CN107225252A - A kind of passivation of lithium microballoon production method - Google Patents

A kind of passivation of lithium microballoon production method Download PDF

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Publication number
CN107225252A
CN107225252A CN201710613292.XA CN201710613292A CN107225252A CN 107225252 A CN107225252 A CN 107225252A CN 201710613292 A CN201710613292 A CN 201710613292A CN 107225252 A CN107225252 A CN 107225252A
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China
Prior art keywords
lithium
metal
passivation
tank
microballoon
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CN201710613292.XA
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Chinese (zh)
Inventor
贾振勇
陈强
牟瀚波
程滋平
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TIANJIN CHINA ENERGY LITHIUM CO Ltd
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TIANJIN CHINA ENERGY LITHIUM CO Ltd
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Priority to CN201710613292.XA priority Critical patent/CN107225252A/en
Publication of CN107225252A publication Critical patent/CN107225252A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14Treatment of metallic powder
    • B22F1/145Chemical treatment, e.g. passivation or decarburisation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/10Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying using centrifugal force
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/02Making metallic powder or suspensions thereof using physical processes
    • B22F9/06Making metallic powder or suspensions thereof using physical processes starting from liquid material
    • B22F9/08Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
    • B22F9/082Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
    • B22F2009/086Cooling after atomisation
    • B22F2009/0876Cooling after atomisation by gas

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

The invention discloses a kind of production method of passive metal lithium microballoon, using following steps:One) drying for filling lithium metal protective gas using vacuumizing, which melts lithium tank and heats lithium metal ingot, is melt into liquid metal lithium to it;Two) passive metal lithium microballoon is prepared in passivation tank, specific method is:Cooling passivation air-flow is formed in the passivation tank, the cooling passivation air-flow is formed by lithium metal protection gas mixing passivator;Liquid metal lithium is atomized using atomizer in the passivation tank; obtain trickle lithium metal droplet distribution to fall, met in scattered dropping process with the cooling passivation air-flow, be frozen into lithium metal microballoon and reacted with passivator; diaphragm is formed on surface, passive metal lithium microballoon is obtained.The present invention uses dry production, and process route is simple, solvent need not be used in preparation process, the lithium metal microsphere surface of preparation is cleaner.

Description

A kind of passivation of lithium microballoon production method
Technical field
The invention belongs to secondary cell field, more particularly to a kind of passive metal lithium microballoon production method.
Background technology
In recent years, as the electric equipment products such as smart mobile phone, tablet personal computer, electric automobile are to high-energy-density electrochmical power source Demand, the specific capacity to secondary cell requires also more and more higher.But existing secondary cell by material because being limited, specific capacity hair Open up space limited, therefore, be badly in need of the battery material of research high power capacity.Passive metal lithium microspheres quality is light, and electrode potential is low, as The cell negative electrode material of high power capacity has many advantages, can be used as lithium-sulfur cell, lithium-air battery, lithium all-solid-state battery, lithium The negative pole of polymer battery and other secondary cells using passive metal lithium microballoon as negative pole;Passive metal lithium microballoon can be with Lithium is mended applied to anode or negative material to use, and the lithium ion of SEI films consumption is formed during supplement circulating battery, reaches and carries The effect of high battery capacity;Passive metal lithium microballoon can also as lithium ion super capacitor lithium source, improve battery appearance Amount.
Current lithium metal microballoon is mainly prepared using wet method, and it is micro- to prepare lithium metal disclosed in patent document CN101213039A The method of ball is:The lithium metal of solid is added in solvent hydrocarbon ils, heating stirring, lithium metal fusing, then pass through high-speed stirred, system It is standby to obtain lithium metal microballoon, add fluorization agent and be passivated, obtain the lithium metal microballoon for thering is lithium fluoride to protect to surface, after pass through Supercooling is filtered, and obtains the lithium metal microballoon for having hydrocarbon ils to surface, by three cleanings of solvent hexane, and solvent pentane is once cleaned, Obtain product.Wet method prepares the problem of existing:1) process route is long, and preparation process is complicated;2) product surface has a small amount of molten Agent (hydrocarbon ils, hexane, pentane) is remained, and the chemical property performance to product has a certain impact.
The content of the invention
The present invention provides a kind of passive metal lithium microballoon production method to solve technical problem present in known technology, This method need not use solvent, and the lithium metal microsphere surface of preparation is cleaner.
