CN109773199B - Rapid preparation method of multi-scale lithium ball - Google Patents
Rapid preparation method of multi-scale lithium ball Download PDFInfo
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- CN109773199B CN109773199B CN201910036379.4A CN201910036379A CN109773199B CN 109773199 B CN109773199 B CN 109773199B CN 201910036379 A CN201910036379 A CN 201910036379A CN 109773199 B CN109773199 B CN 109773199B
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Abstract
Under the protection of inert gas atmosphere, putting lithium raw materials into a lithium melting tank through a feeding port, heating the lithium raw materials to a certain temperature through a heater, extruding liquid lithium in a lithium tube by using inert gas with proper air pressure regulated by an inflation valve, a straight-through valve and a deflation valve, spraying the liquid lithium into a coolant through a small hole of a plug, rapidly cooling and solidifying to obtain lithium balls, regulating the air pressure of the introduced gas to produce the lithium balls with different diameters in a sub-millimeter order, and then carrying out subsequent treatment to obtain the clean multi-scale lithium balls. The invention has the advantages of simple and easy operation, short production period, regular lithium ball forming and controllable size in the sub-millimeter level, can meet the requirements of ELMs (electron cyclotron resonance spectroscopy) injection modulation and plasma cracking protection experiments of the EAST device lithium ball, and provides a good technical basis for the successful application of impurity injection in the fusion reactor in the future.
Description
Technical Field
The invention relates to the technical field of nuclear materials, in particular to a rapid preparation method of a multi-scale lithium ball.
Background
Lithium metal is considered as a possible plasma-facing material, tritium-generating material, etc. due to its unique physicochemical properties (low Z, low melting point, strong chemical activity, etc.). In the last decade, lithium has been used in all forms (e.g., lithium vacuum coating, liquid lithium restrictors, lithium diverters, etc.) in various fusion devices such as EAST, NSTX, FTU, T-10, TJ-II, etc. Recently, a lithium ball injection experiment is carried out on the EAST apparatus, lithium is made into spherical particles and injected into plasma from a midplane, and control of plasma boundary local area modes (ELMs) is realized. In addition, the high-pressure gas is used for driving the small-scale lithium ball to be injected, and the plasma breakage is relieved. In the above applications of the lithium spheres, there are quite high requirements on the size thereof, for example, for control of ELMs, the diameter size of the lithium spheres is required to be between 0.6 and 0.9 mm; in addition, lithium is very active in chemical property and very easy to react with oxygen in the air, which puts extremely high requirements on the preparation of lithium spheres: on one hand, the purity of the lithium ball is required to reach a certain requirement, and new impurities cannot be introduced into the fusion device; on the other hand, the size of the lithium ball needs to meet certain requirements, and the balling rule meets the requirements of physical research.
There are many ways to directly or indirectly prepare particles, such as "top-down" chemical synthesis, physical cutting from "large to small". However, the methods are difficult to control the size and the shape of the generated particles, involve many chemical and physical changes, have complex processes, greatly reduce the balling efficiency and increase the production cost. The invention applies the Tomotika double-flow cylinder model to the preparation of the lithium ball, thereby not only solving the problem that lithium is easy to be oxidized in air, but also having the advantages of simple process, regular balling, easy size control and the like. The lithium ball prepared at the present stage is tested by ELMs (electro-mechanical systems) control on an EAST tokamak fusion device, all indexes reach the expected result of an experiment, and the lithium ball can be applied to industrial production in the later stage in a large scale.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a method for quickly preparing a multi-scale lithium ball.
