CN109773199A - A kind of fast preparation method of multiple dimensioned lithium ball - Google Patents
A kind of fast preparation method of multiple dimensioned lithium ball Download PDFInfo
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- CN109773199A CN109773199A CN201910036379.4A CN201910036379A CN109773199A CN 109773199 A CN109773199 A CN 109773199A CN 201910036379 A CN201910036379 A CN 201910036379A CN 109773199 A CN109773199 A CN 109773199A
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Abstract
The invention discloses a kind of fast preparation methods of multiple dimensioned lithium ball; under atmosphere of inert gases protection; lithium raw material is put into molten lithium tank by feeding port; certain temperature is heated to by heater again; the liquid lithium in lithium pipe is squeezed using the inert gas of charge valve, straight-through valve and Waste gate proper pressure; by the small hole injection of plug into coolant; cooling and solidifying obtains lithium ball rapidly; the air pressure that adjusting is passed through gas can produce the lithium ball of submillimeter magnitude different-diameter, then obtain clean multiple dimensioned lithium ball through subsequent processing.The present invention is simple to operation, it is with short production cycle, the balling-up of lithium ball is regular and size is controllable in submillimeter magnitude, can satisfy the requirement of EAST device lithium ball injection modulation ELMs and Plasma disruption prevention, and the successful application for impurity injection in the following fusion reactor provides good technical foundation.
Description
Technical field
The present invention relates to nuclear material technical field more particularly to a kind of fast preparation methods of multiple dimensioned lithium ball.
Background technique
Lithium metal is considered as one kind because of its unique physicochemical properties (low Z, low melting point, extensive chemical activity etc.)
Possible facing plasma material, tritium generate material etc..Nearly ten years, lithium (such as lithium vacuum coating, liquid lithium in a variety of manners
Limiter, lithium divertor etc.) it is applied in all kinds of fusion facilities such as EAST, NSTX, FTU, T-10, TJ-II.In the recent period in EAST
Lithium ball injection experiments are carried out on device, spherical particles have been made in lithium, and therefrom plane is injected into plasma, is realized
The control of plasma boundary local mode (ELMs).In addition, being injected using the small scale lithium ball of drive of high-pressure gas, also realization pair
The alleviation of Plasma disruption.Above with respect to the application of lithium ball, there is quite high requirement to its size, such as control to ELMs
System, it is desirable that lithium bulb diameter size is between 0.6-0.9mm；In addition, the chemical property of lithium is very active, easily with the oxygen in air
React, this just proposes high requirement to the preparation of lithium ball: on the one hand, the purity of lithium ball will reach certain requirement,
New impurity cannot be introduced in fusion facility；On the other hand, the size of lithium ball will meet certain requirement, and balling-up rule, full
The needs of sufficient physical study.
The method for directly or indirectly preparing particle has very much, such as " from top to bottom " chemical synthesis, by " greatly to small "
Physics cutting method.However these methods are difficult to control the size and pattern for generating particle, and are related to Chemical Physics and change more, process
Complexity greatly reduces balling-up efficiency, increases production cost.Tomotika double fluid type cylinder models are applied to lithium by the present invention
Ball preparation, not only solves the problem of lithium is easily oxidized in air, and the lithium ball of this method preparation has that process is simple,
Many advantages, such as balling-up rule, size is easy to control.The lithium ball prepared at this stage is enterprising in EAST tokamak fusion facility
The test of the ELMs that gone control, indices reach the expected results of experiment, the later period can large-scale application in industrial production.
Summary of the invention
The object of the invention is to remedy the disadvantages of known techniques, provides a kind of quick preparation side of multiple dimensioned lithium ball
Method.
