Analysis method of metal solidified body
By conducting multi-dimensional analysis of the metal solidified body and evaluating the volume percentage of the Fe-Zr intermetallic compound phase and the iron-based solid solution phase, the problem of verifying the performance of the metal solidified body in the prior art has been solved, and the safety and stability of the solidified body of high radioactive waste has been assessed.
Patent Information
- Application Number
- CN202511317882.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-09-15
- Publication Date
- 2026-01-13
AI Technical Summary
Existing technologies are insufficient to effectively analyze the performance of solidified metal bodies, especially the behavior and safety of solidified high-radioactive metal waste during long-term geological disposal. There is a lack of effective analytical methods to verify their corrosion resistance and leaching rate.
By acquiring samples from multiple designated locations, preparing analytical solutions and observing surfaces, determining the concentration of target components and conducting microscopic observations, the volume percentages of Fe-Zr intermetallic compound phases and iron-based solid solution phases are evaluated. Combined with macroscopic sampling and phase characterization methods, the uniformity and stability of the solidified metal are assessed.
It provides multi-dimensional analysis methods, improves the reliability and accuracy of the results, ensures that the performance of solidified metals meets safety requirements, and provides necessary technical support for the disposal of high-level radioactive waste.
Smart Images

Figure CN121324609A_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of radioactive waste treatment technology, and in particular to an analytical method for solidified metal bodies. Background Technology
[0002] This section is intended to provide background or context for embodiments of this application. The description herein is not intended to imply that it is prior art simply because it is included in this section.
[0003] The anode slime produced during the dry electrolytic refining process is a type of high-level radioactive metal waste, containing cladding from spent fuel assemblies, zirconium metal from the fuel, inert fragment products, and small amounts of incompletely electrolyzed actinides. Converting this high-level radioactive metal waste into a chemically stable and corrosion-resistant solidified metal is a crucial step in its safe disposal. One effective solidification method is to melt it at high temperatures and cool it into a solidified metal. This solidified body is a good candidate for containing noble metal fragments, as well as Fe, Zr, and a limited number of actinides, and can encapsulate these nuclides in a compact, high-hardness, and corrosion-resistant high-level radioactive metal waste solidification.
[0004] To ensure that the behavior of metal solidified bodies is predictable and meets safety requirements during long-term geological treatment, it is necessary to analyze the metal solidified bodies, determine the performance of batch-produced metal solidified bodies (such as corrosion resistance and leaching rate), and verify the performance of the metal solidified bodies. Summary of the Invention
[0005] In view of this, embodiments of this application provide an analytical method for metal solidified bodies, which evaluates the metal solidified bodies from multiple dimensions by analyzing the target components, Fe-Zr intermetallic compound phases and iron-based solid solution phases, and verifies the performance of the metal solidified bodies.
[0006] This application provides an analytical method for solidified metal bodies, including: Multiple samples were obtained from multiple designated locations on the solidified metal body; A portion of the sample is dissolved to prepare an analytical solution, and another portion of the sample is prepared to form an observation surface; The concentration of the target component in each of the analytical solutions is obtained, the target component including zirconium; Based on the concentration of the target component in each of the analytical solutions, the average concentration and data dispersion index of the target component are obtained; Microscopic observations were performed on each of the observation surfaces to obtain the volume percentage of the Fe-Zr intermetallic compound phase and the volume percentage of the iron-based solid solution phase in each sample having the observation surface. Determine whether the volume percentage of the Fe-Zr intermetallic compound phase meets a first threshold range, and whether the volume percentage of the iron-based solid solution phase meets a second threshold range.
[0007] In some embodiments, after obtaining the volume percentage of the Fe-Zr intermetallic compound phase and the volume percentage of the iron-based solid solution phase in each sample having the observed surface, the analytical method includes: The distribution characteristics of the target radionuclides in the Fe-Zr intermetallic compound phase and the iron-based solid solution phase of each sample having the observation surface were determined.
[0008] In some embodiments, the target radionuclide includes at least one of uranium, technetium, ruthenium, rhodium, and palladium.