The invention is realized by the following technical scheme:
a quick preparation method of a multi-scale lithium ball comprises an inert gas storage bottle, a lithium melting tank and a beaker, wherein the lithium melting tank is provided with an air inlet and an air outlet, the top end of the lithium melting tank is provided with a feed inlet, the air outlet of the inert gas storage bottle is connected with the air inlet of the lithium melting tank through an air pipe I, the air pipe I is provided with an inflation valve and a straight-through valve, the air outlet of the lithium melting tank is connected with an air pipe II, the air pipe II is provided with an air release valve, a heater is arranged outside the lithium melting tank, the bottom outlet of the lithium melting tank is connected with a lithium pipe, the lithium pipe is provided with a lithium valve, the lower end of the lithium pipe is connected with a plug, the bottom of the plug is provided with a laser hole, the beaker is arranged below the plug, and a coolant is arranged inside the beaker. The operation steps are as follows:
firstly, closing a feed port 4 and an air release valve 5, sequentially opening a lithium valve 11, a straight-through valve 3 and an inflation valve 2, introducing argon gas 1 with 0.02MPa into the preparation device through a first air pipe 8, starting a heater 7, baking and exhausting air for a lithium melting tank 6, a lithium pipe 10, the lithium valve 11 and a plug 12, setting the baking temperature to be 300 ℃, and continuously performing for 12 hours.
Closing the lithium valve 11, adjusting the argon pressure to 0.2MPa, opening the feed port 4, throwing 90g of lithium rods into the lithium melting tank 6 under the protection of argon atmosphere, closing the feed port 4, and then opening the air release valve 5 to release the redundant argon in the lithium melting tank 6.
After feeding, due to the melting of the solid lithium rod, the temperature of the lithium melting tank 6 is firstly reduced and then increased, and the temperatures of the lithium melting tank 6, the lithium tube 10 and the plug 12 are all increased to 300 ℃ and are kept stable.
Fourthly, placing the beaker 14 under the plug 12, wherein the plug 12 extends into the beaker 14 and is about 1/4 away from the cup opening, and then slowly pouring the liquid paraffin 13 into the beaker 14 to ensure that the liquid level is just contacted with the surface of the plug 12.
Fifthly, closing the straight-through valve 3, opening the charging valve 2, presetting a certain air pressure value, opening the deflation valve 5, emptying the air pressure which is increased by temperature rise in the lithium melting tank 6.
Sixthly, opening the lithium valve 11, rapidly opening the straight-through valve 3, and rapidly injecting the pressed liquid lithium into the liquid paraffin 13 through the laser hole 15 of the plug 12 to generate a lithium ball.
And seventhly, closing the lithium valve 11 after liquid lithium in the lithium pipe 10 is sprayed, and collecting the lithium balls floating on the surface of the liquid paraffin.
Adjusting the third step, presetting temperature, presetting air pressure and the aperture of the laser hole 15 to control the size of the lithium ball.
Ninthly, the produced lithium balls are coated with paraffin on the surfaces, mixed and washed by n-hexane, and kept stand for 24h for solution layering, the upper layer is the lithium balls with lower density, the lower layer is the n-hexane solvent with higher density, and the lithium balls are dried in the glove box under the argon atmosphere after being filtered.
Under the protection of inert gas atmosphere, putting lithium raw materials into a lithium melting tank through a feeding port, heating the lithium melting tank to a certain temperature through a heater, extruding liquid lithium in a lithium tube by using inert gas with proper air pressure regulated by an inflation valve, a straight-through valve and a deflation valve, spraying the liquid lithium into a coolant through a small hole of a plug, rapidly cooling and solidifying to obtain lithium balls, regulating the air pressure of the introduced gas to produce the lithium balls with different diameters in a sub-millimeter order, and then carrying out subsequent treatment to obtain the clean multi-scale lithium balls.
The inert gas storage cylinder is an argon cylinder, and the inert gas is argon.
The lithium melting tank is an SUS316 seamless pipe, and a manual gate valve is installed at the feeding port.
The lithium tube is an SUS316 seamless tube, and two ends of the lithium tube are respectively connected with the lithium melting tank and the lithium valve; the first air pipe and the second air pipe are both SUS316 seamless pipes, and are connected with the lithium melting tank through welding.