The present invention is achieved by the following technical solutions:
A kind of fast preparation method of multiple dimensioned lithium ball includes inert gas storage cylinder, molten lithium tank and beaker, melts in described
Lithium tank is equipped with air inlet and air outlet, is equipped with feeding port, the outlet of the inert gas storage cylinder on the top of molten lithium tank
Mouth connects the air inlet of molten lithium tank by tracheae one, is equipped with charge valve and straight-through valve on tracheae one, melts the gas outlet of lithium tank
It is connected with tracheae two, vent valve is installed on tracheae two, having heaters is installed in the outside of molten lithium tank, in the bottom of molten lithium tank
Outlet is connected with lithium pipe, and lithium valve is equipped on lithium pipe, is connected with plug in the lower end of lithium pipe, is provided with laser in the bottom of plug
Hole is equipped with the beaker in the lower section of plug, coolant is equipped with inside beaker.Operating procedure is as follows:
1. closing feeding port 4, vent valve 5, lithium valve 11, straight-through valve 3 and charge valve 2 are successively opened, by tracheae 1 to preparation
0.02MPa argon gas 1 is passed through in device, heater 7 is toasted outlet to molten lithium tank 6, lithium pipe 10, lithium valve 11 and plug 12, dried
Roasting temperature is set as 300 DEG C, is carried out continuously 12h.
2. closing lithium valve 11, ar pressure is adjusted to 0.2MPa, opens feeding port 4, to molten lithium tank under argon atmosphere protection
90g lithium stick is put into 6, closes feeding port 4, is then opened vent valve 5 and is released extra argon gas in molten lithium tank 6.
3. after feeding intake, due to the fusing of solid lithium stick, the temperature of molten lithium tank 6 can first drop to be risen afterwards, lithium tank 6 fusion, lithium pipe 10
300 DEG C of preset temperature are risen to the temperature of plug 12, and remains stable.
4. beaker 14 is placed in immediately below plug 12, in beaker 14 and at rim of a cup about 1/4, then plug 12 is put in
Atoleine 13 is poured slowly into beaker 14, contacts liquid level just with 12 surface of plug.
5. closing straight-through valve 3, charge valve 2 is opened, presets certain atmospheric pressure value, vent valve 5 is opened and is vented molten lithium tank 6
It is middle heating and raised air pressure.
6. opening lithium valve 11, and straight-through valve 3 is opened rapidly, the liquid lithium after compression is fast by the laser hole 15 of plug 12
Speed is ejected into atoleine 13, generates lithium ball.
7. closing lithium valve 11 after liquid lithium has sprayed in lithium pipe 10, the lithium ball of liquid paraffin surface floating is collected.
8. 3. 5. the aperture of preset pressure and laser hole 15 can control lithium ball to regulating step for preset temperature, step
Size.
9. the lithium ball surface produced is coated with paraffin, with n-hexane mixing, washing, stands solution for 24 hours and be layered, upper layer is
The lower lithium ball of density, lower layer is the biggish n-hexane solvent of density, dry under argon atmosphere in glove box after filtering.
Under atmosphere of inert gases protection, lithium raw material put into molten lithium tank by feeding port, then pass through heater by its
It is heated to certain temperature, the liquid in lithium pipe is squeezed using the inert gas of charge valve, straight-through valve and Waste gate proper pressure
State lithium, by the small hole injection of plug into coolant, cooling and solidifying obtains lithium ball rapidly, adjust be passed through the air pressure of gas can be with
The lithium ball of submillimeter magnitude different-diameter is produced, then obtains clean multiple dimensioned lithium ball through subsequent processing.
The inert gas storage cylinder is argon bottle, and inert gas is argon gas.
The molten lithium tank is SUS316 seamless pipe, is equipped with hand operated gate valve at the feeding port.
The lithium pipe is SUS316 seamless pipe, and both ends are connect with molten lithium tank and lithium valve respectively；The tracheae one is gentle
Pipe two is SUS316 seamless pipe, and tracheae one and tracheae two are tank connected with molten lithium by welding.
The lithium valve is bellows valve, and valve body material SUS316 is sealed lithium pipe and plug by clamping sleeve blow-out patch
Connection.
The charge valve includes pressure reducing valve and pressure gauge, and pressure reducing valve air inlet is connected with inert gas storage cylinder, out
Port is connect with tracheae one, the inert gas air pressure after gauge measurement decompression；The straight-through valve is ball valve；The deflation
Valve is the angle valve with flange-interface, is docked by flange with tracheae two, and another flange is opened wide and is communicated with the atmosphere.
