Method for obtaining sizes of fine particle phases in aluminum and nickel-based alloy
By combining synchrotron radiation diffraction and small-angle neutron scattering techniques, the problem of accuracy in determining the size of fine-particle phases in aluminum and nickel-based alloys was solved, achieving high-precision analysis of precipitated phase sizes, simplifying the sample preparation process and reducing equipment costs.
Patent Information
- Application Number
- CN202511168222.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-08-20
- Publication Date
- 2025-11-18
AI Technical Summary
Existing technologies are insufficient to accurately determine the size of fine-particle phases in aluminum and nickel-based alloys. Traditional microscopic observation methods have large errors, X-ray diffraction technology has low sensitivity to light elements, and neutron small-angle scattering equipment is expensive and difficult to popularize.
By combining synchrotron diffraction and small-angle scattering (SAS) techniques, the size of the precipitated phase was calculated through integration of two-dimensional synchrotron diffraction data and fitting of SSA data, and then analyzed using the Modified Williamson-Hall method.
It improves the accuracy and reliability of precipitate size determination, provides statistically significant data support, simplifies the sample preparation process, and reduces equipment costs.
Smart Images

Figure CN120971283A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of high-energy X-ray analysis technology for metallic materials, specifically to a method for obtaining the phase size of fine particles in aluminum and nickel-based alloys using synchrotron radiation diffraction and small-angle neutron scattering. Background Technology
[0002] Aluminum and nickel-based alloys are two very important alloy systems in actual production. In the field of materials science, accurately characterizing the size of precipitates in alloys is crucial for understanding alloy properties. Due to the low strength of solid solution systems, it is always necessary to introduce precipitates into the alloy system to strengthen the alloy in practical applications. The size distribution of precipitates directly affects key indicators such as the mechanical properties and corrosion resistance of the alloy. Therefore, the influence of precipitate size on alloy properties is often critical. Usually, scanning electron microscopy and transmission electron microscopy are used to observe and measure the size of precipitates. However, traditional microscopic observation methods can only obtain the distribution of precipitates in a partial area. If the variance of the precipitate distribution in the alloy is large, the data obtained from partial sampling will have errors with the actual values. Therefore, a more accurate method for calibrating the overall precipitate size of the alloy is needed in practical applications.
[0003] In existing technologies, X-ray diffraction and small-angle scattering (SANS) are two commonly used characterization methods. X-ray diffraction, by analyzing the peak position and width of diffraction peaks, can be used to study the microstructure of materials. Early studies have found that the X-ray spectral broadening of cold-worked metals is related to lattice strain and grain size reduction, and Fourier analysis can verify the influence of defects such as dislocations on spectral broadening. The development of synchrotron X-ray diffraction has further promoted the application of this technology. For example, the improved Williamson-Hall and Warren-Averbach (mWH) methods can be used to calculate the dislocation density of materials, providing a powerful tool for understanding the microstructure evolution during material processing and annealing. In addition, small-angle scattering (SANS) can be combined with different precipitate models to study the morphology and precipitation behavior of precipitates, laying the foundation for analyzing the formation mechanism of nanoscale precipitates.
[0004] In the determination of precipitate data in aluminum and nickel-based alloys, conventional operations are mainly based on the aforementioned techniques. For aluminum alloys, X-ray diffraction is often used to analyze lattice strain and grain size changes generated during cold working, and microstructural information related to the precipitates can be obtained by analyzing spectral broadening phenomena. For nickel-based alloys, such as GH4169 alloy, small-angle neutron scattering combined with spherical and disk-shaped precipitate models can be used to study the size evolution of the γ' and γ” phases during two-stage aging. At the same time, synchrotron X-ray diffraction combined with the mWH method has also been applied to similar alloy systems. By measuring parameters such as dislocation density, the microstructural changes during the formation of precipitates can be indirectly reflected, providing data support for the optimization of the alloy aging process.