The present invention is adopted the technical scheme that to solve technical problem present in known technology:A kind of passive metal lithium The production method of microballoon, using following steps:One) lithium tank heating metal is melted in the drying for filling lithium metal protective gas using vacuumizing Lithium ingot is melt into liquid metal lithium to it;Two) passive metal lithium microballoon is prepared in passivation tank, specific method is:Described blunt Change and cooling passivation air-flow is formed in tank, the cooling passivation air-flow is formed by lithium metal protection gas mixing passivator;Institute State application atomizer in passivation tank to be atomized liquid metal lithium, obtain trickle lithium metal droplet distribution and fall, in scattered whereabouts During with it is described cooling passivation air-flow meet, be frozen into lithium metal microballoon and with passivator react, surface formed diaphragm, Obtain passive metal lithium microballoon.
The step one) the liquid metal lithium that obtains conveyed using the method for air pressure in the molten lithium tank of increase by conveyance conduit In to the atomizer.
Heat preservation structure is set on the conveyance conduit, its outlet temperature is met the atomization need of liquid metal lithium Ask.
The atomizer uses ultrasonic atomizer, and the outlet temperature for controlling the conveyance conduit is 200~1000 DEG C.
The atomizer uses centrifugal atomizer, and the outlet temperature for controlling the conveyance conduit is 200~800 DEG C.
The temperature that the cooling passivating gas stream enters the passivation tank is 0~80 DEG C.
The temperature that the passivation tank is controlled by using the method for cooling is 0~80 DEG C.
The present invention has the advantages and positive effects of:The lithium metal of solid-state is melt into by using dry molten lithium tank The lithium metal of liquid, and in dry passivation tank be atomized into the lithium metal of liquid under trickle lithium metal drop makes it scattered Fall, met in dropping process with cooling passivation air-flow, be cooled and be frozen into lithium metal microballoon, react micro- in lithium metal with passivator The surface of ball forms passivating film, obtains passivated lithium metal microballoon, and surface-active is relatively low.The present invention uses dry production, Process route is simple, solvent need not be used in preparation process, the lithium metal microsphere surface of preparation is cleaner, the passivation of acquisition Lithium metal microsphere diameter is 0.010~0.120mm, the product of different meshes can be sieved into according to different applications, as height Negative pole, secondary battery negative pole or the positive pole of the secondary cell of capacity mend lithium and as lithium ion super capacitor lithium source, can be greatly Improve the capacity of secondary cell in ground.And the present invention can improve production efficiency, it is ensured that product quality.
Brief description of the drawings
Fig. 1 is the structural representation of the first process units of the application present invention;
Fig. 2 is the structural representation of second of process units of the application present invention.
In figure:1st, heater I;2nd, lithium tank is melted;3rd, sifter;4th, splicing funnel;5th, cooler I;6th, it is passivated tank;7th, convey Pipeline;8th, valve;9th, heater II;10-1, ultrasonic atomizer;10-2, centrifugal atomizer;11st, filter;12nd, air exhauster; 13rd, cooler II;14th, air feed pipe, 15, backwind tube;16th, passivator atomizer;17th, collecting box;18th, transition hatch door;19th, argon gas Glove box;20th, high-speed electric expreess locomotive.
Embodiment
In order to further understand the content, features and effects of the present invention, hereby enumerating following examples, and coordinate accompanying drawing Describe in detail as follows:
Refer to Fig. 1~Fig. 2, a kind of production method of passive metal lithium microballoon, using following steps:
One) drying for filling lithium metal protective gas using vacuumizing, which melts lithium tank 2 and heats lithium metal ingot, is melt into liquid to it Lithium metal;Two) passive metal lithium microballoon is prepared in passivation tank 6, specific method is:It is blunt that cooling is formed in the passivation tank 6 Change air-flow, the cooling passivation air-flow is formed by lithium metal protection gas mixing passivator;Mist is applied in the passivation tank 6 Change device to be atomized liquid metal lithium, obtain trickle lithium metal droplet distribution and fall, with the cooling in scattered dropping process Passivation air-flow meets, and is frozen into lithium metal microballoon and is reacted with passivator, forms diaphragm on surface, obtain passive metal lithium micro- Ball.
