CN109482892A - A kind of production method and process units of Li-Si alloy - Google Patents
A kind of production method and process units of Li-Si alloy Download PDFInfo
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- CN109482892A CN109482892A CN201811624922.4A CN201811624922A CN109482892A CN 109482892 A CN109482892 A CN 109482892A CN 201811624922 A CN201811624922 A CN 201811624922A CN 109482892 A CN109482892 A CN 109482892A
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- 229910000676 Si alloy Inorganic materials 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 230000008569 process Effects 0.000 title claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 60
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 27
- 230000008018 melting Effects 0.000 claims abstract description 25
- 238000002844 melting Methods 0.000 claims abstract description 24
- 239000011261 inert gas Substances 0.000 claims abstract description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000013019 agitation Methods 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000005469 granulation Methods 0.000 claims abstract description 5
- 230000003179 granulation Effects 0.000 claims abstract description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 50
- 229910052786 argon Inorganic materials 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 24
- 239000007921 spray Substances 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 15
- 239000000498 cooling water Substances 0.000 claims description 12
- 238000004321 preservation Methods 0.000 claims description 11
- 230000003134 recirculating effect Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 239000000443 aerosol Substances 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 238000000889 atomisation Methods 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 6
- 229910045601 alloy Inorganic materials 0.000 abstract description 4
- 239000000956 alloy Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 238000010907 mechanical stirring Methods 0.000 abstract description 2
- 238000006467 substitution reaction Methods 0.000 abstract description 2
- 238000010410 dusting Methods 0.000 abstract 1
- 238000010309 melting process Methods 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 229910001148 Al-Li alloy Inorganic materials 0.000 description 4
- 229910008290 Li—B Inorganic materials 0.000 description 2
- ZVLDJSZFKQJMKD-UHFFFAOYSA-N [Li].[Si] Chemical compound [Li].[Si] ZVLDJSZFKQJMKD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910007857 Li-Al Inorganic materials 0.000 description 1
- 229910008447 Li—Al Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000012387 aerosolization Methods 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000320 mechanical mixture Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F9/082—Making 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F9/082—Making 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
- B22F2009/0848—Melting process before atomisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F9/082—Making 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
- B22F2009/088—Fluid nozzles, e.g. angle, distance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F9/082—Making 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
- B22F2009/0888—Making 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 casting construction of the melt process, apparatus, intermediate reservoir, e.g. tundish, devices for temperature control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making 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
- B22F9/082—Making 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
- B22F2009/0896—Making 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 particle transport, separation: process and apparatus
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Abstract
The present invention relates to materialogy fields, more particularly to the production method and process units of a kind of Li-Si alloy.Then the present invention dusts raw material lithium and silicon powder melting in proportion the method powder of granulation using inert gas atomizer, melting-powder integral type processed is completed.The production method of Li-Si alloy of the present invention, realizes continuous production, improves production efficiency；Melting and pulverizing process carry out in vacuum protection cover, and substitute mechanical stirring using electromagnetic agitation, are atomized granulation substitution Mechanical Crushing of dusting and are granulated; reduce the introducing of impurity; entire production process is safe and stable, and it is high to obtain powder rate for the alloy powder even particle size distribution of preparation.
Description
Technical field
The present invention relates to materialogy fields, more particularly to the production method and process units of a kind of Li-Si alloy.
Background technique
In thermal cell, thermal cell anode material usually used at present mainly has Li-Al, Li-Si and Li-B alloy.Its
In, Li-Al alloy is the single solid solution phase composition for being 20wt% by an amount containing lithium, therefore its discharge mechanism is fairly simple, only
Show a voltage platform.The lithium content and discharge capacity of Li-B alloy are higher than Li-Si alloy, but because its high activity leads to it
There are security risks in thermal cell work, therefore large-scale promotion does not use.Li-Si alloy is the sun of the step of electric discharge more than one
Pole material can use several voltage platforms in thermal cell design using the flash-over characteristic of Li-Si alloy plurality of voltage platforms,
Therefore its total capacity ratio Li-Al alloy is big, and its large current discharging capability is strong, electrode potential ratio Li-Al alloy is low, comprehensive
Li-Al alloy can be significantly better than.Therefore make the thermal cell of negative electrode material with Li-Si alloy, the more other thermal cell systems of meeting have peace
Quan Xinggao, discharge power are big, specific energy is high, activation is rapid, period of storage is long and it is compact-sized the advantages that.
