A material evolution process test system and method based on fast x-ray imaging

Abstract

A material evolution process testing system based on rapid X-ray imaging includes: a main chamber, a laser heating device, an infrared thermometer, a gas inlet device, and a gas outlet and measurement device. The main chamber is a sealed space, containing an upper clamping device and a lower clamping device. The test piece is clamped by the upper and lower clamping devices, which have high-precision synchronous rotation capabilities. Under the control of an external control system, the upper and lower clamping devices rotate at high speed synchronously together with the clamped test piece. Four laser heaters are evenly distributed around the test piece, forming an angle of approximately 45° with the X-ray imaging beam path. The infrared thermometer forms an angle of approximately 90° with the X-ray imaging beam path. A gas outlet and measurement device is located on the opposite side of the gas inlet device to export the generated gas from the reaction of the test piece under high-temperature conditions for chemical composition determination.

Description

Technical Field

[0001] This invention belongs to the field of aerospace materials oxidation and ablation, specifically relating to an experimental system and method for studying material evolution processes based on rapid X-ray imaging. Background Technology

[0002] C / SiC composites, C / C composites, SiC / SiC composites, phenolic resins, and resin-based composites possess excellent high-temperature mechanical properties and are widely used in aerospace, nuclear energy, and other fields. These materials face extremely harsh thermal environments during service, potentially leading to oxidation and ablation failure. Understanding the structural evolution of materials under extreme conditions and its relationship with chemical reactions is crucial for damage and failure mechanism analysis, process improvement and optimization design, and engineering applications. However, the structural evolution of materials under extreme conditions is very rapid, and they are also affected by strong light and radiation, making existing conventional testing methods difficult to implement.

[0003] Synchrotron X-rays are electromagnetic radiation emitted by relativistically charged particles traveling along curved orbits under the influence of electromagnetic fields. They possess characteristics such as continuous and wide-range spectra, high radiation intensity, high polarization, pulsed time structure, and high collimation, offering advantages such as high spatiotemporal resolution in imaging. By the end of 2025, my country will have completed four generations of synchrotron radiation sources: the Beijing Synchrotron Radiation Facility (Beijing Haidian, first generation), the Hefei Source (Anhui Hefei, second generation), the Shanghai Synchrotron Radiation Facility (Shanghai Pudong, third generation), and the High Energy Synchrotron Radiation Facility (Beijing Huairou, fourth generation). Among them, the 16U2 beamline of the Shanghai Synchrotron Radiation Facility and the Structural Dynamics beamline of the High Energy Synchrotron Radiation Facility have rapid X-ray imaging capabilities, achieving time-resolved imaging at hundreds of picoseconds or even higher.

[0004] Fast X-ray imaging can capture rapid evolution processes, overcome the effects of strong light and radiation, and can be combined with 3D reconstruction technology to obtain CT images. However, existing technologies cannot conduct oxidation and ablation tests on test specimens under extreme thermal environments and determine gas chemical composition using fast X-ray imaging, or perform fast X-ray imaging and gas chemical composition determination on test specimens under extreme thermal environments. Therefore, this invention overcomes the shortcomings of existing technologies and proposes an experimental system and method for studying the oxidation and ablation processes of materials based on fast X-ray imaging technology. This establishes the correlation between the structural evolution of material oxidation and ablation under extreme environments and chemical reactions, providing support for the analysis of material damage and failure mechanisms, process improvement and optimization design, and engineering applications. Summary of the Invention

[0005] To overcome the shortcomings of existing technologies, an experimental system and method based on rapid X-ray imaging for studying the oxidation and ablation processes of materials are proposed. The device simulates extreme environments such as ultra-high temperature during rapid X-ray imaging to obtain digital images of the material evolution process and assists in chemical composition testing, which is used to study the oxidation and ablation processes of materials under extreme conditions.