The lithium valve is a corrugated pipe valve, the valve body is made of SUS316, and the lithium pipe and the plug are connected in a sealing mode through a clamping sleeve joint.
The inflation valve comprises a pressure reducing valve and a pressure gauge, the air inlet of the pressure reducing valve is connected with the inert gas storage bottle, the air outlet of the pressure reducing valve is connected with the first air pipe, and the pressure gauge measures the pressure of the inert gas after pressure reduction; the straight-through valve is a ball valve; the air release valve is an angle valve with a flange interface, is in butt joint with the second air pipe through a flange, and is communicated with the atmosphere through the opening of the other flange.
The heater comprises a direct current power supply and a plurality of armored heating wires, wherein the technical parameters of the direct current power supply are AC 220V/10A input and three paths of DC 0-220V/0-10A output; and a plurality of armored heating wires are respectively wound on the outer sides of the lithium melting tank, the lithium pipe and the plug, are respectively distributed with thermocouples for temperature measurement, and are then wrapped by aluminum foil paper.
The plug is a hollow SUS316 cylinder with an opening at one end, the opening end is connected with the lithium valve, the laser hole is penetrated and corroded at the other end by adopting a laser drilling process, and the plug with different diameters of the round hole can be replaced as required.
The coolant is liquid paraffin, lithium is insoluble in the liquid paraffin, and the lithium and the liquid paraffin exist stably and do not react. In addition, the lithium balls can be protected from air (O)2、H2O、CO2Etc.) are reacted.
The invention has the advantages that: the invention has the advantages of simple and easy operation, short production period, regular lithium ball forming and controllable size in the sub-millimeter level, can meet the requirements of ELMs (electron cyclotron resonance spectroscopy) injection modulation and plasma cracking protection experiments of the EAST device lithium ball, and provides a good technical basis for the successful application of impurity injection in the fusion reactor in the future.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic view of a plug structure.
Detailed Description
As shown in figure 1, the rapid preparation method of the multi-scale lithium ball comprises an inert gas storage bottle 1, a lithium melting tank 6 and a beaker 14, the lithium melting tank 6 is provided with an air inlet and an air outlet, the top end of the lithium melting tank 6 is provided with a feeding port 4, the air outlet of the inert gas storage bottle 1 is connected with the air inlet of the lithium melting tank 6 through an air pipe I8, an inflation valve 2 and a straight-through valve 3 are arranged on the air pipe I8, an air outlet of the lithium melting tank 6 is connected with an air pipe II 9, a deflation valve 5 is arranged on the second air pipe 9, a heater 7 is arranged outside the lithium melting tank 6, a lithium pipe 10 is connected with the outlet at the bottom of the lithium melting tank 6, a lithium valve 11 is installed on the lithium tube 10, a plug 12 is connected with the lower end of the lithium tube 10, a laser hole 15 is opened at the bottom of the plug 12, the beaker 14 is arranged below the plug 12, and the liquid paraffin 13 is arranged in the beaker 14.
The inert gas storage cylinder is an argon cylinder, and the inert gas is argon.
The lithium melting tank 6 is an SUS316 seamless pipe with DN106mm × 200mm and delta 3mm, and one end of the lithium melting tank is welded with a CF100 flange; the other end was blocked with a SUS316 disk of 100mm in diameter and 3mm in diameter, and a lithium tube was welded to the center of the disk through a hole of 13mm in diameter. Two holes with the diameter of 7mm are symmetrically formed in the flange side of the tank body, and a first air pipe and a second air pipe are respectively welded.
The feeding port 4 is a manual gate valve of CF100, the vacuum sealing side is in butt joint with a CF100 flange of the lithium melting tank, and the other side is open and communicated with the atmosphere.
The lithium tube is an SUS316 seamless tube with phi 1/2in and delta 1mm, and two ends of the tube are respectively connected with the lithium melting tank and the lithium valve.