[0005] However, these conventional operating methods have obvious technical limitations: (1) Traditional microscopic observation methods (such as scanning electron microscope and transmission electron microscope) can only obtain precipitate data in some areas. When the variance of precipitate distribution is large, sampling error will cause the measurement results to deviate from the actual values, making it difficult to characterize the overall precipitate size of the alloy. (2) Although X-ray diffraction technology is widely used, synchrotron radiation X-ray diffraction has low sensitivity to light elements and it is difficult to accurately determine the size distribution of nano-sized particles, which limits its application in alloys containing light element precipitates. (3) Although small-angle neutron scattering is suitable for detecting nanostructures, the equipment is expensive and inaccessible, and the measurement results are highly dependent on the sample thickness and scattering contrast, making it difficult to popularize in actual production and research.
[0006] Therefore, this application proposes a method for obtaining the size of fine-particle phases in aluminum and nickel-based alloys to solve the above-mentioned technical problems. Summary of the Invention
[0007] The main objective of this invention is to provide a method for obtaining the size of fine-particle phases in aluminum and nickel-based alloys using synchrotron radiation diffraction and small-angle neutron scattering. This method meets the requirements of high accuracy, simple sample preparation, and statistically significant measurement results, thereby providing accurate experimental basis and data support for the measurement of fine-particle phase sizes in aluminum and nickel-based alloys, and solving the technical problems mentioned in the background art.
[0008] The present invention solves the above-mentioned technical problems by adopting the following technical solutions: A method for obtaining the fine-particle phase size in aluminum and nickel-based alloys includes: Two-dimensional synchrotron radiation diffraction data of the aluminum and nickel-based alloys to be tested were acquired, and the two-dimensional synchrotron radiation diffraction data were integrated to obtain peak position-peak intensity curves. The peak position and full width at half maximum (FWHM) of each diffraction peak of the fine particulate precipitate present in the peak position-peak intensity curve were calibrated. The calibration data is substituted into the calculation equation for the precipitate size to obtain the corresponding precipitate size; The small-angle scattering (SAS) data of the alloy under test is obtained, and the corresponding SAS data model is selected according to the shape of the fine-particle phase. The SAS data is then fitted to obtain the precipitated phase size. The precipitated phase sizes obtained by comparing two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data were used to obtain the phase sizes of fine particles in aluminum and nickel-based alloys.
[0009] Preferably, the equation for calculating the precipitated phase size is: for:
[0010]
[0011] Among them, for dislocation contrast factor , for Dislocation correlation factor of crystal planes For the Burgers vector, For the size of the precipitated phase, For dislocation density, This represents the higher-order infinitesimal within the parentheses. This is a constant related to the actual alloy, with a value of 1. The size is half the height and width. The wavelength of the synchrotron X-rays used. The peak position of the diffraction peak. The constants related to the actual alloy are taken as 0.5. , , These represent the crystal plane indices of the three diffraction peak positions. Preferably, the two-dimensional synchrotron radiation diffraction data is in the form of a Debye ring, and during the integration of the two-dimensional synchrotron radiation diffraction data, a sector integral is performed on the entire two-dimensional diffraction data with the center of the Debye ring as the center.
[0012] Preferably, the diffraction peaks are calibrated using the wavelength of the synchrotron radiation light used for measurement during the calibration process of peak position and full width at half maximum (FWHM).
[0013] Preferably, in the calculation process of obtaining the corresponding precipitate size, the diffraction peaks used have no overlap with other diffraction peaks, and the peak positions and full width at half maximum (FWHM) of the diffraction peaks all originate from the same fine-particle precipitate.
[0014] Preferably, in the calculation process of obtaining the corresponding precipitate size, the peak positions and full width at half maximum (FWHM) of at least three diffraction peaks are substituted into the fitting, and linear fitting is used for the fitting.
[0015] Preferably, the neutron small-angle scattering data has at least one scattering peak, and the neutron small-angle scattering data is a smooth curve.
[0016] Preferably, the shape of the fine particle phase used in the small-angle scattering data model selection process includes spherical and needle-shaped disks.
[0017] As can be seen from the above technical solution, the present invention provides a method for obtaining the particle size of fine particles in aluminum and nickel-based alloys. Compared with the prior art, the present invention has the following advantages: 1. This invention quantifies the size of fine-particle phases in aluminum and nickel-based alloys by combining synchrotron diffraction data and neutron small-angle scattering data. The analysis is based on the peak position and width of the diffraction peaks and the scattering peaks of small-angle scattering, which improves the reliability and accuracy of the results. This allows for accurate determination of the precipitate size and provides reliable data support for the study of precipitate size in aluminum and nickel-based alloys.
