CN119470502B - Method, system and terminal for obtaining the degree of crystal plane rotation in alloy material - Google Patents
Method, system and terminal for obtaining the degree of crystal plane rotation in alloy materialInfo
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- CN119470502B CN119470502B CN202411559645.9A CN202411559645A CN119470502B CN 119470502 B CN119470502 B CN 119470502B CN 202411559645 A CN202411559645 A CN 202411559645A CN 119470502 B CN119470502 B CN 119470502B
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- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
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Abstract
The invention provides a method, a system and a terminal for obtaining the rotation degree of crystal faces in an alloy material, which comprise the steps of obtaining two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, integrating the two-dimensional synchrotron radiation diffraction data, dividing a plurality of sector area integrals and whole diffraction data integrals to respectively obtain corresponding peak position-peak intensity curves, calibrating diffraction peaks of the peak position-peak intensity curves to obtain corresponding diffraction peaks, carrying out normalization processing on peak areas of the diffraction peaks, adding the diffraction peak areas subjected to normalization processing in the same phase to obtain the sum of normalized diffraction peak areas of specific phases of each sector area of the alloy material to be tested, and comparing the sum of normalized diffraction peak areas in each sector area of the alloy material to be tested at each moment to obtain quantitative representation of the rotation of a crystal face of a certain phase in the alloy material to be tested at each moment. The invention has high accuracy, simple sample preparation and nondestructive measurement.
Description
Technical Field
The invention relates to the technical field of metal material diffraction analysis, in particular to a method, a system and a terminal for acquiring the rotation degree of a crystal face in an alloy material by utilizing synchrotron radiation diffraction data.
Background
In the deformation process of the alloy material, three crystal lattice behaviors, namely the change of a crystal lattice constant, the sliding of a crystal face and the rotation of the crystal face, are generated due to the action of internal stress, the three behaviors are needed to be analyzed for better explaining the deformation mechanism of the alloy material, the change of the crystal lattice constant can be calibrated through diffraction peak positions in an in-situ mechanical XRD experiment, the half-width of an XRD diffraction peak can reflect the size of dislocation density to a certain extent, the size of the dislocation density is closely related to the degree of the sliding of the crystal face, and for the measurement of the rotation of the crystal face of the polycrystalline alloy, as the polycrystalline alloy material is not like a single crystal, the rotation of the internal crystal face can be reversely pushed through the change of the diffraction pattern, the diffraction pattern of the polycrystalline alloy material is formed by superposition of a large number of crystal grain diffraction patterns, even if the deformation is subjected to strong plastic deformation, the diffraction pattern is formed by a plurality of Rabye rings, the change cannot be seen intuitively, and the measurement of the rotation of the crystal face cannot be processed like the single crystal alloy material.
There are various ways to study the rotation behavior of crystal planes in alloy materials, and a model estimation method can be used, and s.kok et al (Kok S,Beaudoin AJ,Tortorelli D A.Numerical integration of lattice rotation in polycrystal plasticity[J].International Journal for Numerical Methods in Engineering,2001,52(12):1487-1500.) uses a polycrystalline model to simulate polycrystalline plastic deformation, and proposes a numerical algorithm based on the analysis integral of a lattice rotation evolution equation to estimate the rotation behavior of the crystal lattice. In recent years, with the continued development of spectroscopic techniques, EBSD techniques have been applied to measure lattice rotation, huigang Shi et al (Shi,H.,Chen,J.,Lu,J.,Zhu,L.,Zhang,L.,Li,J.,…Guo,X.(2024).The activation of multiple slip systems in polycrystalline zirconium by using automated lattice rotation framework.Materials Research Letters,12(12),912–920.) analyzed the plastic deformation mechanism of polycrystalline zirconium, wherein slip of alloy materials and lattice rotation have been studied using EBSD techniques, yingbo Bai et al (Bai,Y.,Zhang,R.,Cui,C.,Zhou,Y.,&Sun,X.(2024).In-situ observation of Ni-Co based wrought superalloy high-temperature deformation:lattice rotation and grain boundary response.Materials Research Letters,12(11),869–876.) studied slip and lattice rotation of Ni-Co based alloy grains by EBSD data analysis. However, both the two methods have the defects that the accuracy of the model estimation can only stay on the estimation all the time, and the actual convincing force is insufficient, and the measurement is carried out by using the EBSD technology, so that the measurement of the rotation of the crystal face can only stay in the crystal grains with the surface in the visual field, and the number of the crystal grains is too small.