More specifically method is, the step 2) the liquid metal lithium that obtains using air pressure in the molten lithium tank 2 of increase method It is delivered to by conveyance conduit 7 in the atomizer.Heat preservation structure is set on the conveyance conduit 7, makes its outlet temperature Degree meets the atomization demand of liquid metal lithium.The atomizer uses ultrasonic atomizer 10-1, controls going out for the conveyance conduit 7 Mouth temperature is 200~1000 DEG C.The atomizer uses centrifugal atomizer 10-2, controls the outlet temperature of the conveyance conduit 7 For 200~800 DEG C.The temperature that the cooling passivating gas stream enters the passivation tank 6 is 0~80 DEG C.By using the side of cooling Method controls the temperature of the passivation tank 6 to be 0~80 DEG C.
The application example 1 of the present invention:
Referring to Fig. 1, a kind of productions of use ultrasonic atomizer 10-1 as molten lithium atomizer passive metal lithium microballoon Device, including molten lithium tank 2 and passivation tank 6, the molten lithium tank 2 are provided with heater I 1, and the bottom of the molten lithium tank 2 passes through delivery pipe Road 7 is connected with the top of the passivation tank 6, and the export department of the conveyance conduit 7 is stretched into the passivation tank 6, described blunt Change the top in tank 6 and be fixed with the ultrasonic atomizer 10-1 being connected with conveyance conduit outlet, the passivation tank 6 is cooled down provided with air-flow The circulatory system, the bottom in the passivation tank 6 is provided with the sifter 3 and collecting box 17 being mutually linked, and the collecting box 17 is set Put in the lower section of the sifter 3, transition hatch door 18 is provided with the side wall of passivation tank 6 bottom.
In this example, in order that cooling passivation air-flow and the lithium metal droplet formation convection current of scattered whereabouts, improve passivation Quality, the air-flow cooling recirculation system includes backwind tube 15, air exhauster 12, cooler II 13 and the air feed pipe being sequentially connected 14, the air feed pipe 14 is horizontally set on the bottom in the passivation tank 6, provided with outlet, described time on the air feed pipe 14 Airduct 15 is connected with the top of the passivation tank 6, and filter 11 is provided with the backwind tube 15, and filter 11 is arranged on described The end of backwind tube 15, in the passivation tank 6, the air exhauster 12 and the cooler II 13 are arranged on the passivation tank 6 outside.The use of on-gaseous passivator for convenience, the air-flow cooling recirculation system also includes passivator atomizer 16, The air-flow cooling recirculation system includes the backwind tube 15 being sequentially connected, the air exhauster 12, the cooler II 13, institute Passivator atomizer 16 and the air feed pipe 14 are stated, the passivator atomizer 16 is arranged on the outside of the passivation tank 6.Using The passivator of on-gaseous is atomized by the passivator atomizer 16, passivator is mixed into lithium metal protection gas with steam form, is used Air-flow is passivated in forming cooling.For the ease of the conveying and atomization of lithium metal liquid, in the outside of the conveyance conduit 7 provided with insulation Heating arrangement, the temperature for making conveyance conduit 7 is 200~300 DEG C, and heater II is provided with the export department of the conveyance conduit 7 9, the temperature for making the exit of conveyance conduit 7 is 200~1000 DEG C.In order to prevent trickle lithium metal drop in the mistake of scattered whereabouts Sticked in journey on tank skin, be provided with cooler I 5 on the outside of the middle part of the passivation tank 6, the temperature for making passivation tank is 0~80 DEG C. In order that cooling passivation air-flow is distributed more uniformly across in the horizontal, the air feed pipe 14 uses loop configuration, in annular air feed Pipe is provided with multiple outlets upward.In this example, the discharging portion of the passivation tank 6 is installed in the passivation tank 6 Interior splicing funnel 4, the splicing funnel 4 is located at below the outlet of the air-flow cooling recirculation system.The product screening is received Collect the inside that equipment is arranged on the passivation tank 6, including the sifter 3 and collecting box 17 being connected successively from top to bottom, the sieve Device 3 is divided to be located at the lower section of the splicing funnel 4, the two linking.In order to adjust the flow of control liquid metal lithium, in the conveying Pipeline 7 is provided with valve 8, and the outside of valve 8 is provided with Heat preservation structure.
