Method, system and terminal for obtaining the degree of crystal plane rotation in alloy material

Abstract

The present invention provides a method, system and terminal for obtaining the degree of crystal plane rotation in an alloy material, including: obtaining two-dimensional synchrotron radiation diffraction data of the alloy material to be tested; integrating the two-dimensional synchrotron radiation diffraction data, including dividing the two-dimensional synchrotron radiation diffraction data into a plurality of sector-shaped area integrals and integrating the entire diffraction data, respectively obtaining corresponding peak position-peak intensity curves; performing diffraction peak calibration on the peak position-peak intensity curve to obtain corresponding diffraction peaks; normalizing the peak area of ​​each diffraction peak, adding the normalized diffraction peak areas in phase to obtain the sum of the normalized diffraction peak areas of the specific phases of each sector-shaped area at a certain moment of the alloy material to be tested; comparing the sum of the normalized diffraction peak areas within each sector-shaped area at each moment of the alloy material to be tested, and obtaining a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each moment. The present invention has high accuracy, simple sample preparation and non-destructive measurement.

Description

Technical Field

[0001] The present invention relates to the technical field of diffraction analysis of metallic materials, and in particular to a method, system and terminal for obtaining the degree of crystal plane rotation within an alloy material using synchrotron radiation diffraction data. Background Art

[0002] During the deformation process of alloy materials, due to the action of internal stress, three lattice behaviors will occur, namely, changes in lattice constants, crystal plane slip, and crystal plane rotation. In order to better explain the deformation mechanism of alloy materials, it is often necessary to analyze the above three behaviors. The change in lattice constants can be calibrated by the peak position of diffraction peaks in in-situ mechanical XRD experiments. The half-maximum width of the XRD diffraction peak can reflect the size of the dislocation density to a certain extent. The size of the dislocation density is closely related to the degree of crystal plane slip. For the measurement of crystal plane rotation of polycrystalline alloys, since they do not have only one set of diffraction patterns like single crystals, the rotation of the internal crystal planes can be inferred by the change of the diffraction pattern. Since the diffraction pattern of polycrystalline alloy materials is composed of a large number of grain diffraction patterns superimposed, even after strong plastic deformation, its diffraction pattern is composed of multiple Debye rings, and the changes cannot be intuitively seen. The measurement of its crystal plane rotation cannot be handled like single crystal alloy materials.

[0003] There are many ways to study the rotation behavior of crystal planes in alloy materials. Model estimation methods can be used. S. Kok et al. (Kok S, Beaudoin AJ, Tortorelli DA. Numerical integration of latticerotation in polycrystal plasticity [J]. International Journal for Numerical Methods in Engineering, 2001, 52(12): 1487-1500.) used a polycrystal model to simulate polycrystal plastic deformation and proposed a numerical algorithm based on the analytical integration of the lattice rotation evolution equation to estimate the rotation behavior of the lattice. In recent years, with the continuous development of spectroscopic technology, EBSD technology has been applied to the measurement of 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, in which the slip and lattice rotation of the alloy material were studied using EBSD technology. 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 grainboundary response. Materials Research Letters, 12(11), 869–876.) Using EBSD data analysis, the slip and lattice rotation of Ni-Co-based alloy grains were studied. However, both methods have their own insurmountable shortcomings. The accuracy of the model estimation is always limited to an estimate and lacks practical persuasiveness. Using EBSD technology for measurement, the determination of crystal plane rotation can only be limited to the grains whose surfaces are within the field of view, and the number of grains is too small.

[0004] Therefore, it is necessary to develop a new method to determine the degree of crystal plane rotation inside alloy materials to meet the requirements of high precision, simple sample preparation, non-destructive measurement, and statistically significant measurement results, so as to provide accurate experimental basis and data support for the characterization of the crystal plane rotation process during the plastic deformation of the alloy. Summary of the Invention

[0005] In response to the defects in the prior art, the purpose of the present invention is to provide a method, system and terminal for obtaining the degree of crystal plane rotation in an alloy, and to determine the specific quantitative indicators of the crystal plane rotation process under different states in the target alloy through synchrotron radiation diffraction data analysis.

