Experimental device and experimental method for rapid quenching of radioactive sample

Abstract

The invention relates to the technical field of nuclear fuel circulation and irradiation effect research, and provides a radioactive sample rapid quenching experimental device and experimental method.The radioactive sample rapid quenching experimental device comprises a base and a furnace cover, and the base and the furnace cover define an experimental cavity; the base is in braking connection with a sample rod which is arranged in the experiment chamber and used for being detachably connected with a sample through a brake valve, the base is provided with a water inlet pipe communicated with the experiment chamber, an exhaust pipe and an air inlet pipe used for conveying inert gas, a port, in the experiment chamber, of the water inlet pipe faces the sample, and the base is provided with a blanking hole at the bottom of the experiment chamber; the base is provided with a switch valve at the position of the blanking hole, the base is provided with a water tank below the experimental chamber, and the furnace cover is provided with a heating element surrounding the experimental chamber and used for heating the sample, so that closed heating and multi-atmosphere protection of the radioactive sample are realized, different quenching modes are provided, the stability of the experimental environment is ensured, the operation in the shielding glove box is simplified, and the working efficiency is improved. And the experiment safety and efficiency are improved.

Description

Technical Field

[0001] This invention relates to the field of nuclear fuel cycle and irradiation effect research technology, and more specifically, to an experimental apparatus and method for rapid quenching of radioactive samples. Background Technology

[0002] As a crucial component of clean energy, the core prerequisite for the large-scale safe application of nuclear energy lies in breakthroughs in the performance of nuclear structural and functional materials. These materials must remain stable under extreme conditions such as strong radiation and high temperatures. Therefore, during the research and development phase, a series of heat treatment processes (such as quenching) must be used to simulate the service environment and optimize the microstructure to ensure the long-term reliable operation of nuclear facilities. However, nuclear materials carry extremely high radioactivity after irradiation, making heat treatment operations impossible in conventional environments. They must rely on enclosed protective spaces such as hot chambers or specially shielded glove boxes. This places special and urgent demands on the environmental adaptability, safety, and functionality of heat treatment equipment. In particular, the quenching process, as a critical step affecting the final performance of the material, directly determines the efficiency and safety of nuclear material research and development through the rationality of its equipment design.

[0003] Existing heat treatment equipment is mostly developed based on the processing needs of conventional non-radioactive materials, without fully considering the special limitations of handling radioactive samples. On the one hand, these devices are not structurally optimized for the spatial constraints of the hot chamber or shielded glove box. Most are too large and loosely laid out, making it difficult to fit into the limited operating space of the glove box, thus preventing the completion of the entire quenching process within the protective environment. On the other hand, the cooling functions of existing equipment have significant limitations, generally supporting only a single cooling method (such as air cooling or slow cooling only). If processes requiring high cooling rates, such as water quenching, are needed, it is often necessary to manually remove the high-temperature radioactive sample from the glove box or reach inside for close-range intervention. This process not only exposes operators to radiation risks but may also affect the quenching effect due to temperature fluctuations during sample transfer. Furthermore, contact between the high-temperature sample and air, or improper handling, can easily trigger the spread of radioactive aerosols, exacerbating environmental pollution risks. In addition, some devices lack the ability to precisely control the temperature and monitor the quenching process in real time, resulting in a large cooling response delay. This not only fails to meet the stringent requirements for cooling rate in nuclear material phase transition research, but also makes it difficult to compare the effects of different cooling paths under the same experimental conditions, leading to low comparability of experimental data and hindering the progress of nuclear material performance optimization and mechanism research. Summary of the Invention

[0004] The purpose of this invention is to provide an experimental apparatus and method for rapid quenching of radioactive samples, which solves the problems of existing nuclear material post-irradiation heat treatment equipment, such as single cooling method, poor operational safety, large cooling response delay, and low comparability of multi-path experiments.