The course of work and principle to this example 1 exemplified by using on-gaseous passivator are described as follows:
Lithium ingot is removed after packaging, adds dry molten lithium tank 2, and lithium metal protection gas, in this example, gold are filled after vacuumizing Belong to lithium and protect gas frequently with argon gas.Start heater I 1, by heating lithium metal to melting;Then add in the interior argon gas of molten lithium tank 2 0.005~0.1Mp is pressed, liquid metal lithium is entered in passivation tank 6 by conveyance conduit 7 through valve 8, in passivation tank 6 now Through being formed with cooling passivation air-flow.Conveyance conduit 7 and valve 8 need heating and thermal insulation to 200~300 DEG C;II 9 pairs of conveyings of heater Export department's heating of pipeline 7, it is 200~1000 DEG C to make the temperature at this.The high-temperature metal gone out from the export department's drip of conveyance conduit 7 Lithium liquid enters ultrasonic atomizer 10-1, and the frequency for controlling ultrasonic atomizer is 10~100KHz, and high-temperature metal lithium liquid is atomized into Trickle lithium metal droplet distribution falls.Simultaneously be passivated tank 6 in cooling passivating gas flow through air exhauster 12 be pressurized, cooler II 13 Cooling, into passivator atomizer 16, enters air feed pipe after the passivator of steam form after atomization is mixed into cooling passivation air-flow 14, the outlet through air feed pipe 14 controls 14 exits of air feed pipe cold in the bottom discharge of passivation tank 6 by adjusting cooler II 13 But the temperature of passivation air-flow is 0~80 DEG C.In the presence of air exhauster 12, cooling passivation air-flow slowly equably rises, with dividing The trickle lithium metal droplet formation convection current of whereabouts is dissipated, trickle lithium metal drop is frozen into the presence of cooling passivation air-flow Lithium metal microballoon, while being reacted with the passivator of steam form in cooling passivation air-flow in surface formation diaphragm, is passivated Lithium metal microballoon.Passive metal lithium microballoon falls into sifter 3 through splicing funnel 4 and sieved, and the product of particle diameter falls needed for obtaining Enter collecting box 17.Collecting box 17 can be taken out with the transition hatch door 18 on passivated tank 6.
The application example 2 of the present invention:
Referring to Fig. 2, a kind of productions of use centrifugal atomizer 10-2 as molten lithium atomizer passive metal lithium microballoon Device, including molten lithium tank 2 and passivation tank 6, the molten lithium tank 2 are provided with heater I 1, and the bottom of the molten lithium tank 2 passes through delivery pipe Road 7 is connected with the top of the passivation tank 6, and the export department of the conveyance conduit 7 is stretched into the passivation tank 6, described blunt Change the top in tank 6 and be fixed with the centrifugal atomizer 10-2 being connected with conveyance conduit outlet, the passivation tank 6 is cooled down provided with air-flow The circulatory system, discharging opening, the discharging opening of the passivation tank 6 and entering for argon gas glove box 19 are provided with the bottom of the passivation tank 6 Material mouth is tightly connected, provided with the sifter 3 and collecting box 17 being mutually linked, the collecting box 17 in the argon gas glove box 19 The lower section of the sifter 3 is arranged on, the sifter 3 is connected with the discharging opening of the passivation tank 6, in the argon gas glove box 19 are provided with transition hatch door 18.
In this example, in order that cooling passivation air-flow and the lithium metal droplet formation convection current of scattered whereabouts, improve passivation Quality, the air-flow cooling recirculation system includes backwind tube 15, air exhauster 12, cooler II 13 and the air feed pipe being sequentially connected 14, the outlet of the air feed pipe 14 stretches to the bottom being passivated in tank 6, the top of the backwind tube 15 and the passivation tank 6 Portion is connected, and filter 11 is provided with the backwind tube 15, the air exhauster 12 and the cooler II 13 are arranged on described blunt Change the outside of tank 6.The use of on-gaseous passivator for convenience, the air-flow cooling recirculation system also includes passivator atomizer 16, the air-flow cooling recirculation system includes the backwind tube 15, the air exhauster 12, the cooler II being sequentially connected 13rd, the passivator atomizer 16 and air feed pipe 14, the passivator atomizer 16 are arranged on the outside of the passivation tank 6.For It is easy to the conveying and atomization of lithium metal liquid, Heat preservation structure is provided with the outside of the conveyance conduit 7, for ensures conveying The temperature in the exit of pipeline 7 is 200~800 DEG C.In order to prevent the adhesion during scattered whereabouts of trickle lithium metal drop On tank skin, cooler I 5 is provided with the outside of the middle part of the passivation tank 6, for ensureing that the temperature of passivation tank is relatively low, tank is passivated Temperature be advisable with 0~80 DEG C.In order to ensure that production is smooth, the passivation tank 6 uses the small olive-type structure broad in the middle in two. In this example, the discharging portion of the passivation tank 6 is the discharging opening for being arranged on its bottom, and the product screening collecting device is installed In the lower section of the passivation tank, including argon gas glove box 19 and sifter 3 and receipts in the argon gas glove box 19 Header 17, the feeding mouth of the discharging opening and the argon gas glove box 19 of the passivation tank 6 is tightly connected, and the collecting box 17 is set In the lower section of the sifter 3, the sifter 3 is connected with the discharging opening of the passivation tank 6, on the argon gas glove box 19 Provided with transition hatch door 18.In order to adjust the flow of control liquid metal lithium, valve 8, valve 8 are provided with the conveyance conduit 7 Outside be provided with Heat preservation structure.
