Method, system and terminal for acquiring rotation degree of crystal face in alloy material

Abstract

The invention provides a method, a system and a terminal for acquiring the rotation degree of a crystal face in an alloy material. The method comprises the following steps: acquiring two-dimensional synchrotron radiation diffraction data of a to-be-detected alloy material; carrying out integration on the two-dimensional synchrotron radiation diffraction data, including dividing multiple fan-shaped region integration and whole diffraction data integration, and respectively obtaining corresponding peak position-peak intensity curves; performing diffraction peak calibration on the peak position-peak intensity curve to obtain each corresponding diffraction peak; performing normalization processing on the peak area of each diffraction peak, and adding the diffraction peak areas after normalization processing in the same phase to obtain the sum of the normalized diffraction peak areas of the specific phase of each fan-shaped region of the alloy material to be detected at a certain moment; and comparing the sum of the normalized diffraction peak areas of the alloy material to be detected in each sector region at each moment to obtain quantitative expression of rotation of a certain phase crystal face in the alloy material to be detected at each moment. The method is high in precision, simple in sample preparation and nondestructive in 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 in alloy materials by 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, the change of lattice constant, 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 of lattice constant can be calibrated by the peak position of diffraction peak in in-situ mechanical XRD experiment. The half-width of XRD diffraction peak can reflect the size of dislocation density to a certain extent. The size of dislocation density is closely related to the degree of crystal plane slip. For the determination of crystal plane rotation of polycrystalline alloy, since it does not have only one set of diffraction patterns like single crystal, the rotation of internal crystal plane can be inferred by the change of diffraction pattern. Since the diffraction pattern of polycrystalline alloy material is composed of a large number of grain diffraction patterns, even if it has undergone strong plastic deformation, its diffraction pattern is composed of multiple Debye rings, and the change cannot be intuitively seen. The determination of its crystal plane rotation cannot be handled like single crystal alloy material.

[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 D A. 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 spectroscopy 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 EBSD technology was used to study the slip and lattice rotation of alloy materials. 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.) The slip and lattice rotation of Ni-Co alloy grains were studied by EBSD data analysis. However, both methods have their own shortcomings. The accuracy of the model estimation can only remain at the level of estimation, and the actual persuasiveness is insufficient; the measurement of crystal plane rotation using EBSD technology can only be limited to the grains whose surface is 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 view of 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, there is provided a method for obtaining the degree of crystal plane rotation in an alloy material, comprising:

[0007] Acquire 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 Dodebye rings;

[0008] Performing regional 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 a peak position-peak intensity curve of the entire alloy material to be tested;

[0009] Performing diffraction peak calibration on the peak position-peak intensity curve of each of the fan-shaped regions to obtain the peak area of ​​each diffraction peak corresponding to each of the fan-shaped regions; 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] The peak areas of the diffraction peaks in the sector-shaped regions are normalized by 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 the normalized diffraction peak areas are added in phase to obtain the sum of the normalized diffraction peak areas of the specific phases in 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 time is compared 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 time.

[0012] Optionally, the step of 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 at the same time.

[0015] Optionally, 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.

[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 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:

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

[0020] The integrated intensity of each diffraction peak in each of the sector-shaped regions is divided by the integrated intensity ratio of each diffraction peak to obtain the data of each diffraction peak in each sector-shaped region after eliminating the influence of the difference;

[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 whole alloy to be tested, so as to obtain the normalized peak area of ​​each diffraction peak of each sector area, and complete 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 also includes:

[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, and the changes in the overall situation of the internal crystal plane rotation of the alloy material to be tested at different times are obtained.

[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: 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 Dodebye rings;

[0028] Data integration module: performing regional 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: perform diffraction peak calibration on the peak position-peak intensity curve of each of the fan-shaped areas to obtain the peak area of ​​each diffraction peak corresponding to each of the fan-shaped areas; 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;

[0030] Normalization processing module: using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the whole alloy material to be tested, the peak area of ​​each diffraction peak of each sector area is normalized, and the normalized diffraction peak areas of each sector area are added in the same phase 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 time, and obtains a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each time.

[0032] According to a third aspect of the present invention, there is provided a terminal 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 only samples that can obtain synchrotron radiation diffraction data need to be prepared. Since the data is acquired 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, so 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 invention has the characteristics of high precision, simple sample preparation, non-destructive measurement and statistically significant measurement results. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Other features, objects and advantages of the present invention will become more apparent from the detailed description of non-limiting embodiments made 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 in one embodiment of the present invention;

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

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

[0041] Figure 4 A schematic diagram of a sector-shaped integration region used in an example of the present invention;

[0042] Figure 5 It is a 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 It is a 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 synchrotron radiation diffraction data of Ni-Co-Al alloy in an example of the present invention after sector integration. DETAILED DESCRIPTION

[0045] The present invention is described in detail below in conjunction with specific examples. The following examples will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that, for those of ordinary skill in the art, several variations and improvements can be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.

