can achieve the technical effects of the present invention without the need to pay creative labor.
The invention adopts the diffractometer with no less than four diffraction circles to match with the two-dimensional surface detector to carry out annular symmetrical scanning on the wide-area diffraction reciprocal space, can directly collect the three-dimensional information of a sample due to the adoption of the two-dimensional surface detector for scanning, thereby obtaining more information, and can collect diffraction signals in a larger range due to the adoption of the annular symmetrical scanning mode, so that the invention can realize the collection of most diffraction signals in the wide-area reciprocal space.
Optionally, the method provided in the embodiment of the present invention further includes:
and converting the first diffraction data into reciprocal space coordinates from angle coordinates by using all diffraction fillet values corresponding to the irradiation positions of the straight-through light on the two-dimensional surface detector, wherein the straight-through light is the ray emitted by the X-ray source after passing through the sample.
Wherein the first diffraction data includes but is not limited to: the method comprises the steps of acquiring a two-dimensional data picture by a two-dimensional plane detector, angle values corresponding to four circles of a diffractometer, wavelength lambda (or energy E) of incident X-rays, the size of the two-dimensional plane detector and the size of a pixel point, the irradiation position (Beam center) of through light on the two-dimensional plane detector and the distance L from a sample to the detector.
The angles corresponding to the two-dimensional data picture and the four circles of the diffractometer are both angle coordinates, so that the angle coordinates of the data need to be converted into reciprocal space coordinates, and further data analysis can be performed.
Optionally, in practical application, the foregoing utilize each diffraction fillet value that straight-through light irradiation position on the two-dimensional surface detector corresponds, convert first diffraction data into reciprocal space coordinate by angle coordinate, specifically include:
the method comprises the steps of calculating all diffraction fillet values corresponding to irradiation positions of straight-through light on a two-dimensional detector, calculating all diffraction fillet values of pixel points at other positions on the current two-dimensional detector except the irradiation positions, and calculating emergent light wave vectors corresponding to the pixel points at other positions according to the calculated all diffraction fillet values of the pixel points at other positions, so that first diffraction data are converted into reciprocal space coordinates from angle coordinates.
The invention adopts a matrix operation and matrix transformation mode to quickly and accurately convert diffraction data from a laboratory angle coordinate to a reciprocal space coordinate. Because the data in the two-dimensional data picture is a matrix, the angle rotation can be easily expressed in a matrix form, and the matrix calculation greatly simplifies the calculation process. Because the position of the pixel point on the two-dimensional plane detector is fixed relative to the Beamcenter, and the angular rotation of the pixel point relative to the sample is synchronous and same in size, the method does not need to calculate the angles of four circles corresponding to each pixel point, and only needs four round angle values corresponding to the Beamcenter.
Optionally, in an optional embodiment of the present invention, a specific calculation method for calculating the emergent light wave vector corresponding to each pixel point is as follows:
1. firstly, calculating an incident wave vector corresponding to each pixel point on the two-dimensional plane detector in an initial state (each rotation circle is at a zero point)
And the emergent wave vector
Output of
And
a matrix of N rows and three columns.
2. In the experiment, the angle rotation is represented by a rotation matrix, and the angle rotation is carried out after the rotation
And
calculated by the formulas (2) and (3) (if the six-circle is adopted)Diffraction pattern, adding corresponding rotation matrix).
Where H is the rotation matrix of the ω circle, D is the rotation matrix of the 2 θ circle, X is the rotation matrix of the χ circle, φ is the rotation matrix of the ψ circle:
it is also necessary to calculate the incident wave vector under the initial condition
And the outgoing wave vector
For ease of understanding, reference is made herein to an alternative embodiment of the invention as illustrated in fig. 4- (a) and 4- (b). Under the initial condition, as shown in fig. 4- (a), when the incident X-ray is along the preset Y-axis direction, the corresponding early watt (Ewald) sphere radius is 2 pi/λ, and it can be obtained:
for each pixel on the two-dimensional area Detector (Detector) 401, their values
Are uniform, but corresponding emergent wave vectors
Different, the respective corresponding directions are respectively from the sample center (O point) to each pixel point on the two-dimensional plane detector 401, and the radius is the radius of the early watt sphere. To calculate an arbitrary point M on the detector
As an example, it is assumed that the pixel point is different from the through light irradiation position (Beem center) 402 by m pixel points in the preset X-axis direction, and is different from the through light irradiation position (Beem center) 402 by n pixel points in the preset Z-axis direction. The size of each pixel point in the X-axis direction is preset to be l 1 The dimension in the Z-axis direction is preset to be l 2 And the length from the detector 401 to the center (O point) of the sample is L, the coordinate of the M point in real space at this time can be calculated as (ml) 1 ,L,nl 2 ) Then vector of
Then, the outgoing wave vector corresponding to the M point in the initial state is:
namely:
fig. 4- (b) is a schematic view showing a state in which scanning is performed in association with 2 θ, ω during scanning.
