Preparation method and device of nickel-manganese alloy resistant to high-temperature liquid lithium corrosion

Abstract

The invention relates to the technical field of alloy preparation, and discloses a preparation method and device of nickel-manganese alloy resistant to high-temperature liquid lithium corrosion, and the nickel-manganese alloy preparation device comprises a shell, a cover body, a heating assembly, a stirring assembly, a raw material bin, a vacuum assembly, an inflation assembly and the like. A cavity is formed in the shell, and an opening communicated with the cavity is formed in one end of the shell; the cover body is arranged at the opening end of the shell and is detachably and fixedly mounted and connected with the shell, and the cover body and the cover body are enclosed to form a synthesis cavity; the nickel elementary substance powder and the manganese powder are fed into the high-temperature liquid lithium melt to be dissolved and mixed to form the nickel-manganese alloy, so that the nickel-manganese alloy can obtain excellent lithium corrosion resistance and can be used as a corrosion-resistant material in a high-temperature liquid lithium and lithium alloy environment in engineering systems such as a nuclear fusion reactor.

Description

Technical Field

[0001] The invention relates to the technical field of alloy preparation, and in particular to a method and device for preparing a nickel-manganese alloy resistant to high-temperature liquid lithium corrosion. Background Art

[0002] Magnetic confinement controlled nuclear fusion is one of the important ways to solve human energy and environmental problems. With the continuous upgrading of fusion devices, the interaction between plasma and the wall material facing the plasma (first wall) has gradually become stronger. The first wall material now has two main branches. One is the traditional solid material, mainly beryllium and carbon-based materials; the other is liquid metal, mainly lithium, lithium-lead alloy and lithium-tin alloy. Compared with traditional solid materials, liquid lithium as the first wall material has the following advantages: (1) Lithium is a low-Z material and has good compatibility with plasma; (2) Liquid lithium can withstand 50MW / m 2 heat load; (3) liquid lithium can be continuously renewed and has self-repair capabilities; (4) the flowing liquid lithium can take away heat and protect the high-Z solid wall behind it; (5) lithium atoms can react with fusion neutrons to produce tritium, playing the role of automatic feeding.

[0003] Although liquid lithium has many advantages, lithium is a chemically active alkaline element and is highly corrosive at high temperatures. Commonly used metals such as austenitic stainless steel (304, 316L and 310S stainless steel, etc.), low-activation steel (CLF and CLAM), tungsten-based alloys, molybdenum alloys, etc. will selectively dissolve their components in liquid lithium and chemically react to cause intergranular corrosion, pitting corrosion, etc., which damages the mechanical properties of the components made of the above materials and changes the physical properties of liquid lithium, resulting in unpredictable operating risks and economic losses. Therefore, the development and application of high-temperature resistant liquid lithium and lithium alloy corrosion materials are very important for the development of nuclear fusion reactors.

[0004] SUMMARY OF THE INVENTION

[0005] The technical problem solved by the present invention is to provide an alloy material resistant to corrosion by high-temperature liquid lithium and lithium alloys.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A method for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion comprises the following steps:

[0008] Starting the vacuum assembly to evacuate the synthesis chamber;

[0009] The heating assembly is started to heat the synthesis chamber, and after heating to 800° C., the exhaust process is maintained for 12 hours;

[0010] Turn off the vacuum assembly and heating assembly and cool to room temperature;

[0011] Inert gas is introduced into the synthesis chamber and the raw material bin, and the lithium ingot is placed in the synthesis chamber under the protective atmosphere of the inert gas, and the nickel powder and the manganese powder are placed in the corresponding raw material bins respectively;

[0012] The heating component is started to heat the synthesis chamber to melt the lithium ingot, and then the temperature in the synthesis chamber is adjusted to 500° C.

[0013] Turn on the switch of the raw material bin to send nickel powder and manganese powder into the synthesis chamber;

[0014] Turning on the stirring component to promote the synthesis of nickel powder and manganese powder in the molten lithium solution to form a nickel-manganese alloy;

[0015] After stirring for 5 hours, stop stirring, and after standing for 12 hours, turn off the heating component and cool to room temperature;

[0016] The cover of the synthesis chamber is opened, the solidified lithium is cleaned off with alcohol, and then the synthesized nickel-manganese alloy is taken out.

[0017] In one embodiment of the present invention, after heating and during the process of maintaining the vacuum, the entire preparation device is leak tested to ensure that the overall leakage rate is less than 1.0*10 -9 Pam 3 / s.

