CN103290293A - Lithium-aluminum alloy, and production method and use thereof - Google Patents
Lithium-aluminum alloy, and production method and use thereof Download PDFInfo
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- CN103290293A CN103290293A CN2013102204649A CN201310220464A CN103290293A CN 103290293 A CN103290293 A CN 103290293A CN 2013102204649 A CN2013102204649 A CN 2013102204649A CN 201310220464 A CN201310220464 A CN 201310220464A CN 103290293 A CN103290293 A CN 103290293A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/40—Alloys based on alkali metals
- H01M4/405—Alloys based on lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C24/00—Alloys based on an alkali or an alkaline earth metal
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention relates to lithium-aluminum alloy, and a production method and use thereof, which belong to the technical field of a secondary battery negative material. The lithium-aluminum alloy has a longer charging-discharging cycling life. The lithium-aluminum alloy consists of the following components according to weight percent: 0.1 to 4.0 percent of aluminum, and the balance of lithium and unavoidable impurities. By adding the aluminum in specific content to the lithium, the performance of the pure metal lithium is modified, and not only can the advantages of the lithium capacity be maintained, but also a dendritic crystal inhibition effect can be improved. A single phase is used in the charging and discharging processes, the phase change can be avoided, and thus the charging-discharging cycling life of the lithium-aluminum alloy can be prolonged.
Description
Technical field
The present invention relates to lithium-aluminium alloy and production method thereof and purposes, belong to the secondary battery cathode material technical field.
Background technology
Lithium is a kind of argenteous metal, quality is very light, ductility is good, electroconductibility is strong, and electrochemical properties is quite active, and reductibility is extremely strong, its electrochemical equivalent is very little, be 0.259g/Ah, the theoretical specific capacity of lithium electrode reaches 3860Ah/kg, considerably beyond 820Ah/kg and the 260Ah/kg of lead and the 481Ah/kg of cadmium of zinc.Simultaneously, the exchange current density of lithium electrode is bigger, only has very little polarization to produce in electrode reaction.
Metal lithium electrode uses as secondary lithium battery cathode, have very big defective, major defect is as follows: the lithium metal battery that utilizes lithium anode and common organic electrolyte to form exists problems such as cycle efficiency is low, security is bad, especially safety issue, battery short circuit, overheated, overcharge or the situation of overdischarge under, all the thermal runaway of system may take place, even cause blast.This has brought many problems that are difficult to overcome for the commercialization of lithium metal battery.But essentially, metallic lithium uses as secondary battery negative pole, and main problem is: the lower charge and discharge cycles efficient that (1) complicated surface reaction causes and the continuous increase of interface impedance; (2) generation of " dendrite " and " dead lithium ", the safety issue of bringing and electrode active material loss.
In order to suppress the formation of Li dendrite, people have carried out replacing with lithium alloy many research work of lithium metal negative pole.Disclose a kind of chargeable electrochemical device as patent JP-A-60-167280, the alloy of its use lithium and other metal suppresses the formation of Li dendrite.Compare with pure metal lithium, lithium alloy and electrolytical interface are more stable.So replace lithium as negative pole the safety performance of battery to be improved with lithium alloy.Be a research focus with lithium alloy substituted metal lithium wherein, as lithium-aluminium alloy, lithium-tin alloy etc.Existing experimental study proves: the adding of alloying constituent can make metallic lithium have obviously superior stability in electrolytic solution, reduced to a great extent and electrolytic solution between non-faraday reaction, make the SEI film more even simultaneously, improved the stability of metal lithium electrode.
And for example: application number is that the patent application of CN94104418 discloses a kind of lithium-aluminium alloy for cell negative electrode material and manufacture method thereof, it is a kind of β phase LiAl alloy, its method for making is that raw material is placed melting equipment, vacuumize and charge into argon gas, heating continues to vacuumize, and is heated to 400-450 ℃ and stops to vacuumize, charge into the 0.05-0.5Pa argon, be heated to 710-800 ℃, be incubated 1-5 hour, be chilled to room temperature and make the lithium-aluminium alloy ingot.It is characterized in that, for β phase LiAl alloy, contain lithium 18-24%(weight percentage, down together), contain aluminium 82-76%, 688 ℃ of fusing points.But the lithium-aluminium alloy that aforesaid method makes contains lithium 18-24%(weight percentage), the alloying constituent content of non-lithium is very high, has increased the electrode reaction current potential of lithium metal negative pole, has reduced the specific energy of cathode of lithium.And this negative material can produce phase transformation inevitably in battery charge and discharge process, thereby causes the great variety of volume, causes the quick efflorescence of material, reduces cycle life greatly.The mechanism that discharges and recharges of alloy material no longer has been dissolving one sedimentation mechanism of metallic lithium on negative pole, deviates from mechanism and become the insertion one of lithium ion in lithium alloy.