[0009] In some embodiments, the solidified metal body is cylindrical; The center point of the central axis of the solidified metal, the center of the top surface, and the center of the bottom surface are all the predetermined positions.
[0010] In some embodiments, the cross-section is a plane passing through the center point and perpendicular to the central axis; Any point on the edge of the cross-section of the solidified metal body is one of the designated positions; Any point on the edge line and the point where the line connecting the center point is bisected is a designated position.
[0011] In some embodiments, the analysis method includes: The appearance of the metal solidified body is inspected to obtain its size and surface features.
[0012] In some embodiments, the concentration of the target component in the analytical solution is measured by at least one of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry.
[0013] In some embodiments, the target component includes at least one selected from iron, chromium, nickel, uranium, molybdenum, technetium, ruthenium, rhodium, palladium, and tellurium.
[0014] In some embodiments, the observed surface is observed microscopically using a scanning electron microscope and / or an energy-dispersive X-ray spectrometer.
[0015] The analytical method provided in this application improves the reliability of results by acquiring multiple samples from multiple designated locations. The method directly targets the key characteristics of the solidified metal body. Specifically, it evaluates the uniformity of the target component based on its average concentration and data dispersion index. Furthermore, it compares the volume percentages of the Fe-Zr intermetallic compound phase and the iron-based solid solution phase in different samples based on the volume percentages of these phases in each sample with an observation surface, thus evaluating the predictability and uniformity of the microstructure and phase composition. In this way, by combining macroscopic sampling, batch chemical analysis, and phase characterization, the performance of the solidified metal body product is evaluated from multiple dimensions. This provides necessary technical support and data foundation for process verification, quality control, and the establishment of standards for the reception and disposal of solidified radioactive waste in high-temperature smelting solidification processes for high-level radioactive metal waste. Attached Figure Description
[0016] Figure 1 A schematic flowchart illustrating the analytical method for metal solidified bodies provided in some embodiments of this application; Figure 2 This is a perspective view of a metal-cured body provided in some embodiments of this application; Figure 3 for Figure 2 A schematic diagram of the cross-section of a solidified metal. Detailed Implementation
[0017] The embodiments of this application will be described in further detail below with reference to the accompanying drawings and examples. The following examples are used to illustrate this application, but should not be used to limit the scope of this application.
[0018] The various specific technical features and embodiments described in the detailed embodiments can be combined in any suitable manner without contradiction. For example, different combinations of specific technical features / embodiments can form different implementation methods. To avoid unnecessary repetition, the various possible combinations of various specific technical features / embodiments in this application will not be described separately. In addition, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance. The application will be further described in detail below with reference to the accompanying drawings and specific embodiments.
[0019] In this embodiment, the solidified metal body 1 is produced by high-temperature metal waste through metallurgical melting and solidification. For example, the solidified metal body 1 is formed by mixing radioactive metal waste, then melting and cooling it.
[0020] Radioactive metal waste is radioactive waste generated during the dry reprocessing of spent fuel. It is characterized by high radioactivity, strong heat release, and long half-life. Its safe management requires a combination of technical treatment and engineering isolation measures.
[0021] For example, radioactive metal waste can come from radioactive metal waste such as anode mud and cladding generated during dry electrolytic refining processes. Anode mud contains radioactive nuclides of noble metals such as rhodium, palladium and ruthenium produced by fission, and uranium and zirconium produced from spent fuel electrolysis residues. Cladding contains iron-based materials that are activated by neutron irradiation to form radioactive nuclides (such as cobalt-60, iron-55, etc.).
[0022] Please see Figure 1 This application provides an analytical method for a solidified metal body 1, the analytical method comprising: S100: Obtain multiple samples from multiple designated locations of the metal solidified body; Specifically, please refer to Figure 2 and Figure 3 One or more samples can be obtained at each set location 1a, and the sample is a part of the metal solidified body 1.
[0023] There are no restrictions on the method of obtaining samples from a solidified metal. For example, samples can be separated from a solidified metal by drilling or cutting.
