Test platform, method and application for monitoring in-situ heat treatment process of metal materials

Abstract

The application discloses a test platform, a method and application for monitoring a metal material heat treatment process in situ, wherein the test platform comprises a sample environment control system, a small-angle neutron scattering system, an electrical resistivity and temperature test system and a comprehensive control and collection system, the platform can perform in-situ macroscopic detection on phase transition / precipitation behavior of a metal bulk material in a heat treatment process, is simple to operate, is widely applicable, can measure a temperature range of RT-1200 DEG C, can be additionally provided with a vacuum or a protective atmosphere environment, test results are composed of two parts of electrical resistivity and small-angle scattering results, and mutual interference between the test results is effectively overcome, and the test results are more accurate and reliable. The method is suitable for obtaining relevant quantitative information of precipitation behavior of a metal material in a heat treatment process, and provides a novel and reliable in-situ detection and analysis technology for in-situ tracking and quantitative analysis of phase transition or precipitation behavior of a metal material in a heat treatment process.

Description

Technical Field

[0001] This invention relates to a testing platform and a testing method, specifically to a testing platform, method, and application for in-situ monitoring of the heat treatment process of metallic materials; it belongs to the field of materials analysis and testing technology. Background Technology

[0002] Given the need for in-depth research in materials science, researchers urgently require a grasp of the microscopic information regarding the mechanisms of action, structural and crystal form changes, phase transitions, and factors influencing performance of materials during reaction processes. However, traditional non-in-situ research methods can only test the state before and after the reaction, and cannot achieve dynamic testing during the reaction process, thus failing to adequately meet the needs of cutting-edge research.

[0003] In-situ characterization techniques, which have developed in recent years, utilize specific devices to perform continuous and synchronous analysis of substances and "online" analysis of specific reaction processes. This yields a series of results with time or other relevant conditions as parameters, enabling the analysis of changes in the reaction process. These techniques are dynamic, real-time, and intuitive. Several commonly used in-situ characterization methods include in-situ infrared spectroscopy, in-situ Raman spectroscopy, in-situ X-ray diffraction, and in-situ transmission, which can detect the microstructure and crystal structure of materials.

[0004] We know that the properties of a material are determined by its internal microstructure. Heat treatment is a crucial method for controlling the microstructure of metallic materials, and the evolution of the complex microstructure during heat treatment has a decisive impact on the final comprehensive performance of alloy products. Therefore, elucidating the evolution law of the microstructure of metallic materials during heat treatment and its influence on material structure and properties is of great significance. Researching the fine-tuning of phase transformations / precipitations during the heat treatment of metallic materials, and exploring the heat treatment conditions required for the optimal microstructure characteristics of the material, will allow for the optimization of heat treatment processes based on actual production needs, providing reliable theoretical guidance for the actual production and preparation of metallic materials. Therefore, technologies for in-situ monitoring of various phase transformations and precipitation behaviors during the heat treatment of metallic materials urgently need to be developed. Summary of the Invention

[0005] The purpose of this invention is to address the aforementioned problems in the prior art by providing a testing platform and method for in-situ monitoring of phase transformation and precipitation behavior during the heat treatment of metallic materials. This method is particularly suitable for collecting quantitative information on precipitation behavior of alloys during non-isothermal aging processes and belongs to the field of metallic material structure and characterization technology.

[0006] To achieve the above objectives, the present invention adopts the following technical solution:

[0007] This invention first discloses a testing platform for in-situ monitoring of the heat treatment process of metallic materials, comprising:

[0008] The sample environment control system provides a heat treatment environment for metallic materials and is equipped with a sample clamping structure, an optical entrance window, and an optical exit window.

[0009] A small-angle neutron scattering system is used to generate a neutron beam spot, and small-angle neutron scattering tests on metallic materials are achieved through the optical incident window and the optical exit window.

[0010] The resistivity and temperature testing system is connected to the sample on the sample clamping structure via test leads, and is used to measure the resistance and temperature of metallic materials.

[0011] The integrated control and acquisition system is connected to the small-angle neutron scattering system and the resistivity and temperature testing system to realize the acquisition and control of test data.

[0012] Preferably, the aforementioned sample environment control system is a vertical high-temperature tubular resistance furnace, which may also be equipped with a vacuum pump or auxiliary atmosphere. During the heat treatment process, the vacuum level is maintained at 10... 3 Within a certain range (Pa), or by using a protective gas such as nitrogen, the metal sample can be prevented from undergoing oxidation or other reactions.