[0006] According to one aspect of the present invention, a method for obtaining the degree of crystal plane rotation in an alloy material is provided, comprising:

[0007] Acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, wherein the two-dimensional synchrotron radiation diffraction data is in the form of Dobye rings;

[0008] Performing sector integration on the two-dimensional synchrotron radiation diffraction data to obtain a peak position-peak intensity curve for each sector region; integrating the synchrotron radiation diffraction data for the entire two-dimensional region to obtain a peak position-peak intensity curve for the entire alloy material to be tested;

[0009] Performing diffraction peak calibration on the peak position-peak intensity curve of each of the sector-shaped areas to obtain the peak area of ​​each diffraction peak corresponding to each of the sector-shaped areas; performing diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested;

[0010] Normalizing the peak areas of the diffraction peaks in each sector-shaped region using the standard integrated intensity ratio of each diffraction peak and the peak areas of each diffraction peak of the entire alloy material to be tested, and adding the normalized diffraction peak areas of the same phase to obtain the sum of the normalized diffraction peak areas of the specific phase of each sector-shaped region of the alloy material to be tested at a certain moment;

[0011] The sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment is compared to obtain a quantitative representation of the rotation of a certain phase crystal plane in the alloy material to be tested at each moment.

[0012] Optionally, obtaining two-dimensional synchrotron radiation diffraction data of the alloy material to be tested includes:

[0013] Place the alloy material to be tested by synchrotron radiation transmission or diffraction on the sample stage;

[0014] The state of the alloy material to be tested is changed, and synchrotron radiation diffraction data generated by the alloy material to be tested at different times are obtained from the CCD.

[0015] Optionally, the two-dimensional synchrotron diffraction data is subjected to regional sector integration, wherein the center of the integrated sector area is the center of the Debye ring.

[0016] Optionally, the synchrotron radiation diffraction data of the entire two-dimensional region are integrated, wherein the diffraction data of the entire two-dimensional region are sector-integrated with the center of the Debye ring as the center.

[0017] Optionally, the diffraction peak calibration is performed based on the wavelength of the synchrotron radiation light used for measurement.

[0018] Optionally, the normalizing the peak area of ​​each diffraction peak in each of the sector-shaped regions using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the entire alloy material to be tested comprises:

[0019] Obtaining the integrated intensity ratio of each diffraction peak of the alloy phase of the alloy material to be tested;

[0020] Dividing the integrated intensity of each diffraction peak in each of the sector-shaped areas by the integrated intensity ratio of each diffraction peak to obtain the diffraction peak data of each sector-shaped area after eliminating the difference effect;

[0021] Then, the diffraction peak data of each sector area after eliminating the difference influence is divided by the peak area of ​​each diffraction peak of the entire alloy to be tested to obtain the normalized peak area of ​​each diffraction peak of each sector area, thereby completing the normalization of the diffraction peak area data.

[0022] Optionally, comparing the sum of normalized diffraction peak areas in each sector region of the alloy material to be tested at each time further comprises:

[0023] The sum of the normalized diffraction peak areas of the same alloy material to be tested in different states is divided by the sum of the diffraction peak areas in the initial state, and the sum of the normalized diffraction peak areas is normalized again.

[0024] Optionally, the sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each time is compared, wherein:

[0025] The final normalized sum of the diffraction peak areas is compared, and the comparison reflects the overall situation of the internal crystal plane rotation of the alloy, thereby obtaining the change in the overall situation of the internal crystal plane rotation of the alloy material to be tested at different times.

[0026] According to a second aspect of the present invention, there is provided a system for obtaining the degree of crystal plane rotation in an alloy material, comprising:

[0027] Data acquisition module: acquires two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, wherein the two-dimensional synchrotron radiation diffraction data is in the form of Dobye rings;

[0028] Data integration module: performing sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of each sector region; integrating the synchrotron radiation diffraction data of the entire two-dimensional region to obtain the peak position-peak intensity curve of the entire alloy material to be tested;

[0029] Diffraction peak calibration module: performing diffraction peak calibration on the peak position-peak intensity curve of each of the sector-shaped areas to obtain the peak area of ​​each diffraction peak corresponding to each of the sector-shaped areas; performing diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested;

[0030] Normalization processing module: using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the entire alloy material to be tested, the peak area of ​​each diffraction peak in each sector area is normalized, and the normalized diffraction peak areas of each sector area are added together to obtain the sum of the normalized diffraction peak areas of the specific phase of each sector area of ​​the alloy material to be tested at a certain moment;

[0031] Crystal plane rotation quantitative representation module: compares the sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment, and obtains a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each moment.