[0046] Figure 1 FIG. 1 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, and the method comprises the following steps:

[0047] S100, obtaining 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. 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 a specific embodiment, obtaining two-dimensional synchrotron radiation diffraction data of the sample to be tested may include: using a synchrotron radiation transmission or diffraction sample of a size that meets the requirements, placing it on a sample stage, and performing in-situ mechanical experiments, in-situ electromagnetic experiments, in-situ heating experiments, or other experiments that can change the state of the alloy on the alloy, obtaining synchrotron radiation diffraction data generated by the alloy at different times from the CCD, wherein the diffraction data requires clear and high contrast Debye rings, and sufficient number of them to obtain data with a certain degree of credibility. Specifically, there is no coarse light spot formed by coarse crystals with a width greater than the width of a general Debye ring, the ratio of the intensity at the highest point of the Debye ring diffraction intensity to the background intensity is greater than 100, and the total number of Debye rings must be more than 5.

[0051] In this embodiment, the acquisition of experimental data is non-destructive, and only samples that can obtain synchrotron radiation diffraction data need to be prepared, which is convenient and quick. In addition, the acquisition of synchrotron radiation diffraction data is based on the internal lattice of the entire sample, which has statistical significance for the crystal plane rotation measurement results obtained in the subsequent steps, and the crystal plane rotation of a large number of grains in the alloy material can be obtained.

[0052] S200, performing regional 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, for the regional sector integration, the center of the integrated sector area is the center of the Debye ring. For the integration of the synchrotron radiation diffraction data of the entire two-dimensional area (full data integration), the sector integration of the entire two-dimensional diffraction data is performed with the center of the Debye ring as the center.

[0055] Specifically, refer to Figure 4As shown, the entire two-dimensional region is 0-90 degree integration. Each sector region can be 0 to 45 degree and 45 degree to 90 degree integration or other division methods. The regional sector integration is to first divide each region (different sector ranges) integration, and the different sector ranges can be 0-30, 30-60, 60-90, or 0-45, 45-90, which can be determined according to actual needs, and finally two kinds of curves are obtained: one is 0-90, that is, the peak position-peak intensity curve of the entire alloy material to be tested, and the other is the peak position-peak intensity curve of each sector 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 methods.

[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 by the wavelength of the synchrotron radiation used for measurement. Of course, this is only one method of this embodiment.

[0058] S400, 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, normalizing the peak area of ​​each diffraction peak in each sector-shaped region, adding the normalized diffraction peak areas in the same phase, and obtaining 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;

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

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

[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 integral of the data obtained in S200, so as to normalize the diffraction peak area data, and obtain the normalized diffraction peak area of ​​each sector region;

[0064] Specifically, in S401, the integrated intensity ratio of different diffraction peaks of 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 ratio 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 area 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 The diffraction peak areas were normalized.

[0067] In this step, the diffraction peak area data is 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 time is obtained.

[0069] In this embodiment, since the data is acquired losslessly, the synchrotron radiation diffraction data can be used to quantitatively analyze the degree of crystal plane rotation in the alloy material. By performing analysis based on the peak area of ​​the diffraction peak in the above steps, the final result is highly credible and accurate, thereby enabling quantitative analysis of the degree of crystal plane rotation under in-situ conditions.

[0070] S500, comparing the sum of the 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 above comparison is to compare the final normalized sum of the diffraction peak areas in a table, which can reflect the overall situation of the internal crystal plane rotation of the alloy and obtain the changes in the overall situation of the internal crystal plane rotation of the alloy at different times. Of course, in other embodiments, other comparison methods can also be used, not limited to drawing comparison.

[0073] In the method of the above embodiment of the present invention, the sample metal element, alloy or other material with clear diffraction behavior has clear and distinguishable diffraction peaks, and there is 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, and the two-dimensional synchrotron radiation diffraction data is in the form of Dodebye rings;

[0076] Data integration module: perform sector-by-region integration on the two-dimensional synchrotron radiation diffraction data to obtain the peak position-peak intensity curve of each sector-shaped area; integrate the synchrotron radiation diffraction data of the entire two-dimensional area 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 are added in phase 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;

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

[0080] The technology adopted by each module of 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 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, and the processor is used to execute the method for obtaining the degree of crystal plane rotation in the alloy material in any of the above embodiments when executing the program.

