CN104561617B - A kind of battery grade lithium aluminium alloy synthesis device and synthetic method - Google Patents
A kind of battery grade lithium aluminium alloy synthesis device and synthetic method Download PDFInfo
- Publication number
- CN104561617B CN104561617B CN201510009586.2A CN201510009586A CN104561617B CN 104561617 B CN104561617 B CN 104561617B CN 201510009586 A CN201510009586 A CN 201510009586A CN 104561617 B CN104561617 B CN 104561617B
- Authority
- CN
- China
- Prior art keywords
- synthesis reactor
- melt tank
- heating furnace
- argon
- liquid sealing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to a kind of battery grade lithium aluminium alloy synthesis device and synthetic method, particularly disposable lithium-battery negative material specialized lithium aluminium alloy synthesis device and synthetic method.Including melt tank, the first heating furnace, piping filter, Liquid sealing valve, the second heating furnace, synthesis reactor, the 3rd heating furnace, argon device, vacuum pump and switch board；Melt tank is provided externally with the first heating furnace；Between melt tank and synthesis reactor, it is provided with piping filter and Liquid sealing valve, is provided externally with the second heating furnace at piping filter and Liquid sealing valve；Synthesis reactor is provided externally with the 3rd heating furnace；Described melt tank and synthesis reactor are all connected with outside argon device and vacuum pump；Described melt tank, synthesis reactor, the first heating furnace, the second heating furnace, the 3rd heating furnace, Liquid sealing valve, argon device and vacuum pump are all connected with switch board.Melt operation under total enclosing vacuum condition, produces impurity and is removed, and material completes combination reaction in synthesis reactor, and gained battery grade lithium alloy product quality is good, stable.
Description
Technical field
The present invention relates to a kind of battery grade lithium aluminium alloy synthesis device and synthetic method, particularly disposable lithium-battery negative material specialized lithium aluminium alloy synthesis device and synthetic method.
Background technology
In recent years, along with the development of disposable lithium-battery application, disposable lithium-battery is had higher requirement in electrical property and safety.Practice have shown that a lithium Fe battery adopts battery grade lithium aluminium alloy to make negative material, can obviously improve its discharging voltage characteristic.One time lithium-manganese cell adopts battery grade lithium aluminum alloy materials to make negative pole, can improve its security performance when heavy-current discharge.Therefore the battery grade lithium aluminium alloy as negative material is just being increasingly being applied to disposable lithium-battery industry.
At present, there is purity instability in the battery grade lithium aluminium alloy of traditional process equipment synthesis, and mainly oxygen therein, nitrogen content are higher, and the content of Aluminum in Alloy is uneven.Thus affecting the electrical property quality of disposable lithium-battery and the stability of product.
The synthesis technique of traditional battery grade lithium aluminium alloy mainly has two kinds: one is (relative humidity≤2% in dry air, 20 DEG C) carry out, lithium metal and aluminum are joined by a certain percentage in the uncovered crucible of electric furnace and melt, adopt mechanical agitation mode to synthesize, hand teeming；Another kind is to carry out in the glove box of full argon, lithium metal and aluminum is joined by a certain percentage in the uncovered crucible of electric furnace and melts, and adopts mechanical agitation mode to synthesize, hand teeming.
The synthesis technique of above-mentioned battery grade lithium aluminium alloy is primarily present three problems: one is that the synthesis device of lithium-aluminium alloy is uncovered mechanical agitation mode.When adopting synthesis technique in air drying, even if ensureing that drying room relative humidity is lower than 2%(20 DEG C), owing to lithium metal activity under 200-220 DEG C of condition of synthesis temperature is too strong, more or less impurity can be produced with oxygen, nitrogen generation chemical reaction in air；When adopting synthesis technique in argon glove box, requirement due to operability, glove box can not be accomplished to fully seal, extraneous natural air is easily accessible in glove box and makes argon be contaminated, due to the impact of natural air, lithium-aluminium alloy building-up process also can produce a small amount of lithium oxide, lithium nitride impurity.Two be lithium-aluminium alloy fusing and synthesis all carry out in same equipment, lithium-aluminium alloy fusing and building-up process in generation lithium oxide, lithium nitride impurity can not effectively remove, be brought in product during casting.Three is owing to synthesis device is mechanical agitation mode, need to stop stirring and be operated, therefore influence whether the uniformity of Aluminum in Alloy content during hand teeming.