[0032] According to a third aspect of the present invention, a terminal is provided, comprising a memory, a processor, and a computer program stored in the memory and capable of running on the processor, wherein the processor is used to execute the method for obtaining the degree of crystal plane rotation in an alloy material when executing the program.

[0033] Compared with the prior art, the present invention has at least one of the following beneficial effects:

[0034] The method for obtaining the degree of crystal plane rotation in an alloy material provided by an embodiment of the present invention can use synchrotron radiation diffraction data to quantitatively analyze the degree of crystal plane rotation in an alloy material. Since the analysis is based on the peak area of ​​the diffraction peak, the results obtained are highly reliable and accurate.

[0035] In the embodiment of the present invention, the acquisition of experimental data is non-destructive, and it is only necessary to prepare a sample that can obtain synchrotron radiation diffraction data. Since the data is obtained non-destructively, the present invention realizes the quantitative analysis of the degree of crystal plane rotation under in-situ conditions. The acquisition of synchrotron radiation diffraction data is based on the internal lattice conditions of the entire sample. Therefore, the resulting crystal plane rotation measurement results are statistically significant, and the crystal plane rotation conditions of a large number of grains in the alloy material can be obtained.

[0036] The present invention has the characteristics of high precision, simple sample preparation, non-destructive measurement, and measurement results with statistical significance. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Other features, objects and advantages of the present invention will become more apparent upon reading the detailed description of non-limiting embodiments with reference to the following drawings:

[0038] Figure 1 A flow chart of a method for obtaining the degree of crystal plane rotation in an alloy material according to one embodiment of the present invention;

[0039] Figure 2 Schematic diagram of a specific experimental implementation method in an example of the present invention;

[0040] Figure 3 Schematic diagram of synchrotron radiation diffraction data of Al-Zn alloy in an example of the present invention;

[0041] Figure 4 Schematic diagram of the sector-shaped integration region used in the examples of the present invention;

[0042] Figure 5 Schematic diagram of data obtained by integrating the synchrotron radiation diffraction data of Al-Zn alloy in an example of the present invention after sector integration;

[0043] Figure 6 Schematic diagram of synchrotron radiation diffraction data of Ni-Co-Al alloy in an example of the present invention;

[0044] Figure 7 This is a schematic diagram of the data obtained by integrating the Ni-Co-Al alloy synchrotron radiation diffraction data after sector integration in an example of the present invention. DETAILED DESCRIPTION

[0045] The present invention will be described in detail below with reference to specific examples. The following examples will help those skilled in the art further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that those skilled in the art may make various modifications and improvements without departing from the scope of the present invention. These modifications and improvements fall within the scope of protection of the present invention.

[0046] Figure 1 This is a flow chart of a method for obtaining the degree of crystal plane rotation in an alloy material in one embodiment of the present invention. Figure 1 As shown, this embodiment provides a method for obtaining the degree of crystal plane rotation in an alloy material, the method comprising the following steps:

[0047] S100, acquiring two-dimensional synchrotron radiation diffraction data of the sample to be tested;

[0048] In this step, the sample to be tested refers to a sample made of the alloy material to be tested and suitable for experiment use. The specific sample form, size, etc. can be determined according to the experimental requirements.

[0049] In this step, the two-dimensional synchrotron radiation diffraction data obtained are in the form of Dodebye rings.

[0050] In one specific embodiment, obtaining two-dimensional synchrotron diffraction data of a sample to be tested may include: using a synchrotron transmission or diffraction sample of a desired size, placing it on a sample stage, and acquiring synchrotron diffraction data generated by the alloy at different times from a CCD while conducting in-situ mechanical experiments, in-situ electromagnetic experiments, in-situ heating experiments, or other experiments that can change the alloy's state. The diffraction data must have clear, high-contrast Debye rings and a sufficient number of them to provide reliable data. Specifically, the data must not contain coarse, coarse-grained light spots with a width greater than the width of a typical Debye ring. The ratio of the highest intensity of the Debye ring diffraction to the background intensity must be greater than 100, and the total number of Debye rings must be at least five.