[0005] This invention is achieved through the following technical solution: an experimental device for rapid quenching of radioactive samples, comprising an experimental furnace body disposed within a shielded glove box, the experimental furnace body comprising a base and a furnace cover, the base and the furnace cover forming an experimental chamber, the base being braked and connected by a sample rod disposed within the experimental chamber for detachable connection of the sample via a brake valve, the base being respectively provided with a water inlet pipe, a vacuum pipe and an inlet pipe for conveying inert gas communicating with the experimental chamber, the port of the water inlet pipe within the experimental chamber facing the sample, a material discharge hole being opened at the bottom of the experimental chamber on the base, a switch valve being installed at the material discharge hole on the base, a water tank being disposed below the experimental chamber on the base, and a heating element being disposed around the outside of the experimental chamber for heating the sample on the furnace cover.

[0006] Furthermore, the base is equipped with a lifting mechanism that connects to the furnace cover and is used to drive the furnace cover to move vertically up and down.

[0007] Furthermore, the sample rod is made of boron carbide ceramic material.

[0008] Furthermore, the furnace lid is made of transparent ceramic.

[0009] Furthermore, a sealing gasket is installed between the base and the furnace cover.

[0010] Furthermore, the top of the furnace lid is equipped with an infrared thermometer for detecting the temperature inside the experimental chamber and a barometer for detecting the air pressure inside the experimental chamber.

[0011] Furthermore, an exhaust pipe is connected to the upper part of the furnace cover, and the exhaust pipe is connected to a nuclear-grade filter via an exhaust fan.

[0012] An experimental method comprising the following steps: Step S1: Lift the furnace cover, fix the sample to the end of the sample rod through the operating hole of the shielded glove box, and fix the sample rod through the brake valve to seal the furnace cover and base. Step S2: Heat the experimental chamber to a preset temperature using a heating element and then maintain the temperature at a constant level; Step S3: After maintaining the temperature for the preset time, select the quenching method; When the jet cooling is applied, the water inlet pipe is turned on to connect the cooling water and spray it evenly onto the sample. During rapid water quenching, the switch valve is opened, triggering the brake valve and releasing the sample rod, allowing the sample to fall into the water tank. Step S4: Complete the quenching and remove the sample.

[0013] Furthermore, in step S2, if vacuum heating is to be performed, a vacuum mechanism is connected through the evacuation pipe to evacuate the vacuum; if inert gas protection heating is to be performed, argon gas is introduced through the inlet pipe.

[0014] Furthermore, in step S4, if the quenching method is jet cooling, the sample is removed using a long-handled tool after the air pressure in the experimental chamber returns to atmospheric pressure; if the quenching method is rapid water quenching, the sample is directly removed from the water tank using a long-handled tool.

[0015] The present invention has at least the following advantages and beneficial effects: (1) The base and furnace cover form a closed experimental chamber. The sample rod connected by the brake valve, the exhaust pipe connected to the experimental chamber, the inert gas inlet pipe, the water inlet pipe facing the sample, the material drop hole with switch valve at the bottom of the base and the water tank below, and the heating element surrounding the experimental chamber enable precise heating of radioactive samples in a closed environment, multi-atmosphere protection and jet cooling and rapid water quenching. It effectively prevents the leakage of radioactive aerosol, ensures temperature control accuracy and experimental environment stability, adapts to the quenching requirements of different nuclear materials, simplifies the operation inside the shielded glove box, and improves experimental safety and efficiency.

[0016] (2) By sealing the sample, heating to a constant temperature, selecting the quenching method according to the requirements, and then completing the sampling, the entire process of radioactive sample loading and sampling is safe and controllable, adapting to the cooling rate requirements of different samples, avoiding sample contamination and personnel radiation exposure risks during the experiment, and fully ensuring the reliability and nuclear safety requirements of nuclear material quenching experiments. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the experimental apparatus and method for rapid quenching of radioactive samples provided by the present invention.

[0018] Reference numerals: 1-Base, 10-Discharge hole, 11-Brake valve, 12-Water inlet pipe, 13-Exhaust pipe, 14-Air inlet pipe, 15-Switch valve, 2-Furnace cover, 20-Experimental chamber, 21-Heating element, 22-Exhaust pipe, 3-Sample, 4-Sample rod, 5-Water tank, 6-Lifting mechanism, 7-Infrared thermometer, 8-Pressure gauge. Detailed Implementation

[0019] The specific implementation method is described below with reference to the accompanying drawings.