[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 the 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, wherein 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 is used, the thickness of the synchrotron radiation light penetration side of the sample is thinned to a thickness sufficient to allow the synchrotron radiation light to penetrate the sample, an in-situ stretching experiment is performed on a stretching test bench, and a CCD is 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 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 0-45 degree sector and 45-90 degree sector integrals are performed as the area for studying the crystal plane rotation, and the 0-90 degree sector integral is performed as the integral data of the alloy as a whole. The schematic diagram of the sector integral area used is as follows Figure 4 As shown, the integral data is as follows Figure 5 Of course, in other embodiments, it can also be a fan-shaped area with other angles and an overall integral.

[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 the

[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 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 first diffraction peak areas of each sector region after normalization are added in the same phase, that is, the sum of the normalized diffraction peak areas of the specific phase of each sector region of a certain sample at a certain time is obtained;

[0093] In this step, the literature is consulted to obtain the relative peak intensities of different diffraction peaks. 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 time, and obtain a quantitative representation of the rotation of a crystal plane of a certain phase in the alloy material to be tested at each time.

[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 decreases, 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 increases, 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 specific method:

[0103] S1. Use a dog-bone Ni-Co-Al alloy sample, reduce the thickness of the synchrotron radiation light penetration side to a thickness sufficient to allow the synchrotron radiation light to penetrate the sample, perform an in-situ stretching experiment on a stretching test bench, and use a CCD 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 6 As shown, the synchrotron radiation data are matched one-to-one with the stages of the in-situ stretching 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 and 45-90 degree sectors as the area for studying crystal plane rotation. Perform 0-90 degree sector integration again as the integral data of the alloy material as a whole. The schematic diagram of the sector integration area used is shown in 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 stretching, the initial plastic deformation and the final plastic deformation respectively. All the

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

[0108] In this step, the literature is consulted to obtain the relative peak intensities of different diffraction peaks. 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 They are 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 as the tension progresses at different stages

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

[0112] The above describes the specific embodiments of the present invention. It should be understood that the present invention is not limited to the above specific embodiments, and those skilled in the art can make various modifications or variations within the scope of the claims, which does not affect the essence of the present invention. The above preferred features can be used in any combination without conflicting with each other.

Claims

1. A method for obtaining the degree of crystal plane rotation in an alloy material, characterized in that: include: Acquire 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 Dodebye rings; Performing regional 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 a peak position-peak intensity curve of the entire alloy material to be tested; Performing diffraction peak calibration on the peak position-peak intensity curve of each of the fan-shaped regions to obtain the peak area of ​​each diffraction peak corresponding to each of the fan-shaped regions; 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; The peak areas of the diffraction peaks in the sector-shaped regions are normalized by 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 the normalized diffraction peak areas are added in phase to obtain the sum of the normalized diffraction peak areas of the specific phases in 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 time is compared 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 time.

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 at the same time.

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 step of normalizing 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; The integrated intensity of each diffraction peak in each of the sector-shaped regions is divided by the integrated intensity ratio of each diffraction peak to obtain the data of each diffraction peak in each sector-shaped region after eliminating the influence of the difference; 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 whole alloy to be tested, so as to obtain the normalized peak area of ​​each diffraction peak of each sector area, and complete 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 normalized diffraction peak areas in each sector region of the alloy material to be tested at each time also includes: 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, and the changes in the overall situation of the internal crystal plane rotation of the alloy material to be tested at different times are obtained.

9. A system for obtaining the degree of crystal plane rotation in an alloy material, characterized in that: include: Data acquisition module: 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 Dodebye rings; Data integration module: performing regional 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: perform diffraction peak calibration on the peak position-peak intensity curve of each of the fan-shaped areas to obtain the peak area of ​​each diffraction peak Pi corresponding to each of the fan-shaped areas; 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; Normalization processing module: using the standard integrated intensity ratio of each diffraction peak and the peak area of ​​each diffraction peak of the whole alloy material to be tested, the peak area of ​​each diffraction peak of each sector area is normalized, and the normalized diffraction peak areas of each sector area are added in the same phase 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 time, and obtains a quantitative representation of the crystal plane rotation of a certain phase in the alloy material to be tested at each time.

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: The processor is used to execute the method for obtaining the degree of crystal plane rotation in an alloy material as described in any one of claims 1 to 8 when executing the program.

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