Therefore, a new method needs to be developed to measure the rotation degree of the internal crystal face of the alloy material so as to meet the requirements of high accuracy, simple sample preparation, nondestructive measurement, statistical significance of measurement results and the like, thereby providing accurate experimental basis and data support for the description of the rotation process of the crystal face in the plastic deformation process of the alloy.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method, a system and a terminal for acquiring the rotation degree of a crystal face in an alloy, and specific quantitative indexes of the crystal face rotation process in different states in a target alloy are determined through synchrotron radiation diffraction data analysis.
According to one aspect of the present invention, there is provided a method for obtaining a degree of rotation of a crystal plane in an alloy material, comprising:
Acquiring two-dimensional synchrotron radiation diffraction data of an alloy material to be measured, wherein the two-dimensional synchrotron radiation diffraction data is in a multi-Debye ring form;
Carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of all sector areas;
Calibrating diffraction peaks of peak position-peak intensity curves of the fan-shaped areas to obtain peak areas of diffraction peaks corresponding to the fan-shaped areas; calibrating diffraction peaks of the peak position-peak intensity curve of the whole alloy material to be tested to obtain peak areas of diffraction peaks of the whole alloy material to be tested;
Normalizing the peak areas of the diffraction peaks of each sector area by using the standard integral intensity ratio of the diffraction peaks and the peak areas of the diffraction peaks of the whole alloy material to be measured, and adding the same phases of the normalized areas of the diffraction peaks to obtain the sum of the normalized areas of the diffraction peaks of the specific phases of each sector area of the alloy material to be measured at a certain moment;
and comparing the sum of normalized diffraction peak areas in each sector area of the alloy material to be measured at each moment to obtain quantitative representation of rotation of a certain phase crystal face in the alloy material to be measured at each moment.
Optionally, the acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be measured includes:
placing an alloy material to be tested, which transmits or diffracts synchronous radiation, on a sample table;
Changing the state of the alloy material to be measured, and simultaneously acquiring synchronous radiation diffraction data generated by the alloy material to be measured at different moments from a CCD.
Optionally, the two-dimensional synchrotron radiation diffraction data is subjected to zonal sector integration, wherein the circle center of the integral sector area is the circle center of the debye ring.
Optionally, the integration of the synchrotron radiation diffraction data of the whole two-dimensional area is performed, wherein the diffraction data of the whole two-dimensional area is fan-shaped integrated by taking the circle center of the debye ring as the circle center.
Optionally, the diffraction peak is calibrated at a wavelength used for the synchrotron radiation light for measurement.
Optionally, the normalizing the peak area of each diffraction peak in each sector area by using the standard integral intensity ratio of each diffraction peak and the peak area of each diffraction peak in the whole alloy material to be measured includes:
Obtaining the integral intensity ratio of each diffraction peak of the phases in the alloy of the alloy material to be measured;
Dividing the integral intensity of each diffraction peak of each sector area by the integral intensity ratio of each diffraction peak to obtain each diffraction peak data of each sector area after eliminating the influence of the difference;
dividing the diffraction peak data of each sector area after eliminating the influence of the difference by the peak area of each diffraction peak of the whole alloy to be measured to obtain the peak area of each diffraction peak normalized by each sector area, and completing the normalization of the diffraction peak area data.
Optionally, comparing the sum of normalized diffraction peak areas in each sector area at each moment of the alloy material to be measured, further includes:
dividing the sum of normalized diffraction peak areas of different states of the same alloy material to be measured by the sum of diffraction peak areas of the initial state, and normalizing the sum of normalized diffraction peak areas again.
Optionally, comparing the sum of normalized diffraction peak areas in each sector area at each moment of the alloy material to be measured, wherein:
And comparing the sum of the final normalized diffraction peak areas, wherein the comparison reflects the overall situation of the rotation of the internal crystal face of the alloy, and the change of the overall situation of the rotation of the internal crystal face of the alloy material to be measured at different times is obtained.