[0018] It should be understood that the descriptions in this section are not intended to identify key or essential features of embodiments of the invention, nor are they intended to limit the scope of the invention. Other features of the invention will become readily apparent from the following description. Of course, implementing any product of the invention does not necessarily require achieving all of the advantages described above simultaneously. Attached Figure Description
[0019] The accompanying drawings, which form part of this application, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an undue limitation of the invention. In the drawings: Figure 1 This is a schematic diagram of the overall process of the present invention; Figure 2 This is a schematic diagram of two-dimensional synchrotron radiation diffraction data of Al-Zn alloy in an embodiment of the present invention; Figure 3 This is a schematic diagram of the integrated results of synchrotron radiation diffraction data of Al-Zn alloy in an embodiment of the present invention; Figure 4 This is a schematic diagram of the linear fitting process of Al-Zn alloy synchrotron radiation diffraction data integration using the mWH method in an embodiment of the present invention. Figure 5 This is a schematic diagram of the original data and fitting results of small-angle scattering of neutrons in Al-Zn alloy in an embodiment of the present invention. Detailed Implementation
[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. Unless otherwise specified, the embodiments and features in the embodiments of this application can be combined with each other. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0021] For details in the embodiments, please refer to Figures 1 to 5 .
[0022] like Figure 1 As shown. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys using synchrotron radiation diffraction and small-angle neutron scattering proposed in this embodiment of the invention includes the following steps: S1. Obtain two-dimensional synchrotron radiation diffraction data of the aluminum and nickel-based alloys to be tested. The alloys to be tested are processed into sizes suitable for two-dimensional synchrotron radiation measurement, and their two-dimensional synchrotron radiation diffraction data are measured using two-dimensional synchrotron radiation technology. The final two-dimensional synchrotron radiation diffraction data obtained is in the form of Dodeby rings.
[0023] At this point, the two-dimensional synchrotron radiation diffraction data is further integrated using software such as Fit2D to obtain the peak position-peak intensity curve. During the integration process, the entire two-dimensional diffraction data is integrated with the center of the Debye ring as the center.
[0024] In a specific implementation, acquiring two-dimensional synchrotron radiation diffraction data of the sample to be tested may include: using a synchrotron radiation transmission diffraction sample of the required size, placing it on the sample stage, and acquiring the synchrotron radiation diffraction data generated by the alloy from the CCD. The diffraction data requires that the Debye rings be clear and have high contrast, with an intensity ratio of more than 10, and that there be enough Debye rings, at least three or more.
[0025] S2. The peak positions and full width at half maximum (FWHM) of each diffraction peak of the fine particulate precipitate present in the peak position-peak intensity curve are calibrated.
[0026] The diffraction peak calibration is performed using the wavelength of the synchrotron radiation light used for the measurement. The precipitates in aluminum alloys can be zinc and other precipitates commonly found in aluminum alloys. The precipitates in nickel-based alloys can be γ' phase and other precipitates commonly found in nickel-based alloys.
[0027] The peak positions and full width at half maximum (FWHM) of the diffraction peaks can be determined using X-ray diffraction data processing software such as Origin and Jade.
[0028] In summary, the above operations acquire experimental data in a non-destructive manner. Only samples capable of providing synchrotron diffraction and small-angle neutron scattering data are required. This enables the same sample to be analyzed in multiple experimental environments, thereby improving sample utilization and analytical flexibility, and facilitating a more comprehensive study of the fine-particle phase size in alloys.
[0029] S3. Substitute the calibration data into the following equation to calculate the precipitate size:
[0030]
[0031] Among them, for dislocation contrast factor , for Dislocation correlation factor of crystal planes For the Burgers vector, For the size of the precipitated phase, For dislocation density, This represents the higher-order infinitesimal within the parentheses. This is a constant related to the actual alloy, with a value of 1. The size is half the height and width. The wavelength of the synchrotron X-rays used. The peak position of the diffraction peak. The constants related to the actual alloy are taken as 0.5. , , These represent the crystal plane indices of the three diffraction peak positions.