[0013] Preferably, the aforementioned resistivity and temperature testing system includes a resistance tester and a temperature tester to detect and record the change in resistivity with temperature during heat treatment.

[0014] More preferably, the aforementioned vertical high-temperature tubular resistance furnace has an optical incident window on its first sidewall and an optical exit window on the opposite side of the first sidewall. The sample clamping structure is located between the optical incident window and the optical exit window. Both the optical incident window and the optical exit window are made of sapphire and are used for the incident and exit of the neutron beam spot.

[0015] More preferably, the optical emission channel between the aforementioned sample clamping structure and the optical emission window is a trumpet-shaped structure with a smaller inner diameter and a larger outer diameter, which facilitates the collection of scattered neutrons.

[0016] More preferably, one end of the aforementioned vertical high-temperature tubular resistance furnace is equipped with a vent valve and a wire outlet, while the other end is equipped with a pressure relief valve and a vacuum valve. The test leads of the resistance tester and temperature tester are fixedly connected to the sample through the wire outlet. To ensure reliable connection, spot welding can be used to fix the test leads to the sample. The test leads can be made of materials such as copper, aluminum, and nickel, suitable for testing different types of metal materials. Furthermore, the test leads are sheathed with a high-temperature resistant insulating material, capable of withstanding temperatures up to 1200℃.

[0017] Preferably, the in-situ resistivity test employs a four-point method. To minimize errors, four test leads are connected to the sample via spot welding. Simultaneously, to accurately measure real-time temperature changes, two temperature test leads are welded onto the sample. The test leads must not interfere with each other and must not pass through the space through which the neutron beam passes. Therefore, the sample clamping structure secures both the sample and the six test leads. A high-temperature resistant (1200℃) and insulating sheath is used to re-wrap all the test leads. This not only prevents mutual interference between the test leads but also meets the requirements of the high-temperature testing environment. If a test lead becomes worn, it can be reused by adjusting the sheath length. This structural design fulfills the fundamental requirements for both in-situ resistivity and neutron scattering testing.

[0018] Furthermore, to better meet the requirements of the sample testing environment, such as vacuum and temperature control accuracy, it is essential to ensure that the outlet of the test leads is insulated and sealed. To achieve this high standard, a threaded outlet and a sealing valve were first made on the valve of the quartz tube of the resistance furnace. Then, the sealing port of the sealing valve was removed, making it resemble a hollow spiral tube. The test leads were then passed through one by one, and finally, they were fixed and sealed with resin.

[0019] More preferably, the aforementioned vertical high-temperature tubular resistance furnace is equipped with an upper flange and a lower flange at both ends, respectively. The upper flange has a positioning structure, and when the upper flange is installed, the sample clamping structure is installed and positioned through the positioning structure.

[0020] This invention also discloses a testing method for in-situ monitoring of the heat treatment process of metallic materials using the aforementioned testing platform, the specific steps of which are as follows:

[0021] S1. Prepare the sample of the material to be tested. The surface of the sample should be as flat as possible.

[0022] S2. Load the sample onto the sample clamping structure, spot weld the test wires and thermocouple wires to ensure normal readings of the resistance meter and temperature meter, and then fix the sample clamping structure to the upper flange of the vertical high temperature tubular resistance furnace and achieve positioning through the positioning structure.

[0023] S3. Prepare the test environment according to the test requirements, set the temperature control program according to the heat treatment process, and after the temperature rises, monitor and record the resistivity and temperature in situ, and at the same time perform small-angle neutron scattering test.

[0024] S4. Perform preliminary processing on the small-angle neutron scattering data and resistivity data to obtain the neutron scattering intensity distribution, resistivity and temperature change patterns at any time point during the experimental test, and analyze the relevant quantitative information on phase transition or precipitation of the sample during the heat treatment process.

[0025] Preferably, the aforementioned test environment is a vacuum environment or a protective atmosphere.

[0026] The in-situ monitoring test method for the heat treatment process of metallic materials, as described above, has excellent application prospects in the quantitative information collection of precipitation behavior during the non-isothermal aging process of alloys.