According to a second aspect of the present invention, there is provided a system for obtaining the degree of rotation of a crystal plane in an alloy material, comprising:
the data acquisition module is used for acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be detected, wherein the two-dimensional synchrotron radiation diffraction data are in a multi-Debye ring form;
The data integration module is used for carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of all sector areas;
The diffraction peak calibration module is used for carrying out diffraction peak calibration on the peak position-peak intensity curve of each sector area to obtain the peak area of each diffraction peak corresponding to each sector area;
The normalization processing module is used for carrying out normalization processing on the peak areas of the diffraction peaks of each sector area by utilizing the standard integral intensity ratio of the diffraction peaks and the peak areas of the diffraction peaks of the whole alloy material to be measured, and adding the areas of the diffraction peaks after normalization processing in the same phase to obtain the sum of the normalized diffraction peak areas of the specific phases of each sector area of the alloy material to be measured at a certain moment;
and the crystal face rotation quantitative representation module is used for comparing the sum of normalized diffraction peak areas in all sector areas of the alloy material to be detected at all times to obtain quantitative representation of the rotation of a certain phase crystal face in the alloy material to be detected at all times.
According to a third aspect of the present invention there is provided a terminal comprising a memory, a processor and a computer program stored on the memory and capable of running on the processor, the processor when executing the program being adapted to perform the method of obtaining the degree of rotation of the crystal plane within an alloy material.
Compared with the prior art, the invention has at least one of the following beneficial effects:
The method for obtaining the rotation degree of the crystal face in the alloy material provided by the embodiment of the invention can quantitatively analyze the rotation degree of the crystal face in the alloy material by utilizing the synchrotron radiation diffraction data, and the obtained result has higher reliability and better accuracy because the analysis is based on the peak area of the diffraction peak.
In the embodiment of the invention, the experimental data are obtained without damage, and only a sample capable of obtaining the synchrotron radiation diffraction data is needed, and the quantitative analysis of the crystal face rotation degree under the in-situ condition is realized because the data are obtained without damage, and the synchrotron radiation diffraction data are obtained based on the internal crystal lattice condition of the whole sample, so that the crystal face rotation measurement result obtained therewith has statistical significance, and the crystal face rotation condition of a large number of crystal grains in the alloy material can be obtained.
The invention has the characteristics of high accuracy, simple sample preparation, nondestructive measurement and statistical significance of measurement results.
Drawings
Other features, objects and advantages of the present invention will become more apparent upon reading of the detailed description of non-limiting embodiments, given with reference to the accompanying drawings in which:
FIG. 1 is a flow chart of a method for obtaining the rotation degree of a crystal plane in an alloy material according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of an embodiment of the experiment in the example of the invention;
FIG. 3 is a graph showing the diffraction data of Al-Zn alloy synchrotron radiation in the example of the present invention;
FIG. 4 is a schematic view of a sector integration region used in an example of the present invention;
FIG. 5 is a schematic diagram of the data obtained by integrating the diffraction data of the Al-Zn alloy synchrotron radiation by sector integration in the example of the invention;
FIG. 6 is a graph showing synchrotron radiation diffraction data of Ni-Co-Al alloy in the example of the present invention;
FIG. 7 is a graph showing the data obtained by integrating the diffraction data of the synchrotron radiation of the Ni-Co-Al alloy in the example of the present invention after sector integration.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the present invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications could be made by those skilled in the art without departing from the inventive concept. These are all within the scope of the present invention.
FIG. 1 is a flow chart of a method for obtaining the rotation degree of the crystal face in the alloy material according to an embodiment of the invention. Referring to fig. 1, the present embodiment provides a method for obtaining a degree of rotation of a crystal plane in an alloy material, the method including the steps of:
S100, acquiring two-dimensional synchrotron radiation diffraction data of a sample to be detected;
in the step, the sample to be tested refers to a sample which is made of an alloy material to be tested and is suitable for experiments, and the specific sample forms, the specific sample sizes and the like can be carried out according to the experimental requirements.
In this step, the two-dimensional synchrotron radiation diffraction data is obtained in the form of a multiple debye ring.
In a specific embodiment, obtaining the two-dimensional synchrotron radiation diffraction data of the sample to be measured can include using a synchrotron radiation transmission or diffraction sample with a size meeting the requirement, placing the sample on a sample stage, and obtaining synchrotron radiation diffraction data generated by the alloy at different moments from a CCD when an in-situ mechanical experiment, an in-situ electromagnetic experiment, an in-situ heating experiment or other experiments capable of changing the alloy state are performed on the alloy, wherein the diffraction data require that the clear contrast of the Rakah circle is high and enough to obtain data with certain credibility. Specifically, the laser does not contain coarse light spots which are formed by coarse crystals and have a width larger than that of a general debye ring, the ratio of the highest diffraction intensity of the debye ring to the intensity of the back substrate is larger than 100, and the total number of the debye rings is more than 5.