[0020] Example like Figure 1 As shown in the figure, this embodiment mainly discloses an experimental device for rapid quenching of radioactive samples, which includes an experimental furnace body set in a shielded glove box. The experimental furnace body includes a base 1 and a furnace cover 2.

[0021] The base 1 and the furnace cover 2 together form an experimental chamber 20. The experimental chamber 20 is a closed chamber, which can prevent the aerosols and dust generated by the radioactive sample 3 during heating and quenching from leaking into the shielded glove box.

[0022] The base 1 is braked and connected to a sample rod 4, which is arranged inside the experimental chamber 20 and is used for detachable connection of the sample 3, via a brake valve 11. Specifically, the sample rod 4 is connected to the base 1 via the brake valve 11, which can precisely fix the sample 3 in the position inside the chamber, ensuring that the sample 3 is stably located in the heating area inside the experimental chamber 20. The sample 3 is detachably connected to the end of the sample rod 4 by a boron carbide screw. The brake valve 11 is a pneumatic brake valve 11 of the prior art, and its brake clamp at the actuation end locks and releases the sample rod 4, which is suitable for the limited operating space inside the shielded glove box.

[0023] The base 1 is equipped with a water inlet pipe 12, a vacuum pipe 13, and an inlet pipe 14 for transporting inert gas, all connected to the experimental chamber 20. The end of the water inlet pipe 12 inside the experimental chamber 20 faces the sample 3. The vacuum pipe 13 can be connected to an external vacuum system (such as a two-stage "molecular pump-mechanical pump") to achieve 10⁻ 5 The high vacuum of Pa meets the oxidation-free heating requirements of easily oxidized nuclei; the inlet pipe 14 can be connected to an external inert gas source to provide an inert protective atmosphere for the sample 3, preventing the sample 3 from reacting with oxygen and water vapor at high temperatures; the water inlet pipe 12 has its port directly facing the sample 3, allowing the cooling water to be precisely applied to the surface of the sample 3 during jet cooling, improving cooling efficiency and uniformity. This overcomes the limitation of traditional devices that can only heat in a single environment, expanding the applicable scenarios of the device.

[0024] The base 1 has a material discharge hole 10 at the bottom of the experimental chamber 20. A switch valve 15 is installed at the material discharge hole 10 on the base 1. A water tank 5 is set below the experimental chamber 20 on the base 1. The material discharge hole 10 at the bottom of the base 1, together with the switch valve 15, can quickly open the channel during quenching. The water tank 5 below directly receives the falling sample 3, realizing rapid cooling, avoiding the temperature loss of the sample 3 in the traditional manual transfer process, ensuring the consistency of the quenching effect, and reducing the operation steps in the shielded glove box, thus improving experimental efficiency.

[0025] The furnace cover 2 is equipped with a heating element 21 surrounding the experimental chamber 20 for heating the sample 3. The heating element 21 can be an induction heating resistance wire in the prior art, which surrounds the experimental chamber 20 to form a uniform heating field in the chamber, avoid local overheating or excessive temperature gradient, and ensure the accuracy of experimental data.

[0026] Furthermore, in a specific implementation, a lifting mechanism 6 is provided on the base 1 provided in the embodiment of the present invention, which is connected to the furnace cover 2 for driving the furnace cover 2 to rise and fall vertically. Specifically, the lifting mechanism 6 includes a guide rod and a lead screw, which are arranged vertically and parallel to each other. A drive motor is driven to the end of the lead screw, and a connecting block for connecting the furnace cover 2 is threaded to the lead screw. At the same time, the connecting block slides with the guide rod to limit the movement, thereby realizing the vertical rise and fall of the furnace cover 2 and reducing the complexity of operation. When loading samples, after the furnace cover 2 is raised, the sample rod 4 in the experimental chamber 20 is exposed, which makes it easier for long-handled tools to fix the sample 3. The same applies when taking samples, which reduces the frequency of contact between the operator and the device and reduces the risk of radioactive contamination.