[0024] The shape of the sample is not limited; for example, the sample can be in the form of fragments or blocks.
[0025] S200: Dissolve a portion of the sample to prepare an analytical solution, and prepare another portion of the sample to form an observation surface; The solvent used to dissolve a portion of the sample to prepare an analytical solution is not limited. For example, a mixed acid consisting of hydrochloric acid, nitric acid, and hydrofluoric acid, i.e., a mixed acid consisting of HCl, HNO3, and HF, can be used as a solvent to dissolve the sample and prepare an analytical solution.
[0026] Before preparing the analytical solution, the sample needs to be cleaned and weighed. Cleaning removes dust and impurities from the sample; for example, deionized water can be used. Weighing is used to obtain the mass of the sample to determine the amount of solvent to be used.
[0027] Understandably, one, two, or more samples may be used to prepare an analytical solution, with one analytical solution corresponding to one sample.
[0028] Another portion of the sample is used to prepare the observation surface. In other words, this portion of the sample will not be dissolved and will remain in a solid state. Each sample can correspond to one observation surface.
[0029] For example, multiple samples may be acquired at a designated location 1a, wherein a portion of the samples acquired at the designated location 1a are prepared into an analytical solution, and another portion is prepared into an observation surface.
[0030] For example, a sample can be obtained at a designated location 1a, and this sample can be used to prepare an analytical solution or to observe a surface.
[0031] The observation surface can be a basically flat plane used to observe the microscopic morphology of the sample.
[0032] In some embodiments, the sample can be embedded in the support structure. Since the sample is too small to be easily handled, embedding the sample in the support structure allows the sample to be retrieved by gripping the support structure.
[0033] The support structure can be formed by curing a gel-like substance, such as epoxy resin or other gel-like substances. Specifically, liquid epoxy resin can be used to encapsulate part of the sample structure, leaving the observation surface exposed. Once the liquid epoxy resin cures, a support structure is formed.
[0034] The sample can be ground and polished to form an observation surface. The smoothness of the observation surface can be set as needed; for example, the observation surface can be ground to 1200 grit, but this application embodiment does not limit it.
[0035] S300, Obtain the concentration of the target component in each of the analytical solutions, wherein the target component includes zirconium; S400. Based on the concentration of the target component in each of the analytical solutions, obtain the average concentration and data dispersion index of the target component; The concentration of zirconium is a process control indicator for the solidification of radioactive waste into a solidified metal body 1.
[0036] The average concentration of the target component is the arithmetic mean of the concentrations of the target component in all analytical solutions.
[0037] The data dispersion index for target components is used to measure the degree of dispersion of the concentration of the target component in various analytical solutions. Taking zirconium as an example, the average concentration of zirconium (Zr) is the arithmetic mean of the concentrations of zirconium in all analytical solutions.
[0038] Taking zirconium as an example, the zirconium data dispersion index is used to measure the degree of dispersion of zirconium concentration in various analytical solutions.
[0039] Data dispersion metrics may include at least one of standard deviation, relative standard deviation, and variance.
[0040] In some embodiments, the data dispersion metric may include standard deviation, relative standard deviation, or variance.
[0041] In some embodiments, the data dispersion metric may include any two or three of the following: standard deviation, relative standard deviation, and variance.
[0042] The average concentration and data dispersion index of zirconium can be used to assess the spatial uniformity of zirconium distribution throughout the solidified metal.
[0043] In some embodiments, the average concentration of the target component is compared with the standard concentration to determine whether the target component meets the requirements.
[0044] By comparing the average concentration of zirconium with the standard concentration, it can be determined whether the zirconium content meets the requirements.
[0045] For example, the standard concentration of zirconium can be 5 wt%-20 wt%.
[0046] If the average concentration of zirconium is within the standard concentration range, for example, between 5 wt% and 20 wt%, then the zirconium content in the solidified metal 1 meets the requirements. If the average concentration of zirconium is outside the standard concentration range, for example, less than 5 wt%, or greater than 20 wt%, then the zirconium content in the solidified metal 1 does not meet the requirements.