In the embodiment, the experimental data are obtained without damage, and only a sample capable of obtaining the synchrotron radiation diffraction data is needed to be prepared, so that the method is convenient and quick. And the acquisition of the synchrotron radiation diffraction data is based on the internal lattice condition of the whole sample, has statistical significance on crystal face rotation measurement results obtained in the subsequent steps, and can acquire crystal face rotation conditions of a large number of crystal grains in the alloy material.
S200, carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data obtained in the step S100 to obtain peak position-peak intensity curves of all sector areas;
In this step, the integration process can be performed by using synchrotron radiation data processing software, for example, GSAS-II or similar processing software, so that the integration of the sector integration in the area and the integration of the whole data (data total integration) can be conveniently realized.
In the step, the sector integration is carried out on the divided areas, wherein the circle center of the integrated sector area is the circle center of the debye ring. The integration (data total integration) of the synchrotron radiation diffraction data of the whole two-dimensional area is to integrate the whole two-dimensional diffraction data in a sector mode by taking the circle center of the debye ring as the circle center.
Specifically, referring to FIG. 4, the entire two-dimensional area is integrated at 0-90 degrees. The individual sectors may be integrated at 0 to 45 degrees and 45 to 90 degrees or other dividing methods. The zoned sector integration is to divide each zone (different sector ranges) into first and second areas, wherein the different sector ranges can be 0-30,30-60,60-90, 0-45,45-90, and can be determined according to actual requirements, and finally two curves are obtained, namely a peak position-peak intensity curve of the whole alloy material to be measured, namely 0-90, and a peak position-peak intensity curve of each sector, namely a peak position-peak intensity curve of each zone determined by 0-45,45-90 or 0-30,30-60,60-90 or other division methods.
S300, carrying out diffraction peak calibration on the peak position-peak intensity curves of all the sector areas to obtain peak areas of all the diffraction peaks Pi corresponding to all the sector areas, and simultaneously carrying out diffraction peak calibration on the peak position-peak intensity curves of the whole alloy material to be tested to obtain the peak areas of all the diffraction peaks of the whole alloy material to be tested;
In this step, the peak position of the diffraction peak is calibrated at the wavelength used for the synchrotron radiation light for measurement. Of course, this is just one way of this embodiment.
S400, carrying out normalization processing on the peak areas of all diffraction peaks of all sector areas by using the standard integral intensity ratio of all diffraction peaks and the peak areas of all diffraction peaks of the whole alloy material to be detected, and adding the same phases of all diffraction peak areas after the normalization processing to obtain the sum of normalized diffraction peak areas of specific phases of all sector areas of the alloy material to be detected at a certain moment;
to better achieve the final crystal plane rotation measurement, in a specific embodiment, S400 may employ the following steps:
s401, obtaining integral intensity ratios of different diffraction peaks of phases in the alloy;
In this step, the integrated intensity ratio of the different diffraction peaks of the phases in the alloy can be obtained by looking up an ICSD database or other literature.
S402, dividing the diffraction peak area of each diffraction peak corresponding to each sector area by the integral intensity ratio of different diffraction peaks detected in S401, so as to eliminate the influence of the difference of the diffraction integral intensity (namely diffraction peak area) of each diffraction peak;
S403, dividing the data obtained in S402 by the integral intensity of the corresponding diffraction peak in the total integral of the data obtained in S200 to normalize the diffraction peak area data to obtain the diffraction peak area of each sector area after normalization;
Specifically, in S401, the integral intensity ratio of the different diffraction peaks of the phases in the alloy may be expressed in terms of relative peak intensities, where the integral intensity of the diffraction peak with the highest peak intensity is 1, and the ratio of the remaining diffraction peaks to the diffraction peak with the highest peak intensity is I k,Ik, that is, the integral intensity ratio representing the different diffraction peaks, and then I k is normalized as the integral intensity ratio in the normalization step.