[0051] In this example, the experimental data is obtained non-destructively, requiring only the preparation of a sample for which synchrotron diffraction data can be obtained. This is a quick and convenient process. Furthermore, the synchrotron diffraction data are obtained based on the entire internal lattice of the sample, providing statistical significance for the crystal plane rotation measurements obtained in subsequent steps. This allows for the determination of the crystal plane rotation of a large number of grains within the alloy material.

[0052] S200, performing sector integration on the two-dimensional synchrotron radiation diffraction data obtained in S100 to obtain a peak position-peak intensity curve for each sector region; integrating the synchrotron radiation diffraction data for the entire two-dimensional region to obtain a peak position-peak intensity curve for the entire alloy material to be tested;

[0053] In this step, the above-mentioned integration processing can be performed using synchrotron radiation data processing software, for example, GSAS-II or similar processing software with similar functions can be used, so that regional sector integration and overall data integration (full data integration) can be very conveniently achieved.

[0054] In this step, the sector integration is performed by taking the center of the Debye ring as the center of the sector. The integration of the synchrotron diffraction data of the entire two-dimensional region (full data integration) is performed by taking the center of the Debye ring as the center of the sector integration.

[0055] Specifically, refer to Figure 4Shown, whole two-dimensional region, is 0-90 degree integration.Each fan-shaped region, can be 0 to 45 degree and 45 degree to 90 degree integration or other division method etc.Dividing region fan-shaped integration is to first divide each region (different fan-shaped scope) integration, different fan-shaped scope can be 0-30,30-60,60-90, also can be 0-45,45-90, can be determined according to actual demand, finally obtain two kinds of curves: one is 0-90, that is, the peak position-peak intensity curve of the alloy material to be measured overall, and another is the peak position-peak intensity curve of each fan-shaped region, that is, 0-45,45-90 or 0-30,30-60,60-90 or the peak position-peak intensity curve corresponding to each region determined by other division method.

[0056] S300, performing diffraction peak calibration on the peak position-peak intensity curve of each sector-shaped area to obtain the peak area of ​​each diffraction peak Pi corresponding to each sector-shaped area, and at the same time, performing diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested;

[0057] In this step, the peak position of the diffraction peak is calibrated based on the wavelength of the synchrotron radiation used for measurement. Of course, this is only one method of this embodiment.

[0058] S400, normalizing the peak areas of the diffraction peaks in each sector-shaped region using the standard integrated intensity ratio of each diffraction peak and the peak areas of each diffraction peak of the entire alloy material to be tested, and adding the normalized diffraction peak areas of the same phase to obtain the sum of the normalized diffraction peak areas of the specific phase in each sector-shaped region of the alloy material to be tested at a certain moment;

[0059] In order to better achieve the final crystal plane rotation measurement, in a specific embodiment, S400 can adopt the following steps:

[0060] S401, obtaining the integrated intensity ratio of different diffraction peaks of the alloy phase;

[0061] In this step, the integrated intensity ratios of different diffraction peaks of the alloy phases can be obtained by searching the ICSD database or other literature.

[0062] S402, dividing the diffraction peak area of ​​each diffraction peak corresponding to each sector region by the integrated intensity ratio of different diffraction peaks found in S401, so as to eliminate the influence of the difference in the diffraction integrated intensity (i.e., the diffraction peak area) of each diffraction peak itself;

[0063] S403, dividing the data obtained in S402 by the integrated intensity of the corresponding diffraction peak in the full integration of the data obtained in S200 to normalize the diffraction peak area data to obtain the normalized diffraction peak area of ​​each sector region;

[0064] Specifically, in S401, the integrated intensity ratio of different diffraction peaks in the alloy phase can be expressed in the form of relative peak intensity, with the integrated intensity of the diffraction peak with the highest peak intensity being 1, and the ratios of the remaining diffraction peaks to the diffraction peak with the highest peak intensity being 1. k , I k The ratio between them represents the integrated intensity ratio of different diffraction peaks. k Normalization was performed as the integrated intensity ratio in the normalization step.