[0006] Working principle: A material evolution process test system based on rapid X-ray imaging, including: main chamber, laser heating device, infrared temperature measuring device, gas inlet device, and gas outlet and measuring device; The main chamber is a cylindrical, sealed space. All screw connections are sealed with sealing rings, and other seams are sealed with sealant to ensure good airtightness. The main chamber includes an upper clamping device and a lower clamping device. The test piece is clamped by the upper and lower clamping devices. The upper and lower clamping devices have a high-precision synchronous rotation function, with an error of no more than 0.01° per 360° rotation. Under the control of the external control system, the clamped test piece and the device rotate together at high speed, with a maximum speed of 3600° / s, which meets the requirements of high-speed CT imaging. The supporting structure of the annular side surface of the main body is made of a material that has a certain supporting strength while allowing X-rays, laser heating and infrared thermometry to pass through. Four 200W laser heaters and an infrared temperature measuring device are at the same horizontal level as the X-ray imaging area of ​​the test, that is, at the same horizontal height as the X-ray and the detector. The four laser heaters are evenly distributed around the test piece, forming an angle of about 45° with the X-ray imaging optical path, to ensure that the test piece is heated evenly without affecting the X-ray. The infrared thermometer forms an angle of approximately 90° with the X-ray imaging optical path. Through an external temperature control system, a closed-loop control feedback is formed between the infrared thermometer and the laser heating device. A gas inlet device is set on the opposite side of the infrared thermometer. In addition to controlling the introduction of air, oxygen, and inert gas to simulate the gas environment inside the main cabin, the gas inlet device also simulates the effect of high-speed scouring airflow. A gas outlet and measurement device is set on the opposite side of the gas inlet device to export the generated gas from the reaction of the test piece under high temperature environment and to measure its chemical composition.

[0007] Furthermore, acrylic material was chosen for the support structure of the main cabin.

[0008] Furthermore, the following steps are included: Step 1: Select a high-energy or medium-energy synchrotron radiation source X-ray imaging beamline as a fast X-ray imaging facility, install the material evolution process test system based on fast X-ray imaging on the optical platform of the fast X-ray imaging facility, and install the test specimen inside the main cabin. Step 2: Apply extreme environment to the test piece using the test system. As needed for the research, start the rapid X-ray imaging facility in a timely manner to carry out the imaging capture test process. If only two-dimensional imaging research is carried out, the upper clamping device and the lower clamping device do not need to start the rotation function. If three-dimensional imaging research is carried out, the upper clamping device and the lower clamping device will rotate synchronously with high precision. The specific parameters are determined according to the imaging parameters and research needs. The third step: The gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines the results with the X-ray images obtained during the test to study the oxidation and ablation process of materials under extreme conditions.

[0009] Furthermore, in the first step, the 16U2 synchrotron radiation source beamline was selected as the rapid X-ray imaging facility, and the test specimen was a C / SiC composite material. The second step also includes the following specific contents: applying a nitrogen inert gas environment to the test piece, and heating it to 1300°C using a laser heating device after the gas environment stabilizes to the specified oxygen content. The rapid X-ray imaging facility is then activated to perform the imaging capture test process, with an exposure time of 0.2ms in white light mode. The upper and lower clamping devices are controlled to perform high-precision synchronous rotation to acquire three-dimensional imaging projection images. The rotation speed is 0.1s per 180° rotation to acquire 500 projection images for reconstruction. After acquiring a set of CT projections after each 180° rotation, the rotation is paused for 10s before continuing, and so on, until the oxidation and ablation process is completed. The third step also includes the following specific content: the gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines it with the subsequent reconstructed X-ray CT images to carry out the study of the material oxidation and ablation process under extreme conditions. A series of three-dimensional CT images during the test show the structural evolution process of C / SiC composite material under extreme conditions, while gas measurement distinguishes the gases generated. At the same time, energy dispersive spectroscopy is further used to perform composition analysis on the C / SiC composite material residue after the test, and the correlation between structural evolution and chemical changes is comprehensively studied.

[0010] Furthermore, in the first step, a high-energy synchrotron radiation facility structural dynamics beamline is selected as a rapid X-ray imaging facility, and the C / C composite material test specimen to be tested is installed inside the main cabin. The second step also includes the following: using the test system to apply an argon inert gas environment to the test piece, and after the gas environment stabilizes to the specified oxygen content, heating it to 2000°C using a laser heater, starting the rapid X-ray imaging facility to perform the imaging capture test process, with an exposure time of 50µs in white light mode, and performing high-speed two-dimensional imaging acquisition until the oxidation and ablation process is completed. The third step also includes the following: the gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines it with two-dimensional X-ray images to study the oxidation and ablation process of materials under extreme conditions. A series of X-ray images during the test show the structural evolution process of C / C composite materials under extreme conditions, while gas measurement distinguishes the gases produced. At the same time, energy dispersive spectroscopy is further used to analyze the composition of the C / C composite material residues after the test, and the correlation between structural evolution and chemical changes is studied in a comprehensive manner.