Specifically, in S402, a symbol may be usedIn order to calculate the integral intensity of diffraction peaks of each sector area conveniently, m represents the time of the sample, particularly the initial stage, the middle stage and the final stage of the experiment, n represents different phases in the alloy sample, particularly FCC, BCC or any other phase with a crystal structure, j represents different sector areas, particularly 0-30 degrees, 30-60 degrees or other sector areas, k represents the kth diffraction peak, particularly the diffraction peak of (001), (111) crystal face family of face-centered cubic crystals or other diffraction peaks,Calculating diffraction peak area representing the kth diffraction peak of phase n in the sector integration region j in the alloy sample at time mTo eliminate the influence of the difference in diffraction integrated intensity (diffraction peak area) of each diffraction peak itself.
Specifically, in S403, a symbol may be usedTo facilitate calculation of the integrated intensity of the corresponding diffraction peak in the total integral of the data obtained in S200, which represents the diffraction peak area of the kth diffraction peak of phase n in the total integral of the data in the alloy sample at time m, calculation ofTo normalize the diffraction peak areas.
In the step, the diffraction peak area data is normalized by the normalization method, and the normalization operation can be used for quantitative analysis of the crystal face rotation degree under the in-situ condition.
S404, normalizing diffraction peak areas of diffraction peaks in the same phase of the alloy material sample to be measured at the same time, which is obtained in S403Adding, passing throughAnd obtaining the sum of normalized diffraction peak areas of specific phases of all sector areas at a certain moment of a certain sample.
In the embodiment, as the data are obtained without damage, quantitative analysis can be performed on the rotation degree of the crystal face in the alloy material by utilizing the synchrotron radiation diffraction data, and analysis is performed on the basis of the peak area of the diffraction peak in the steps, the reliability of the obtained result is higher, the accuracy is better, and the quantitative analysis on the rotation degree of the crystal face under the in-situ condition can be realized.
S500, comparing the sum of normalized diffraction peak areas in different sector areas of the alloy material to be measured at different moments to obtain quantitative representation of rotation of a certain phase crystal face in the alloy at different moments.
In the step, the sum of normalized diffraction peak areas of different states of the same alloy material sample to be detected is divided by the sum of diffraction peak areas of the initial state, so that the sum of normalized diffraction peak areas is subjected to normalization again.
In the step, the comparison is performed by taking the sum of the final normalized diffraction peak areas as a table, so that the overall situation of the rotation of the internal crystal face of the alloy can be reflected, and the change of the overall situation of the rotation of the internal crystal face of the alloy at different moments can be obtained. Of course, in other embodiments, other comparison modes may be used, and are not limited to graphical comparison.
According to the method in the embodiment of the invention, the metal simple substance, alloy and other materials with definite diffraction behaviors of the sample to be detected are obtained. Diffraction peaks are clear and distinguishable, and interference among different diffraction peaks is less.
Based on the same technical conception, in another embodiment of the invention, a system for acquiring the rotation degree of the crystal face in the alloy material by using the synchrotron radiation diffraction data is further provided, and the system comprises a data acquisition module, a data integration module, a diffraction peak calibration module, a normalization processing module and a crystal face rotation quantitative representation module, wherein:
The data acquisition module is used for acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be detected, wherein the two-dimensional synchrotron radiation diffraction data is in a multi-Debye ring form;
The data integration module is used for carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of all sector areas;
The diffraction peak calibration module is used for carrying out diffraction peak calibration on the peak position-peak intensity curve of each sector area to obtain the peak area of each diffraction peak Pi corresponding to each sector area;
the normalization processing module is used for carrying out normalization processing on the peak areas of the diffraction peaks of all the sector areas by utilizing the standard integral intensity ratio of the diffraction peaks and the peak areas of the diffraction peaks of the whole alloy material to be measured, and adding the areas of the diffraction peaks after the normalization processing in the same phase to obtain the sum of the areas of the normalized diffraction peaks of the specific phases of all the sector areas of the alloy material to be measured at a certain moment;
And the crystal face rotation quantitative representation module is used for comparing the sum of normalized diffraction peak areas in each sector area of the alloy material to be detected at each moment to obtain quantitative representation of the rotation of a certain phase crystal face in the alloy material to be detected at each moment.
In the system for obtaining the rotation degree of the crystal face in the alloy material by using the synchrotron radiation diffraction data in the above embodiment of the present invention, the technology adopted by each module may refer to the steps corresponding to the above method embodiment for obtaining the rotation degree of the crystal face in the alloy material, which are not described herein again.