The first air pipe 8 and the second air pipe 9 are two SUS316 seamless pipes with phi 1/4in and delta 1mm, one ends of the SUS316 seamless pipes are welded on the lithium melting tank, and the other ends of the SUS316 seamless pipes are respectively connected with a precision pressure gauge and a CF16 flange.
The lithium valve 11 is an SS-8UW type bellows valve, the valve body is made of SUS316, the valve body can resist high temperature of 482 ℃, and can be hermetically connected with a lithium pipe and a plug through a phi 1/2in ferrule sleeve joint to control the on-off of liquid lithium in the lithium pipe.
The charging valve 2 comprises a YQAr-720 type pressure reducing valve and a YB-150A type precision pressure gauge, the air inlet of the pressure reducing valve is connected with an argon steel cylinder, and the air outlet is connected with an air pipe; the precise pressure gauge measures the argon pressure after decompression, the measurement range is 0-0.4MPa, and the precision is 0.4 grade.
The straight-through valve 3 is an SS-43GS4 type ball valve, and can rapidly control the on-off of the gas path. The pressure reducing valve, the precision pressure gauge and the ball valve are connected with the air pipe through phi 1/4in ferrule fittings.
The air release valve 5 is an angle valve with two CF16 flange interfaces, a bellows seal is used as a transmission seal, a flange exposing the bellows is butted with a CF16 flange led out from a lithium melting tank, and the other flange is opened to be communicated with the atmosphere.
The heater 7 comprises a direct current power supply and three armored heating wires, wherein the technical parameters of the direct current power supply are AC 220V/10A input and three paths of DC 0-220V/0-10A output; three armoured heating wires are respectively wound on the outer sides of the lithium melting tank, the lithium pipe (including a lithium valve) and the plug, thermocouples are respectively arranged for measuring temperature, and then aluminum foil paper is used for wrapping to realize the effects of uniform heating and heat preservation, and the power of each heating wire is 1 KW.
The lithium raw material is a lithium rod with the size of phi 25mm multiplied by 57mm, and the single piece is about 15 g.
As shown in fig. 2, the plug 12 is a hollow SUS316 cylinder with a diameter of 1/2in and a diameter of 1mm, one end of the hollow SUS316 cylinder is open, the open end is connected with a lithium valve, and the other end of the hollow SUS316 cylinder is drilled through a circular hole with a diameter of 0.5mm by a laser drilling process.
The coolant is liquid paraffin, lithium is insoluble in the liquid paraffin, and the lithium and the liquid paraffin exist stably and do not react; in addition, since the liquid paraffin is coated on the surface of the lithium ball, the lithium ball is protected from air (O)2、H2O、CO2Etc.) are reacted.
As shown in fig. 1 and 2, the operation steps are as follows:
firstly, closing a feed port 4 and an air release valve 5, sequentially opening a lithium valve 11, a straight-through valve 3 and an inflation valve 2, introducing argon gas 1 with 0.02MPa into the preparation device through a first air pipe 8, starting a heater 7, baking and exhausting air for a lithium melting tank 6, a lithium pipe 10, the lithium valve 11 and a plug 12, setting the baking temperature to be 300 ℃, and continuously performing for 12 hours.
Closing the lithium valve 11, adjusting the argon pressure to 0.2MPa, opening the feed port 4, throwing 90g of lithium rods into the lithium melting tank 6 under the protection of argon atmosphere, closing the feed port 4, and then opening the air release valve 5 to release the redundant argon in the lithium melting tank 6.
After feeding, due to the melting of the solid lithium rod, the temperature of the lithium melting tank 6 is firstly reduced and then increased, and the temperatures of the lithium melting tank 6, the lithium tube 10 and the plug 12 are all increased to 300 ℃ and are kept stable.
Fourthly, placing the beaker 14 under the plug 12, wherein the plug 12 extends into the beaker 14 and is about 1/4 away from the cup opening, and then slowly pouring the liquid paraffin 13 into the beaker 14 to ensure that the liquid level is just contacted with the surface of the plug 12.