Therefore, traditional process equipment synthesis battery grade lithium alloy product difficult quality guarantee and less stable.Simultaneously as equipment is uncovered mechanical agitation mode, there is bigger potential safety hazard.
Summary of the invention
It is an object of the invention to provide a kind of battery grade lithium aluminium alloy synthesis device and synthetic method thereof for above-mentioned weak point, utilize this equipment and the synthetic method can when total enclosing, fine vacuum and high-purity argon gas, without any mechanical stirring device, produce heavy-duty battery level lithium-aluminium alloy product.
A kind of battery grade lithium aluminium alloy synthesis device and synthetic method thereof realize by the following technical solutions:
A kind of battery grade lithium aluminium alloy synthesis device includes melt tank, the first heating furnace, piping filter, Liquid sealing valve, the second heating furnace, synthesis reactor, the 3rd heating furnace, argon device, vacuum pump and switch board；Melt tank is provided externally with the first heating furnace；Between melt tank and synthesis reactor, it is provided with piping filter and Liquid sealing valve, is provided externally with the second heating furnace at piping filter and Liquid sealing valve；Synthesis reactor is provided externally with the 3rd heating furnace；Described melt tank and synthesis reactor are all connected with outside argon device and vacuum pump；Described melt tank, synthesis reactor, the first heating furnace, the second heating furnace, the 3rd heating furnace, Liquid sealing valve, argon device and vacuum pump are all connected with switch board.
Described side, melt tank top is provided with melt tank vacuum tube and melt tank tunger tube, and described melt tank vacuum tube and melt tank tunger tube couple with outside vacuum pump and argon device respectively；The cover of melt tank and tank body are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；Melt pot bottom is provided with melt tank discharge nozzle.
Described side, synthesis reactor top is provided with synthesis reactor feed pipe, is provided with synthesis reactor discharge nozzle bottom synthesis reactor；Synthesis reactor top opposite side is provided with tunger tube on synthesis reactor vacuum tube and synthesis reactor, and on described synthesis reactor vacuum tube and synthesis reactor, tunger tube couples with outside vacuum pump and argon device respectively；In synthesis reactor, bottom is provided with argon allotter, is along the circumferential direction evenly equipped with aperture on argon allotter；Argon allotter couples with the argon device of outside by being arranged under the synthesis reactor of synthesis reactor bottom tunger tube；The kettle cover of synthesis reactor and kettle are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；The kettle cover of synthesis reactor is provided with pneumatic valve barrel, and pneumatic valve barrel is coupled by flange seal with the long stem valve in synthesis reactor, pneumatic valve barrel control the open and close of long stem valve.
Filtering accuracy≤2 micron of described piping filter.
Being equipped with thermal detector in melt tank, Liquid sealing valve, synthesis reactor and the first heating furnace, the second heating furnace and the 3rd heating furnace, described thermal detector adopts industrial thermal detector, and the change of the temperature measured by thermal detector reflects state and the trend of material.
Described melt tank, Liquid sealing valve, synthesis reactor, the first heating furnace, the second heating furnace, the 3rd heating furnace, argon device and vacuum pump are all connected with switch board, thus realizing the safety in production that overall process automatically controls.
Described equipment adopts pipe flange connecting mode to be connected into one by airtight for whole component parts so that this equipment carries out melt and synthetic job when total enclosing, fine vacuum and high-purity argon gas.