Based on the same technical concept, in another embodiment of the present invention, there is also provided a terminal including a memory, a processor, and a computer program stored on the memory and capable of running on the processor, where the processor executes the program to perform the method for obtaining the rotation degree of the crystal plane in the alloy material in any one of the above embodiments.
In order to better understand the above technical solution, the method for obtaining the rotation degree of the crystal plane in the alloy material in the specific embodiment of the present invention is further described below, and it should be understood that the present invention is not limited to the following embodiment.
Example 1
The embodiment obtains the crystal face rotation degree of an Al phase in the Al-Zn alloy, and the specific method comprises the following steps:
s1, acquiring two-dimensional synchrotron radiation diffraction data of an alloy material to be detected, wherein the two-dimensional synchrotron radiation diffraction data are in a multi-Debye ring form.
Specifically, in this embodiment, a dog-bone-shaped Al-Zn alloy sample is used, the thickness of the light transmission side of the sample is reduced sufficiently to enable the synchrotron radiation light to penetrate the sample, an in-situ stretching experiment is performed on a stretching experiment table, and a CCD is used to obtain synchrotron radiation light generated by penetrating an alloy material at different moments, the specific experimental implementation is shown in fig. 2, the obtained experimental data is shown in fig. 3 and is in a multi-debye ring form, and the synchrotron radiation diffraction data corresponds to the performed in-situ stretching experiment stages one by one.
S2, carrying out zonal sector integration on the obtained synchrotron radiation diffraction data by using synchrotron radiation data processing software, and integrating the whole synchrotron radiation diffraction data of the alloy.
Specifically, the point position of the transmitted light of the synchrotron radiation light is taken as the center of a circle, the horizontal right is taken as the starting point, the rotation angle towards the anticlockwise direction is taken as the positive, the sector integration of the sectors of 0-45 degrees and the sectors of 45-90 degrees is respectively carried out, the sector integration is taken as the area for researching the rotation of the crystal face, the sector integration of 0-90 degrees is carried out, the integral data of the whole alloy is taken as the integral data of the alloy, the schematic diagram of the sector integration area is shown in fig. 4, and the integral data is shown in fig. 5. Of course, in other embodiments, other angular sector areas and integral integrations are possible.
And S3, calibrating diffraction peaks of all the fan-shaped and alloy integral data.
For example, the number of the cells to be processed,Representing the peak area of the k diffraction peak in the 0-45 degree sector integration of the Al-Zn sample, in this example, k is three, namely 111 peak, 200 peak and 220 peak of Al, m represents the mth state, m in this example takes 1, 2 and 3, respectively represents the moment of the initial stretching stage, the initial plastic deformation stage and the final plastic deformation stage, and all the moments are calibrated and recorded respectively
And S4, performing peak shape fitting on diffraction peaks based on the integral data of each sector and the alloy to obtain peak areas of diffraction peaks of each sector.
Specifically, the standard integral intensity ratio of each first diffraction peak and the area of each diffraction peak of the alloy are utilized to normalize the peak areas of each diffraction peak of each sector, and the areas of each first diffraction peak of each sector after normalization are added in phase, so that the sum of normalized diffraction peak areas of specific phases of each sector at a certain moment of a certain sample is obtained;
in this step, the literature data is referred to obtain relative peak intensities I k of different diffraction peaks, the 111 diffraction peak of Al is 1, the 200 diffraction peak is 0.47,220 diffraction peak is 0.22, and calculation is performed AndTo normalize and sum the diffraction peak intensities.
Calculating samples at different momentsAndAnd calculateAnd
S5, comparing the sum of normalized diffraction peak areas in all sector areas of the alloy material to be measured at all times to obtain quantitative representation of rotation of a crystal face of a certain phase in the alloy material to be measured at all times.
In this stepAndListed in table 1 and analyzed as follows:
TABLE 1 variation of the total diffraction peak areas of the Al phase in different sector areas with different stages of stretching in the Al-Zn alloy of this example
According to the above table of the present invention,The smaller represents a decrease in the area of the diffraction peak compared with the initial state, the total number of crystal planes which generate diffraction at the sector is decreased, the crystal planes are rotated from the sector to the other sector, the larger represents an increase in the area of the diffraction peak compared with the initial state, the total number of crystal planes which generate diffraction at the sector is increased, and the crystal planes are rotated from the other sector to the sector.