[0047] S500. Perform microscopic observation on each of the observation surfaces to obtain the volume percentage of Fe-Zr intermetallic compound phase and the volume percentage of iron-based solid solution phase in each sample having the observation surface. Fe-Zr intermetallic compound phases can form stable compounds with precious metal fragment products, radionuclides such as uranium, etc., reducing the migration of radioactive elements in the disposal environment, and can also improve the structural strength of the solidified metal body.
[0048] Iron-based solid solutions use α (body-centered cubic) or γ (face-centered cubic) iron as the matrix and form substitutional or interstitial solid solutions through the solid solution of alloying elements (such as Cr, Ni, etc.), which significantly improves the mechanical strength of the solidified metal. Iron-based solid solutions can dissolve some radionuclides to form a stable solid solution structure and reduce the migration of nuclides in the disposal environment.
[0049] The volume percentage of the Fe-Zr intermetallic compound phase is the percentage of the volume of the Fe-Zr intermetallic compound phase to the volume of the sample in which it is located.
[0050] The volume percentage of the iron-based solid solution phase is the percentage of the volume of the iron-based solid solution phase to the volume of the sample in which it is contained.
[0051] In some embodiments, the morphology, size, and spatial distribution characteristics of the Fe-Zr intermetallic compound phase and the iron-based solid solution phase in each sample with an observation surface can also be identified by microscopic observation.
[0052] Microscopic observation is a method of obtaining the volume percentage, morphology, size, and spatial distribution characteristics of Fe-Zr intermetallic compound phases and iron-based solid solutions at or below micrometers by magnifying them using optical or electronic devices.
[0053] S600. Determine whether the volume percentage of the Fe-Zr intermetallic compound phase meets the first threshold range, and whether the volume percentage of the iron-based solid solution phase meets the second threshold range.
[0054] An excessively high volume percentage of Fe-Zr intermetallic compound phases may lead to increased melting temperature and reduced mechanical properties; an excessively high volume percentage of iron-based solid solution phases may lead to reduced nuclide containment and increased risk of radionuclide leaching in acidic environments.
[0055] Therefore, determining whether the volume percentage of the Fe-Zr intermetallic compound phase meets the first threshold range and whether the volume percentage of the iron-based solid solution phase meets the second threshold range can be used to evaluate the stability of the solidified metal.
[0056] The first threshold range and the second threshold range can be set according to requirements.
[0057] In some embodiments, the first threshold range can be 20 vol%-40 vol%. That is, the volume percentage of the Fe-Zr intermetallic compound phase can be X. If 20 vol% ≤ X ≤ 40 vol%, then the volume percentage of the Fe-Zr intermetallic compound phase meets the threshold range, and the content of the Fe-Zr intermetallic compound phase meets the requirements. If X < 20 vol%, or X > 40 vol%, then the volume percentage of the Fe-Zr intermetallic compound phase does not meet the threshold range, and the content of the Fe-Zr intermetallic compound phase does not meet the requirements.
[0058] In some embodiments, the second threshold range can be 60 vol%-80 vol%. That is, the volume percentage of the iron-based solid solution phase can be Y. If 60 vol% ≤ Y ≤ 80 vol%, then the volume percentage of the iron-based solid solution phase meets the threshold range, and the content of the iron-based solid solution phase meets the requirements. If Y < 60 vol%, or Y > 80 vol%, then the volume percentage of the iron-based solid solution phase does not meet the threshold range, and the content of the iron-based solid solution phase does not meet the requirements.
[0059] For example, the volume percentage X of the Fe-Zr intermetallic compound phase is between 20 vol% and 40 vol%, and the volume percentage Y of the iron-based solid solution phase is between 60 vol% and 80 vol%. This can reduce the melting process temperature, form a two-phase microstructure, and have better containment effect and mechanical properties, thereby obtaining a stable, dense, and corrosion-resistant solidified metal body.
[0060] It can calculate at least one of the standard deviation, relative standard deviation, and variance of the volume percentage of Fe-Zr intermetallic compound phases, which can be used to evaluate the spatial distribution uniformity of Fe-Zr intermetallic compound phases.