[0018] A preparation device for a nickel-manganese alloy resistant to high temperature liquid lithium corrosion, used to implement the above preparation method, comprising:

[0019] A shell, wherein a cavity is formed in the shell, and an opening communicating with the cavity is provided at one end of the shell;

[0020] A cover body, which is arranged at the open end of the shell and is detachably fixedly connected to the shell, and is enclosed with the cover body to form a synthetic chamber;

[0021] A heating component, the heating component is used to heat the synthesis chamber;

[0022] A stirring assembly, the stirring assembly comprising a power source and a stirring rod, the power source drivingly connected to the stirring rod, one end of the stirring rod passing through the cover body and disposed in the synthesis chamber;

[0023] A plurality of raw material bins, each of which is connected to the cover body and can communicate with the synthesis chamber;

[0024] A vacuum component, which can be in communication with the synthesis chamber and is used to evacuate the synthesis chamber;

[0025] An inflation component, wherein the inflation component can be communicated with the synthesis chamber and is used for filling the synthesis chamber with an inert gas.

[0026] In one embodiment of the present invention, the cavity is a columnar structure.

[0027] In one embodiment of the present invention, the cavity is in a cylindrical structure.

[0028] In one embodiment of the present invention, the open end of the shell is connected to the cover body via a knife-edge flange.

[0029] In one embodiment of the present invention, the cover body is a multifunctional flange.

[0030] In one solution of the present invention: a temperature sensor is provided on the shell, and the temperature sensor is connected to a temperature controller, and the temperature controller is used to control the start and stop of the heating component.

[0031] In one embodiment of the present invention, the inert gas is argon.

[0032] Beneficial effects of the present invention:

[0033] The present application provides a nickel-manganese alloy preparation device and preparation method, which forms a nickel-manganese alloy by feeding nickel element powder and manganese powder into a high-temperature liquid lithium melt to dissolve and mix, so that the nickel-manganese alloy can obtain excellent lithium corrosion resistance and can be used as a corrosion-resistant material in high-temperature liquid lithium and lithium alloy environments in engineering systems such as nuclear fusion reactors.

[0034] Additional aspects and advantages of the present invention will be given in part in the following description and in part will be obvious from the following description, or will be learned through practice of the present invention. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] The above and / or additional aspects and advantages of the present invention will become apparent and easily understood from the description of the embodiments in conjunction with the following drawings, in which:

[0036] Figure 1 It is a schematic structural diagram of the preparation device of the present invention.

[0037] The reference numerals in the figure are: 1. shell; 2. cover; 3. heating component; 4. stirring component; 5. raw material bin; 6. vacuum component; 7. inflation component; 8. temperature controller. DETAILED DESCRIPTION

[0038] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0039] In the description of the present invention, it should be understood that descriptions involving orientations, such as up, down, front, back, left, right, etc., and orientations or positional relationships indicated are based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0040] In the description of the present invention, "several" means one or more, "more" means more than two, "greater than", "less than", "exceed" etc. are understood as not including the number itself, and "above", "below", "within" etc. are understood as including the number itself. If there is a description of "first" or "second", it is only used for the purpose of distinguishing the technical features, and cannot be understood as indicating or implying the relative importance or implicitly indicating the number of the indicated technical features or implicitly indicating the order of the indicated technical features.

[0041] See also Figure 1 The present invention is a preparation device for a nickel-manganese alloy resistant to high-temperature liquid lithium corrosion, comprising a shell 1, a cover 2, a heating component 3, a stirring component 4, a raw material bin 5, a vacuum component 6, and an inflation component 7. The shell 1 has a cavity, and the upper end of the shell 1 has an opening connected to the cavity; the cover 2 is arranged at the open end of the shell 1 and is detachably fixedly connected to the shell 1, and is enclosed with the cover 2 to form a synthesis chamber; the cavity can be a columnar structure. Specifically, the cavity can be a cylindrical structure. The synthesis chamber can be set as a cylindrical structure with a length of 500mm, an outer diameter of 110mm, and an inner diameter of 100mm.

[0042] See also Figure 1 In one embodiment of the present invention, the opening of the shell 1 can be sealed by a knife-edge flange and can be used for connection with the cover 2. The cover 2 can be a multifunctional flange. The top of the cover 2 can be provided with two CF16 flange interfaces for connection with the raw material bin 5; the top center of the cover 2 can be provided with another CF35 flange interface for subsequent connection with the stirring bracket. A pipeline connected to the synthesis chamber can be provided on the side of the cover 2, and a CF16 flange interface can be welded on the end of the pipeline away from the cover 2 for subsequent connection with the vacuum component 6 and the exhaust component.