Example 2
In this embodiment, the rotation degree of the crystal plane of the Ni phase in the Ni-Co-Al alloy is obtained by the following specific method:
S1, using a dog-bone-shaped Ni-Co-Al alloy sample, thinning the thickness of a synchronous radiation light penetrating side sufficiently to enable synchronous radiation light to penetrate the sample, carrying out in-situ stretching experiments on a stretching experiment table, using a CCD to obtain synchronous radiation light generated by penetrating alloy materials at different moments, wherein the specific experimental implementation mode is shown in fig. 2, the obtained experimental data are shown in fig. 6, and the synchronous radiation data are in one-to-one correspondence with the implemented in-situ stretching experimental stages.
S2, carrying out sector integration on the obtained data by using synchrotron radiation data processing software, taking the point position of the transmitted light of synchrotron radiation light as the center of a circle, taking the horizontal right as the starting point, setting the rotation angle towards the anticlockwise direction as positive, respectively carrying out sector integration of 0-45-degree sectors and 45-90-degree sectors as the area for researching crystal face rotation, carrying out sector integration of 0-90 degrees, and taking the integrated data as integral data of the alloy material, wherein the schematic diagram of the sector integration area is shown in fig. 4, and the integrated data is shown in fig. 7.
And S3, calibrating diffraction peaks of all the fan-shaped and alloy integral data.
For exampleRepresenting the peak area of the k diffraction peak in the 0-45 degree sector integration of the Ni-Co-Al sample, in this example, k has three, namely 111, 200 and 220 peaks of Ni, m represents the mth state, m in this example takes 1, 2 and 3, respectively represents the initial stretching stage, the initial plastic deformation stage and the final plastic deformation stage, and all the moments are calibrated and recorded respectively
And S4, performing peak shape fitting based on the integral data of each sector and the alloy material to obtain the peak areas of diffraction peaks of each sector.
In this step, the literature data is referred to obtain relative peak intensities I k of different diffraction peaks, the 111 diffraction peak of Ni is 1, the 200 diffraction peak is 0.42,220 diffraction peak is 0.21, and calculation is performedAndTo normalize and sum the diffraction peak intensities.
Calculating samples at different momentsAndAnd calculateAnd
S5, willAndListed in table 2, and analyzed,The smaller represents a decrease in the area of the diffraction peak compared with the initial state, the total number of crystal planes which generate diffraction at the sector is decreased, the crystal planes are rotated from the sector to the other sector, the larger represents an increase in the area of the diffraction peak compared with the initial state, the total number of crystal planes which generate diffraction at the sector is increased, and the crystal planes are rotated from the other sector to the sector. TABLE 2 variation of total area of diffraction peaks of Ni phase in different sector areas with different stages of drawing in Ni-Co-Al alloy
| Time m | Sector Y value of 0-45 degree | Fan Y value of 45-90 degrees |
| 1 (Initial stage of stretching) | 1 | 1 |
| 2 (Initial stage of plastic deformation) | 0.9521 | 0.9329 |
| 3 (Plastic deformation end stage) | 0.8098 | 1.1651 |
The foregoing describes specific embodiments of the present invention. It is to be understood that the invention is not limited to the particular embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the claims without affecting the spirit of the invention. The above-described preferred features may be used in any combination without collision.
Claims (10)
1. A method for obtaining the degree of rotation of a crystal plane in an alloy material, comprising:
Acquiring two-dimensional synchrotron radiation diffraction data of an alloy material to be measured, wherein the two-dimensional synchrotron radiation diffraction data is in a multi-Debye ring form;
Carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of all sector areas;
Calibrating diffraction peaks of peak position-peak intensity curves of the fan-shaped areas to obtain peak areas of diffraction peaks corresponding to the fan-shaped areas; calibrating diffraction peaks of the peak position-peak intensity curve of the whole alloy material to be tested to obtain peak areas of diffraction peaks of the whole alloy material to be tested;
Normalizing the peak areas of the diffraction peaks of each sector area by using the standard integral intensity ratio of the diffraction peaks and the peak areas of the diffraction peaks of the whole alloy material to be measured, and adding the same phases of the normalized areas of the diffraction peaks to obtain the sum of the normalized areas of the diffraction peaks of the specific phases of each sector area of the alloy material to be measured at a certain moment;
and comparing the sum of normalized diffraction peak areas in each sector area of the alloy material to be measured at each moment to obtain quantitative representation of rotation of a certain phase crystal face in the alloy material to be measured at each moment.