[0061] It can calculate at least one of the standard deviation, relative standard deviation, and variance of the volume percentage of the iron-based solid solution phase, and can be used to evaluate the spatial distribution uniformity of the iron-based solid solution phase.
[0062] The analytical method provided in this application improves the reliability of results by acquiring multiple samples from multiple designated locations 1a. The method directly targets the key characteristics of the solidified metal body 1. Specifically, it evaluates the uniformity of the target component based on its average concentration and data dispersion index. Furthermore, it compares the volume percentages of the Fe-Zr intermetallic compound phase and the iron-based solid solution phase in different samples based on the volume percentages of the Fe-Zr intermetallic compound phase and the iron-based solid solution phase in each sample with an observation surface, thereby evaluating the predictability and uniformity of the microstructure and phase composition. Thus, by combining macroscopic sampling, batch chemical analysis, and phase characterization, the consistency of the solidified metal body 1 product performance is verified and evaluated from multiple dimensions. This provides necessary technical support and data foundation for process verification, quality control, and the final reception and disposal of the solidified metal body in the high-temperature melting process of high-level radioactive metal waste.
[0063] In some embodiments, after obtaining the volume percentage of the Fe-Zr intermetallic compound phase and the volume percentage of the iron-based solid solution phase in each sample having the observed surface, the analytical method includes: S700. Determine the distribution characteristics of the target radionuclide in the Fe-Zr intermetallic compound phase and the iron-based solid solution phase in each sample having the observation surface.
[0064] The distribution characteristics of the target radionuclides in the Fe-Zr intermetallic compound phase and the iron-based solid solution phase of each sample with the observation surface can be determined by micro-area elemental analysis.
[0065] Micro-area elemental analysis technology enables in-situ detection of chemical components in tiny areas by focusing on the micrometer to nanometer scale.
[0066] In this embodiment, by determining the distribution characteristics of the target radionuclides in different phases, it is verified whether these target radionuclides preferentially enrich or dissolve in a specific stable phase as expected, thereby determining the fixation effect of the target radionuclides.
[0067] In some embodiments, the target radionuclide includes at least one of uranium (U), technetium (Tc), ruthenium (Ru), rhodium (Rh), and palladium (Pd).
[0068] For example, the target radionuclide includes one of uranium, technetium, ruthenium, rhodium, and palladium.
[0069] For example, the target radionuclides include multiple elements such as uranium, technetium, ruthenium, rhodium, and palladium.
[0070] For example, the target radionuclides include all of the elements uranium, technetium, ruthenium, rhodium, and palladium.
[0071] Uranium can originate from residues from spent fuel separation processes.
[0072] Technetium, ruthenium, rhodium, and palladium are fission products of precious metals.
[0073] In this embodiment, the distribution characteristics of at least one of uranium, technetium, ruthenium, rhodium, and palladium in the Fe-Zr intermetallic compound phase and the iron-based solid solution phase are determined to verify whether these target radionuclides are preferentially enriched or dissolved in specific stable phases as expected. For example, whether uranium (U), ruthenium (Ru), rhodium (Rh), and palladium (Pd) are mainly present in the Fe-Zr intermetallic compound phase, and the distribution of technetium (Tc), etc., thereby confirming the fixation effect.
[0074] In some embodiments, please refer to Figure 2 The solidified metal body 1 is cylindrical; the center point 11 of the central axis 1b of the solidified metal body 1, the center 12 of the top surface and the center 13 of the bottom surface are all set at position 1a.
[0075] In the process of solidifying radioactive metal waste, a cylindrical solidified metal body 1 can be manufactured using a vacuum metal melting device.
[0076] The center point 11 of the central axis 1b of the solidified metal body 1, the center 12 of the top surface, and the center 13 of the bottom surface are all designated positions 1a. In this way, three or more samples can be obtained from the above positions.
[0077] The center of the top surface 12 is the center of one of the circular surfaces of the cylinder, and the center of the bottom surface 13 is the center of the other circular surface of the cylinder.