The emergent light wave vector can be calculated by combining formula (1), formula (2), formula (3), formula (4), formula (5) and formula (6)
Since its expression is too long and too complex, it is not expanded here.
Alternatively, in other alternative embodiments of the present invention, a person skilled in the art can combine the above 6 formulas to perform numerical operations without creative efforts, and does not need arithmetic expressions. In the actual calculation process, the matrix operation mode is adopted to simultaneously calculate the point correspondences of all the pixel points
It is stored in a matrix of N rows and 3 columns.
Optionally, the method provided in the embodiment of the present invention further includes:
and (3) performing interpolation reconstruction on the reciprocal space coordinates by using a parallel interpolation algorithm to obtain a diffraction intensity value on an interpolation point in the target reciprocal space.
In practical applications, the distribution of the first diffraction data in the target reciprocal space is not uniform after the transformation, and thus the first diffraction data cannot be used for quantitative analysis. If the data is to be quantitatively analyzed, for example, structural information such as a crystal domain proportion and the like is obtained by integrating diffraction peak intensities, data interpolation processing needs to be performed on the data first to obtain diffraction intensity values on uniform grid points (i.e., the interpolation points) in the reciprocal space.
Optionally, the performing interpolation reconstruction on the reciprocal space coordinate by using the parallel interpolation algorithm to obtain the diffraction intensity value on the interpolation point in the target reciprocal space specifically includes:
and determining a regular three-dimensional grid according to the space range to be interpolated and the interpolation step length, wherein the diffraction intensity value of each grid point to be interpolated is equal to the average diffraction intensity value of all original data points, the original data points are positioned in a cube range taking the grid point to be interpolated as the center and the interpolation step length as the side length, and the original data points are points corresponding to reciprocal space coordinates.
The intensities of the original data points in the same cube range are added to the grid point to be interpolated in the center of the cube.
And determining an arithmetic mean value of the intensity added to each grid point to be interpolated respectively, and determining the arithmetic mean value as a diffraction intensity value on the interpolation point in the target reciprocal space.
In practical applications, fast interpolation reconstruction of large amounts of data is a difficult point. In order to ensure that the wide-area three-dimensional diffraction result still has enough resolution, the data picture acquired by one experiment of wide-area three-dimensional diffraction is more than thousands of frames, and the number of data points exceeds 10 9 The total amount of the original data exceeds 2G; on the other hand, the user also wants that the experimental result can be presented in front of the user within minutes after the data collection, so as to judge whether the data is available and take the next experimental measures. The interpolation reconstruction of such a large amount of data is very difficult to complete within several minutes, and therefore, the above parallel interpolation algorithm needs to be used for fast interpolation reconstruction of the large amount of data.
Optionally, in an optional embodiment of the present invention, before performing interpolation, a spatial range to be interpolated and an interpolation step size (interpolation precision) need to be determined, where the spatial range to be interpolated may be determined according to an actually measured target reciprocal spatial range, the interpolation step size cannot be higher than a resolution of data itself in a reciprocal space, and if the interpolation density is low, the precision of a final result may be reduced. After the interpolation space range and the interpolation step length are determined, a regular three-dimensional grid can be constructed, and then how to calculate the diffraction signal intensity on the grid point (interpolation point), namely interpolation.
Alternatively, as shown in fig. 5, in another alternative embodiment of the present invention, the value of each grid point to be interpolated (blue point) is equal to the average intensity of all original data points in a square range centered on the point and having the interpolation step as the side length.
The black lattice is a regular grid constructed according to a diffraction space range and an interpolation step length, the black points are the points to be interpolated, the white points are original data points which are unevenly distributed in a reciprocal space, and as shown in fig. 5, the interpolation is the diffraction intensity value of the black point at the center of a frame, which is the arithmetic average value of the white points in the frame. Where the initial value of all black dots is set to 0.