The synthetic method of a kind of battery grade lithium aluminium alloy synthesis device, comprises the steps:
1) when melt tank is full of argon, open melt cover and maintenance passes into argon, close melt cover after Battery grade lithium metal and high-purity aluminum foil being fed in raw material by the weight of required proportioning, simultaneously close off melt tank tunger tube valve.
2) open melt tank vacuum tube valve and melt tank is carried out evacuation operation, as vacuum≤1Pa in melt tank, open the first heating furnace melt tank is heated, when in melt tank, temperature of charge reaches 200-220 DEG C, in melt tank, material is in complete molten condition, keep heated at constant temperature after 1 hour, open the involutory one-tenth still of synthesis reactor vacuum tube valve and carry out evacuation operation.
3) as vacuum≤1Pa in synthesis reactor, the second heating furnace outside piping filter and Liquid sealing valve is opened；In Liquid sealing valve, the change of temperature of charge shows conducting and the closure state of Liquid sealing valve, and when in Liquid sealing valve, temperature of charge is more than 180 DEG C, material is molten condition, and Liquid sealing valve is in the conduction state；When in Liquid sealing valve, temperature of charge is less than 180 DEG C, material is curdled appearance, and Liquid sealing valve is in closure state；When Liquid sealing valve turns on, close the first heating furnace outside melt tank, simultaneously close off melt tank vacuum tube valve, stop the evacuation operation of melt tank, open melt tank tunger tube valve and pass into argon in melt tank, whole for the material in melt tank filter pressings are flowed in synthesis reactor；After above-mentioned material filter pressing, close melt tank tunger tube valve, stop passing into argon in melt tank, synthesis reactor is heated by the 3rd heating furnace opened outside synthesis reactor simultaneously, keep temperature of charge in synthesis reactor to be 200-220 DEG C, close the second heating furnace outside piping filter and Liquid sealing valve.
4) when in Liquid sealing valve, temperature of charge naturally cools to less than 180 DEG C, the Liquid sealing valve between melt tank and synthesis reactor is in closure state, is namely in, between melt tank and synthesis reactor, the state of being fully disconnected；Now open the valve of tunger tube under the synthesis reactor of synthesis reactor bottom, pass into argon to the argon allotter of synthesis reactor bottom and material in synthesis reactor is sufficiently stirred for.After argon passes into material, discharge from the synthesis reactor vacuum tube on synthesis reactor top, regulate synthesis reactor vacuum tube valve, make argon pass into and outflow be in balance and ensure that in synthesis reactor, material is sufficiently stirred for.
5) when in synthesis reactor material temperature be pass under 200-220 DEG C of condition argon be sufficiently stirred for 1 little time after, close the 3rd heating furnace outside synthesis reactor.
6) open pneumatic long stem valve in synthesis reactor and carry out the casting of lithium-aluminium alloy ingot.
In described step (1), in battery grade lithium aluminium alloy, the content of aluminum is: 0.1-3%.
In described step (2), heating-up temperature is maintained at 200-220 DEG C, because when in melt tank, temperature of charge reaches 200-220 DEG C, it was shown that in tank, material is in complete molten condition.In tank, the change of temperature of charge reflects the fusion process of material.
In step (5), synthesis temperature is 200-220 DEG C, and argon stirs 1 hour.Because material can be sufficiently complete the combination reaction between lithium aluminum metal with this understanding.
In step (6) casting cycle, material is in argon stirring all the time.
One novel battery level lithium-aluminium alloy synthesis device simple in construction of the present invention, easy and simple to handle, production run is safe and reliable, it may be achieved overall process automatically controls production.Melt tank and synthesis reactor separate design is adopted due to this equipment; melt operation is carried out under total enclosing vacuum condition; the micro-oxidation lithium, the impurity such as lithium nitride that produce in melt process are being removed through piping filter filter pressing; being sufficiently complete intermetallic combination reaction under the protection of lithium-aluminium alloy material high-purity argon gas in synthesis reactor and stirring condition, during casting, material is in stirring all the time.Therefore, the battery grade lithium alloy product quality obtained is good, stable.