[0078] The central axis 1b is a straight line that extends axially along the cylinder and connects the center of the top surface 12 and the center of the bottom surface 13.
[0079] The center point 11 of the central axis 1b is the bisection point 15 of the central axis 1b.
[0080] In this embodiment, during the solidification process of radioactive metal waste to form a solidified metal body, specifically, for example, during the solidification process, the cooling rate of the surface and the central region of the solidified metal body is significantly different. For example, the surface region cools faster, forming a fine-grained region, and impurities or low-melting-point elements are easily pushed to the final solidified central region. The central region cools slowly, and the elements diffuse sufficiently, but it is easy to enrich segregated elements. Moreover, radionuclides have different dissolution and migration behaviors, and are easy to accumulate in different parts. Sampling the center 12 of the top surface and the center 13 of the bottom surface of the solidified metal body can be used to represent the surface characteristics, while sampling the center point of the solidified metal body is beneficial to represent the characteristics of the central region.
[0081] In some embodiments, please refer to Figure 2 and Figure 3 The cross-section is a plane that passes through the center point and is perpendicular to the central axis 1b; Any point 14 on the edge of the cross-section of the solidified metal 1 is a designated position 1a; Any point 14 on the edge line and the bisection point 15 of the line connecting the center point are designated positions 1a.
[0082] In this embodiment, sampling is performed on the edge of the cross-section, i.e. the circumferential surface of the metal solidified body, and the central region to further improve the comprehensiveness and authenticity of the data.
[0083] In some embodiments, the analysis method includes: S800. Inspect the appearance of the metal solidified body 1 and obtain the size and surface features of the metal solidified body 1.
[0084] Taking a cylindrical solidified metal body 1 as an example, the dimensions of the solidified metal body 1 may include its height along the axial direction, diameter, volume, area of the top surface, and area of the bottom surface.
[0085] Surface features may include, but are not limited to, the presence of dents, cracks, and / or pores on the surface. Surface features are used to determine the surface integrity of a solidified metal and can be used to characterize whether there are obvious manufacturing defects on the surface of the solidified metal.
[0086] In some embodiments, the concentration of the target component in the analytical solution is measured by at least one of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry.
[0087] For example, the concentration of a target component in a solution can be measured and analyzed by one of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry.
[0088] For example, the concentration of a target component in a solution can be analyzed by two methods: inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS).
[0089] Inductively Coupled Plasma Atomic Emission Spectrometry (ICP-AES) is an analytical technique based on the emission characteristic spectra of elements in a sample excited by high-temperature plasma. It is used for the qualitative and quantitative determination of the concentration of target components in solutions.
[0090] Inductively Coupled Plasma Mass Spectrometry (ICP-MS) uses high-temperature plasma to ionize target components in the analytical solution, and then uses mass spectrometry to accurately separate and detect the ions, thus achieving quantitative analysis of ultra-trace elements.
[0091] In this embodiment, elemental quantitative analysis of analytical solutions at different sampling locations is performed using at least one of inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). This can be used to determine the concentrations of major elements (such as Fe, Cr, Ni, Zr, U) and key noble metal fission products (such as Mo, Tc, Ru, Rh, Pd, Te). By comparing the chemical composition data (e.g., arithmetic mean, standard deviation, relative standard deviation, and / or variance) of samples at different locations, the spatial homogeneity of the entire metal solidification body in terms of chemical composition can be evaluated.
[0092] In some embodiments, the target component includes at least one of iron (Fe), chromium (Cr), nickel (Ni), uranium (U), molybdenum (Mo), technetium (Tc), ruthenium (Ru), rhodium (Rh), palladium (Pd), and tellurium (Te).
[0093] For example, the target component includes one of the following elements: iron, chromium, nickel, uranium, molybdenum, technetium, ruthenium, rhodium, palladium, and tellurium.
[0094] For example, the target components include multiple elements selected from iron, chromium, nickel, uranium, molybdenum, technetium, ruthenium, rhodium, palladium, and tellurium.