[0011] The beneficial effects of this invention are as follows: An experimental system and method based on rapid X-ray imaging for studying the oxidation and ablation processes of materials can be used to visually characterize the structural evolution of materials under extreme environments. The experimental system based on rapid X-ray imaging can capture the dynamic processes of ablation and oxidation of materials under extreme environments through two-dimensional or three-dimensional imaging, visually demonstrating these processes.

[0012] A novel experimental system and method based on rapid X-ray imaging for studying the oxidation and ablation processes of materials can support the study of chemical reactions in materials under extreme environments, helping to establish the correlation between chemical reactions and structural evolution. The developed experimental system can analyze the chemical composition of gases generated during the oxidation or ablation of materials under extreme environments, further establishing the correlation between the structural evolution of materials under extreme conditions and chemical reactions. Attached Figure Description

[0013] Figure 1 It is a forward oblique view of the system.

[0014] Figure 2 This is a top view of the test system.

[0015] Figure 3 This is a side view of the system.

[0016] The components include: 1. Main cabin; 2. Laser heating device; 3. Infrared temperature measuring device; 4. Gas inlet device; 5. Gas outlet and measuring device; 6. Upper clamping device; 7. Lower clamping device; 8. Test piece; 9. Support structure; 10. X-ray; and 11. Detector. Detailed Implementation

[0017] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection claimed by the present invention.

[0018] Example 1 A material evolution process test system based on rapid X-ray imaging includes a main chamber 1, a laser heating device 2, an infrared temperature measuring device 3, a gas inlet device 4, and a gas outlet and measuring device 5. The main chamber 1 is a sealed space. All screw connections are sealed with sealing rings, and other joints are sealed with sealant to ensure good airtightness. The main chamber 1 includes an upper clamping device 6 and a lower clamping device 7. The test piece 8 is clamped by the upper clamping device 6 and the lower clamping device 7. The upper clamping device 6 and the lower clamping device 7 have a high-precision synchronous rotation function. The error of each 360° rotation does not exceed 0.01°. Under the control of the external control system, the test piece 8 and the clamped device 7 rotate together at high speed. The fastest speed can reach 3600° / s, which meets the requirements of high-speed CT imaging. The supporting structure 9 of the main body 1 needs to be selected with a certain supporting strength, and at the same time, it needs to be made of materials that allow X-rays 10, laser heating and infrared thermometry to pass through. The four 200W laser heaters 2, the infrared temperature measuring device 3 and the X-ray imaging area of ​​the test piece 8 are on the same horizontal direction, that is, at the same horizontal height as X-ray 10 and detector 11. The four laser heaters 2 are evenly distributed around the test piece 8, forming an angle of about 45° with the imaging optical path of X-ray 10, which can ensure that the test piece is heated evenly, while not affecting the X-ray. The infrared temperature measuring device 3 forms an angle of approximately 90° with the X-ray imaging optical path of the X-ray 10. Through an external temperature control system, a closed-loop control feedback is formed between the infrared temperature measuring device 3 and the laser heating device 2. A gas inlet device 4 is set on the opposite side of the infrared temperature measuring device 3. In addition to controlling the introduction of air, oxygen and inert gas to simulate the gas environment inside the main cabin 1, the gas inlet device 4 also simulates the effect of high-speed scouring airflow. A gas outlet and measuring device 5 is set on the opposite side of the gas inlet device 4 to outlet the generated gas of the test piece reaction under high temperature environment and to measure the chemical composition.

[0019] The supporting structure 9 of the main cabin 1 must be made of acrylic material, which has a certain supporting strength and can allow X-rays 10, laser heating and infrared thermometry to pass through.

[0020] An experimental method for studying the oxidation and ablation processes of materials based on rapid X-ray imaging, utilizing a developed experimental system for studying the oxidation and ablation processes of materials under extreme conditions, combined with rapid X-ray imaging facilities, specifically includes the following steps: (3) Select a high-energy or medium-energy synchrotron radiation source X-ray imaging beamline as a fast X-ray imaging facility, install the material evolution process test system based on fast X-ray imaging on the optical platform of the fast X-ray imaging facility, and install the test specimen to be tested inside the main cabin 1. (4) The experimental system based on rapid X-ray imaging for studying the oxidation and ablation process of materials is developed to apply extreme environment to the test piece. According to the research needs, the rapid X-ray imaging facility is activated in time to carry out the imaging capture test process. If only two-dimensional imaging research is carried out, the upper clamping device 6 and the lower clamping device 7 do not need to activate the rotation function. If three-dimensional imaging research is carried out, the upper clamping device 6 and the lower clamping device 7 will rotate synchronously with high precision. The specific parameters are determined according to the imaging parameters and research needs. (5) Gas extraction and measurement device 5 performs chemical composition analysis on the gas components during the test process, and conducts research on the oxidation and ablation process of materials under extreme conditions in conjunction with the X-ray images obtained during the test.