Accompanying drawing explanation
Below with reference to accompanying drawing, the invention will be further described:
Fig. 1 is the structural representation of a kind of battery grade lithium aluminium alloy synthesis device of the present invention.
In figure: 1, melt tank, 2, first heating furnace, 3, tank body, 4, cover, 5, piping filter, 6, Liquid sealing valve, 7, second heating furnace, 8, synthesis reactor, 9, 3rd heating furnace, 10, argon allotter, 11, long stem valve, 12, kettle, 13, kettle cover, 14, pneumatic valve barrel, 15, argon device, 16, vacuum pump, 17, switch board, a, melt tank vacuum tube, b, melt tank tunger tube, c, melt tank discharge nozzle, d, synthesis reactor feed pipe, e, synthesis reactor discharge nozzle, f, tunger tube under synthesis reactor, g, synthesis reactor vacuum tube, h, tunger tube on synthesis reactor.
Detailed description of the invention
With reference to Fig. 1, a kind of battery grade lithium aluminium alloy synthesis device includes melt tank the 1, first heating furnace 2, piping filter 5, Liquid sealing valve the 6, second heating furnace 7, synthesis reactor the 8, the 3rd heating furnace 9, argon device 15, vacuum pump 16 and switch board 17；Melt tank 1 is provided externally with the first heating furnace 2；Between melt tank 1 and synthesis reactor 8, it is provided with piping filter 5 and Liquid sealing valve 6, is provided externally with the second heating furnace 7 at piping filter 5 and Liquid sealing valve 6；Synthesis reactor 8 is provided externally with the 3rd heating furnace 9；Described melt tank 1 and synthesis reactor 8 are all connected with outside argon device 15 and vacuum pump 16；Described melt tank 1, synthesis reactor the 8, first heating furnace the 2, second heating furnace the 7, the 3rd heating furnace 9, Liquid sealing valve 6, argon device 15 and vacuum pump 16 are all connected with switch board 17.
Described side, melt tank 1 top is provided with melt tank vacuum tube a and melt tank tunger tube b, described melt tank vacuum tube a and melt tank tunger tube b and couples with outside vacuum pump 16 and argon device 15 respectively；The cover 4 of melt tank 1 and tank body 3 are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；Melt tank discharge nozzle c it is provided with bottom melt tank 1.
Described side, synthesis reactor 8 top is provided with synthesis reactor feed pipe d, is provided with synthesis reactor discharge nozzle e bottom synthesis reactor 8；Synthesis reactor 8 top opposite side is provided with tunger tube h on synthesis reactor vacuum tube g and synthesis reactor, and on described synthesis reactor vacuum tube g and synthesis reactor, tunger tube h couples with outside vacuum pump 16 and argon device 15 respectively；In synthesis reactor 8, bottom is provided with argon allotter 10, is along the circumferential direction evenly equipped with aperture on argon allotter 10；Argon allotter 10 couples with the argon device 15 of outside by being arranged under the synthesis reactor of synthesis reactor 8 bottom tunger tube f；The kettle cover 13 of synthesis reactor 8 and kettle 12 are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；The kettle cover 13 of synthesis reactor 8 is provided with pneumatic valve barrel 14, and pneumatic valve barrel 14 is coupled by flange seal with the long stem valve 11 in synthesis reactor 8, pneumatic valve barrel 14 control the open and close of long stem valve 11.
Filtering accuracy≤2 micron of described piping filter 5.
Being equipped with thermal detector in melt tank 1, Liquid sealing valve 6, synthesis reactor 8 and first heating furnace the 2, second heating furnace 7 and the 3rd heating furnace 9, described thermal detector adopts industrial thermal detector, and the change of the temperature measured by thermal detector reflects state and the trend of material.
Melt tank 1, Liquid sealing valve 6, synthesis reactor the 8, first heating furnace the 2, second heating furnace the 7, the 3rd heating furnace 9, argon device 15 and vacuum pump 16 are all connected with switch board 17, thus realizing the safety in production that overall process automatically controls.