[0032] During the calculation, the fine particulate precipitate phase must be the same as the fine particulate precipitate phase present in the peak position-peak intensity curve.
[0033] It should be noted that in the process of calculating the size of the precipitated phase, the diffraction peaks of the fine-particle precipitated phase must be sufficiently strong, have no overlap with other diffraction peaks, and the peak position and full width at half maximum (FWHM) must originate from the same fine-particle precipitated phase. In addition, it should be noted that during the calculation process, the peak positions and full width at half maximum (FWHM) of at least three diffraction peaks must be substituted into the fitting, and linear fitting should be used for the fitting.
[0034] S4. Obtain neutron small-angle scattering (SAS) data of the alloy to be tested, and select the corresponding SAS data model according to the shape of the fine-particle phase. Fit the SAS data to obtain the precipitated phase size.
[0035] At this point, the neutron small-angle scattering data contains at least one scattering peak. The neutron small-angle scattering data is a smooth curve, and the scattering peak needs to be obvious, with a certain height and width.
[0036] Furthermore, the scattering peak needs to be distinct, with a height of at least 10% relative to the baseline and an Å value of not less than 0.03 Å. -1 The width.
[0037] Furthermore, in the specific implementation process, a suitable small-angle scattering data model can be selected, where the shape of the fine particle phase may be spherical, needle-like, or disk-like, and data models such as spherical, needle-like, and disk-like can be selected respectively.
[0038] Furthermore, Sasview and other similar fitting software can be used to fit the small-angle neutron scattering data.
[0039] S5. The precipitated phase sizes obtained by comparing and analyzing two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data are used to obtain the phase sizes of fine particles in aluminum and nickel-based alloys.
[0040] At this point, the above operation is based on the acquisition of synchrotron diffraction and small-angle neutron scattering data of the entire sample, which can make the obtained fine particle phase size statistically significant, thereby obtaining the average result of most fine particle phase size in the alloy material, so as to more accurately reflect the overall precipitated phase size of the alloy.
[0041] In one specific embodiment, if the precipitate size obtained from two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data differs by more than 10%, it is necessary to analyze the reasons for the deviation in precipitate size obtained from the two experimental conditions in order to obtain results that are closer to the actual situation.
[0042] In summary, the method for obtaining the fine particle phase size in aluminum and nickel-based alloys using synchrotron diffraction and small-angle scattering (SAS) provided in this application embodiment can quantitatively analyze the fine particle phase size in aluminum and nickel-based alloys using synchrotron diffraction data and SAS data. Since the analysis is based on the peak position and peak width of the diffraction peaks and the scattering peaks of the small-angle scattering, the results obtained have high reliability and good accuracy.
[0043] Furthermore, in this embodiment of the invention, the acquisition of experimental data is non-destructive. Only a sample capable of acquiring synchrotron diffraction and small-angle scattering (SAS) data is required. Since the data acquisition is non-destructive, this invention achieves the effect of joint analysis of the same sample under multiple experimental conditions. The acquisition of synchrotron diffraction and SAS data is based on the entire sample condition, so the resulting fine particle phase size is statistically significant, and the average result of most of the fine particle phase size in the alloy material can be obtained.
[0044] In a further specific embodiment, the precipitated Zn phase size in an Al-Zn alloy is obtained using the following steps: S1. Obtain two-dimensional synchrotron radiation diffraction data of the aluminum and nickel-based alloys to be tested. The two-dimensional synchrotron radiation diffraction data is in the form of Dodeby rings. Integrate the two-dimensional synchrotron radiation diffraction data to obtain the peak position-peak intensity curve. Specifically, in this embodiment, the alloy tested is an Al-Zn alloy. The thickness of the sample on the synchrotron radiation penetration side was reduced to a level sufficient for synchrotron radiation to penetrate the sample. A CCD was then used to acquire the synchrotron radiation generated by the penetration of the alloy material. The obtained data are as follows: Figure 2 As shown, the peak position-peak intensity curve is obtained by integrating the obtained two-dimensional synchrotron radiation diffraction data in the form of a Dodeby ring. The data are as follows: Figure 3 As shown.