[0021] Example 2 The study of material oxidation and ablation processes under extreme environments includes the following steps: (1) The Shanghai Synchrotron Radiation Facility 16U2 beamline was selected as the fast X-ray imaging facility. The experimental system developed in step one based on fast X-ray imaging to study the oxidation and ablation process of materials was installed on the optical platform of the fast X-ray imaging facility. The C / SiC composite material test specimen to be tested was installed in the main cabin (1). (2) Using the experimental system developed in step one for studying the oxidation and ablation process of materials based on rapid X-ray imaging, nitrogen inert gas environment is applied to the test piece. After the gas environment stabilizes to the specified oxygen content, the laser heating device 2 is used to heat it to 1300℃. The rapid X-ray imaging facility is started to carry out the imaging capture test process. The exposure time in white light mode is 0.2ms. The upper clamping device 6 and the lower clamping device 7 are controlled to perform high-precision synchronous rotation to acquire three-dimensional imaging projection images. The rotation speed is 0.1s to rotate 180° to acquire 500 projection images for reconstruction. After acquiring a set of CT projections after each 180° rotation, the rotation is paused for 10s and then continued. This process is repeated until the oxidation and ablation process is completed. (3) Gas extraction and measurement device 5 performs chemical composition analysis on the gas components during the test process. Combined with the later reconstructed X-ray CT images, it conducts research on the oxidation and ablation process of materials under extreme conditions. A series of three-dimensional CT images during the test process show the structural evolution process of C / SiC composite material under extreme conditions, while gas measurement distinguishes the gases generated. At the same time, energy dispersive spectrometer is used to further analyze the composition of C / SiC composite material residues after the test, and comprehensively study the relationship between structural evolution and chemical changes.

[0022] Example 3 The study of material oxidation and ablation processes under extreme environments includes the following steps: (1) The structural dynamics beamline of the High Energy Synchrotron Radiation Facility (HEPS) in Huairou, Beijing was selected as the fast X-ray imaging facility. The experimental system based on fast X-ray imaging to study the oxidation and ablation process of materials was installed on the optical platform of the fast X-ray imaging facility, and the C / C composite material test specimen to be tested was installed in the main cabin 1. (2) Using the test system based on rapid X-ray imaging to study the oxidation and ablation process of materials, an argon inert gas environment is applied to the test piece. After the gas environment stabilizes to the specified oxygen content, it is heated to 2000℃ using a laser heater. The rapid X-ray imaging facility is started to carry out the imaging capture test process. The exposure time is 50u in white light mode. High-speed two-dimensional imaging acquisition is carried out until the oxidation and ablation process is completed. (3) Gas extraction and measurement device 5 performs chemical composition analysis on the gas components during the test process, and conducts research on the oxidation and ablation process of materials under extreme conditions in combination with two-dimensional X-ray images. A series of X-ray images during the test process show the structural evolution process of C / C composite material under extreme conditions, while gas measurement distinguishes the gas generated in the reaction. At the same time, energy dispersive spectrometer is used to further analyze the composition of C / C composite material residues after the test, and comprehensively study the relationship between structural evolution and chemical changes.