[0065] Specifically, in S402, the symbol In order to facilitate the calculation of the integrated intensity of the diffraction peaks in each sector area, m represents the time of the sample, which can be the initial stage of the experiment, the middle stage of the experiment, and the end stage of the experiment; n represents the different phases in the alloy sample, which can be FCC, BCC or any other phase with a crystal structure; j represents different sector areas, which can be 0-30 degrees, 30-60 degrees or other sector areas; k represents the kth diffraction peak, which can be the (001) and (111) crystal plane family diffraction peaks of the face-centered cubic crystal or other diffraction peaks. Represents the diffraction peak area of ​​the kth diffraction peak of phase n in the sector integration region j of the alloy sample at time m, calculated This is to eliminate the influence of the difference in the diffraction integrated intensity (diffraction peak area) of each diffraction peak itself.

[0066] Specifically, in S403, the symbol To facilitate the calculation of the integral intensity of the corresponding diffraction peak in the full integral of the data obtained in S200, which represents the diffraction peak area of ​​the kth diffraction peak of phase n in the full integral of the data in the alloy sample at time m, calculate To normalize the diffraction peak area.

[0067] In this step, the diffraction peak area data are normalized by the above-mentioned normalization method. This normalization operation can be used for quantitative analysis of the degree of crystal plane rotation under in-situ conditions.

[0068] S404, the normalized diffraction peak area of ​​each diffraction peak in the same phase of the alloy material sample to be tested at the same time obtained in S403 Addition, through The sum of the normalized diffraction peak areas of the specific phase in each sector region of a sample at a certain moment is obtained.

[0069] In this embodiment, since the data is obtained non-destructively, the degree of crystal plane rotation in the alloy material can be quantitatively analyzed using synchrotron radiation diffraction data. By performing analysis based on the peak area of ​​the diffraction peak in the above steps, the final result obtained has high credibility and good accuracy, thereby enabling quantitative analysis of the degree of crystal plane rotation under in-situ conditions.

[0070] S500, comparing the sums of normalized diffraction peak areas in different sector-shaped regions of the alloy material to be tested at different times, to obtain a quantitative representation of the rotation of a crystal plane of a certain phase in the alloy at different times.

[0071] In this step, the sum of the normalized diffraction peak areas of the same alloy material sample under different states is divided by the sum of the diffraction peak areas under the initial state, so that the sum of the normalized diffraction peak areas is normalized again.

[0072] In this step, the comparison is performed by tabulating the sum of the final normalized diffraction peak areas. This can reflect the overall state of crystal plane rotation within the alloy and determine the overall changes in crystal plane rotation within the alloy at different times. Of course, in other embodiments, other comparison methods can be used, and are not limited to graphical comparison.

[0073] In the method of the above embodiment of the present invention, the sample metal element, alloy, or other material having a clear diffraction behavior has clear and distinguishable diffraction peaks, with little interference between different diffraction peaks.

[0074] Based on the same technical concept, in another embodiment of the present invention, a system for obtaining the degree of crystal plane rotation in an alloy material using synchrotron radiation diffraction data is provided, comprising: a data acquisition module, a data integration module, a diffraction peak calibration module, a normalization processing module, and a crystal plane rotation quantitative representation module, wherein:

[0075] Data acquisition module: obtains two-dimensional synchrotron radiation diffraction data of the alloy material to be tested. The two-dimensional synchrotron radiation diffraction data is in the form of Dodebye rings;

[0076] Data integration module: Performs sector-wise integration on the two-dimensional synchrotron diffraction data to obtain the peak position-peak intensity curve of each sector; integrates the synchrotron diffraction data of the entire two-dimensional region to obtain the peak position-peak intensity curve of the entire alloy material to be tested;

[0077] Diffraction peak calibration module: perform 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; perform diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested;

[0078] Normalization processing module: using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the entire alloy material to be tested, the peak area of ​​each diffraction peak in each sector area is normalized, and the normalized diffraction peak areas of each sector area are added together to obtain the sum of the normalized diffraction peak areas of the specific phase of the alloy material to be tested at a certain moment;

[0079] Crystal plane rotation quantitative representation module: compares the sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment, and obtains a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each moment.

[0080] The system for obtaining the degree of crystal plane rotation in alloy materials using synchrotron radiation diffraction data in the above embodiment of the present invention, the technology adopted by each module can refer to the corresponding steps of the above embodiment of the method for obtaining the degree of crystal plane rotation in alloy materials, and will not be repeated here.