The heater includes DC power supply and Duo Gen armouring heater strip, and the technical parameter of the DC power supply is
AC 220V/10A input, three road DC 0-220V/0-10A output；More armouring heater strips be respectively wound around molten lithium tank, lithium pipe and
The outside of plug, and it is respectively arranged thermocouple temperature measurement, then wrapped up with aluminium-foil paper.
The plug is hollow SUS316 cylindrical body open at one end, and open end is connect with lithium valve, and the other end is using sharp
The technique of light punching wears erosion laser hole, can according to need the different plug of replacement Circularhole diameter.
The coolant is atoleine, and lithium does not dissolve in atoleine, and the two is stabilized without reacting.This
Outside, can protect lithium ball not with air (O2、H2O、CO2Deng) reaction.
The invention has the advantages that the present invention is simple to operation, with short production cycle, the balling-up of lithium ball is regular and size is in submillimeter
Magnitude is controllable, can satisfy the requirement of EAST device lithium ball injection modulation ELMs and Plasma disruption prevention, is future
The successful application that impurity injects in fusion reactor provides good technical foundation.
Detailed description of the invention
Fig. 1 is the structural diagram of the present invention.
Fig. 2 is stopper structure schematic diagram.
Specific embodiment
As shown in Figure 1, a kind of fast preparation method of multiple dimensioned lithium ball, includes inert gas storage cylinder 1, molten lithium tank 6
With beaker 14, it is equipped with air inlet and air outlet on the molten lithium tank 6, is equipped with feeding port 4 on the top of molten lithium tank 6, it is described
The gas outlet of inert gas storage cylinder 1 air inlet of molten lithium tank 6 is connected by tracheae 1, inflation is installed on tracheae 1
The gas outlet of valve 2 and straight-through valve 3, molten lithium tank 6 is connected with tracheae 29, vent valve 5 is equipped on tracheae 29, in molten lithium tank 6
Outside having heaters 7 is installed, be connected with lithium pipe 10 in the outlet at bottom of molten lithium tank 6, lithium valve 11 be installed on lithium pipe 10,
The lower end of lithium pipe 10 is connected with plug 12, is provided with laser hole 15 in the bottom of plug 12, is equipped in the lower section of plug 12 described
Beaker 14 is equipped with atoleine 13 inside beaker 14.
The inert gas storage cylinder is argon bottle, and inert gas is argon gas.
The molten lithium tank 6 is DN106mm*200mm, and the SUS316 seamless pipe of δ 3mm, CF100 flange is welded in one end；Separately
The SUS316 disk of one end φ 100mm, δ 3mm are blocked, and open the hole φ 13mm welding lithium pipe in its center.In tank flange side pair
Title opens two holes φ 7mm, and tracheae one and tracheae two is respectively welded.
The feeding port 4 is the hand operated gate valve of CF100, and vacuum sealing side is docked with molten lithium tank CF100 flange, another
Side is opened wide and is communicated with the atmosphere.
The lithium pipe is φ 1/2in, and the SUS316 seamless pipe of δ 1mm, both ends are connect with molten lithium tank and lithium valve respectively.
The tracheae 1 and tracheae 29 is the SUS316 seamless pipe of two φ 1/4in, δ 1mm, their one end welding
On molten lithium tank, the other end respectively with precision pressure gauge and CF16 flanged joint.
The lithium valve 11 is SS-8UW type bellows valve, and valve body material SUS316, resistance to 482 °C of high temperature can pass through
φ 1/2in clamping sleeve blow-out patch and lithium pipe and plug are tightly connected, and control the on-off of liquid lithium in lithium pipe.
The charge valve 2 includes a YQAr-720 type pressure reducing valve and a YB-150A type precision pressure gauge, pressure reducing valve
Air inlet is connected with argon gas steel cylinder, and gas outlet is connect with tracheae；Ar pressure after precision pressure gauge measurement decompression, measures model
Enclosing is 0-0.4MPa, 0.4 grade of precision.
The straight-through valve 3 is SS-43GS4 type ball valve, can control gas path on-off rapidly.Pressure reducing valve, precision pressure gauge
It with tracheae is interconnected by φ 1/4in clamping sleeve blow-out patch with ball valve.