The course of work and principle to this example exemplified by using on-gaseous passivator are described as follows:
Lithium ingot is removed after packaging, adds dry molten lithium tank 2, and lithium metal protection gas, in this example, gold are filled after vacuumizing Category lithium protection gas uses argon gas.Start heater I 1, by heating lithium metal to melting;Then argon pressurization is used in molten lithium tank 2 0.005~0.1Mp, liquid metal lithium is entered in passivation tank 6 by conveyance conduit 7 through valve 8, in passivation tank 6 now It is formed with cooling passivation air-flow.Conveyance conduit 7 and valve 8 need heating and thermal insulation, and the temperature for making the exit of conveyance conduit 7 is 200 ~800 DEG C;The high-temperature metal lithium liquid gone out from the outlet of conveyance conduit 7 drip enters centrifugal atomizer 10-2, centrifugal atomizer 10-2 Driven by high-speed electric expreess locomotive 20, the rotating speed of high-speed electric expreess locomotive 20 is up to 1~80,000 revs/min.High-temperature metal lithium liquid is by centrifugal atomizer 10-2 Trickle lithium metal droplet distribution is atomized into fall.The cooling passivating gas being passivated simultaneously in tank 6 flows through air exhauster 12 and is pressurized, through cold But device II 13 is cooled down, into passivator atomizer 16, the passivator of steam form after atomization is mixed into cooling passivation air-flow laggard Enter air feed pipe 14, through being discharged for wind tube outlet in the bottom of passivation tank 6, control air feed pipe 14 to export by adjusting cooler II 13 The temperature of place's cooling passivation air-flow is 0~80 DEG C.In the presence of air exhauster 12, cooling passivation air-flow slowly equably rises, With the trickle lithium metal droplet formation convection current of scattered whereabouts, trickle lithium metal drop coagulates in the presence of cooling passivation air-flow Consolidate into lithium metal microballoon, while forming diaphragm, acquisition on surface with the passivator reaction of steam form in cooling passivation air-flow Passive metal lithium microballoon.Passive metal lithium microballoon is by being passivated the screening that the discharging opening of the bottom of tank 6 is fallen into argon gas glove box 19 Device 3 is sieved, and the product of particle diameter falls into collecting box 17 needed for obtaining.Collecting box 17 can be through the transition on argon gas glove box 19 Hatch door 18 takes out.
In the present invention, it is that the lithium metal protection gas incorporation passivator in passivation tank is formed that above-mentioned cooling, which is passivated air-flow, , passivator be used for lithium metal microsphere surface is passivated, can using phosphoric acid class, phosphoric acid ester, sulfuric acid, thio-alcohol, Type siloxane, fluorine-containing compound and atoleine etc., it would however also be possible to employ the gas such as carbon dioxide and oxygen mix.If used Gaseous state passivator, only need to directly be filled with passivation tank by gaseous state passivator, and gaseous state passivator is mixed with the lithium metal protection gas in tank, Cooling passivation air-flow is formed in the presence of air-flow cooling recirculation system, now the air-flow cooling recirculation system does not include passivation Agent atomizer 16.If using on-gaseous passivator, it is necessary to which after on-gaseous passivator is atomized, passivator atomizing steam is added Lithium metal protects gas, and cooling passivation air-flow is formed in the presence of air-flow cooling recirculation system, now the air-flow cooling circulation System should include passivator atomizer 16.Lithium metal protects gas that inertia that argon gas etc. do not react with lithium metal or stably can be used Gas.