There are mainly two types of currently used Li-Si alloy powder preparation methods: one is by by high-purity lithium and silicon powder
After mechanical mixture melting, Li-Si Alloy Powder is obtained after grinding is mechanically pulverized in obtained Li-Si alloy ingot；Another method be by
High-purity lithium powder obtains Li-Si Alloy Powder after grinding is mechanically pulverized after being sintered under high temperature or high pressure after mixing in proportion with silicon powder.
It will be appreciated, however, that due to Li-Si alloy have very high activity, it is therefore desirable to full of argon gas glove box in into
Row preparation, the Li-Si alloy of preparation is at high cost, complex process, yield and safety are low, is not suitable for large-scale production.
Summary of the invention
The present invention provided aiming at above-mentioned defect it is a kind of it is safe and reliable, totally-enclosed it is pollution-free, can stablize and criticize
The production method of amount synthesis Li-Si alloy.The present invention realizes the conjunction of lithium silicon using vacuum induction melting, inert gas atomizer technology
Golden melting-powder integral type processed is completed, and is simplified technique, is improved the safety of equipment operation, ensure that and prepare the high-purity of product
Degree and particle size uniformity.
A kind of preparation method technical solution of Li-Si alloy powder of the invention are as follows: a kind of production method of Li-Si alloy,
The following steps are included: by the melting in proportion of raw material lithium and silicon powder, then dusted the method powder of granulation using inert gas atomizer,
Melting-powder integral type processed is completed, specifically includes the following steps:
(1) raw material lithium and silicon powder are fitted into melting kettle in proportion, seal logical argon and replaces to water, oxygen content≤10PPm.
(2) electromagnetic heater is opened, temperature programming is controlled to 300-400 DEG C, opens recirculating cooling water system；Open low frequency
Magnetic stirrer is continuously heating to 700-800 DEG C, and constant temperature stirs 20-60min.
(3) Li-Si alloy that above-mentioned reaction obtains being transferred in heat preservation crucible, control temperature is constant at 700-800 DEG C,
Control melt is entered at the high-pressure inert gas nozzle of spray chamber by diversion pipe, and high-speed flow impact grinding melt is atomized into liquid
Li-Si alloy powder is frozen into after drop.
(4) the Li-Si alloy powder obtained collects another part powder in level-one powder container by cyclone separation system
End is collected in second level powder container, and gas part is discharged after filtering via accurate filter.
The form of raw material lithium is one or more of lithium grain, lithium piece or lithium ingot, purity >=99% in the step (1)；
The raw material silicon powder is purity >=99.9%, and the granularity of silicon powder is 100-500 mesh.
Raw material order of addition is lithium after first silicon in the step (1).
It is 65-100% that lithium metal gross mass is added in the step (1) and accounts for the percentage of addition raw silicon quality.
In the step (2), the power for controlling electromagnetic heater in reaction process is 30-50KW, recirculated cooling water
Flow is 30-80m3/ h, electromagnetic agitation frequency are as follows: 1-20HZ, electromagnetic agitation electric current are 200-500A.
In the step (3), the flow of control atomization process mesohigh inert gas is 1-50m3/min。
In the step (4), the partial size of Li-Si alloy powder product collected by vacuum aerosolization is 40-300 mesh.
The invention also discloses a kind of process units of Li-Si alloy, including device noumenon, it is arranged on described device ontology
There are sealing cover and cooling jacket, the water inlet of the cooling jacket is connect with recirculating cooling water system；Described device ontology includes
Working chamber and spray chamber are provided with melting kettle and heat preservation crucible in the working chamber, and the melting kettle bottom is provided with low
Frequency magnetic stirrer；The argon gas import for being provided with vacuum orifice in the working chamber and being connected to high-purity argon gas source；The atomization
Ceiling portion is provided with high-pressure inert gas nozzle, and the air inlet of the high-pressure inert gas nozzle is connected to high-purity argon gas source, institute
The feed inlet for stating high-pressure inert gas nozzle is connect by diversion pipe with the discharge port for keeping the temperature crucible bottom；The spray chamber bottom
It is provided with second level powder container, aerosol outlet, the aerosol outlet and cyclone separation system are provided in the spray chamber
Feed inlet connection, the discharge port of the cyclone separation system bottom connect with level-one powder container, the cyclone separation system
Gas outlet connect with accurate filter.