The vent valve 5 is that there are two the angle valves of CF16 flange-interface for band, using sylphon seal as transmission seal,
The flange of exposure bellows is docked with the CF16 flange that molten lithium tank is drawn, and another flange is opened wide and is communicated with the atmosphere.
The heater 7 includes a DC power supply and three armouring heater strips, the technical parameter of DC power supply are AC
220V/10A input, three road DC 0-220V/0-10A output；Three armouring heater strips are respectively wound around molten lithium tank, lithium pipe (containing lithium
Valve) and plug outside, and be respectively arranged thermocouple temperature measurement, then may be implemented to be evenly heated and keep the temperature with aluminium-foil paper package
Effect, the power of single heater strip are 1KW.
The lithium raw material is having a size of φ 25mm × 57mm lithium stick, Dan Meiyue 15g.
As shown in Fig. 2, the plug 12 is φ 1/2in, the hollow SUS316 cylindrical body open at one end of δ 1mm, opening
End is connect with lithium valve, and the other end uses the technique of laser boring to wear erosion diameter as the circular hole of 0.5mm.
The coolant is atoleine, and lithium does not dissolve in atoleine, and the two is stabilized without reacting；This
Outside, due to atoleine be coated in lithium ball surface, thus protect lithium ball not with air (O2、H2O、CO2Deng) reaction.
As illustrated in fig. 1 and 2, operating procedure is as follows:
1. closing feeding port 4, vent valve 5, lithium valve 11, straight-through valve 3 and charge valve 2 are successively opened, by tracheae 1 to preparation
0.02MPa argon gas 1 is passed through in device, heater 7 is toasted outlet to molten lithium tank 6, lithium pipe 10, lithium valve 11 and plug 12, dried
Roasting temperature is set as 300 DEG C, is carried out continuously 12h.
2. closing lithium valve 11, ar pressure is adjusted to 0.2MPa, opens feeding port 4, to molten lithium tank under argon atmosphere protection
90g lithium stick is put into 6, closes feeding port 4, is then opened vent valve 5 and is released extra argon gas in molten lithium tank 6.
3. after feeding intake, due to the fusing of solid lithium stick, the temperature of molten lithium tank 6 can first drop to be risen afterwards, lithium tank 6 fusion, lithium pipe 10
300 DEG C of preset temperature are risen to the temperature of plug 12, and remains stable.
4. beaker 14 is placed in immediately below plug 12, in beaker 14 and at rim of a cup about 1/4, then plug 12 is put in
Atoleine 13 is poured slowly into beaker 14, contacts liquid level just with 12 surface of plug.
5. closing straight-through valve 3, charge valve 2 is opened, presets certain atmospheric pressure value, vent valve 5 is opened and is vented molten lithium tank 6
It is middle heating and raised air pressure.
6. opening lithium valve 11, and straight-through valve 3 is opened rapidly, the liquid lithium after compression is fast by the laser hole 15 of plug 12
Speed is ejected into atoleine 13, generates lithium ball.
7. closing lithium valve 11 after liquid lithium has sprayed in lithium pipe 10, the lithium ball of liquid paraffin surface floating is collected.
8. 3. 5. the aperture of preset pressure and laser hole 15 can control lithium ball to regulating step for preset temperature, step
Size.
9. the lithium ball surface produced is coated with paraffin, with n-hexane mixing, washing, stands solution for 24 hours and be layered, upper layer is
The lower lithium ball of density, lower layer is the biggish n-hexane solvent of density, dry under argon atmosphere in glove box after filtering.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although above-described embodiment to the present invention into
Gone detailed description, the related technical personnel of this field it is understood that can modify to the present invention or replace on an equal basis, but
Any modification and part replacement for not departing from spirit and scope of the invention should all be covered in scope of the presently claimed invention.