[0043] See also Figure 1In one embodiment of the present invention, the heating component 3 is used to heat the synthesis chamber; the heating component 3 may include an electric heating structure, or other heating structures may be selected as needed. As an example, the heating component 3 may include an electric heating wire arranged around the shell 1 and a heating power supply for power supply. An insulation layer may be arranged on the outside of the shell 1 to enclose the heating chamber. The shell 1 is located in the heating chamber to ensure the heating effect, and at the same time, it can play a protective and heat-insulating role to reduce heat loss. The device may also include a heating control component, which may include a temperature controller 8 and a temperature sensor arranged on the shell 1. The temperature sensor may be a thermocouple or other types of sensors used to detect the temperature in the synthesis chamber, and the temperature controller 8 is used to adjust the power of the heating component 3 to regulate the temperature in the synthesis chamber. Furthermore, a paperless recorder may be provided to record relevant temperature data.

[0044] See also Figure 1 In one embodiment of the present invention, the stirring assembly 4 includes a power source and a stirring rod, the power source drives the stirring rod, and the power source can be a servo motor connected to a DC power supply. An air device or a control switch can be provided on it to control the start and stop of the stirring assembly 4. The end of the stirring rod away from the power source passes through the cover 2 and is arranged in the synthesis chamber; specifically, the stirring rod can include a vertical rod and a horizontal rod, the vertical rod can be used as a stirring shaft connected to the power source, the horizontal rod can include a plurality of support rods distributed around the vertical rod and fixedly connected to the vertical rod, and the other end of the support rod is connected to a round rod. That is, the round rod forms a circular structure around several support rods. The round rod and the support rod are in the same plane, and the plane can be tilted, that is, the angle between the plane where the round rod is located and the vertical rod is less than 90°. In this way, the vertical rod can drive the materials at different heights above and below to stir in the process of driving the horizontal rod to rotate, thereby promoting the effect of alloy mixing and synthesis. Ensure the uniformity and quality of the alloy. A stirring frame can be connected to the cover 2 through a CF35 flange interface to ensure the stability of the stirring assembly 4.

[0045] See also Figure 1 In one embodiment of the present invention, a plurality of raw material bins 5 are connected to the cover 2 and can communicate with the synthesis chamber; specifically, the raw material bin 5 can be arranged above the synthesis chamber, a tube body can be arranged at the lower end of the raw material bin 5 and a CF16 flange can be welded for subsequent connection with the cover 2, and a control valve is arranged on the tube body for controlling the on-off of the tube body. As an example, the raw material bin 5 can be a cylindrical structure with a length of 300 mm, an outer diameter of 40 mm, an inner diameter of 35 mm and a knife-edge flange sealing, so as to be used to contain nickel powder and manganese powder respectively.

[0046] See also Figure 1 In one embodiment of the present invention, the vacuum component 6 can be connected to the synthesis chamber to evacuate the synthesis chamber; the vacuum component 6 can include a molecular pump group, a mass spectrometer and a pipeline for connecting the cover body 2, and a valve is provided on the pipeline for controlling the on-off. The inflation component 7 can be connected to the synthesis chamber to fill the synthesis chamber with an inert gas. The inflation component 7 can include a gas cylinder, a pressure reducing valve and a pipeline for connecting the cover body 2, and a valve is provided on the pipeline for controlling the on-off. A protective atmosphere can be formed by the inert gas during the process of adding materials to avoid the introduction of impurities. As an example, the inert gas can be argon.

[0047] Working principle of the present invention:

[0048] That is, the method for preparing a nickel-manganese alloy resistant to high-temperature liquid lithium corrosion using the above-mentioned device includes the following steps: First, assemble the preparation device used in this application and prepare relevant materials. Start the vacuum component 6 to evacuate the synthesis chamber; the evacuation process can be carried out at normal temperature / room temperature, and the room temperature environment is the temperature of the environment in which the equipment is located, and the same applies below. Specifically, the room temperature can refer to a temperature range between 15°C and 25°C, and the user can operate the specific temperature value according to needs.

[0049] While performing the evacuation (vacuuming) step, the heating component 3 is started to heat the synthesis chamber. The heating process is monitored and regulated by the heating control component. After the synthesis chamber is heated to 800°C, the evacuation process is maintained for 12 hours; thereby ensuring the vacuuming effect and avoiding residual gas and impurities that affect the subsequent preparation process. During the evacuation process, the entire preparation device is leak-checked to ensure that the overall leakage rate is less than 1.0*10 -9 Pam 3 / s. The leak detection process can be performed multiple times during the heating and maintaining the exhaust process.