In order to perform parallel interpolation operation, that is, perform interpolation operation on N original data maps simultaneously, the parallel interpolation algorithm provided in the embodiment of the present disclosure further includes another important strategy, that is, add the intensity of an original data point to its nearest neighboring interpolation point, record a first number of original data points to which the interpolation point has been added, and calculate an average value of diffraction intensity values of the first number of original data points.
The parallel interpolation algorithm can conveniently perform parallel calculation, namely original scattered point data can be split into a plurality of processes for processing, calculation is not required to be performed after all the original scattered point data are completely obtained, and the calculation speed is improved.
Optionally, the spatial range to be interpolated may be determined according to a range of the target reciprocal space.
The interpolation step is not greater than the resolution of the reciprocal space coordinates in the target reciprocal space.
Optionally, in the method provided by the embodiment of the present invention, the two-dimensional surface detector is located on a diffractometer, and the diffractometer is a diffractometer with no less than four diffraction circles.
In practical application, the invention adopts the diffractometer with at least four diffraction circles to match the two-dimensional plane detector to perform annular symmetrical scanning on the wide-area diffraction reciprocal space, can directly acquire the three-dimensional information of a sample due to the adoption of the two-dimensional plane detector for scanning, thereby acquiring more information, and can acquire diffraction signals in a wider range due to the adoption of the annular symmetrical scanning mode, so that the invention can realize the acquisition of most diffraction signals in the wide-area reciprocal space. Meanwhile, the method processes the acquired data by utilizing the matrix operation, the matrix transformation and the parallel interpolation algorithm, realizes the rapid processing of the diffraction signal, shortens the processing time of the data, and further plays a promoting role in improving the acquisition speed of the diffraction signal.
Therefore, the invention realizes the rapid and efficient acquisition of most diffraction signals in the wide-area reciprocal space by adopting the diffractometer with at least four diffraction circles, matching with the two-dimensional surface detector and assisting with the parallel interpolation algorithm and the data coordinate conversion.
Corresponding to the above embodiment of the method for acquiring X-ray diffraction signals, the present invention further provides an acquisition system for X-ray diffraction signals, as shown in fig. 6, the acquisition system for X-ray diffraction signals includes:
the light source module 601 emits X-rays through the X-ray source to irradiate the sample.
The acquisition module 602 performs circular symmetric reciprocal space scanning on a target reciprocal space of a sample through a two-dimensional plane detector to obtain first diffraction data in the target reciprocal space.
The circular symmetric reciprocal space scanning specifically comprises:
using a two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to be 0, wherein omega is the angle of the sample rotating around the preset X axis, chi is the angle of the sample rotating around the preset Y axis, psi is the angle of the sample rotating around the preset Z axis, and 2 theta is the angle of the two-dimensional detector rotating around the preset X axis.
The sample was controlled to rotate 360 degrees around the psi circle.
Determining whether scanning of the part with the target reciprocal space Qz under the current 2 theta and omega values being positive is finished, if not, controlling the x change delta x, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle; if yes, the target reciprocal space is judged to be scanned completely, if the target reciprocal space is not scanned completely, 2 theta is controlled to change delta 2 theta, omega is controlled to change delta omega, wherein 2 delta omega = delta 2 theta, and the step is returned to control the sample to rotate 360 degrees along the psi circle; and if the target reciprocal space is scanned completely, ending the processing.
And the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
Optionally, the system further includes:
and the coordinate conversion module converts the first diffraction data into reciprocal space coordinates from angle coordinates by using various diffraction fillet values corresponding to the irradiation positions of the direct light on the two-dimensional detector, wherein the direct light is the ray emitted by the X-ray source after passing through the sample.
Optionally, the coordinate transformation module may be specifically configured to:
the method comprises the steps of calculating all diffraction fillet values corresponding to irradiation positions of direct light on a two-dimensional detector, calculating all diffraction fillet values of pixel points at other positions on the current two-dimensional detector except the irradiation positions, and calculating emergent light wave vectors corresponding to the pixel points at other positions according to the calculated all diffraction fillet values of the pixel points at other positions, so that first diffraction data are converted into reciprocal space coordinates from angle coordinates.
Optionally, the system further includes:
and the interpolation reconstruction module performs interpolation reconstruction on the reciprocal space coordinates by using a parallel interpolation algorithm to obtain a diffraction intensity value on an interpolation point in the target reciprocal space.