Summary of the invention
Technical problem to be solved by this invention provides the higher lithium-aluminium alloy of a kind of charge and discharge circulation life.
Lithium-aluminium alloy of the present invention is made up of following components in weight percentage: aluminium 0.1～4.0wt%, surplus is lithium and unavoidable impurities.
Further, as optimized technical scheme, lithium-aluminium alloy of the present invention is made up of following components in weight percentage: aluminium 0.1～1wt%, surplus is lithium and unavoidable impurities.
Further, the present invention also provides a kind of method of producing lithium-aluminium alloy.
The method that the present invention produces lithium-aluminium alloy comprises the steps: metallic lithium and aluminium by weight 24～1000:1 mixing, then under inert atmosphere in 190～300 ℃ of meltings, cooling makes lithium-aluminium alloy.The inventive method adopts 190～300 ℃ low smelting heat to produce lithium-aluminium alloy, and energy consumption is reduced, and product percent of pass is improved greatly.
Wherein, the effect of the inert atmosphere in the aforesaid method be prevent lithium, aluminium is oxidized or nitrogenize, described inert atmosphere is preferably helium, neon, argon or krypton atmosphere, the oxygen in the atmosphere, nitrogen total amount is preferred≤15ppm.Further, described inert atmosphere most preferably is argon atmospher.
Wherein, the too high easy generation safety problem of heat-up rate, heat-up rate is crossed low then production efficiency and is descended, and in order to guarantee production process safety, simultaneously production efficiency is maintained in the tolerance interval, and the heat-up rate of aforesaid method melting preferably is controlled to be 200～300 ℃/h.
Wherein, in the aforesaid method, the time of general melting is controlled to be 1～8h and can melting finishes.
Further, according to concrete needs, in the aforesaid method, also be cooled to 190～230 ℃ after melting finishes, cast, after casting is finished, be cooled to room temperature, the demoulding makes lithium-aluminium alloy.
The present invention also provides the purposes of above-mentioned lithium-aluminium alloy in the preparation cell negative electrode material.
Lithium-aluminium alloy of the present invention by adding the aluminium of certain content, has been done modification to the performance of pure metal lithium, both keep lithium capacity advantage, improved the dendrite inhibition again, be single phase during it discharges and recharges, can not undergo phase transition, improve the charge and discharge circulation life of lithium-aluminium alloy.
Embodiment
Lithium-aluminium alloy of the present invention is made up of following components in weight percentage: aluminium 0.1～4.0wt%, surplus is lithium and unavoidable impurities.
Further, as optimized technical scheme, lithium-aluminium alloy of the present invention is made up of following components in weight percentage: aluminium 0.1～1wt%, surplus is lithium and unavoidable impurities.
Further, the present invention also provides a kind of method of producing lithium-aluminium alloy.
The method that the present invention produces lithium-aluminium alloy comprises the steps: metallic lithium and aluminium by weight 24～1000:1 mixing, then under inert atmosphere in 190～300 ℃ of meltings, cooling makes lithium-aluminium alloy.The inventive method adopts 190～300 ℃ low smelting heat to produce lithium-aluminium alloy, and energy consumption is reduced, and product percent of pass is improved greatly.
Wherein, the effect of the inert atmosphere in the aforesaid method be prevent lithium, aluminium is oxidized or nitrogenize, described inert atmosphere is preferably helium, neon, argon or krypton atmosphere, the oxygen in the atmosphere, nitrogen total amount is preferred≤15ppm.Further, described inert atmosphere most preferably is argon atmospher.
Wherein, the too high easy generation safety problem of heat-up rate, heat-up rate is crossed low then production efficiency and is descended, and in order to guarantee production process safety, simultaneously production efficiency is maintained in the tolerance interval, and the heat-up rate of aforesaid method melting preferably is controlled to be 200～300 ℃/h.
Wherein, in the aforesaid method, the time of general melting is controlled to be 1～8h and can melting finishes.
Further, according to concrete needs, in the aforesaid method, also be cooled to 190～230 ℃ after melting finishes, cast, after casting is finished, be cooled to room temperature, the demoulding makes lithium-aluminium alloy.
The present invention also provides the purposes of above-mentioned lithium-aluminium alloy in the preparation cell negative electrode material.
Be further described below in conjunction with the specific embodiment of the present invention of embodiment, therefore do not limit the present invention among the described scope of embodiments.
The preparation of embodiment 1 lithium-aluminium alloy of the present invention
Ready metallic lithium, metallic aluminium are weight ratio by the lithium al proportion in the 99.80:0.15(embodiment of the invention) put into crucible, vacuumize (0.1Pa), logical argon gas (9 * 10
4Pa) displacement twice guarantees that a jar interior oxygen, nitrogen total amount are not more than 15ppm.Begin to heat up (300 ℃/h), temperature rises to 220 ℃, smelting time 2h.After alloying is finished, be cooled to 210 ℃, cast.After casting is finished, after the temperature of alloy pig reaches envrionment temperature, open tank body and carry out demoulding sampling.The sample that takes out vacuumizes packing rapidly, weighs, record.Gained lithium-aluminium alloy composition sees the following form 1.