Described equipment adopts pipe flange connecting mode to be connected into one by airtight for whole component parts so that this equipment carries out melt and synthetic job when total enclosing, fine vacuum and high-purity argon gas.
The synthetic method of a kind of battery grade lithium aluminium alloy synthesis device, comprises the steps:
1) when melt tank 1 is full of argon, open cover 4 and maintenance passes into argon, close cover 4 after Battery grade lithium metal and high-purity aluminum foil being fed in raw material by the weight of required proportioning, simultaneously close off melt tank tunger tube b valve.
2) open melt tank vacuum tube a valve and melt tank 1 is carried out evacuation operation, as vacuum≤1Pa in melt tank 1, open the first heating furnace 2 melt tank 1 is heated, when in melt tank 1, temperature of charge reaches 200-220 DEG C, in melt tank 1, material is in complete molten condition, keep heated at constant temperature after 1 hour, open synthesis reactor vacuum tube g valve and synthesis reactor 8 is carried out evacuation operation.
3) as vacuum≤1Pa in synthesis reactor 8, the second heating furnace 7 outside piping filter 5 and Liquid sealing valve 6 is opened；In Liquid sealing valve 6, the change of temperature of charge shows conducting and the closure state of Liquid sealing valve 6, and when in Liquid sealing valve 6, temperature of charge is more than 180 DEG C, material is molten condition, and Liquid sealing valve 6 is in the conduction state；When in Liquid sealing valve 6, temperature of charge is less than 180 DEG C, material is curdled appearance, and Liquid sealing valve 6 is in closure state；When Liquid sealing valve 6 turns on, close the first heating furnace 2 outside melt tank 1, simultaneously close off melt tank vacuum tube a valve, stop the evacuation operation of melt tank 1, open melt tank tunger tube b valve and pass into argon in melt tank 1, whole for the material in melt tank 1 filter pressings are flowed in synthesis reactor 8；After above-mentioned material filter pressing, close melt tank tunger tube b valve, stop passing into argon in melt tank 1, synthesis reactor 8 is heated by the 3rd heating furnace 9 opened outside synthesis reactor 8 simultaneously, keep temperature of charge in synthesis reactor 8 to be 200-220 DEG C, close the second heating furnace 7 outside piping filter 5 and Liquid sealing valve 6.
4) when in Liquid sealing valve 6, temperature of charge naturally cools to less than 180 DEG C, the Liquid sealing valve 6 between melt tank 1 and synthesis reactor 8 is in closure state, is namely in, between melt tank 1 and synthesis reactor 8, the state of being fully disconnected；Now opening the valve of tunger tube f under synthesis reactor 8 bottom synthesis reactor, in synthesis reactor 8, the argon allotter 10 of bottom passes into argon material in synthesis reactor 8 is sufficiently stirred for；After argon passes into material, discharge from the synthesis reactor vacuum tube g on synthesis reactor 8 top；Regulate synthesis reactor vacuum tube g valve, make argon pass into and outflow be in balance and ensure that in synthesis reactor 8, material is sufficiently stirred for.
5) when in synthesis reactor 8 material temperature be pass under 200-220 DEG C of condition argon be sufficiently stirred for 1 little time after, close the 3rd heating furnace outside synthesis reactor 8.
6) open pneumatic long stem valve 11 in synthesis reactor 8 and carry out the casting of lithium-aluminium alloy ingot.
In described step (1), in battery grade lithium aluminium alloy, the content of aluminum is: 0.1-3%.
In described step (2), heating-up temperature is maintained at 200-220 DEG C, because when in melt tank, temperature of charge reaches 200-220 DEG C, it was shown that in tank, material is in complete molten condition.In tank, the change of temperature of charge reflects the fusion process of material.
In step (5), synthesis temperature is 200-220 DEG C, and argon stirs 1 hour, because material can be sufficiently complete the combination reaction between lithium aluminum metal with this understanding.