Beneficial effect
Compared with the method for Li-Si Alloy Powder is prepared by Mechanical Crushing again after traditional method of smelting prepares Li-Si alloy ingot,
The production method of Li-Si alloy of the present invention realizes the conjunction of lithium silicon using vacuum induction melting, inert gas atomizer technology
Golden melting-powder integral type processed is completed, and is realized continuous production, is simplified technique, improves production efficiency；Melting and powder mistake processed
Cheng Jun is carried out in vacuum protection cover, and substitutes mechanical stirring using electromagnetic agitation, improves the safety of equipment operation；This hair
Bright atomization, which is dusted, is granulated substitution Mechanical Crushing granulation, reduces the introducing of impurity, entire production process is safe and stable, preparation
Alloy powder even particle size distribution, it is high to obtain powder rate, ensure that the high-purity and particle size uniformity for preparing product.
Detailed description of the invention:
Fig. 1 show the structural schematic diagram of Li-Si Alloy Powder process units of the present invention；
In figure, 1. working chambers, 2. spray chambers, 3. sealing covers, 4. high-purity argon gas sources, 5. first pressure regulator valves, 6. melting kettles, 7. electricity
Magnetic heater, 8. recirculating cooling water systems, 9. magnetic stirrers, 10. heat preservation crucibles, 11. diversion pipes, 12. high-pressure inert gas
Nozzle, 13. second pressure regulator valves, 14. cyclone separation systems, 15. level-one powder containers, 16. second level powder containers, 17. accurate mistakes
Filter, 18. cooling jackets.
Specific embodiment:
For a better understanding of the present invention, below with specific example come the technical solution that the present invention will be described in detail, but it is of the invention
It is not limited thereto.
The form of the raw materials used lithium of following embodiment is one or more of lithium grain, lithium piece or lithium ingot, purity >=99%；
The raw material silicon powder is purity >=99.9%, and the granularity of silicon powder is 100-500 mesh.
Embodiment 1
As shown in Figure 1, a kind of process units of Li-Si alloy, including device noumenon, sealing cover 3 is provided on described device ontology
It is connect with the water inlet of cooling jacket 18, the cooling jacket with recirculating cooling water system 8；Described device ontology includes working chamber
1 and spray chamber 2, melting kettle 6 and heat preservation crucible 10 are provided in the working chamber 1, and the melting kettle bottom is provided with electricity
Magnetic stirrer 9；The argon gas import for being provided with vacuum orifice in the working chamber and being connected to high-purity argon gas source 4；The spray chamber
Top is provided with high-pressure inert gas nozzle 12, and the air inlet of the high-pressure inert gas nozzle is connected to 4 with high-purity argon gas source, institute
The feed inlet for stating high-pressure inert gas nozzle is connect by diversion pipe 11 with the discharge port for keeping the temperature 10 bottom of crucible；The spray chamber
2 bottoms are provided with second level powder container 16, and aerosol outlet, the aerosol outlet and whirlwind point are provided in the spray chamber
Feed inlet connection from system 14, the discharge port of the cyclone separation system bottom are connect with level-one powder container 15, the rotation
The gas outlet of wind separation system is connect with accurate filter 17.
Embodiment 2
A kind of production method of Li-Si alloy, comprising the following steps:
(1) 1.3kg, 200 mesh silicon powders are first packed into 6 bottom of melting kettle in working chamber 1, then 1kg lithium grain is packed into melting earthenware
Adjusted in crucible 6, after sealing the first pressure regulator valve 5 control high-purity argon gas source 4 argon flow lead to argon replace to water, oxygen content≤
10PPm。
(2) electromagnetic heater 7 is opened, controls temperature programming to 300 DEG C；Recirculating cooling water system 8 is opened, control flow is
30m3/h；Low frequency electromagnetic blender 9 is opened, control electromagnetic agitation frequency is 10HZ, and electromagnetic agitation electric current is 200A, continues to heat up
To 700 DEG C, constant temperature stirs 40min.
(3) Li-Si alloy that above-mentioned reaction obtains is transferred in heat preservation crucible 10, control temperature is constant at 750 DEG C, control
Melt processed is entered by diversion pipe 11 at the high-pressure inert gas nozzle 12 of spray chamber 2, and the second pressure regulator valve 13 control high speed is adjusted
Air-flow is with 20m3/ min impact grinding melt is frozen into Li-Si alloy powder after being atomized into drop.