[0081] Based on the same technical concept, in another embodiment of the present invention, a terminal is also provided, including a memory, a processor, and a computer program stored in the memory and capable of running on the processor. When the processor executes the program, it is used to execute the method for obtaining the degree of crystal plane rotation in the alloy material in any of the above embodiments.

[0082] In order to better understand the above technical solution, the method for obtaining the degree of crystal plane rotation in the alloy material in a specific embodiment of the present invention is further described below. It should be understood that the present invention is not limited to the following embodiments.

[0083] Example 1

[0084] This embodiment obtains the degree of crystal plane rotation of the Al phase in an Al-Zn alloy, and the specific method is as follows:

[0085] S1. Obtain two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, where the two-dimensional synchrotron radiation diffraction data is in the form of Dodebye rings.

[0086] Specifically, in this embodiment, a dog-bone Al-Zn alloy sample was used. The thickness of the synchrotron radiation light penetration side of the sample was thinned to a thickness sufficient to allow the synchrotron radiation light to penetrate the sample. An in-situ tensile test was performed on a tensile test bench, and a CCD was used to obtain the synchrotron radiation light generated by penetrating the alloy material at different times. The specific experimental implementation method is as follows: Figure 2 The experimental data obtained are shown in Figure 3 As shown, it is in the form of Dodebye rings, which corresponds the synchrotron radiation diffraction data to the stages of the in situ stretching experiment implemented.

[0087] S2. Use synchrotron radiation data processing software to perform partition sector integration on the obtained synchrotron radiation diffraction data, and to integrate the overall synchrotron radiation diffraction data of the alloy.

[0088] Specifically, with the point of the transmitted light of the synchrotron radiation as the center of the circle, the horizontal right as the starting point, and the counterclockwise rotation angle as positive, the sector integrals of 0-45 degrees and 45-90 degrees are performed as the area for studying the rotation of the crystal plane, and the sector integral of 0-90 degrees is performed as the integral data of the entire alloy. The schematic diagram of the sector integral area used is shown as follows: Figure 4 As shown, the integral data is as follows Figure 5 Of course, in other embodiments, fan-shaped areas at other angles and overall integrals may also be used.

[0089] S3. Calibrate the diffraction peaks of each sector and the overall integrated data of the alloy.

[0090] For example, It represents the peak area of ​​the k diffraction peak in the 0-45 degree sector integral of the Al-Zn sample. In this example, there are three k, namely the 111 peak, 200 peak and 220 peak of Al. m represents the mth state. In this embodiment, m is 1, 2 and 3, representing the initial stretching, the initial plastic deformation and the final plastic deformation, respectively. All are calibrated and recorded.

[0091] S4. Perform peak shape fitting based on the diffraction peaks of each sector and the overall integral data of the alloy to obtain the peak area of ​​each diffraction peak of each sector.

[0092] Specifically, the peak area of ​​each diffraction peak in each sector-shaped region is normalized using the standard integrated intensity ratio of each first diffraction peak and the area of ​​each diffraction peak of the alloy, and the normalized first diffraction peak areas of each sector-shaped region are added together in the same phase to obtain the sum of the normalized diffraction peak areas of the specific phase of each sector-shaped region of a certain sample at a certain time;

[0093] In this step, the relative peak intensities of different diffraction peaks were obtained by consulting the literature. k The 111 diffraction peak of Al is 1, the 200 diffraction peak is 0.47, and the 220 diffraction peak is 0.22. as well as The diffraction peaks were normalized and summed.

[0094] Calculate the samples at different times as well as and calculate as well as

[0095] S5. Compare the sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment to obtain a quantitative representation of the rotation of a crystal plane of a certain phase in the alloy material to be tested at each moment.

[0096] In this step, as well as They are listed in Table 1 and analyzed as follows:

[0097] Table 1. Changes in the total area of ​​diffraction peaks of the Al phase in different fan-shaped regions in the Al-Zn alloy of this example at different stretching stages

[0098]

[0099]

[0100] According to the above table, The smaller it is, the smaller the diffraction peak area is compared to the initial state, the total number of crystal planes producing diffraction in this sector is reduced, and the crystal planes rotate from this sector area to other sector areas. The larger it is, the larger the diffraction peak area is compared to the initial state, the total number of crystal planes producing diffraction in this sector is increased, and the crystal planes rotate from other sector areas to this sector area.