[0027] Small-angle neutron scattering (SANS) instruments are used to detect microscopic and mesoscopic structures ranging from 1 to 100 nm within materials due to density or compositional inhomogeneities, making them an important tool for obtaining nanoscale structural information about materials. In neutron scattering experiments, a neutron beam irradiates a sample, causing scattering or diffraction, which is then received by a detector at a certain distance. Analysis of this data reveals the internal microstructure of the tested sample. However, this analysis typically requires supplementary characterization techniques, such as using an atomic probe microanalysis (APT) to measure the density and composition of precipitated phases within the sample, or using electron microscopy (TEM) to determine the size and distribution of the microstructure. These characterization methods are usually non-in-situ and microscopically localized, and are easily affected by field-of-view selection, thus impacting the reliability and accuracy of the neutron data analysis results.

[0028] Furthermore, for metallic materials, resistivity reflects the overall average of electron scattering effects in all directions within their microstructure. Variations in the resistivity of metallic materials are influenced by various internal defects, such as point defects (vacancies), solid-solution atoms, line defects (dislocations), and surface defects (grain boundaries). These defects disrupt the integrity of the internal structure of metallic materials, interfere with the free electron scattering process, and thus affect the overall resistivity value. Therefore, in-situ resistivity testing technology has emerged, enabling in-situ quantitative analysis of the dynamic evolution of the microstructure within materials during heat treatment, such as the composition and volume fraction of precipitated phases. Compared to traditional microstructure testing methods such as electron microscopy, it offers significant advantages, including simple operation, accurate results, and measurement independence from field-of-view selection.

[0029] The advantages of this invention are:

[0030] (1) This invention proposes and constructs a testing platform and method for in-situ monitoring of phase transformation and precipitation behavior during the heat treatment of metallic materials. The testing platform includes a sample environment control system, a small-angle neutron scattering system, a resistivity and temperature testing system, and a comprehensive control and acquisition system. The small-angle neutron scattering system is located outside the sample environment control system. The incident neutron beam interacts with the sample through the optical incident window on the sample environment system, and the scattered neutrons are collected through the optical exit window, thus realizing neutron scattering detection. The resistivity and temperature testing system is directly connected to the sample under test, and through a clever structural design, it is made independent of the neutron scattering detection and does not interfere with it. The scattering detection results, resistivity, and temperature data are collected and controlled synchronously in real time through the comprehensive control and acquisition system.

[0031] (2) The test platform and test method of the present invention successfully combine two powerful microstructure characterization methods: in-situ resistivity test and neutron small-angle scattering technology. It can perform in-situ macroscopic detection of phase transformation / precipitation behavior during the heat treatment of bulk metal materials. It is simple to operate, has wide applicability, and can measure a temperature range of RT - 1200 ℃. It can be supplemented with a vacuum or protective atmosphere environment to meet the required environment or conditions of the sample, such as non-isothermal heating and cooling processes, high temperature, vacuum or introduction of protective atmosphere, etc. The test results are accurate and reliable, consisting of resistivity and small-angle scattering.

[0032] (3) The test method of the present invention is simple to operate and easy to implement. It can easily obtain the neutron scattering intensity distribution, resistivity and degree change law at any time during the test process. Further analysis can obtain the relevant quantitative information of phase transformation or precipitation of the sample during heat treatment. It is suitable for obtaining the relevant quantitative information of precipitation behavior of materials such as Al-Zn-Mg-Cu alloy and Inconel 718 high temperature alloy during non-isothermal aging process. It provides a new and reliable in-situ detection and analysis technology for in-situ tracking and quantitative analysis of phase transformation or precipitation behavior of metal materials during heat treatment. Attached Figure Description

[0033] Figure 1 This is a schematic diagram of the module structure of the test platform of the present invention;

[0034] Figure 2 This is a schematic diagram of the sample environment control system in the testing platform of the present invention;

[0035] Figure 3 This is a schematic diagram of the dimensions of the metallic material sample measured by the testing platform of this invention;

[0036] Figure 4 This is a partial experimental result diagram obtained by the method of Embodiment 2 of the present invention;

[0037] Figure 5 This is a partial experimental result diagram obtained by the method of Embodiment 3 of the present invention;

[0038] Figure 6 This is a partial experimental result diagram obtained by the method of Embodiment 4 of the present invention;

[0039] Figure 7 This is a partial experimental result diagram obtained by the method of Embodiment 5 of the present invention;

[0040] The meanings of the reference numerals in the figure are as follows: 1-Optical exit window, 2-Vent valve, 3-Outlet hole, 4-Flange (upper flange / lower flange), 5-Fastening screw, 6-Sample clamping structure, 7-Furnace tube fixing clamp, 8-Furnace body, 9-Optical entrance window, 10-Window fixing device, 11-Sample, 12-Pressure relief valve, 13-Vacuum valve, 14-Supporting leg. Detailed Implementation

[0041] The present invention will now be described in detail with reference to the accompanying drawings and specific embodiments.