[0045] S2. The peak position and full width at half maximum (FWHM) of each diffraction peak of the fine particulate precipitate present in the peak position-peak intensity curve are calibrated. Specifically, the peak positions and full width at half maximum (FWHM) of the (002), (100), (101), and (102) diffraction planes of the precipitated phase HCP-Zn were calibrated, and the specific values were recorded.
[0046] S3. Substitute the peak positions and full width at half maximum (FWH) of each diffraction peak of the fine-grained precipitates present in the alloy into the equation of the Modified Williamson-Hall (mWH) method to calculate the size of the precipitates. Specifically, the equation for the Modified Williamson-Hall (mWH) method is as follows:
[0047] in , These are the parameters used in the auxiliary calculation, namely the dislocation comparison factor. , ρ is the dislocation contrast factor of the h00 crystal plane, b is the Burgers vector (0.2665 nm in this embodiment), D is the precipitated phase size, and ρ is the dislocation density. The parentheses represent higher-order infinitesimals, which can be ignored in actual calculations. M is a constant related to the actual alloy, with a value of 1. β is the full width at half maximum (FWHM). λ is the wavelength of the synchrotron X-rays used, which is 0.06887 nm in this embodiment. θ is the peak position of the diffraction peak. q is a constant related to the actual alloy, with a value of 0.5. hkl represents the exponent of the (hkl) peak position. The specific fitting process is as follows... Figure 4 As shown.
[0048] S4. Obtain neutron small-angle scattering data of the alloy, wherein the neutron small-angle scattering data has at least one scattering peak; Specifically, when the same sample was used in a small-angle neutron scattering experiment, the obtained data showed a scattering peak with a scattering vector Q value of approximately 0.06 Å⁻¹, as shown in the following figures. Figure 4 As shown.
[0049] S5. Based on the shape of the fine particle phase, select a suitable small-angle scattering data model, fit the neutron small-angle scattering data, and obtain the precipitated phase size; Specifically, in this embodiment, Zn exists in a needle-like form, and a sphere model suitable for needle-like models is used for fitting. The specific fitting results are as follows: Figure 4 As shown.
[0050] S6. Compare and analyze the precipitate size obtained from two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data; Specifically, the precipitate sizes obtained from two-dimensional synchrotron diffraction data and neutron small-angle scattering data are listed in the table below and analyzed as follows:
[0051] According to the table above, the precipitate size obtained from the two-dimensional synchrotron radiation diffraction data and the small-angle scattering data of neutrons in the Al-Zn alloy of this embodiment is compared. The difference between the two is more than 50%. After analysis, it was found that there are two sizes of Zn particles in this alloy. The two-dimensional synchrotron radiation diffraction data is the average size of the larger particles, while the small-angle scattering data is the average size of the smaller particles. Both size distributions exist. This embodiment has successfully obtained multiple size distributions of the precipitate phase.
[0052] In a further specific embodiment two, the size of the fine γ' (Ni3Al) precipitates in the cast GH4169 alloy is obtained using the following method: S1. Obtain two-dimensional synchrotron radiation diffraction data of the aluminum and nickel-based alloys to be tested. The two-dimensional synchrotron radiation diffraction data is in the form of Dodeby rings. Integrate the two-dimensional synchrotron radiation diffraction data to obtain the peak position-peak intensity curve. Specifically, in this embodiment, the alloy being tested is a cast GH4169 alloy. The thickness of the synchrotron radiation penetrating side of the sample is reduced to a level sufficient to allow the synchrotron radiation to penetrate the sample. A CCD is used to acquire the synchrotron radiation generated by penetrating the alloy material, which is in the form of a Dodeby ring. The obtained two-dimensional synchrotron radiation diffraction data is then integrated to obtain the peak position-peak intensity curve.
[0053] S2. The peak position and full width at half maximum (FWHM) of each diffraction peak of the fine particulate precipitate present in the peak position-peak intensity curve are calibrated. Specifically, the peak positions and full width at half maximum (FWHM) of the (100), (110), (422), and (511) diffraction planes of the precipitated phase γ' (Ni3Al) were calibrated, and the specific values were recorded.