2. The method for obtaining the rotation degree of the crystal plane in the alloy material according to claim 1, wherein the obtaining the two-dimensional synchrotron radiation diffraction data of the alloy material to be measured comprises:
placing an alloy material to be tested, which transmits or diffracts synchronous radiation, on a sample table;
Changing the state of the alloy material to be measured, and simultaneously acquiring synchronous radiation diffraction data generated by the alloy material to be measured at different moments from a CCD.
3. The method for obtaining the rotation degree of the crystal face in the alloy material according to claim 1, wherein the two-dimensional synchrotron radiation diffraction data is subjected to zonal sector integration, and the circle center of the sector integration area is the circle center of the debye ring.
4. The method for obtaining the rotation degree of the crystal face in the alloy material according to claim 1, wherein the integration of the synchrotron radiation diffraction data of the whole two-dimensional area is performed by taking the circle center of the debye ring as the circle center, and the sector integration is performed on the diffraction data of the whole two-dimensional area.
5. The method of claim 1, wherein the diffraction peak is calibrated at a wavelength used for the synchrotron radiation light for measurement.
6. The method for obtaining the rotation degree of the crystal plane in the alloy material according to claim 1, wherein the normalizing the peak area of each diffraction peak in each sector area by using the standard integral intensity ratio of each diffraction peak and the peak area of each diffraction peak in the whole alloy material to be measured comprises:
Obtaining the integral intensity ratio of each diffraction peak of the phases in the alloy of the alloy material to be measured;
Dividing the integral intensity of each diffraction peak of each sector area by the integral intensity ratio of each diffraction peak to obtain each diffraction peak data of each sector area after eliminating the influence of the difference;
dividing the diffraction peak data of each sector area after eliminating the influence of the difference by the peak area of each diffraction peak of the whole alloy to be measured to obtain the peak area of each diffraction peak normalized by each sector area, and completing the normalization of the diffraction peak area data.
7. The method for obtaining the rotation degree of the crystal face in the alloy material according to claim 1, wherein comparing the sum of normalized diffraction peak areas in each sector area at each moment of the alloy material to be measured, further comprises:
dividing the sum of normalized diffraction peak areas of different states of the same alloy material to be measured by the sum of diffraction peak areas of the initial state, and normalizing the sum of normalized diffraction peak areas again.
8. The method for obtaining the rotation degree of the crystal face in the alloy material according to claim 7, wherein the comparison is performed on the sum of normalized diffraction peak areas in each sector area at each moment of the alloy material to be measured, wherein:
And comparing the sum of the final normalized diffraction peak areas, wherein the comparison reflects the overall situation of the rotation of the internal crystal face of the alloy, and the change of the overall situation of the rotation of the internal crystal face of the alloy material to be measured at different times is obtained.
9. A system for obtaining the degree of rotation of a crystal plane within an alloy material, comprising:
the data acquisition module is used for acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be detected, wherein the two-dimensional synchrotron radiation diffraction data are in a multi-Debye ring form;
The data integration module is used for carrying out regional sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of all sector areas;
The diffraction peak calibration module is used for carrying out diffraction peak calibration on the peak position-peak intensity curve of each sector area to obtain the peak area of each diffraction peak Pi corresponding to each sector area;
The normalization processing module is used for carrying out normalization processing on the peak areas of the diffraction peaks of each sector area by utilizing the standard integral intensity ratio of the diffraction peaks and the peak areas of the diffraction peaks of the whole alloy material to be measured, and adding the areas of the diffraction peaks after normalization processing in the same phase to obtain the sum of the normalized diffraction peak areas of the specific phases of each sector area of the alloy material to be measured at a certain moment;
and the crystal face rotation quantitative representation module is used for comparing the sum of normalized diffraction peak areas in all sector areas of the alloy material to be detected at all times to obtain quantitative representation of the rotation of a certain phase crystal face in the alloy material to be detected at all times.
10. A terminal comprising a memory, a processor and a computer program stored on the memory and capable of running on the processor, wherein the processor is configured to execute the method for obtaining the degree of rotation of the crystal plane in the alloy material according to any one of claims 1 to 8 when the processor executes the program.
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