[0042] Example 1

[0043] See Figure 1 The in-situ monitoring test platform for the heat treatment process of metallic materials of the present invention includes: a sample environment control system, a small-angle neutron scattering system, a resistivity and temperature testing system, and a comprehensive control and acquisition system.

[0044] Among them, the sample environment control system provides a heat treatment environment for metallic materials, and can be selected from, such as Figure 2 The self-designed vertical high-temperature tubular resistance furnace shown includes a furnace body 8, a sample placement tube vertically installed inside the furnace body 8 for loading the sample 11, and a support frame 14 for supporting the furnace body 8. The sample placement tube can be a vertical quartz tube, which is transparent and detachable. To facilitate sample positioning, the vertical position of the quartz tube can be finely adjusted using a clamping device.

[0045] An optical incident window 9 is provided on the first side wall of the vertical high-temperature tubular resistance furnace, and an optical exit window 1 is provided on the opposite side of the first side wall. Both the optical incident window 9 and the optical exit window 1 are made of sapphire and are installed on the side wall by a window fixing device 10. They are used for the incident and exit of the neutron beam generated by the small-angle neutron scattering system. A sample clamping structure 6 is located between the optical incident window 9 and the optical exit window 1, and the optical exit channel between the sample clamping structure 6 and the optical exit window 1 is a trumpet-shaped structure with a smaller inner diameter and a larger outer diameter.

[0046] See Figure 2 The vertical high-temperature tubular resistance furnace has a vent valve 2 and a cable outlet 3 at its upper end, and a pressure relief valve 12 and a vacuum valve 13 at its lower end. Both ends are fixed in place using upper and lower flanges 4 respectively, secured with fastening screws 5. A furnace tube fixing clamp 7 is also provided at the connection between the sample placement tube and the furnace body 8. Furthermore, a positioning structure is formed on the upper flange 4, which allows for the positioning of the sample clamping structure 6 during installation. Alternatively, this positioning structure can be a positioning mark; positioning arrows corresponding to the positioning structure can be placed at appropriate positions on the vertical high-temperature tubular resistance furnace to achieve positioning.

[0047] Furthermore, the sample environmental control system can also be equipped with a vacuum pump or auxiliary atmosphere. During heat treatment, the vacuum level is maintained at 10... 3 The pressure is kept below 10 Pa, or a protective gas such as nitrogen is introduced to prevent oxidation or other reactions from occurring in the metal material sample 11 during the heat treatment process.

[0048] The resistivity and temperature testing system is used to measure the resistance and monitor the temperature of metallic materials. It specifically includes a resistance tester and a temperature tester. The test leads are fixedly connected to the sample 11 through the lead outlet 3. To ensure reliable connection, it is best to use spot welding to fix the test leads to the sample 11. The test leads can be made of copper, aluminum, nickel, or other materials, suitable for testing different types of metallic materials. The outer sheath of the test leads is made of high-temperature resistant insulating material, capable of withstanding temperatures up to 1200℃.

[0049] Finally, the integrated control and acquisition system is connected to the small-angle neutron scattering system and the resistivity and temperature testing system to collect and control the test data, and send the data to the background for analysis to obtain the relevant test results.

[0050] Example 2

[0051] The Al-Zn-Mg-Cu alloy with a Zn content of 6% was tested using the test platform of Example 1. The specific steps are as follows:

[0052] S1. An Al-Zn-Mg-Cu alloy with a Zn content of 6% was subjected to solution treatment. The solution treatment process was: treatment at 475±5℃ for 2 h, followed by cold water quenching. Then, the sample to be tested, 11, was prepared by wire electrical discharge machining. The dimensions of sample 11 are as follows: Figure 3 As shown.

[0053] S2. Clamp sample 11 on sample clamping structure 6, and spot weld aluminum test wire and thermocouple wire using a spot welding machine. Confirm that the resistance meter and temperature meter are reading normally, and then fix sample clamping structure 6 to the upper flange 4 of vertical high temperature tubular resistance furnace to ensure fixation and positioning.