Optionally, the interpolation reconstruction module may be specifically configured to:
and determining a regular three-dimensional grid according to the space range to be interpolated and the interpolation step length, wherein the diffraction intensity value of each grid point to be interpolated is equal to the average diffraction intensity value of all original data points, the original data points are positioned in a cube range which takes the grid point to be interpolated as the center and takes the interpolation step length as the side length, and the original data points are points corresponding to reciprocal space coordinates.
The intensities of the original data points in the same cube range are added to the grid point to be interpolated in the center of the cube.
And determining an arithmetic mean value of the intensity added to each grid point to be interpolated respectively, and determining the arithmetic mean value as a diffraction intensity value on the interpolation point in the target reciprocal space.
Optionally, the spatial range to be interpolated may be determined according to a range of the target reciprocal space.
The interpolation step is not greater than the resolution of the reciprocal space coordinates in the target reciprocal space.
Optionally, in the system, the two-dimensional plane detector is located on a diffractometer, and the diffractometer is a diffractometer with at least four diffraction circles.
In practical application, the invention adopts the diffractometer with no less than four diffraction circles to match the two-dimensional surface detector to perform annular symmetric scanning on the wide-area diffraction reciprocal space, and can directly acquire the three-dimensional information of a sample to acquire more information due to the adoption of the two-dimensional surface detector for scanning. Meanwhile, the method processes the acquired data by utilizing the matrix operation, the matrix transformation and the parallel interpolation algorithm, realizes the rapid processing of the diffraction signal, shortens the processing time of the data, and further plays a promoting role in improving the acquisition speed of the diffraction signal.
As shown in fig. 7, an embodiment of the present invention further provides an apparatus for acquiring an X-ray diffraction signal, including:
a processor 701.
A memory 702 for storing processor-executable instructions.
Wherein the processor is configured to execute the instructions to implement the method of acquiring X-ray diffraction signals as in any one of the above.
A computer readable storage medium, wherein instructions, when executed by a processor of an electronic device, enable the electronic device to perform any one of the methods of X-ray diffraction signal acquisition described above.
Computer-readable media, including both permanent and non-permanent, removable and non-removable media, may implement the information storage by any method or technology. The information may be computer readable instructions, data structures, modules of a program, or other data. Examples of computer storage media include, but are not limited to, phase change memory (PRAM), static Random Access Memory (SRAM), dynamic Random Access Memory (DRAM), other types of Random Access Memory (RAM), read Only Memory (ROM), electrically Erasable Programmable Read Only Memory (EEPROM), flash memory or other memory technology, compact disc read only memory (CD-ROM), digital Versatile Disks (DVD) or other optical storage, magnetic cassettes, magnetic tape magnetic disk storage or other magnetic storage devices, or any other non-transmission medium, which can be used to store information that can be accessed by a computing device. As defined herein, a computer readable medium does not include a transitory computer readable medium such as a modulated data signal and a carrier wave.
As will be appreciated by one skilled in the art, embodiments of the present application may be provided as a method, system, or computer program product. Accordingly, the present application may take the form of an entirely hardware embodiment, an entirely software embodiment or an embodiment combining software and hardware aspects. Furthermore, the present application may take the form of a computer program product embodied on one or more computer-usable storage media (including, but not limited to, disk storage, CD-ROM, optical storage, and the like) having computer-usable program code embodied therein.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrases "comprising a," "8230," "8230," or "comprising" does not exclude the presence of additional identical elements in the process, method, article, or apparatus comprising the element.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A method for acquiring X-ray diffraction signals, comprising:
emitting X-rays to irradiate the sample through an X-ray source;
performing annular symmetrical reciprocal space scanning on a target reciprocal space of the sample by using a two-dimensional detector to obtain first diffraction data in the target reciprocal space;
the annular symmetrical reciprocal space scanning specifically comprises:
using the two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to be 0, wherein omega is the angle of the sample rotating around a preset X axis, chi is the angle of the sample rotating around a preset Y axis, psi is the angle of the sample rotating around a preset Z axis, and 2 theta is the angle of the two-dimensional plane detector rotating around the preset X axis;
controlling the sample to rotate 360 degrees along a psi circle;
judging whether scanning of the part with the target reciprocal space Qz under the current 2 theta and omega values being positive is finished, if not, controlling the x change delta x, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle; if yes, judging whether the target reciprocal space is scanned completely, if not, controlling 2 theta to change delta 2 theta and controlling omega to change delta omega, wherein 2 delta omega is not larger than delta 2 theta, and returning to the step to control the sample to rotate 360 degrees along the psi circle; if the target reciprocal space is scanned completely, ending the processing;
and the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
2. The method of claim 1, further comprising:
and converting the first diffraction data into reciprocal space coordinates from angle coordinates by using diffraction fillet values corresponding to irradiation positions of straight-through light on the two-dimensional surface detector, wherein the straight-through light is the ray emitted by the X-ray source after passing through the sample.