Table 1
The preparation of embodiment 2 lithium-aluminium alloys of the present invention
Ready metallic lithium, metallic aluminium are put into crucible by 99.85:0.1, vacuumize (0.1Pa), logical argon gas (9 * 10
4Pa) displacement twice guarantees that a jar interior oxygen, nitrogen total amount are not more than 15ppm.Begin to heat up (300 ℃/h), temperature rises to 190 ℃, smelting time 8h.After alloying is finished, be cooled to 190 ℃, cast.After casting is finished, after the temperature of alloy pig reaches envrionment temperature, open tank body and carry out demoulding sampling.The sample that takes out vacuumizes packing rapidly, weighs, record.Gained lithium-aluminium alloy composition sees the following form 2.
Table 2
The preparation of embodiment 3 lithium-aluminium alloys of the present invention
Ready metallic lithium, metallic aluminium are put into crucible by 96:4, vacuumize (0.1Pa), logical argon gas (9 * 10
4Pa) displacement twice guarantees that a jar interior oxygen, nitrogen total amount are not more than 15ppm.Begin to heat up (300 ℃/h), temperature rises to 300 ℃, smelting time 1h.After alloying is finished, be cooled to 210 ℃, cast.After casting is finished, after the temperature of alloy pig reaches envrionment temperature, open tank body and carry out demoulding sampling.The sample that takes out vacuumizes packing rapidly, weighs, record.Gained lithium-aluminium alloy composition sees the following form 3.
Table 3
| Composition | Li | Al | N | Na | K | Ca | Si | Fe | Ni | Cl | Cu |
| Content (%) | 95.93 | 3.98 | 0.01 | 0.01 | 0.01 | 0.025 | 0.005 | 0.002 | 0.003 | 0.004 | 0.003 |
The preparation of embodiment 4 lithium-aluminium alloys of the present invention
Ready metallic lithium, metallic aluminium by putting into crucible shown in the table 4, are vacuumized (0.1Pa), logical argon gas (9 * 10
4Pa) displacement twice guarantees that a jar interior oxygen, nitrogen total amount are not more than 15ppm.Begin to heat up (200～300 ℃/h), temperature rises to 190～300 ℃, smelting time 1～8h.After alloying is finished, be cooled to 190～230 ℃, cast.After casting is finished, after the temperature of alloy pig reaches envrionment temperature, open tank body and carry out demoulding sampling.The sample that takes out vacuumizes packing rapidly, weighs, record.Gained lithium-aluminium alloy composition sees Table 5.
Table 4
Table 5
Test example 1
The lithium-aluminium alloy of embodiment 1,2,3,4 preparations is discharged and recharged experiment as negative material, measure the performance of lithium-aluminium alloy of the present invention.The iron lithium phosphate that positive electrode material adopts Sichuan Tianqi Lithium Industries.Inc. to produce, tackiness agent is 5% in the positive plate; Barrier film adopts three layers of PP/PE/PP; Make the 1Ah flexible-packed battery.Adopt 1C to charge and discharge the cycle performance of (charging stopping potential 3.8V, discharge cut-off voltage 2.0V) electricity assessment battery.
In addition, prepare lithium-aluminium alloy with the method for CN94104418, discharge and recharge experiment under the equal conditions.
Measurement result is as shown in table 6 below.The lithium-aluminium alloy numbering of producing among the embodiment 4 is corresponding with table 6.
Table 6
| Numbering | Full piezoelectric voltage V | Cycle index | Capacity keeps | Cycle index | Capacity keeps |
| Embodiment 1 | 3.80 | 50 | 93% | 150 | 85% |
| Embodiment 2 | 3.80 | 50 | 90% | 150 | 84% |
| Embodiment 3 | 3.80 | 50 | 91% | 150 | 85% |
| 4-1 | 3.80 | 50 | 90% | 150 | 83% |
| 4-2 | 3.80 | 50 | 90% | 150 | 82% |
| 4-3 | 3.78 | 50 | 89% | 150 | 80% |
| 4-4 | 3.75 | 50 | 88% | 150 | 77% |
| 4-5 | 3.75 | 50 | 85% | 150 | 75% |
| 4-6 | 3.75 | 50 | 85% | 150 | 70% |
| 4-7 | 3.73 | 50 | 83% | 150 | 70% |
| 4-8 | 3.7 | 50 | 83% | 150 | 70% |
| 4-9 | 3.7 | 50 | 80% | 150 | 68% |
| 4-10 | 3.7 | 50 | 80% | 150 | 65% |
| CN94104418 | 3.5 | 50 | 75% | 150 | 50% |
Claims (8)
1. lithium-aluminium alloy, it is characterized in that being made up of following components in weight percentage: aluminium 0.1～4.0wt%, surplus is lithium and unavoidable impurities.