Above-mentioned process units be there are certain requirements to the relative humidity of environment, and preferably passivation tank is placed in drying room.On Stating passive metal lithium microballoon includes doping aluminium element in passivation pure metal lithium microballoon, in addition to passivation lithium metal, element silicon, boron member The lithium alloy microballoon of the other elements such as element, magnesium elements, phosphide element, Zn-ef ficiency, doping way can use unit, binary, ternary Or multi-element doping, the content of doped chemical is 0.01%~40%.For example:It is passivated lithium-aluminium alloy microballoon, passivation of lithium magnesium boron alloy Microballoon, passivation of lithium magnesium borosilicate alloy microballoon etc..
Although the preferred embodiments of the present invention are described above in conjunction with accompanying drawing, the invention is not limited in upper The embodiment stated, above-mentioned embodiment is only schematical, be not it is restricted, this area it is common Technical staff is under the enlightenment of the present invention, in the case where not departing from present inventive concept and scope of the claimed protection, also Many forms can be made, these are belonged within protection scope of the present invention.

Claims (7)

1. a kind of production method of passive metal lithium microballoon, it is characterised in that use following steps:
One) drying for filling lithium metal protective gas using vacuumizing, which melts lithium tank and heats lithium metal ingot, is melt into liquid metal to it Lithium;
Two) passive metal lithium microballoon is prepared in passivation tank, specific method is:Cooling passivating gas is formed in the passivation tank Stream, the cooling passivation air-flow is formed by lithium metal protection gas mixing passivator;Atomizer is applied in the passivation tank Liquid metal lithium is atomized, trickle lithium metal droplet distribution is obtained and falls, is passivated in scattered dropping process with the cooling Air-flow meets, and is frozen into lithium metal microballoon and is reacted with passivator, forms diaphragm on surface, obtain passive metal lithium microballoon.
2. the production method of passive metal lithium microballoon according to claim 1, it is characterised in that the step one) obtain Liquid metal lithium be delivered to using the method for air pressure in the molten lithium tank of increase by conveyance conduit in the atomizer.
3. the production method of passive metal lithium microballoon according to claim 2, it is characterised in that on the conveyance conduit Heat preservation structure is set, its outlet temperature is met the atomization demand of liquid metal lithium.
4. the production method of passive metal lithium microballoon according to claim 3, it is characterised in that the atomizer is using super Sound atomizer, the outlet temperature for controlling the conveyance conduit is 200~1000 DEG C.
5. the production method of passive metal lithium microballoon according to claim 3, it is characterised in that the atomizer use from Heart atomizer, the outlet temperature for controlling the conveyance conduit is 200~800 DEG C.
6. the production method of passive metal lithium microballoon according to claim 1, it is characterised in that the cooling is passivated air-flow Temperature into the passivation tank is 0~80 DEG C.
7. the production method of passive metal lithium microballoon according to claim 1, it is characterised in that by using the side of cooling Method controls the temperature of the passivation tank to be 0~80 DEG C.