3. The method according to claim 2, wherein the converting the first diffraction data from angular coordinates to reciprocal space coordinates by using each diffraction fillet value corresponding to an irradiation position of the direct light on the two-dimensional surface detector comprises:
the method comprises the steps of calculating all diffraction fillet values corresponding to irradiation positions of direct light on a two-dimensional detector, calculating all diffraction fillet values of pixel points at other positions on the two-dimensional detector except the irradiation positions, and calculating emergent light wave vectors corresponding to the pixel points at other positions according to the calculated all diffraction fillet values of the pixel points at other positions, so that the first diffraction data are converted into reciprocal space coordinates from angle coordinates.
4. The method of claim 2 or 3, further comprising:
and carrying out interpolation reconstruction on the reciprocal space coordinates by using a parallel interpolation algorithm to obtain a diffraction intensity value on an interpolation point in the target reciprocal space.
5. The method according to claim 4, wherein the performing interpolation reconstruction on the reciprocal space coordinates by using a parallel interpolation algorithm to obtain diffraction intensity values at interpolation points in the target reciprocal space specifically includes:
determining a regular three-dimensional grid according to a space range to be interpolated and an interpolation step length, wherein the diffraction intensity value of each grid point to be interpolated is equal to the average diffraction intensity value of all original data points, the original data points are positioned in a cube range taking the grid point to be interpolated as the center and the interpolation step length as the side length, and the original data points are points corresponding to the reciprocal space coordinates;
adding the intensity of each original data point in the same cube range to a grid point to be interpolated in the center of the cube;
and determining an arithmetic mean value of the intensity added to each grid point to be interpolated respectively, and determining the arithmetic mean value as a diffraction intensity value on the interpolation point in the target reciprocal space.
6. The method according to claim 5, characterized in that the spatial range to be interpolated is determined according to the range of the target reciprocal space;
the interpolation step is not greater than a resolution of the reciprocal space coordinate in the target reciprocal space.
7. The method of claim 1, wherein the two-dimensional area detector is located on a diffractometer that is not less than four diffraction circles.
8. An X-ray diffraction signal acquisition system, comprising:
the light source module is used for emitting X rays to irradiate the sample through the X-ray source;
the acquisition module is used for performing annular symmetrical reciprocal space scanning on a target reciprocal space of the sample through a two-dimensional plane detector to obtain first diffraction data in the target reciprocal space;
the acquisition module carries out annular symmetrical reciprocal space scanning and specifically sets as:
using the two-dimensional surface detector to perform continuous scanning, and performing the following processing in the continuous scanning process:
initializing 2 theta, omega, chi and psi to be 0, wherein omega is the angle of the sample rotating around a preset X axis, chi is the angle of the sample rotating around a preset Y axis, psi is the angle of the sample rotating around a preset Z axis, and 2 theta is the angle of the two-dimensional plane detector rotating around the preset X axis;
controlling the sample to rotate 360 degrees along a psi circle;
determining whether scanning of a part with a positive target reciprocal space Qz under the current 2 theta and omega values is finished, if not, controlling the x change delta x, and returning to the step of controlling the sample to rotate 360 degrees along the psi circle; if so, judging that the target reciprocal space is scanned completely, if not, controlling 2 theta to change delta 2 theta, controlling omega to change delta omega, wherein 2 delta omega =delta2 theta, and returning to the step to control the sample to rotate 360 degrees along the psi circle; if the target reciprocal space is scanned completely, ending the processing;
and the target reciprocal space Qz is a coordinate axis of the target reciprocal space along the normal direction of the sample.
9. An apparatus for acquiring X-ray diffraction signals, comprising:
a processor;
a memory for storing processor-executable instructions;
wherein the processor is configured to execute the instructions to implement the method of acquiring X-ray diffraction signals of any of claims 1 to 7.
10. A computer readable storage medium, instructions in which, when executed by a processor of an electronic device, enable the electronic device to perform the method of acquiring X-ray diffraction signals of any one of claims 1 to 7.
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