[0054] S3. Substitute the peak positions and full width at half maximum (FWH) of each diffraction peak of the fine-grained precipitates present in the alloy into the equation of the Modified Williamson-Hall (mWH) method to calculate the size of the precipitates. Specifically, the equation for the Modified Williamson-Hall (mWH) method is as follows:
[0055] in , Dislocation contrast factor b is the Burgers vector, which is 0.252nm in this embodiment. M is 1. β is the full width at half maximum (FWHM). λ is the wavelength of the synchrotron X-rays used, which is 0.06887nm in this embodiment. θ is the position of the diffraction peak. q is 0.5. hkl represents the index of the (hkl) peak position.
[0056] S4. Obtain neutron small-angle scattering data of the alloy, wherein the neutron small-angle scattering data has at least one scattering peak; Specifically, when the same sample was used in a small-angle neutron scattering experiment, the obtained data showed a scattering peak with a scattering vector Q value of around 0.03 Å⁻¹.
[0057] S5. Based on the shape of the fine particle phase, select a suitable small-angle scattering data model, fit the neutron small-angle scattering data, and obtain the precipitated phase size; Specifically, in this embodiment, γ'(Ni3Al) exists in a spherical shape, and the sphere model, which is suitable for spherical models, is used for fitting.
[0058] S6. Compare and analyze the precipitate size obtained from two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data; Specifically, the precipitate sizes obtained from two-dimensional synchrotron diffraction data and neutron small-angle scattering data are listed in the table below and analyzed as follows:
[0059] According to the table above, the difference between the precipitate size obtained from the two-dimensional synchrotron radiation diffraction data and the small-angle neutron scattering data of the γ'(Ni3Al) phase in the cast GH4169 alloy of this embodiment is less than 10%, which proves that the precipitate size in the actual alloy is close to this result.
[0060] Furthermore, compared with existing technologies, the existing technologies (such as the TWIP steel dislocation density calculation method based on neutron diffraction and synchrotron X-ray diffraction mentioned in Acta Metallurgica Sinica, Vol. 56, No. 4) employ similar neutron diffraction and synchrotron X-ray diffraction calculations.
[0061] It is necessary to further explain that neutron diffraction and small-angle neutron scattering are two completely different experimental methods. Both use neutrons as high-energy rays, but their experimental principles, testing procedures, analytical equipment, and experimental results differ, and the data processing procedures are also entirely different. These differences are illustrated here with a data table comparison:
[0062] Therefore, it is evident that the combined technique of neutron small-angle scattering and synchrotron radiation diffraction in this application is significantly superior to existing technologies in the relevant technical field.
[0063] In addition, it can be summarized that this method has the characteristics of high accuracy, simple sample preparation, non-destructive nature in practical use, and the measurement results are statistically significant.
[0064] In another aspect, the present invention also discloses a computer-readable storage medium storing a computer program, which, when executed by a processor, causes the processor to perform the steps of the above-described calculation method for obtaining the fine particle phase size in aluminum and nickel-based alloys.
[0065] In another aspect, the present invention also discloses a computer device, including a memory and a processor, wherein the memory stores a computer program, and when the computer program is executed by the processor, the processor performs the steps of the above-described calculation method for obtaining the fine particle phase size in aluminum and nickel-based alloys.
[0066] In another embodiment provided in this application, a computer program product containing instructions is also provided, which, when run on a computer, causes the computer to execute any of the calculation methods described above for obtaining the fine particle phase size in aluminum and nickel-based alloys.
[0067] It is understood that the system provided in the embodiments of the present invention corresponds to the method provided in the embodiments of the present invention, and the explanation, examples and beneficial effects of the relevant content can be referred to the corresponding parts of the above methods.