CN201710613292.XA 2017-07-25 2017-07-25 A kind of passivation of lithium microballoon production method Pending CN107225252A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108015294A (en) * 2017-12-13 2018-05-11 天齐锂业股份有限公司 The preparation method and device of passive metal lithium powder
CN108161016A (en) * 2017-12-13 2018-06-15 天齐锂业股份有限公司 The method for preparing passivation of lithium powder
CN108176859A (en) * 2017-12-05 2018-06-19 天齐锂业股份有限公司 The preparation method of passivation of lithium powder
CN108461724A (en) * 2018-03-05 2018-08-28 苏州大学 A kind of preparation method of high security metal composite negative pole
CN109037627A (en) * 2018-07-20 2018-12-18 浙江大学 A kind of alkali metal base composite negative pole and its application
CN109482892A (en) * 2018-12-28 2019-03-19 山东重山光电材料股份有限公司 A kind of production method and process units of Li-Si alloy
CN110148719A (en) * 2019-05-10 2019-08-20 浙江大学 The preparation method and applications of modification thin-walled multi-stage porous carbon for lithium-sulfur cell

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1311537A (en) * 2000-10-31 2001-09-05 周炳利 High specific energy mercury-free alloy zinc powder for alkaline battery, preparation method and device thereof
WO2003099920A1 (en) * 2002-05-17 2003-12-04 Polyone Corporation Composition and method for improvement of resin flow in polymer processing equipment
CN101418406A (en) * 2008-11-18 2009-04-29 天津中能锂业有限公司 Purification lithium and purification method
CN103708419A (en) * 2013-12-27 2014-04-09 北京科技大学 Method for preparing of high-activity LiH microspheres through wet process
CN104259455A (en) * 2014-09-17 2015-01-07 长沙市宇顺显示技术有限公司 Online coating production method and device of nanometer copper powder
CN105271139A (en) * 2015-04-21 2016-01-27 四川展祥特种合金科技有限公司 Method and device for preparing aluminum nitride powder through atomization
CN106450229A (en) * 2016-11-22 2017-02-22 深圳市鑫永丰科技有限公司 Lithium metal powder coated by conductive polymer and preparation method and device of lithium metal powder
CN205996194U (en) * 2016-08-31 2017-03-08 郑州机械研究所 Powder passivation equipment and its powder passivation device
CN106735274A (en) * 2017-04-08 2017-05-31 长沙唯特冶金工程技术有限公司 A kind of equipment and technique for preparing globular metallic powder
CN206316380U (en) * 2016-12-20 2017-07-11 上海四驱新能源科技有限公司 A kind of preparation facilities for preparing high stability lithium metal microsphere powder

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1311537A (en) * 2000-10-31 2001-09-05 周炳利 High specific energy mercury-free alloy zinc powder for alkaline battery, preparation method and device thereof
WO2003099920A1 (en) * 2002-05-17 2003-12-04 Polyone Corporation Composition and method for improvement of resin flow in polymer processing equipment
CN101418406A (en) * 2008-11-18 2009-04-29 天津中能锂业有限公司 Purification lithium and purification method
CN103708419A (en) * 2013-12-27 2014-04-09 北京科技大学 Method for preparing of high-activity LiH microspheres through wet process
CN104259455A (en) * 2014-09-17 2015-01-07 长沙市宇顺显示技术有限公司 Online coating production method and device of nanometer copper powder
CN105271139A (en) * 2015-04-21 2016-01-27 四川展祥特种合金科技有限公司 Method and device for preparing aluminum nitride powder through atomization
CN205996194U (en) * 2016-08-31 2017-03-08 郑州机械研究所 Powder passivation equipment and its powder passivation device
CN106450229A (en) * 2016-11-22 2017-02-22 深圳市鑫永丰科技有限公司 Lithium metal powder coated by conductive polymer and preparation method and device of lithium metal powder
CN206316380U (en) * 2016-12-20 2017-07-11 上海四驱新能源科技有限公司 A kind of preparation facilities for preparing high stability lithium metal microsphere powder
CN106735274A (en) * 2017-04-08 2017-05-31 长沙唯特冶金工程技术有限公司 A kind of equipment and technique for preparing globular metallic powder

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108176859A (en) * 2017-12-05 2018-06-19 天齐锂业股份有限公司 The preparation method of passivation of lithium powder
CN108015294A (en) * 2017-12-13 2018-05-11 天齐锂业股份有限公司 The preparation method and device of passive metal lithium powder
CN108161016A (en) * 2017-12-13 2018-06-15 天齐锂业股份有限公司 The method for preparing passivation of lithium powder
CN108015294B (en) * 2017-12-13 2024-09-20 天齐锂业股份有限公司 Method and device for preparing passivated metal lithium powder
CN108461724A (en) * 2018-03-05 2018-08-28 苏州大学 A kind of preparation method of high security metal composite negative pole
CN109037627A (en) * 2018-07-20 2018-12-18 浙江大学 A kind of alkali metal base composite negative pole and its application
CN109482892A (en) * 2018-12-28 2019-03-19 山东重山光电材料股份有限公司 A kind of production method and process units of Li-Si alloy
CN109482892B (en) * 2018-12-28 2024-01-23 山东重山光电材料股份有限公司 Production method and production device of lithium silicon alloy
CN110148719A (en) * 2019-05-10 2019-08-20 浙江大学 The preparation method and applications of modification thin-walled multi-stage porous carbon for lithium-sulfur cell

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