[0101] Example 2

[0102] In this embodiment, the degree of crystal plane rotation of the Ni phase in the Ni-Co-Al alloy is obtained by the following method:

[0103] S1. Using a dog-bone Ni-Co-Al alloy sample, the thickness of the synchrotron radiation light penetration side was reduced to a thickness sufficient to allow the synchrotron radiation light to penetrate the sample. An in-situ tensile test was performed on a tensile test bench, and a CCD was used to obtain the synchrotron radiation light generated by the alloy material at different times. The specific experimental implementation method is as follows: Figure 2 The experimental data obtained are shown in Figure 6 As shown, the synchrotron radiation data are matched one-to-one with the stages of the in situ tensile experiment implemented.

[0104] S2. Use synchrotron radiation data processing software to perform sector integration on the data obtained. Take the point of the transmitted light of the synchrotron radiation light as the center of the circle, horizontally to the right as the starting point, set the counterclockwise rotation angle as positive, and perform sector integration of 0-45 degree sector and 45-90 degree sector respectively as the area for studying crystal plane rotation. Then perform 0-90 degree sector integration as the integral data of the entire alloy material. The schematic diagram of the sector integration area used is shown as follows: Figure 4 As shown, the integral data is as follows Figure 7 shown.

[0105] S3. Calibrate the diffraction peaks of each sector and the overall integrated data of the alloy.

[0106] For example It represents the peak area of ​​the k diffraction peak in the 0-45 degree sector integral of the Ni-Co-Al sample. In this example, there are three k, namely the 111 peak, 200 peak and 220 peak of Ni. m represents the mth state. In this example, m is 1, 2 and 3, representing the initial stage of stretching, the initial stage of plastic deformation and the final stage of plastic deformation, respectively. All are calibrated and recorded.

[0107] S4. Perform peak shape fitting based on each sector and the overall integral data of the alloy material to obtain the peak area of ​​each diffraction peak in each sector.

[0108] In this step, the relative peak intensities of different diffraction peaks were obtained by consulting the literature. k , the 111 diffraction peak of Ni is 1, the 200 diffraction peak is 0.42, and the 220 diffraction peak is 0.21. as well as The diffraction peaks were normalized and summed.

[0109] Calculate the samples at different times as well as and calculate as well as

[0110] S5. as well as Listed in Table 2 and analyzed. The smaller the value, the smaller the diffraction peak area is compared to the initial state, the total number of crystal planes that produce diffraction in this sector is reduced, and the crystal planes rotate from this sector area to other sector areas. The larger the value, the larger the diffraction peak area is compared to the initial state, the total number of crystal planes that produce diffraction in this sector is increased, and the crystal planes rotate from other sector areas to this sector area. Table 2. Changes in the total diffraction peak area of ​​Ni phase in different sector areas in a Ni-Co-Al alloy at different stages of stretching

[0111] Time m 0-45 degree sector Y value 45-90 degree sector Y value 1 (initial stretching) 1 1 2 (early stage of plastic deformation) 0.9521 0.9329 3 (end of plastic deformation) 0.8098 1.1651

[0112] The above describes specific embodiments of the present invention. It should be understood that the present invention is not limited to the specific embodiments described above, and those skilled in the art may make various modifications or variations within the scope of the claims without affecting the essence of the present invention. The above preferred features may be used in any combination as long as they do not conflict with each other.

Claims

1. A method for obtaining the degree of crystal plane rotation in an alloy material, characterized in that: include: Acquiring two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, wherein the two-dimensional synchrotron radiation diffraction data is in the form of Dobye rings; Performing sector integration on the two-dimensional synchrotron radiation diffraction data to obtain a peak position-peak intensity curve for each sector region; integrating the synchrotron radiation diffraction data for the entire two-dimensional region to obtain a peak position-peak intensity curve for the entire alloy material to be tested; Performing diffraction peak calibration on the peak position-peak intensity curve of each of the sector-shaped areas to obtain the peak area of ​​each diffraction peak corresponding to each of the sector-shaped areas; performing diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested; Normalizing the peak areas of the diffraction peaks in each sector-shaped region using the standard integrated intensity ratio of each diffraction peak and the peak areas of each diffraction peak of the entire alloy material to be tested, and adding the normalized diffraction peak areas of the same phase to obtain the sum of the normalized diffraction peak areas of the specific phase of each sector-shaped region of the alloy material to be tested at a certain moment; The sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment is compared to obtain a quantitative representation of the rotation of a certain phase crystal plane in the alloy material to be tested at each moment.

2. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The step of obtaining two-dimensional synchrotron radiation diffraction data of the alloy material to be tested comprises: Place the alloy material to be tested by synchrotron radiation transmission or diffraction on the sample stage; The state of the alloy material to be tested is changed, and synchrotron radiation diffraction data generated by the alloy material to be tested at different times are obtained from the CCD.

3. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The two-dimensional synchrotron radiation diffraction data is subjected to regional sector integration, wherein the center of the integrated sector area is the center of the Debye ring.

4. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The synchrotron radiation diffraction data of the entire two-dimensional region are integrated, wherein the diffraction data of the entire two-dimensional region are sector-integrated with the center of the Debye ring as the center.

5. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The diffraction peak calibration is performed based on the wavelength of the synchrotron radiation used for measurement.

6. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The normalizing process of the peak area of ​​each diffraction peak in each sector region by using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the entire alloy material to be tested comprises: Obtaining the integrated intensity ratio of each diffraction peak of the alloy phase of the alloy material to be tested; Dividing the integrated intensity of each diffraction peak in each of the sector-shaped areas by the integrated intensity ratio of each diffraction peak to obtain the diffraction peak data of each sector-shaped area after eliminating the difference effect; Then, the diffraction peak data of each sector area after eliminating the difference influence is divided by the peak area of ​​each diffraction peak of the entire alloy to be tested to obtain the normalized peak area of ​​each diffraction peak of each sector area, thereby completing the normalization of the diffraction peak area data.

7. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 1, characterized in that: The comparing the sum of the normalized diffraction peak areas in each sector region at each moment of the alloy material to be tested further comprises: The sum of the normalized diffraction peak areas of the same alloy material to be tested in different states is divided by the sum of the diffraction peak areas in the initial state, and the sum of the normalized diffraction peak areas is normalized again.

8. The method for obtaining the degree of crystal plane rotation in an alloy material according to claim 7, characterized in that: The sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each time is compared, wherein: The final normalized sum of the diffraction peak areas is compared, and the comparison reflects the overall situation of the internal crystal plane rotation of the alloy, thereby obtaining the change in the overall situation of the internal crystal plane rotation of the alloy material to be tested at different times.

9. A system for obtaining the degree of crystal plane rotation in an alloy material, characterized in that: include: Data acquisition module: acquires two-dimensional synchrotron radiation diffraction data of the alloy material to be tested, wherein the two-dimensional synchrotron radiation diffraction data is in the form of Dobye rings; Data integration module: performing sector integration on the two-dimensional synchrotron radiation diffraction data to obtain peak position-peak intensity curves of each sector region; integrating the synchrotron radiation diffraction data of the entire two-dimensional region to obtain the peak position-peak intensity curve of the entire alloy material to be tested; Diffraction peak calibration module: performing diffraction peak calibration on the peak position-peak intensity curve of each sector-shaped area to obtain the peak area of ​​each diffraction peak Pi corresponding to each sector-shaped area; performing diffraction peak calibration on the peak position-peak intensity curve of the entire alloy material to be tested to obtain the peak area of ​​each diffraction peak of the entire alloy material to be tested; Normalization processing module: using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the entire alloy material to be tested, the peak area of ​​each diffraction peak in each sector area is normalized, and the normalized diffraction peak areas of each sector area are added together to obtain the sum of the normalized diffraction peak areas of the specific phase of each sector area of ​​the alloy material to be tested at a certain moment; Crystal plane rotation quantitative representation module: compares the sum of the normalized diffraction peak areas in each sector region of the alloy material to be tested at each moment, and obtains a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each moment.

10. A terminal comprising a memory, a processor, and a computer program stored in the memory and capable of running on the processor, characterized in that: When the processor executes the program, it is used to execute the method for obtaining the degree of crystal plane rotation in the alloy material according to any one of claims 1 to 8.

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