(4) the 100-200 mesh Li-Si alloy powder obtained is collected by cyclone separation system 14 in level-one powder container 15
In, another part powder is collected in second level powder container 16, and gas part is discharged after filtering via accurate filter 17.
Embodiment 3
A kind of production method of Li-Si alloy, comprising the following steps:
(1) 1kg, 200 mesh silicon powders are first packed into 6 bottom of melting kettle in working chamber 1, then 1kg lithium grain is packed into melting kettle 6
In, the logical argon of argon flow that the first pressure regulator valve 5 control high-purity argon gas source 4 is adjusted after sealing is replaced to water, oxygen content≤10PPm.
(2) electromagnetic heater 7 is opened, controls temperature programming to 350 DEG C；Recirculating cooling water system 8 is opened, control flow is
35m3/h；Low frequency electromagnetic blender 9 is opened, control electromagnetic agitation frequency is 12HZ, and electromagnetic agitation electric current is 250A, continues to heat up
To 750 DEG C, constant temperature stirs 50min.
(3) Li-Si alloy that above-mentioned reaction obtains is transferred in heat preservation crucible 10, control temperature is constant at 800 DEG C, control
Melt processed is entered by diversion pipe 11 at the high-pressure inert gas nozzle 12 of spray chamber 2, and the second pressure regulator valve 13 control high speed is adjusted
Air-flow is with 30m3/ min impact grinding melt is frozen into Li-Si alloy powder after being atomized into drop.
(4) the 50-150 mesh Li-Si alloy powder obtained is collected by cyclone separation system 14 in level-one powder container 15
In, another part powder is collected in second level powder container 16, and gas part is discharged after filtering via accurate filter 17.
Embodiment 4
A kind of production method of Li-Si alloy, comprising the following steps:
1) 2kg, 300 mesh silicon powders are first packed into indoor 6 bottom of melting kettle of melting, then 1.6kg lithium grain is packed into melting kettle 6
In, the logical argon of argon flow that the first pressure regulator valve 5 control high-purity argon gas source 4 is adjusted after sealing is replaced to water, oxygen content≤10PPm.
(2) electromagnetic heater 7 is opened, controls temperature programming to 300 DEG C；Recirculating cooling water system 8 is opened, control flow is
30m3/h；Low frequency electromagnetic blender 9 is opened, control electromagnetic agitation frequency is 15HZ, and electromagnetic agitation electric current is 230A, continues to heat up
To 700 DEG C, constant temperature stirs 60min.
(3) Li-Si alloy that above-mentioned reaction obtains is transferred in heat preservation crucible 10, control temperature is constant at 750 DEG C, control
Melt processed is entered by diversion pipe 11 at the high-pressure inert gas nozzle 12 of spray chamber 2, and the second pressure regulator valve 13 control high speed is adjusted
Air-flow is with 25m3/ min impact grinding melt is frozen into Li-Si alloy powder after being atomized into drop.
(4) the 100-200 mesh Li-Si alloy powder obtained is collected by cyclone separation system 14 in level-one powder container 15
In, another part powder is collected in second level powder container 16, and gas part is discharged after filtering via accurate filter 17.
Embodiment 5
A kind of production method of Li-Si alloy, comprising the following steps:
1) 1.5kg, 250 mesh silicon powders are first packed into 6 bottom of melting kettle in working chamber 1, then 1kg lithium grain is packed into melting kettle
The logical argon of argon flow that the first pressure regulator valve 5 control high-purity argon gas source 4 is adjusted in 6, after sealing is replaced to water, oxygen content≤10PPm.
(2) electromagnetic heater 7 is opened, controls temperature programming to 400 DEG C；Recirculating cooling water system 8 is opened, control flow is
30m3/h；Low frequency electromagnetic blender 9 is opened, control electromagnetic agitation frequency is 20HZ, and electromagnetic agitation electric current is 300A, continues to heat up
To 750 DEG C, constant temperature stirs 40min.
(3) Li-Si alloy that above-mentioned reaction obtains is transferred in heat preservation crucible 10, control temperature is constant at 750 DEG C, control
Melt processed is entered by diversion pipe 11 at the high-pressure inert gas nozzle 12 of spray chamber 2, and the second pressure regulator valve 13 control high speed is adjusted
Air-flow is with 25m3/ min impact grinding melt is frozen into Li-Si alloy powder after being atomized into drop.