[0027] Furthermore, in specific implementation, the sample rod 4 provided in the embodiments of the present invention is made of boron carbide ceramic material, which has the characteristics of high temperature resistance (can withstand high temperatures above 1500℃ and have a stable structure without deformation), neutron absorption capability (can reduce the radiation dose generated by the decay of radioactive sample 3 and is suitable for nuclear material experimental environment) and chemical inertness (resistant to corrosion by gas and quenching medium in experimental chamber 20 and does not react with sample 3 to contaminate sample 3). This ensures the stable use of sample rod 4 in high temperature experiments, avoids radioactive risks and sample 3 contamination problems, and is suitable for the quenching requirements of radioactive sample 3.

[0028] Furthermore, in specific implementations, the furnace cover 2 provided in this embodiment of the invention is made of transparent ceramic, which has good corrosion resistance and high-temperature stability. It is colorless and transparent, and can withstand continuous burning at 1500℃ or even higher temperatures without discoloration. The state of the sample 3 during heating can be observed from the outside through the transparent ceramic. In addition, a camera can be arranged next to the transparent ceramic to observe blind spots and record the state of the sample 3 during heating and isothermal treatment.

[0029] Furthermore, in specific implementation, a sealing gasket is provided between the base 1 and the furnace cover 2 provided in the embodiments of the present invention. Specifically, the upper edge of the base 1 and the lower edge of the furnace cover 2 can be stepped together to form a labyrinth seal; the sealing gasket can be set on the edge of the base 1 and / or the furnace cover 2, and the sealing gasket is pressed tightly by the gravity of the furnace cover 2 and the self-locking of the screw in the lifting mechanism 6, so as to avoid the leakage of radioactive aerosols and dust and reduce the radiation risk.

[0030] Furthermore, in a specific implementation, an infrared thermometer 7 for detecting the temperature inside the experimental chamber 20 and a pressure gauge 8 for detecting the gas pressure inside the experimental chamber 20 are provided at the top of the furnace cover 2 provided in this embodiment of the invention. Specifically, the infrared thermometer 7 adopts existing technology and monitors the temperature of the sample 3 in real time through a non-contact temperature measurement method and feeds it back to an external computer; the pressure gauge 8 adopts existing technology and can intuitively display the pressure of the experimental chamber 20 in real time, which is convenient for judging whether the vacuum degree meets the standard, whether the inert gas pressure is appropriate, etc., to ensure the accuracy and safety of the experiment.

[0031] Furthermore, in a specific implementation, an exhaust pipe 22 is connected to the upper part of the furnace cover 2 provided in the embodiment of the present invention, and the exhaust pipe 22 is connected to a nuclear-grade filter via an exhaust fan. The nuclear-grade filter can filter radioactive dust and aerosols generated during the heat treatment process, efficiently intercepting radioactive materials discharged from the experimental chamber 20; and preventing radioactive materials from entering the hot chamber and spreading and polluting the environment.

[0032] In this embodiment, an experimental method is also disclosed, including the following steps: Step S1: Lift the furnace cover 2, fix the sample 3 to the end of the sample rod 4 through the operation hole of the shielded glove box, and fix the sample rod 4 through the brake valve 11 to seal the furnace cover 2 and the base 1. Specifically, drive the furnace cover 2 vertically upward through the lifting mechanism 6 until the experimental chamber 20 is fully exposed. The operator uses long-handled tweezers through the special operation hole of the shielded glove box to accurately fix the radioactive sample 3 to be tested to the end of the sample rod 4.

[0033] Step S2: Heat the experimental chamber 20 to the preset temperature using the heating element 21 and maintain the temperature at a constant temperature. Adjust the environment of the experimental chamber 20 according to the characteristics of the sample 3. If the sample 3 is an easily oxidized nucleus material, vacuum heating is performed. Vacuum is then performed by connecting the vacuum mechanism through the evacuation pipe 13 to remove the air in the chamber. If inert gas protection is required, inert gas protection heating is performed by introducing argon gas through the inlet pipe 14 while monitoring the pressure gauge 8.

[0034] Step S3: After maintaining the temperature for the preset time, select the quenching method; When using jet cooling, turn on the water inlet pipe 12 to connect the cooling water and spray it evenly onto the sample 3. Jet cooling is suitable for sample 3 that is sensitive to cooling rate (e.g., brittle core material). It is necessary to avoid cracking due to excessive cooling. During rapid water quenching, the switch valve 15 is opened, triggering the brake valve 11 and releasing the sample rod 4, causing the sample 3 to fall into the water tank 5. Rapid water quenching is suitable for samples 3 that require high cooling rates (such as high-strength nuclear structural steel).