[0068] In the above embodiments, implementation can be achieved entirely or partially through software, hardware, firmware, or any combination thereof. When implemented using software, it can be implemented entirely or partially in the form of a computer program product. The computer program product includes one or more computer instructions. When the computer program instructions are loaded and executed on a computer, all or part of the processes or functions described in the embodiments of this application are generated. The computer can be a general-purpose computer, a special-purpose computer, a computer network, or other programmable device. The computer instructions can be stored in a computer-readable storage medium or transmitted from one computer-readable storage medium to another. For example, the computer instructions can be transmitted from one website, computer, server, or data center to another website, computer, server, or data center via wired (e.g., coaxial cable, fiber optic, digital subscriber line) or wireless (e.g., infrared, wireless, microwave, etc.) means. The computer-readable storage medium can be any available medium that a computer can access or a data storage device such as a server or data center that integrates one or more available media. The available medium can be a magnetic medium (e.g., floppy disk, hard disk, magnetic tape), an optical medium (e.g., DVD), or a semiconductor medium (e.g., solid-state drive), etc.
[0069] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.
[0070] Furthermore, it should be noted that if any directional indication (such as up, down, left, right, front, back, etc.) is involved in the embodiments of the present invention, the directional indication is only used to explain the relative positional relationship and movement of each component in a specific posture. If the specific posture changes, the directional indication will also change accordingly.
[0071] Furthermore, if the embodiments of this invention involve descriptions such as "first" or "second," these descriptions are for descriptive purposes only and should not be construed as indicating or implying their relative importance or implicitly specifying the number of technical features indicated. Therefore, a feature defined with "first" or "second" may explicitly or implicitly include at least one of those features. Additionally, the meaning of "and / or" throughout the text includes three parallel solutions; for example, "A and / or B" includes solution A, solution B, or a solution where both A and B are satisfied simultaneously. Furthermore, in the embodiments of this invention, "multiple" refers to two or more. Moreover, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or impossible to implement, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by this invention.
Claims
1. A method for obtaining the size of fine-particle phases in aluminum and nickel-based alloys, characterized in that, include: Two-dimensional synchrotron radiation diffraction data of the aluminum and nickel-based alloys to be tested were acquired, and the two-dimensional synchrotron radiation diffraction data were integrated to obtain peak position-peak intensity curves. The peak position and full width at half maximum (FWHM) of each diffraction peak of the fine particulate precipitate present in the peak position-peak intensity curve were calibrated. The calibration data is substituted into the calculation equation for the precipitate size to obtain the corresponding precipitate size; The small-angle scattering (SAS) data of the alloy under test is obtained, and the corresponding SAS data model is selected according to the shape of the fine-particle phase. The SAS data is then fitted to obtain the precipitated phase size. The precipitated phase sizes obtained by comparing two-dimensional synchrotron radiation diffraction data and neutron small-angle scattering data were used to obtain the phase sizes of fine particles in aluminum and nickel-based alloys.
2. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, The equation for calculating the size of the precipitated phase is: for: Among them, for dislocation contrast factor , for Dislocation correlation factor of crystal planes For the Burgers vector, For the size of the precipitated phase, For dislocation density, This represents the higher-order infinitesimal within the parentheses. This is a constant related to the actual alloy, with a value of 1. The size is half the height and width. The wavelength of the synchrotron X-rays used. The peak position of the diffraction peak. The constants related to the actual alloy are taken as 0.
5. , , These represent the crystal plane indices of the three diffraction peak positions.
3. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, The two-dimensional synchrotron radiation diffraction data is in the form of a Debye ring. During the integration of the two-dimensional synchrotron radiation diffraction data, a sector integral is performed on the entire two-dimensional diffraction data with the center of the Debye ring as the center.
4. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, During the calibration of peak position and half-width at half-maximum (WHM), the diffraction peaks are calibrated using the wavelength of the synchrotron radiation light used for measurement.
5. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, In the calculation process to obtain the corresponding precipitate size, the diffraction peaks used have no overlap with other diffraction peaks, and the peak positions and full width at half maximum (FWHM) of the diffraction peaks all originate from the same fine-particle precipitate.
6. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, In the calculation process to obtain the corresponding precipitate size, the peak positions and full width at half maximum (FWHM) of at least three diffraction peaks are substituted into the fitting, and linear fitting is used for the fitting.
7. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, The neutron small-angle scattering data has at least one scattering peak, and the neutron small-angle scattering data is a smooth curve.
8. The method for obtaining the fine-particle phase size in aluminum and nickel-based alloys as described in claim 1, characterized in that, In the process of selecting the small-angle scattering data model, the shapes of the fine particle phases used include spherical and needle-like disk shapes.