2. lithium-aluminium alloy according to claim 1, it is characterized in that being made up of following components in weight percentage: aluminium 0.1～1wt%, surplus is lithium and unavoidable impurities.
3. produce the method for lithium-aluminium alloy, it is characterized in that comprising the steps: with metallic lithium and aluminium by weight 24～1000:1 mixing, then under inert atmosphere in 190～300 ℃ of meltings, cooling makes lithium-aluminium alloy.
4. the method for production lithium-aluminium alloy according to claim 3, it is characterized in that: described inert atmosphere is helium, neon, argon or krypton atmosphere, the oxygen in the atmosphere, nitrogen total amount≤15ppm.
5. according to the method for claim 3 or 4 described production lithium-aluminium alloys, it is characterized in that: the heat-up rate of melting is 200～300 ℃/h.
6. according to the method for each described production lithium-aluminium alloy of claim 3～5, it is characterized in that: the time of melting is 1～8h.
7. according to the method for each described production lithium-aluminium alloy of claim 3～5, it is characterized in that: also be cooled to 190～230 ℃ after melting finishes, cast, after casting is finished, be cooled to room temperature, the demoulding makes lithium-aluminium alloy.
8. claim 1 or 2 described lithium-aluminium alloys are in the purposes of preparation in the cell negative electrode material.
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| CN201310220464.9A CN103290293B (en) | 2013-06-05 | 2013-06-05 | Lithium-aluminium alloy and production method thereof and purposes |
| PCT/CN2014/074187 WO2014194709A1 (en) | 2013-06-05 | 2014-03-27 | Lithium-aluminium alloy and production method and use thereof |
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| CN104060141A (en) * | 2014-07-14 | 2014-09-24 | 四川天齐锂业股份有限公司 | Vacuum synthesis method of lithium-aluminum alloy |
| WO2014194709A1 (en) * | 2013-06-05 | 2014-12-11 | 四川天齐锂业股份有限公司 | Lithium-aluminium alloy and production method and use thereof |
| CN105552348A (en) * | 2015-11-23 | 2016-05-04 | 天津赫维科技有限公司 | Making method of 3V chargeable button lithium battery lithium-aluminum alloy negative electrode |
| CN106816578A (en) * | 2016-12-12 | 2017-06-09 | 佛山市尚好门窗有限责任公司 | A kind of lithium La-Al alloy |
| CN107068964A (en) * | 2016-12-29 | 2017-08-18 | 中国电子科技集团公司第十八研究所 | Lithium aluminum alloy surface modified lithium cathode and solid-state battery thereof |
| CN108376764A (en) * | 2018-03-23 | 2018-08-07 | 西北工业大学 | Lithium secondary battery anode surface modifying method is modified lithium electrode and application using Ag made from this method |
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| CN109830646A (en) * | 2019-01-12 | 2019-05-31 | 哈尔滨工业大学 | A kind of composite metal negative pole and the battery comprising the cathode |
| CN110120502A (en) * | 2018-02-05 | 2019-08-13 | 中国科学院物理研究所 | A kind of lithium metal alloy material of cathode and its preparation method and application |
| CN111048744A (en) * | 2018-10-11 | 2020-04-21 | 中国科学技术大学 | Metallic lithium alloy electrode material, preparation method thereof and metallic lithium secondary battery |
| CN111916815A (en) * | 2019-05-08 | 2020-11-10 | 宁德时代新能源科技股份有限公司 | Lithium metal battery |
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| US12107254B2 (en) * | 2018-10-08 | 2024-10-01 | University Of Electronic Science And Technology Of China | Lithium alloy as an anode material and a preparation method thereof |
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| CN111916815A (en) * | 2019-05-08 | 2020-11-10 | 宁德时代新能源科技股份有限公司 | Lithium metal battery |
| CN114097109A (en) * | 2020-05-08 | 2022-02-25 | 株式会社Lg新能源 | Lithium-free battery and preparation method thereof |
| CN114050253A (en) * | 2021-10-21 | 2022-02-15 | 中山大学 | Preparation method and application of nano lithium alloy |
| CN114050253B (en) * | 2021-10-21 | 2024-08-13 | 中山大学 | Preparation method and application of nano lithium alloy |
| CN116072859A (en) * | 2023-02-10 | 2023-05-05 | 深圳市新固能科技有限公司 | Preparation method and application of Li-Al negative electrode material applied to solid-state battery |
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| CN103290293B (en) | 2016-02-24 |
| WO2014194709A1 (en) | 2014-12-11 |
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