(4) the 100-200 mesh Li-Si alloy powder obtained is collected by cyclone separation system 14 in level-one powder container 15
In, another part powder is collected in second level powder container 16, and gas part is discharged after filtering via accurate filter 17.
Claims (9)
1. a kind of production method of Li-Si alloy, which comprises the following steps: melt raw material lithium and silicon powder in proportion
Refining, is then dusted the method powder of granulation using inert gas atomizer, and melting-powder integral type processed is completed.
2. the production method of Li-Si alloy according to claim 1, which is characterized in that specifically includes the following steps:
(1) raw material lithium and silicon powder are fitted into melting kettle in proportion, be passed through after sealing argon gas replace to system water, oxygen content≤
10PPm；
(2) electromagnetic heater is opened, control is warming up to 300-400 DEG C, opens recirculating cooling water system；Open low frequency electromagnetic stirring
Device is continuously heating to 700-800 DEG C, and constant temperature stirs 20-60min, obtains Li-Si alloy；
(3) obtained Li-Si alloy is transferred in heat preservation crucible, control temperature is constant at 700-800 DEG C, then control heat preservation
Melt in crucible is entered at the high-pressure inert gas nozzle of spray chamber by diversion pipe, the atomization of high-speed flow impact grinding melt
At being frozen into Li-Si alloy powder after drop；
(4) the Li-Si alloy powder obtained is collected in level-one powder container by cyclone separation system, and another part powder is received
Collection in the second level powder container of spray chamber bottom, discharge after filtering via accurate filter by gas part.
3. the production method of Li-Si alloy according to claim 2, which is characterized in that raw material lithium in the step (1)
Form be one or more of lithium grain, lithium piece or lithium ingot, purity >=99%；The raw material silicon powder is purity >=99.9%,
The granularity of silicon powder is 100-500 mesh.
4. the production method of Li-Si alloy according to claim 2, which is characterized in that raw material adds in the step (1)
Add sequence that lithium is then added for silicon is first added.
5. a kind of production method of Li-Si alloy according to claim 2, which is characterized in that add in the step (1)
It is 65-100% that the gross mass for entering lithium metal, which accounts for and the percentage of raw silicon quality is added,.
6. a kind of production method of Li-Si alloy according to claim 2, which is characterized in that in the step (2), control
The power of electromagnetic heater is 30-50KW in reaction process processed, and the flow of recirculated cooling water is 30-80m3/ h, electromagnetic agitation frequency
Rate are as follows: 1-20HZ, electromagnetic agitation electric current are 200-500A.
7. a kind of production method of Li-Si alloy according to claim 2, which is characterized in that in the step (3), control
The flow of atomization process mesohigh inert gas processed is 1-50m3/min。
8. a kind of production method of Li-Si alloy according to claim 2, which is characterized in that in the step (4), institute
The partial size of the Li-Si alloy powder product of collection is 40-300 mesh.
9. a kind of process units of Li-Si alloy, which is characterized in that including device noumenon, sealing is provided on described device ontology
Lid and cooling jacket, the water inlet of the cooling jacket are connect with recirculating cooling water system；Described device ontology includes working chamber
And spray chamber, melting kettle and heat preservation crucible are provided in the working chamber, the melting kettle bottom is provided with low frequency electromagnetic
Blender；The argon gas import for being provided with vacuum orifice in the working chamber and being connected to high-purity argon gas source；At the top of the spray chamber
It is provided with high-pressure inert gas nozzle, the air inlet of the high-pressure inert gas nozzle is connected to high-purity argon gas source, the high pressure
The feed inlet of inert gas nozzle is connect by diversion pipe with the discharge port for keeping the temperature crucible bottom；The spray chamber bottom is provided with
Second level powder container is provided with aerosol outlet, the charging of the aerosol outlet and cyclone separation system in the spray chamber
Mouth connection, the discharge port of the cyclone separation system bottom are connect with level-one powder container, the outlet of the cyclone separation system
Mouth is connect with accurate filter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811624922.4A CN109482892B (en) | 2018-12-28 | 2018-12-28 | Production method and production device of lithium silicon alloy |
Applications Claiming Priority (1)
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