[0054] S3. Fix the high-temperature tubular resistance furnace onto the small-angle neutron scattering test platform, position the sample, and then evacuate to maintain a vacuum level of 10. 3 Within Pa. After setting the heating and cooling program, this embodiment performs non-isothermal aging treatment on the sample, with a heating rate of 0.5℃ / min, and continues to heat up to 220℃, while simultaneously collecting resistivity and temperature data and performing small-angle neutron tests.

[0055] S4. At this point, the phase transition test experiment was completed, and the small-angle neutron scattering data and resistivity change data of the sample during the non-isothermal aging process were successfully measured. Figure 4 These are some of the experimental results obtained. Among them, Figure 4 Figure (a) shows the resistivity as a function of temperature. Figure 4 Figure (b) shows the correlation results of small-angle neutron scattering intensity.

[0056] The obtained experimental data were analyzed and compared to determine whether the phase transition and precipitation behaviors were consistent. Figure 4 As shown in Figure (a), the resistivity difference (Δρ) of the Al-Zn-Mg-Cu alloy with a Zn content of 6% decreases with increasing temperature, indicating the precipitation of nanophases in the alloy, and the increasing number of nanophases with increasing temperature. Meanwhile, Figure 4 Similar results are reflected in the small-angle scattering data in Figure (b)—the peak in the curve gradually shifts to the left as the temperature increases, indicating that the size of the nanophase in the alloy increases with temperature.

[0057] Based on the above analysis and comparison, it can be seen that the small-angle neutron scattering data and resistivity data have good consistency. The test method of this invention can obtain the neutron scattering intensity distribution, resistivity and temperature change law at any time during the experimental test. Further analysis can obtain relevant quantitative information on the precipitation behavior of Al-Zn-Mg-Cu alloy with 6% Zn content during non-isothermal aging.

[0058] Example 3

[0059] The Al-Zn-Mg-Cu alloy with a Zn content of 8% was tested using the test platform of Example 1. The specific steps are as follows:

[0060] S1. An Al-Zn-Mg-Cu alloy with a Zn content of 8% was subjected to solution treatment. The solution treatment process was as follows: treatment at 475±5℃ for 2 h, followed by cold water quenching. Then, the sample to be tested was prepared by wire electrical discharge machining. The sample dimensions are as follows. Figure 3 As shown.

[0061] S2. Clamp the sample onto the sample clamping structure 6, and spot weld the aluminum test wire and thermocouple wire using a spot welding machine. Confirm that the resistance meter and temperature meter are reading normally, and then fix the sample clamping structure 6 onto the upper flange 4 of the vertical high-temperature tubular resistance furnace to ensure fixation and positioning.

[0062] S3. Fix the high-temperature tubular resistance furnace onto the small-angle neutron scattering test platform, position the sample, and then evacuate to maintain a vacuum level of 10. 3 Within Pa. After setting the heating and cooling program, this embodiment performs non-isothermal aging treatment on the sample, with a heating rate of 0.5℃ / min, and continues to heat up to 220℃, while simultaneously collecting resistivity and temperature data and performing small-angle neutron tests.

[0063] S4. At this point, the phase transition test experiment was completed, and the small-angle neutron scattering data and resistivity change data of the sample during the non-isothermal aging process were successfully measured. Figure 5 These are some of the experimental results obtained. Among them, Figure 5 Figure (a) shows the resistivity as a function of temperature. Figure 5 Figure (b) shows the correlation results of small-angle neutron scattering intensity.

[0064] The obtained experimental data were analyzed and compared to determine whether the phase transition and precipitation behaviors were consistent. Figure 5 As shown in Figure (a), the resistivity difference (Δρ) of the Al-Zn-Mg-Cu alloy with 8% Zn content decreases with increasing temperature, indicating the precipitation of nano-phases in the alloy, and the increasing number of nano-phases with increasing temperature. Meanwhile, Figure 5 Similar results are reflected in the small-angle scattering data in Figure (b)—the peak in the curve gradually shifts to the left as the temperature increases, indicating that the size of the nanophase in the alloy increases with temperature.

[0065] Based on the above analysis and comparison, it can be seen that the small-angle neutron scattering data and resistivity data have good consistency. The test method of this invention can obtain the neutron scattering intensity distribution, resistivity and temperature change law at any time during the experimental test. Further analysis can obtain relevant quantitative information on the precipitation behavior of Al-Zn-Mg-Cu alloy with 8% Zn content during non-isothermal aging.