In step (6) casting cycle, material is in argon stirring all the time.
Below in conjunction with embodiment, this equipment operation principle is explained.
Example 1: 1) when melt tank 1 is full of argon, unlatching cover 4 maintenance pass into argon.Weigh 30Kg Battery grade lithium metal and join in tank, weigh 30g high-purity aluminum foil and join in tank, close cover 4, simultaneously close off argon pipeline b valve and stop passing into argon.
2) by synthetic method 2)-6) step be operated, obtain containing the battery grade lithium alloy product that aluminum is 0.1%.
Example 2: 1) when melt tank 1 is full of argon, unlatching cover 4 maintenance pass into argon.Weigh 30Kg Battery grade lithium metal and join in tank, weigh 300g high-purity aluminum foil and join in tank, close cover 4, simultaneously close off argon pipeline b valve and stop passing into argon.
2) by synthetic method 2)-6) step be operated, obtain containing the battery grade lithium alloy product that aluminum is 1%.
Example 3: 1) when melt tank 1 is full of argon, unlatching cover 4 maintenance pass into argon.Weigh 30Kg Battery grade lithium metal and join in tank, weigh 900g high-purity aluminum foil and join in tank, close cover 4, simultaneously close off argon pipeline b valve and stop passing into argon.
2) by synthetic method 2)-6) step be operated, obtain containing the battery grade lithium alloy product that aluminum is 3%.
Claims (6)
1. a battery grade lithium aluminium alloy synthesis device, it is characterised in that: include melt tank, the first heating furnace, piping filter, Liquid sealing valve, the second heating furnace, synthesis reactor, the 3rd heating furnace, argon device, vacuum pump and switch board；Melt tank is provided externally with the first heating furnace；Between melt tank and synthesis reactor, it is provided with piping filter and Liquid sealing valve, is provided externally with the second heating furnace at piping filter and Liquid sealing valve；Synthesis reactor is provided externally with the 3rd heating furnace；Described melt tank and synthesis reactor are all connected with outside argon device and vacuum pump；Described melt tank, synthesis reactor, the first heating furnace, the second heating furnace, the 3rd heating furnace, Liquid sealing valve, argon device and vacuum pump are all connected with switch board；
Described side, melt tank top is provided with melt tank vacuum tube and melt tank tunger tube, and described melt tank vacuum tube and melt tank tunger tube couple with outside vacuum pump and argon device respectively；The cover of melt tank and tank body are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；Melt pot bottom is provided with melt tank discharge nozzle；
Described side, synthesis reactor top is provided with synthesis reactor feed pipe, is provided with synthesis reactor discharge nozzle bottom synthesis reactor；Synthesis reactor top opposite side is provided with tunger tube on synthesis reactor vacuum tube and synthesis reactor, and on described synthesis reactor vacuum tube and synthesis reactor, tunger tube couples with outside vacuum pump and argon device respectively；In synthesis reactor, bottom is provided with argon allotter, is along the circumferential direction evenly equipped with aperture on argon allotter；Argon allotter couples with the argon device of outside by being arranged under the synthesis reactor of synthesis reactor bottom tunger tube；The kettle cover of synthesis reactor and kettle are by the hermetically sealed connection of flange, and flange seal ring is provided with upper and lower water-cooling jacket；The kettle cover of synthesis reactor is provided with pneumatic valve barrel, and pneumatic valve barrel is coupled by flange seal with the long stem valve in synthesis reactor, pneumatic valve barrel control the open and close of long stem valve.
2. battery grade lithium aluminium alloy synthesis device according to claim 1, it is characterised in that: filtering accuracy≤2 micron of described piping filter.
3. battery grade lithium aluminium alloy synthesis device according to claim 1, it is characterized in that: in melt tank, Liquid sealing valve, synthesis reactor and the first heating furnace, the second heating furnace and the 3rd heating furnace, be equipped with thermal detector, described thermal detector adopts industrial thermal detector, and the change of the temperature measured by thermal detector reflects state and the trend of material.