Fifthly, closing the straight-through valve 3, opening the charging valve 2, presetting a certain air pressure value, opening the deflation valve 5, emptying the air pressure which is increased by temperature rise in the lithium melting tank 6.
Sixthly, opening the lithium valve 11, rapidly opening the straight-through valve 3, and rapidly injecting the pressed liquid lithium into the liquid paraffin 13 through the laser hole 15 of the plug 12 to generate a lithium ball.
And seventhly, closing the lithium valve 11 after liquid lithium in the lithium pipe 10 is sprayed, and collecting the lithium balls floating on the surface of the liquid paraffin.
Adjusting the third step, presetting temperature, presetting air pressure and the aperture of the laser hole 15 to control the size of the lithium ball.
Ninthly, the produced lithium balls are coated with paraffin on the surfaces, mixed and washed by n-hexane, and kept stand for 24h for solution layering, the upper layer is the lithium balls with lower density, the lower layer is the n-hexane solvent with higher density, and the lithium balls are dried in the glove box under the argon atmosphere after being filtered.
The above embodiments are only used for illustrating but not limiting the technical solutions of the present invention, and although the above embodiments describe the present invention in detail, those skilled in the art should understand that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and any modifications and equivalents may fall within the scope of the claims.
Claims (1)
1. A method for rapidly preparing multi-scale lithium spheres is characterized by comprising the following steps: comprises an inert gas storage bottle (1), a lithium melting tank (6) and a beaker (14), wherein the lithium melting tank (6) is provided with an air inlet and an air outlet, the top end of the lithium melting tank (6) is provided with a feeding port (4), the air outlet of the inert gas storage bottle (1) is connected with the air inlet of the lithium melting tank (6) through an air pipe I (8), the air pipe I (8) is provided with an inflation valve (2) and a straight-through valve (3), the air outlet of the lithium melting tank (6) is connected with an air pipe II (9), the air pipe II (9) is provided with an air release valve (5), a heater (7) is arranged outside the lithium melting tank (6), the bottom outlet of the lithium melting tank (6) is connected with a lithium pipe (10), the lithium pipe (10) is provided with a lithium valve (11), the lower end of the lithium pipe (10) is connected with a plug (12), the bottom of the plug (12) is provided with a laser hole (15), the beaker (14) is arranged below the plug (12), the beaker (14) is internally provided with a coolant, and the operation steps are as follows:
firstly, closing a feed port (4) and an air release valve (5), sequentially opening a lithium valve (11), a straight-through valve (3) and an inflation valve (2), introducing argon gas of 0.02MPa into a preparation device through a gas pipe I (8), starting a heater (7), baking a lithium melting tank (6), a lithium pipe (10), the lithium valve (11) and a plug (12) to give out gas, setting the baking temperature to be 300 ℃, and continuously performing for 12 hours;
closing a lithium valve (11), adjusting the argon pressure to 0.2MPa, opening a feed port (4), putting 90g of lithium rods into the lithium melting tank (6) under the protection of argon atmosphere, closing the feed port (4), and then opening a gas release valve (5) to release redundant argon in the lithium melting tank (6);
after feeding, due to the melting of the solid lithium rod, the temperature of the lithium melting tank (6) is firstly reduced and then increased, and the temperatures of the lithium melting tank (6), the lithium tube (10) and the plug (12) are all increased to 300 ℃ which is preset and kept stable;
placing the beaker (14) under the plug (12), wherein the plug (12) extends into the beaker (14) and is about 1/4 away from the cup opening, and then slowly pouring the liquid paraffin (13) into the beaker (14) to ensure that the liquid level is just contacted with the surface of the plug (12);
closing the straight-through valve (3), opening the inflation valve (2), presetting a certain air pressure value, opening the deflation valve (5), emptying the air pressure increased by temperature rise in the lithium melting tank (6);