[0095] It can determine the concentration of at least one of the following elements: iron, chromium, nickel, uranium, molybdenum, technetium, ruthenium, rhodium, palladium, and tellurium, and calculate the average concentration, standard deviation, relative standard deviation, and variance of these elements.
[0096] In some embodiments, only the concentration, average concentration, and data dispersion index of zirconium may be measured.
[0097] In some embodiments, the observed surface is observed microscopically using a scanning electron microscope and / or an energy-dispersive X-ray spectrometer.
[0098] For example, the surface can be observed microscopically using either a scanning electron microscope or an energy-dispersive X-ray spectrometer.
[0099] For example, the surface can be observed microscopically using multiple scanning electron microscopes.
[0100] Scanning electron microscopy (SEM) can be used to observe the morphology, size, and spatial distribution characteristics of Fe-Zr intermetallic compound phases and iron-based solid solution phases.
[0101] Energy-dispersive X-ray spectrometers (EDS / EDX) can be used to identify elements from boron (B) to uranium (U), especially radionuclides, and generate elemental surface distribution maps to locate segregation regions.
[0102] In the description of this specification, the references to the terms "an embodiment," "some embodiments," and "exemplary" refer to specific features, structures, materials, or characteristics described in connection with that embodiment or example, which are included in at least one embodiment or example of the embodiments of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.
[0103] The various embodiments / implementations provided in this application can be combined with each other without creating contradictions. The above descriptions are merely preferred embodiments of this application and are not intended to limit this application. For those skilled in the art, this application can have various modifications and variations. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.
Claims
1. A method for analyzing solidified metal bodies, characterized in that, include: Multiple samples were obtained from multiple predetermined locations on the solidified metal body; A portion of the sample is dissolved to prepare an analytical solution, and another portion of the sample is prepared to form an observation surface; The concentration of the target component in each of the analytical solutions is obtained, the target component including zirconium; Based on the concentration of the target component in each of the analytical solutions, the average concentration and data dispersion index of the target component are obtained; Microscopic observations were performed on each of the observation surfaces to obtain the volume percentage of the Fe-Zr intermetallic compound phase and the volume percentage of the iron-based solid solution phase in each sample having the observation surface. Determine whether the volume percentage of the Fe-Zr intermetallic compound phase meets a first threshold range, and whether the volume percentage of the iron-based solid solution phase meets a second threshold range.
2. The analytical method according to claim 1, characterized in that, After obtaining the volume percentage of the Fe-Zr intermetallic compound phase and the volume percentage of the iron-based solid solution phase in each sample having the observed surface, the analytical method includes: The distribution characteristics of the target radionuclides in the Fe-Zr intermetallic compound phase and the iron-based solid solution phase of each sample having the observation surface were determined.
3. The analytical method according to claim 2, characterized in that, The target radionuclides include at least one of uranium, technetium, ruthenium, rhodium, and palladium.
4. The analytical method according to claim 1, characterized in that, The solidified metal body is cylindrical; The center point of the central axis of the solidified metal, the center of the top surface, and the center of the bottom surface are all the predetermined positions.
5. The analytical method according to claim 4, characterized in that, The cross-section is a plane passing through the center point and perpendicular to the central axis; Any point on the edge of the cross-section of the solidified metal body is one of the designated positions; Any point on the edge line and the point where the line connecting the center point is bisected is a designated position.
6. The analytical method according to claim 1, characterized in that, The analytical method includes: The appearance of the metal solidified body is inspected to obtain its size and surface features.
7. The analytical method according to claim 1, characterized in that, The concentration of the target component in the analytical solution is measured by at least one of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry.
8. The analytical method according to claim 1, characterized in that, The target components include at least one of the following elements: iron, chromium, nickel, uranium, molybdenum, technetium, ruthenium, rhodium, palladium, and tellurium.
9. The analytical method according to claim 1, characterized in that, Microscopic observations were performed on the observed surface using a scanning electron microscope and / or an energy-dispersive X-ray spectrometer.