[0066] Example 4

[0067] The Al-Zn-Mg-Cu alloy with a Zn content of 10% was tested using the test platform of Example 1. The specific steps are as follows:

[0068] S1. An Al-Zn-Mg-Cu alloy with a Zn content of 10% was subjected to solution treatment. The solution treatment process was as follows: treatment at 475±5℃ for 2 h, followed by cold water quenching. Then, the sample to be tested was prepared by wire electrical discharge machining. The sample dimensions are as follows. Figure 3 As shown.

[0069] S2. Clamp the sample onto the sample clamping structure 6, and spot weld the aluminum test wire and thermocouple wire using a spot welding machine. Confirm that the resistance meter and temperature meter are reading normally, and then fix the sample clamping structure 6 onto the upper flange 4 of the vertical high-temperature tubular resistance furnace to ensure fixation and positioning.

[0070] S3. Fix the high-temperature tubular resistance furnace onto the small-angle neutron scattering test platform, position the sample, and then evacuate to maintain a vacuum level of 10. 3Within Pa. After setting the heating and cooling program, this embodiment performs non-isothermal aging treatment on the sample, with a heating rate of 0.5℃ / min, and continues to heat up to 220℃, while simultaneously collecting resistivity and temperature data and performing small-angle neutron tests.

[0071] S4. At this point, the phase transition test experiment was completed, and the small-angle neutron scattering data and resistivity change data of the sample during the non-isothermal aging process were successfully measured. Figure 6 These are some of the experimental results obtained. Among them, Figure 6 Figure (a) shows the resistivity as a function of temperature. Figure 6 Figure (b) shows the correlation results of small-angle neutron scattering intensity.

[0072] The obtained experimental data were analyzed and compared to determine whether the phase transition and precipitation behaviors were consistent. Figure 6 As shown in Figure (a), the resistivity difference (Δρ) of the Al-Zn-Mg-Cu alloy with a Zn content of 10% decreases with increasing temperature, indicating the precipitation of nanophases in the alloy, and the increasing number of nanophases with increasing temperature. Meanwhile, Figure 6 Similar results are reflected in the small-angle scattering data in Figure (b)—the peak in the curve gradually shifts to the left as the temperature increases, indicating that the size of the nanophase in the alloy increases with temperature.

[0073] Based on the above analysis and comparison, it can be seen that the small-angle neutron scattering data and resistivity data have good consistency. The test method of this invention can obtain the neutron scattering intensity distribution, resistivity and temperature change law at any time during the experimental test. Further analysis can obtain relevant quantitative information on the precipitation behavior of Al-Zn-Mg-Cu alloy with 10% Zn content during non-isothermal aging.

[0074] Example 5

[0075] The 3D-printed Inconel 718 high-temperature alloy was tested using the test platform of Example 1. The specific steps are as follows:

[0076] S1. The 3D-printed Inconel 718 high-temperature alloy was divided into two groups. The first group underwent no further treatment; the second group underwent solution treatment, which consisted of treatment at 1000±5℃ for 1 h followed by cold water quenching. Subsequently, both groups of samples were prepared for testing using wire electrical discharge machining (EDM). Sample dimensions are as follows... Figure 3 As shown.

[0077] S2. Clamp the sample onto the sample clamping structure 6, and spot weld the aluminum test wire and thermocouple wire using a spot welding machine. Confirm that the resistance meter and temperature meter are reading normally, and then fix the sample clamping structure 6 onto the upper flange 4 of the vertical high-temperature tubular resistance furnace to ensure fixation and positioning.

[0078] S3. Fix the high-temperature tubular resistance furnace onto the small-angle neutron scattering test platform, position the sample, and then evacuate the vacuum, maintaining a vacuum level of 10. 3 Within Pa. The heating and cooling programs were set. In this embodiment, the heat treatment process for the first group of samples was as follows: heating rate of 0.5 ℃ / min, heating to 1000 ℃, and holding for 1 h. The heat treatment process for the second group of samples was as follows: heating rate of 0.5 ℃ / min, heating to 1000 ℃, holding for 0.5 h, and then cooling at a rate of 0.5 ℃ / min.