[0023] The above description of the disclosed embodiments enables those skilled in the art to make or use the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the scope of the invention. Therefore, the invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A material evolution process experimental system based on rapid X-ray imaging, characterized in that, include: Main cabin, laser heating device, infrared temperature measuring device, gas inlet device, gas outlet and measuring device; The main chamber is a cylindrical, sealed space. All screw connections are sealed with sealing rings, and other seams are sealed with sealant to ensure good airtightness. The main chamber includes an upper clamping device and a lower clamping device. The test piece is clamped by the upper and lower clamping devices. The upper and lower clamping devices have a high-precision synchronous rotation function, with an error of no more than 0.01° per 360° rotation. Under the control of the external control system, the clamped test piece and the device rotate together at high speed, with a maximum speed of 3600° / s, which meets the requirements of high-speed CT imaging. The supporting structure of the annular side surface of the main body is made of a material that has a certain supporting strength while allowing X-rays, laser heating and infrared thermometry to pass through. Four 200W laser heaters and an infrared temperature measuring device are at the same horizontal level as the X-ray imaging area of ​​the test, that is, at the same horizontal height as the X-ray and the detector. The four laser heaters are evenly distributed around the test piece, forming an angle of about 45° with the X-ray imaging optical path, to ensure that the test piece is heated evenly without affecting the X-ray. The infrared thermometer forms an angle of approximately 90° with the X-ray imaging optical path. Through an external temperature control system, a closed-loop control feedback is formed between the infrared thermometer and the laser heating device. A gas inlet device is set on the opposite side of the infrared thermometer. In addition to controlling the introduction of air, oxygen, and inert gas to simulate the gas environment inside the main cabin, the gas inlet device also simulates the effect of high-speed scouring airflow. A gas outlet and measurement device is set on the opposite side of the gas inlet device to export the generated gas from the reaction of the test piece under high temperature environment and to measure its chemical composition.

2. The material evolution process testing system according to claim 3, characterized in that, The main cabin's supporting structure is made of acrylic material.

3. A method for testing material evolution processes based on rapid X-ray imaging, characterized in that, Includes the following steps: Step 1: Select a high-energy or medium-energy synchrotron radiation source X-ray imaging beamline as a fast X-ray imaging facility, install the material evolution process test system based on fast X-ray imaging on the optical platform of the fast X-ray imaging facility, and install the test specimen inside the main cabin. Step 2: Apply extreme environment to the test piece using the test system. As needed for the research, start the rapid X-ray imaging facility in a timely manner to carry out the imaging capture test process. If only two-dimensional imaging research is carried out, the upper clamping device and the lower clamping device do not need to start the rotation function. If three-dimensional imaging research is carried out, the upper clamping device and the lower clamping device will rotate synchronously with high precision. The specific parameters are determined according to the imaging parameters and research needs. The third step: The gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines the results with the X-ray images obtained during the test to study the oxidation and ablation process of materials under extreme conditions.

4. The experimental method for material evolution process according to claim 3, characterized in that, The first step selects the 16U2 synchrotron radiation source beamline as the fast X-ray imaging facility, and the test specimen is a C / SiC composite material. The second step also includes the following specific contents: applying a nitrogen inert gas environment to the test piece, and heating it to 1300°C using a laser heating device after the gas environment stabilizes to the specified oxygen content. The rapid X-ray imaging facility is then activated to perform the imaging capture test process, with an exposure time of 0.2ms in white light mode. The upper and lower clamping devices are controlled to perform high-precision synchronous rotation to acquire three-dimensional imaging projection images. The rotation speed is 0.1s per 180° rotation to acquire 500 projection images for reconstruction. After acquiring a set of CT projections after each 180° rotation, the rotation is paused for 10s before continuing, and so on, until the oxidation and ablation process is completed. The third step also includes the following specific content: the gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines it with the subsequent reconstructed X-ray CT images to carry out the study of the material oxidation and ablation process under extreme conditions. A series of three-dimensional CT images during the test show the structural evolution process of C / SiC composite material under extreme conditions, while gas measurement distinguishes the gases generated. At the same time, energy dispersive spectroscopy is further used to perform composition analysis on the C / SiC composite material residue after the test, and the correlation between structural evolution and chemical changes is comprehensively studied.

5. The experimental method for material evolution process according to claim 3, characterized in that, The first step involves selecting the structural dynamics beamline of the high-energy synchrotron radiation facility as a rapid X-ray imaging facility and installing the C / C composite material test specimen to be tested inside the main cabin. The second step also includes the following: using the test system to apply an argon inert gas environment to the test piece, and after the gas environment stabilizes to the specified oxygen content, heating it to 2000°C using a laser heater, starting the rapid X-ray imaging facility to perform the imaging capture test process, with an exposure time of 50µs in white light mode, and performing high-speed two-dimensional imaging acquisition until the oxidation and ablation process is completed. The third step also includes the following: the gas extraction and measurement device performs chemical composition analysis on the gas components during the test, and combines it with two-dimensional X-ray images to study the oxidation and ablation process of materials under extreme conditions. A series of X-ray images during the test show the structural evolution process of C / C composite materials under extreme conditions, while gas measurement distinguishes the gases produced. At the same time, energy dispersive spectroscopy is further used to analyze the composition of the C / C composite material residues after the test, and the correlation between structural evolution and chemical changes is studied in a comprehensive manner.

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