[0035] Step S4: Complete quenching and remove sample 3. Specifically, if the quenching method is jet cooling, wait for the air pressure in the experimental chamber 20 to return to atmospheric pressure before using a long-handled tool to remove sample 3; if the quenching method is rapid water quenching, directly use a long-handled tool to remove sample 3 from the water tank 5. After sampling, control the lifting mechanism 6 to lower the furnace cover 2, resealing the experimental chamber 20; turn on the exhaust fan and nuclear-grade filter of the exhaust pipe 22, using the nuclear-grade filter to filter the airflow, while simultaneously drying and venting the experimental chamber 20 to remove residual moisture or dust, preparing for the next experiment.

Claims

1. An experimental apparatus for rapid quenching of radioactive samples, comprising an experimental furnace body disposed within a shielded glove box, characterized in that, The experimental furnace body includes a base (1) and a furnace cover (2); The base (1) and the furnace cover (2) together form an experimental chamber (20). The base (1) is braked by a brake valve (11) to connect a sample rod (4) arranged in the experimental chamber (20) for detachable connection of the sample (3). The base (1) is respectively provided with a water inlet pipe (12), a gas extraction pipe (13) and a gas inlet pipe (14) for conveying inert gas, which are connected to the experimental chamber (20). The port of the water inlet pipe (12) in the experimental chamber (20) faces the sample (3). The base (1) has a material drop hole (10) at the bottom of the experimental chamber (20). The base (1) is equipped with a switch valve (15) at the material drop hole (10). The base (1) is provided with a water tank (5) below the experimental chamber (20). The furnace cover (2) is provided with a heating element (21) surrounding the experimental chamber (20) for heating the sample (3).

2. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, The base (1) is provided with a lifting mechanism (6) connected to the furnace cover (2) for driving the furnace cover (2) to rise and fall vertically.

3. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, The sample rod (4) is made of boron carbide ceramic material.

4. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, The furnace cover (2) is made of transparent ceramic.

5. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, A sealing gasket is provided between the base (1) and the furnace cover (2).

6. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, The top of the furnace cover (2) is equipped with an infrared thermometer (7) for detecting the temperature inside the experimental chamber (20) and a barometer (8) for detecting the air pressure inside the experimental chamber (20).

7. The experimental apparatus for rapid quenching of radioactive samples according to claim 1, characterized in that, The upper part of the furnace cover (2) is connected to an exhaust pipe (22), and the exhaust pipe (22) is connected to a nuclear-grade filter through an exhaust fan.

8. An experimental method for a rapid quenching experimental apparatus for radioactive samples according to any one of claims 1-7, characterized in that, Includes the following steps: Step S1: Lift the furnace cover (2), fix the sample (3) to the end of the sample rod (4) through the operation hole of the shielded glove box, and fix the sample rod (4) through the brake valve (11) to seal and fasten the furnace cover (2) to the base (1); Step S2: Heat the experimental chamber (20) to a preset temperature using the heating element (21) and maintain the temperature at a constant temperature; Step S3: After maintaining the temperature for the preset time, select the quenching method; When the jet is cooled, the water inlet pipe (12) is turned on to connect the cooling water and spray it evenly onto the sample (3); When rapid water quenching occurs, the switch valve (15) is opened, the brake valve (11) is triggered, the sample rod (4) is released, and the sample (3) falls into the water tank (5). Step S4: Complete the quenching and remove the sample (3).

9. The experimental method according to claim 8, characterized in that, In step S2, if vacuum heating is performed, the vacuum mechanism is connected through the evacuation pipe (13) to evacuate the vacuum; if inert gas protection heating is performed, argon gas is introduced through the inlet pipe (14).

10. The experimental method according to claim 8, characterized in that, In step S4, if the quenching method is jet cooling, the sample (3) is removed using a long-handled tool after the air pressure in the experimental chamber (20) is restored to atmospheric pressure; if the quenching method is rapid water quenching, the sample (3) is removed directly from the water tank (5) using a long-handled tool.

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