4. the synthetic method of a kind of battery grade lithium aluminium alloy synthesis device according to claim 1, it is characterised in that comprise the steps:
1) when melt tank is full of argon, open cover and maintenance passes into argon, close cover after Battery grade lithium metal and high-purity aluminum foil being fed in raw material by the weight of required proportioning, simultaneously close off melt tank tunger tube valve；
2) open melt tank vacuum tube valve and melt tank is carried out evacuation operation, as vacuum≤1Pa in melt tank, open the first heating furnace melt tank is heated, when in melt tank, temperature of charge reaches 200-220 DEG C, in melt tank, material is in complete molten condition, keep heated at constant temperature after 1 hour, open the involutory one-tenth still of synthesis reactor vacuum tube valve and carry out evacuation operation；
3) as vacuum≤1Pa in synthesis reactor, the second heating furnace outside piping filter and Liquid sealing valve is opened；In Liquid sealing valve, the change of temperature of charge affects conducting and the closure state of Liquid sealing valve, and when in Liquid sealing valve, temperature of charge is more than 180 DEG C, material is molten condition, and Liquid sealing valve is in the conduction state；When in Liquid sealing valve, temperature of charge is less than 180 DEG C, material is curdled appearance, and Liquid sealing valve is in closure state；When Liquid sealing valve turns on, close the first heating furnace outside melt tank, simultaneously close off melt tank vacuum tube valve, stop the evacuation operation of melt tank, open melt tank tunger tube valve and pass into argon in melt tank, whole for the material in melt tank filter pressings are flowed in synthesis reactor；After above-mentioned material filter pressing, close melt tank tunger tube valve, stop passing into argon in melt tank, synthesis reactor is heated by the 3rd heating furnace opened outside synthesis reactor simultaneously, keep temperature of charge in synthesis reactor to be 200-220 DEG C, close the second heating furnace outside piping filter and Liquid sealing valve；
4) when in Liquid sealing valve, temperature of charge naturally cools to less than 180 DEG C, the Liquid sealing valve between melt tank and synthesis reactor is in closure state, is namely in, between melt tank and synthesis reactor, the state of being fully disconnected；Now opening the valve of tunger tube under synthesis reactor bottom synthesis reactor, in synthesis reactor, the argon allotter of bottom passes into argon material in synthesis reactor is sufficiently stirred for；After argon passes into material, discharge from the synthesis reactor vacuum tube on synthesis reactor top；Regulate synthesis reactor vacuum tube valve, make argon pass into and outflow be in balance and ensure that in synthesis reactor, material is sufficiently stirred for；
5) when in synthesis reactor material temperature be pass under 200-220 DEG C of condition argon be sufficiently stirred for 1 little time after, close the 3rd heating furnace outside synthesis reactor；
6) open pneumatic long stem valve in synthesis reactor and carry out the casting of lithium-aluminium alloy ingot.
5. the synthetic method of a kind of battery grade lithium aluminium alloy synthesis device according to claim 4, it is characterised in that: in step (1), in battery grade lithium aluminium alloy, the content of aluminum is 0.1-3%.