[0050] After heating, vacuuming and leak detection are completed, the vacuum component 6 and the heating component 3 are closed, the vacuuming and heating are stopped, and the mixture is cooled to room temperature; the valve of the inflation system is opened, and the valve of the raw material bin 5 is opened, and inert gas is introduced into the synthesis chamber and the raw material bin 5, and the lithium ingot is placed in the synthesis chamber under the protective atmosphere of the inert gas, and the nickel powder and manganese powder are placed in the corresponding raw material bins 5 respectively.

[0051] After adding the raw materials, start the heating component 3 to heat the synthesis chamber to promote the melting of the lithium ingot to form a lithium melt, and then adjust the temperature in the synthesis chamber to 500°C and maintain a constant temperature; while keeping the temperature, turn on the switch of the raw material bin 5 to send nickel powder and manganese powder into the synthesis chamber, so that the nickel powder and manganese powder are dissolved in the liquid lithium; while adding the nickel powder and manganese powder raw materials, turn on the stirring component 4 to promote the synthesis of nickel powder and manganese powder in the molten lithium solution to form a nickel-manganese alloy; stop stirring after stirring for 5 hours, turn off the heating component 3 after standing for 12 hours, and cool to room temperature; after the synthesis chamber is cooled to room temperature, open the cover 2 of the synthesis chamber, because the nickel-manganese alloy is insoluble in alcohol, and use alcohol to wash away the solidified lithium, and then take out the synthesized nickel-manganese alloy.

[0052] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made according to the scope of application of the present invention should still fall within the scope of the claims of the present invention.

Claims

1. A method for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion, characterized in that: The steps include: Starting the vacuum component (6) to evacuate the synthesis chamber; The heating component (3) is started to heat the synthesis chamber, and after heating to 800° C., the exhaust process is maintained for 12 hours; Turn off the vacuum assembly (6) and the heating assembly (3), and cool to room temperature; Inert gas is introduced into the synthesis chamber and the raw material bin (5), and a lithium ingot is placed in the synthesis chamber under the protective atmosphere of the inert gas, and nickel powder and manganese powder are placed in corresponding raw material bins (5); Starting the heating component (3) to heat the synthesis chamber to promote the melting of the lithium ingot, and then regulating the temperature in the synthesis chamber to 500° C. for insulation; The switch of the raw material bin (5) is turned on to feed nickel powder and manganese powder into the synthesis chamber; Turning on the stirring assembly (4) to promote the synthesis of nickel powder and manganese powder in the molten lithium solution to form a nickel-manganese alloy; After stirring for 5 hours, the stirring was stopped, and after standing for 12 hours, the heating component (3) was turned off and the mixture was cooled to room temperature; The cover (2) of the synthesis chamber is opened, the solidified lithium is cleaned off with alcohol, and then the synthesized nickel-manganese alloy is taken out.

2. The method for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 1, characterized in that: After heating and maintaining the process of pumping, the entire preparation device is leak tested to ensure that the overall leakage rate is less than 1.0*10 -9 Pam 3 / s.

3. A device for implementing the method for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to any one of claims 1 to 2, characterized in that: include: A shell (1), wherein a cavity is provided in the shell (1), and an opening communicating with the cavity is provided at one end of the shell (1); A cover body (2), the cover body (2) being arranged at the open end of the shell (1) and being detachably fixedly connected to the shell (1), and enclosing the cover body (2) to form a synthetic chamber; A heating component (3), the heating component (3) being used to heat the synthesis chamber; A stirring assembly (4), the stirring assembly (4) comprising a power source and a stirring rod, the power source drivingly connected to the stirring rod, one end of the stirring rod passing through the cover (2) and arranged in the synthesis chamber; A plurality of raw material bins (5), wherein the raw material bins (5) are connected to the cover body (2) and are capable of communicating with the synthesis chamber; A vacuum component (6), the vacuum component (6) being able to communicate with the synthesis chamber and being used to evacuate the synthesis chamber; An inflation component (7), wherein the inflation component (7) can be in communication with the synthesis chamber and is used to fill the synthesis chamber with an inert gas.

4. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 3, characterized in that: The cavity is in a columnar structure.

5. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 4, characterized in that: The cavity is in a cylindrical structure.

6. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 3, characterized in that: The open end of the shell (1) is connected to the cover body (2) via a knife-edge flange.

7. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 6, characterized in that: The cover body (2) is a multifunctional flange.

8. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 3, characterized in that: The housing (1) is provided with a temperature sensor, the temperature sensor is connected to a temperature controller (8), and the temperature controller (8) is used to control the start and stop of the heating component (3).

9. The device for preparing a nickel-manganese alloy resistant to high temperature liquid lithium corrosion according to claim 3, characterized in that: The inert gas is argon.

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