Claims (9)
1. a kind of fast preparation method of multiple dimensioned lithium ball, it is characterised in that: include inert gas storage cylinder, molten lithium tank and burning
Cup is equipped with air inlet and air outlet on the molten lithium tank, is equipped with feeding port, the inert gas on the top of molten lithium tank
The gas outlet of storage cylinder connects the air inlet of molten lithium tank by tracheae one, is equipped with charge valve and straight-through valve on tracheae one, melts
The gas outlet of lithium tank is connected with tracheae two, is equipped with vent valve on tracheae two, installs having heaters in the outside of molten lithium tank,
The outlet at bottom of molten lithium tank is connected with lithium pipe, and lithium valve is equipped on lithium pipe, plug is connected in the lower end of lithium pipe, in plug
Bottom is provided with laser hole, is equipped with the beaker in the lower section of plug, coolant is equipped with inside beaker；Specific preparation step is such as
Under:
(1) feeding port, vent valve are closed, lithium valve, straight-through valve and charge valve is successively opened, is passed through by tracheae one into molten lithium tank
The inert gas of 0.02MPa, heater toast outlet to molten lithium tank, lithium pipe, lithium valve and plug, and baking temperature is set as
300 DEG C, it is carried out continuously 12h；
(2) lithium valve is closed, inert gas air pressure is adjusted to 0.2MPa, feeding port is opened, to molten lithium under atmosphere of inert gases protection
90g lithium stick is put into tank, closes feeding port, is then opened vent valve and is released inert gas extra in molten lithium tank；
(3) after feeding intake, due to the fusing of solid lithium stick, the temperature of molten lithium tank can first drop to be risen afterwards, lithium tank fusion, lithium pipe and plug
Temperature rises to 300 DEG C of preset temperature, and remains stable；
(4) it places the beaker immediately below plug, plug is put in beaker and at rim of a cup 1/4, the liquid level and plug of coolant
Surface contact；
(5) straight-through valve is closed, charge valve is opened, preset pressure value is opened and heated up and raised gas in the molten lithium tank of vent valve emptying
Pressure；
(6) lithium valve is opened, and opens straight-through valve, the liquid lithium after compression is quickly ejected into coolant by the laser hole of plug
In, generate lithium ball；
(7) lithium valve is closed after liquid lithium has sprayed in lithium pipe, collects the lithium ball of coolant surface flotation；
(8) aperture of regulating step (3) preset temperature, step (5) preset pressure and laser hole controls the size of lithium ball.
2. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the indifferent gas
Body storage cylinder is argon bottle, and inert gas is argon gas.
3. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the molten lithium tank
It is SUS316 seamless pipe, hand operated gate valve is installed at the feeding port.
4. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the lithium pipe is
SUS316 seamless pipe, both ends are connect with molten lithium tank and lithium valve respectively；The tracheae one and tracheae two is SUS316 seamless pipe,
Tracheae one and tracheae two are tank connected with molten lithium by welding.
5. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the lithium valve is
Lithium pipe and plug are tightly connected by bellows valve, valve body material SUS316 by clamping sleeve blow-out patch.
6. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the charge valve
It include pressure reducing valve and pressure gauge, pressure reducing valve air inlet is connected with inert gas storage cylinder, and gas outlet is connect with tracheae one, pressure
Inert gas air pressure after table measurement decompression；The straight-through valve is ball valve；The vent valve is the angle valve with flange-interface,
It is docked by flange with tracheae two, another flange is opened wide and is communicated with the atmosphere.
7. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the heater
It include DC power supply and Duo Gen armouring heater strip, the technical parameter of the DC power supply is AC 220V/10A input, three tunnels
DC 0-220V/0-10A output；More armouring heater strips are respectively wound around the outside of molten lithium tank, lithium pipe and plug, and cloth respectively
Thermocouple temperature measurement is set, is then wrapped up with aluminium-foil paper.
8. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the plug is
Hollow SUS316 cylindrical body open at one end, open end are connect with lithium valve, and the other end wears erosion laser using the technique of laser boring
Hole.
9. a kind of fast preparation method of multiple dimensioned lithium ball according to claim 1, it is characterised in that: the coolant
It is atoleine.
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| CN111063458A (en) * | 2019-12-25 | 2020-04-24 | 中国科学院合肥物质科学研究院 | Device and method for accurately calibrating plasma injection impurities |
| CN111081389A (en) * | 2019-12-09 | 2020-04-28 | 中国科学院合肥物质科学研究院 | Mechanism and method for injecting plasma impurities into fusion device |
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| CN109773199B (en) | 2021-05-28 |
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