[0079] S4. At this point, the phase transition test experiment was completed, and the small-angle neutron scattering data and resistivity change data of the sample during the heat treatment process were successfully measured. Figure 7 These are some of the experimental results obtained. Among them, Figure 7 Figure (a) shows the resistivity as a function of temperature. Figure 7 Figures (b) and (c) show the correlation results of small-angle neutron scattering intensity.

[0080] By processing and analyzing small-angle neutron scattering data and resistivity data, the distribution of neutron scattering intensity, resistivity, and temperature variation patterns at any time point during the experimental test can be obtained. Further analysis can yield quantitative information on the solid solution and precipitation of Inconel 718 high-temperature alloys in different states during heat treatment.

[0081] In summary, the test platform and method for in-situ monitoring of phase transformation and precipitation behavior during the heat treatment of metallic materials of the present invention, based on a self-designed and constructed synchronous in-situ measurement platform of "small-angle neutron scattering + resistivity", provides a new and reliable in-situ detection and analysis technology for in-situ tracking and quantitative analysis of phase transformation or precipitation behavior during the heat treatment of metallic materials.

[0082] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the above embodiments do not limit the present invention in any way, and all technical solutions obtained by equivalent substitution or equivalent transformation fall within the protection scope of the present invention.

Claims

1. A testing platform for in-situ monitoring of the heat treatment process of metallic materials, characterized in that, include: The sample environment control system provides a heat treatment environment for metallic materials and is equipped with a sample clamping structure, an optical entrance window, and an optical exit window. The small-angle neutron scattering system enables the testing of small-angle neutron scattering on metallic materials through the optical incident window and the optical exit window. The resistivity and temperature testing system is connected to the sample on the sample clamping structure via test leads, and is used to measure the resistance and temperature of metallic materials. The integrated control and acquisition system is connected to the small-angle neutron scattering system and the resistivity and temperature testing system to realize the acquisition and control of test data.

2. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 1, characterized in that, The sample environment control system is a vertical high-temperature tubular resistance furnace, which is also equipped with a vacuum pump or auxiliary atmosphere.

3. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 1, characterized in that, The resistivity and temperature testing system includes a resistance tester and a temperature tester.

4. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 2, characterized in that, The vertical high-temperature tubular resistance furnace has an optical incident window on its first side wall and an optical exit window on the opposite side of the first side wall. The sample clamping structure is located between the optical incident window and the optical exit window.

5. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 2, characterized in that, The vertical high-temperature tubular resistance furnace is equipped with a vent valve and a wire outlet at one end, and a pressure relief valve and a vacuum valve at the other end; the test leads of the resistance tester and temperature tester are fixedly connected to the sample through the wire outlet.

6. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 4, characterized in that, Both the optical incident window and the optical exit window are made of sapphire, and the optical exit channel between the sample clamping structure and the optical exit window is a trumpet-shaped structure with a smaller inner diameter and a larger outer diameter.

7. The testing platform for in-situ monitoring of the heat treatment process of metallic materials according to claim 4, characterized in that, The vertical high-temperature tubular resistance furnace is equipped with an upper flange and a lower flange at both ends, and a positioning structure is formed at the upper flange.

8. A testing method for in-situ monitoring of the heat treatment process of metallic materials using the testing platform described in any one of claims 1 to 7, characterized in that, The specific steps are as follows: S1. Prepare a sample of the material to be tested, the sample surface of which is flat; S2. Load the sample onto the sample clamping structure, spot weld the test wires and thermocouple wires to ensure normal readings of the resistance meter and temperature meter, and then fix the sample clamping structure to the upper flange of the vertical high temperature tubular resistance furnace and achieve positioning through the positioning structure. S3. Prepare the test environment according to the test requirements, set the temperature control program according to the heat treatment process, and after the temperature rises, monitor and record the resistivity and temperature in situ, and at the same time perform small-angle neutron scattering test. S4. Perform preliminary processing on the small-angle neutron scattering data and resistivity data to obtain the neutron scattering intensity distribution, resistivity and temperature change patterns at any time point during the experimental test, and analyze the relevant quantitative information on phase transition or precipitation of the sample during the heat treatment process.

9. The test method for in-situ monitoring of the heat treatment process of metallic materials according to claim 8, characterized in that, The test environment is a vacuum environment or a protective atmosphere.

10. The application of the in-situ monitoring test method for heat treatment of metallic materials as described in claim 8 in the collection of relevant quantitative information on precipitation behavior during non-isothermal aging of alloys.

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