sixthly, opening the lithium valve (11), quickly opening the straight-through valve (3), and quickly injecting the pressed liquid lithium into the liquid paraffin (13) through the laser hole (15) of the plug (12) to generate a lithium ball;
seventhly, after liquid lithium in the lithium pipe (10) is sprayed, closing a lithium valve (11), and collecting lithium balls floating on the surface of liquid paraffin (13);
adjusting the third step, presetting temperature, presetting air pressure and the aperture of the laser hole (15) to control the size of the lithium ball;
ninthly, coating paraffin on the surface of the produced lithium ball, mixing and washing with n-hexane, standing for 24h for layering of the solution, wherein the upper layer is a lithium ball with lower density, the lower layer is a n-hexane solvent with higher density, and drying in a glove box under the argon atmosphere after filtering;
under the protection of inert gas atmosphere, putting lithium raw materials into a lithium melting tank (6) through a feeding port (4), heating the lithium raw materials to a certain temperature through a heater (7), extruding liquid lithium in a lithium tube (10) by using inert gas with proper air pressure regulated by an inflation valve (2), a straight-through valve (3) and a deflation valve (5), spraying the liquid lithium into a coolant through a small hole of a plug (12), rapidly cooling and solidifying to obtain lithium balls, regulating the air pressure of the introduced gas to produce the lithium balls with sub-millimeter magnitude and different diameters, and then carrying out subsequent treatment to obtain clean multi-scale lithium balls;
the inert gas storage cylinder (1) is an argon cylinder, and the inert gas is argon;
the lithium melting tank (6) is an SUS316 seamless pipe, and a manual gate valve is arranged at the feeding port (4);
the lithium tube (10) is an SUS316 seamless tube, and two ends of the lithium tube are respectively connected with the lithium melting tank (6) and the lithium valve (11); the first air pipe (8) and the second air pipe (9) are SUS316 seamless pipes, and the first air pipe (8) and the second air pipe (9) are connected with the lithium melting tank (6) through welding;
the lithium valve (11) is a corrugated pipe valve, the valve body is made of SUS316, and the lithium pipe (10) and the plug (12) are connected in a sealing mode through a clamping sleeve joint;
the inflation valve (2) comprises a pressure reducing valve and a pressure gauge, the air inlet of the pressure reducing valve is connected with the inert gas storage bottle (1), the air outlet of the pressure reducing valve is connected with the first air pipe (8), and the pressure gauge measures the pressure of the decompressed inert gas; the straight-through valve (3) is a ball valve; the air release valve (5) is an angle valve with a flange interface, is butted with the second air pipe (9) through a flange, and the other flange is opened to be communicated with the atmosphere;
the heater (7) comprises a direct current power supply and a plurality of armored heating wires, and the technical parameters of the direct current power supply are AC 220V/10A input and three paths of DC 0-220V/0-10A output; a plurality of armored heating wires are respectively wound on the outer sides of the lithium melting tank (6), the lithium pipe (10) and the plug (12), are respectively provided with thermocouples for measuring temperature, and are then wrapped by aluminum foil paper;
the plug (12) is a hollow SUS316 cylinder with an opening at one end, the opening end is connected with the lithium valve (11), the laser hole (15) is penetrated and etched at the other end by adopting a laser drilling process, and the plug (12) with different circular hole diameters can be replaced according to the requirement;
the coolant is liquid paraffin (13), lithium is insoluble in the liquid paraffin (13), the lithium and the liquid paraffin are stably present and do not react, and in addition, the lithium spheres can be protected from reacting with air.
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| CN111081389B (en) * | 2019-12-09 | 2022-08-16 | 中国科学院合肥物质科学研究院 | Mechanism and method for injecting plasma impurities into fusion device |
| CN111063458B (en) * | 2019-12-25 | 2022-08-16 | 中国科学院合肥物质科学研究院 | Device and method for accurately calibrating plasma injection impurities |
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