6. the synthetic method of a kind of battery grade lithium aluminium alloy synthesis device according to claim 4, it is characterised in that: in step (6) casting cycle, material is in argon stirring all the time.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009586.2A CN104561617B (en) | 2015-01-09 | 2015-01-09 | A kind of battery grade lithium aluminium alloy synthesis device and synthetic method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510009586.2A CN104561617B (en) | 2015-01-09 | 2015-01-09 | A kind of battery grade lithium aluminium alloy synthesis device and synthetic method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104561617A CN104561617A (en) | 2015-04-29 |
| CN104561617B true CN104561617B (en) | 2016-07-06 |
Family
ID=53078685
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510009586.2A Active CN104561617B (en) | 2015-01-09 | 2015-01-09 | A kind of battery grade lithium aluminium alloy synthesis device and synthetic method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104561617B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111180698B (en) * | 2019-12-31 | 2021-04-23 | 中国科学院宁波材料技术与工程研究所 | Metal lithium composite negative electrode, preparation method thereof and lithium metal secondary battery |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4638002B2 (en) * | 2000-07-21 | 2011-02-23 | 高周波熱錬株式会社 | Method and apparatus for manufacturing silicon for solar cell |
| JP5977831B2 (en) * | 2011-10-24 | 2016-08-24 | エルジー・ケム・リミテッド | Method for manufacturing negative electrode active material, negative electrode active material, and lithium secondary battery including the same |
| CN202658215U (en) * | 2012-05-11 | 2013-01-09 | 重庆昆瑜锂业有限公司 | Equipment for making lithium-aluminum alloy with doping method |
| CN104060141B (en) * | 2014-07-14 | 2017-01-11 | 天齐锂业股份有限公司 | Vacuum synthesis method of lithium-aluminum alloy |
-
2015
- 2015-01-09 CN CN201510009586.2A patent/CN104561617B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104561617A (en) | 2015-04-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN204545419U (en) | A kind of high vacuum induction is without crucible and have crucible inert gas atomizer powder manufacturing apparatus | |
| CN110238356B (en) | Melt pouring device and method for aluminum-lithium alloy DC casting | |
| CN104561617B (en) | A kind of battery grade lithium aluminium alloy synthesis device and synthetic method | |
| JPH11285810A (en) | Method for melting reactive metallic material and melting device | |
| CN101880788A (en) | Method for enhancing SiC particle grinding of magnesium aluminum alloy | |
| CN109402425B (en) | Superaudio induction heating light alloy vacuum smelting pouring furnace | |
| CN103484898B (en) | A kind of vacuum high-temperature continuous electrolysis furnace system and electrolysis process | |
| CN104946904A (en) | Industrial-grade metal lithium refining equipment and refining method | |
| CN209006634U (en) | A kind of magnesium lithium alloy ingot casting preparation facilities | |
| CN204584231U (en) | Titanium-base alloy induction melting leakage type suction pouring equipment | |
| CN109579530A (en) | A kind of the material alloying mechanism and its charging process of vacuum induction furnace zone preservative pipe | |
| CN110528087B (en) | Apparatus for producing refractory oxide single crystal | |
| CN208711536U (en) | A kind of building coating stirred tank | |
| CN110273048A (en) | A kind of VD furnace online processing position threads feeding apparatus and method | |
| CN108947204A (en) | A kind of automatic feed agitating device for glass production | |
| CN204211787U (en) | Magnesium chloride is two-mand ladle | |
| CN206131717U (en) | Lead smelting furnace | |
| CN108069462A (en) | A kind of one-step method batch synthesizes the device and method of high-purity cobalt disulfide | |
| CN103866145A (en) | Al-V-Sn-Fe-Cu alloy used for preparing titanium alloy, and preparation method thereof | |
| CN209054943U (en) | Crucible device and agglomerating plant | |
| CN110206906A (en) | Feed vacuum separation valve on a kind of vaccum sensitive stove | |
| CN202116632U (en) | Magnesium alloy vacuum melting device | |
| US3431345A (en) | Electrical resistance furnaces | |
| CN111912223A (en) | Atmosphere protection type high-purity magnesium alloy smelting furnace and smelting process thereof | |
| CN206680551U (en) | A kind of vertical skull crucible of vacuum consumable electrode electric arc |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191219 Address after: 226400 No.9, Zhenxing 1st Road, juegang Town, Rudong County, Nantong City, Jiangsu Province Patentee after: Nantong Shengneng New Material Technology Co., Ltd Address before: 214121 Wuxi high school, Wuxi Institute of Technology, West Road, Jiangsu, No. 1600 Patentee before: Wuxi Institute of Technology |
|
| TR01 | Transfer of patent right |