CN105826545A - Preparation method for lithium powder or lithium alloy powder - Google Patents
Preparation method for lithium powder or lithium alloy powder Download PDFInfo
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- CN105826545A CN105826545A CN201610346059.5A CN201610346059A CN105826545A CN 105826545 A CN105826545 A CN 105826545A CN 201610346059 A CN201610346059 A CN 201610346059A CN 105826545 A CN105826545 A CN 105826545A
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- lithium
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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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- 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
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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
- 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 invention discloses a preparation method for lithium powder or lithium alloy powder .The preparation method includes the following steps that 1, lithium or lithium alloy is added to a container containing an inert organic solvent, wherein the inert organic solvent does not react with lithium or lithium alloy; 2, through ultrasonic treatment, the lithium powder or lithium alloy powder stored in the organic solvent is obtained .The product can be prepared through the preparation method under the condition that the temperature is lower than the melting point of lithium, operation is simple, the requirements for equipment are low, and the micron level lithium powder or lithium alloy powder can be obtained.
Description
Technical field
The present invention relates to a kind of lithium powder or the preparation method of lithium alloy powder.
Background technology
Metallic lithium powder and lithium alloy pruinescence are widely used in the applications such as lithium alkylide, catalyst, polymer, lithium battery and Aero-Space.But, owing to lithium metal has high reactivity, bigger viscosity and relatively low fusing point (180.5 DEG C), so metallic lithium powder and lithium alloy powder are difficult to pulverize preparation by conventional breaking methods such as mechanical activation comminution.At present, commonly used melted dispersion method prepares metallic lithium powder and lithium alloy powder.The method is a kind of lithium metal or lithium alloy to be heated to fusing and by high-speed stirred or atomization pelletize to transform into drop, then cools down the method making powder.The method needs to apply nearly 200 DEG C or higher operation temperature, inert protective atmosphere in preparation process; but also often need to use high boiling hydrocarbon ils and the low boiling hydrocarbon ils for washing, have that preparation cost is high, preparation efficiency is low, harsh to equipment requirements, the problems such as aspherical lithium powder and lithium alloy powder cannot be prepared.
Summary of the invention
In order to solve above-mentioned technical problem, the present invention provides a kind of lithium powder or the preparation method of lithium alloy powder, and it can prepare product under the temperature conditions less than the fusing point of lithium, simple to operate, low for equipment requirements, can obtain micron order lithium powder or lithium alloy powder.
To this end, technical scheme is as follows:
A kind of lithium powder or the preparation method of lithium alloy powder, comprise the steps:
1) lithium or lithium alloy are added in the container filling inert organic solvents；Described inert organic solvents is the organic solvent not reacted with lithium or lithium alloy；
2) sonicated, the described lithium powder must being saved in organic solvent or lithium alloy powder.
Preferably, step 2) sonicated after, also through filtering, be dried, obtain described lithium powder or lithium alloy powder.
Preferably, described lithium alloy is the alloy of Li and at least one composition in Be, Mg, Ti, Zr, V, Nb, Cr, Cu, Al, Sn and Sr.
Preferably, described lithium or lithium alloy mass percent in described inert organic solvents are 0.01～40%.
Preferably, it is x that described lithium accounts for the mass percent of lithium alloy, and meets 3%≤x ＜ 100%.
Preferably, described inert organic solvents is varsol, esters solvent, amide solvent or ether solvent.It is further preferred that described varsol is hexamethylene, normal hexane or paraffin；Described esters solvent dimethyl carbonate or ethyl acetate；Described amide solvent is N-Methyl pyrrolidone；Described ether solvent is 1,3-dioxy ring penta.
Preferably, the size in described lithium or at least one dimension of lithium alloy is not more than 10mm；When the size of described lithium or three dimensions of lithium alloy is all higher than 10mm, need to process through mechanical force, such as ball milling or cal rolling so that it is size meets requirement.The described size in a dimension can be the size of granule, the thickness of sheet, rod or the diameter of silk, the wall thickness of porous material.
Preferably, step 2) time of supersound process is 1～600min；The temperature processed is less than 180 DEG C, preferably 10～100 DEG C.
Further, seal after being full of dry air or noble gas in described container, then carry out ultrasound procedure；When the temperature of supersound process is higher than 100 DEG C, seals after filling with inert gas protection in described container and carry out ultrasound procedure again.
Described lithium powder or lithium alloy powder are through filtering and preserving in an inert atmosphere after dried.
Lithium powder or lithium alloy powder that the present invention prepares can apply to lithium battery, solve, by " benefit lithium ", the problem that its initial coulomb efficiency is low；Meanwhile, it can be used for preparing lithium alkylide, shortens manufacturing cycle and improves product yield.
The present invention, by ultrasonic applications broken lithium metal or method of lithium alloy in liquid phase, prepares micron order lithium powder or lithium alloy powder.This is a kind of new to prepare lithium powder or the method for lithium alloy powder, compared with prior art has the advantage that
1) producing temperature to need not carry out under the high temperature more than lithium metal and alloy melting point thereof, and can also at room temperature carry out, the harshest to equipment requirements, production security is high；
2) the optional wide ranges of inert organic solvents, it is not necessary to use high boiling solvent, save the subsequent processing steps of high boiling solvent；
3) noble gas such as unnecessary Ar of protective atmosphere, can select dry air to replace；
4) except spherical metal lithium powder or lithium alloy powder can be prepared, the aspherical metallic lithium powders such as lamellar or lithium alloy powder are also prepared；Reactivity is good；
5) Ultrasonic Pulverization technique is simple, and easy and simple to handle, production cost is low, efficiency is high, and equipment requirements is low, maintenance is easy.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of the lithium powder that embodiment 1 prepares；
Fig. 2 is the XRD figure spectrum of the lithium powder that embodiment 1 prepares；
Fig. 3 be the lithium powder for preparing of embodiment 1 put lithium capacity curve；
Fig. 4 is first all charging and discharging curves of the silicon-carbon cathode material containing the prepared lithium powder of embodiment 1.
Detailed description of the invention
Below in conjunction with drawings and Examples, technical scheme is described in detail.
Embodiment 1
In the plastic bottle of 200ml, load battery grade lithium paper tinsel and the 45g dimethyl carbonate of 5g, then plastic bottle is sealed；Supersound process 180min in the ultrasonic instrument of 100W, temperature is not higher than 50 DEG C, then filters and be vacuum dried, and obtains lithium powder.This lithium powder is carried out performance test, obtains such as Fig. 1～4.
Fig. 1 is the SEM photograph of the lithium powder that the present embodiment obtains, it can be seen that metallic lithium powder is laminated structure, thickness is 5～50 μm, and width is 100～300 μm, and radius-thickness ratio is about 3～30.
Fig. 2 is the XRD spectra of the lithium powder that the present embodiment obtains, and shows that its thing is Li mutually, and there is LiOH.Understanding in conjunction with SEM and XRD analysis result, metallic lithium powder is lamellar, and some little granules that its surface exists are LiOH.LiOH is to be reacted by the minor amount of water in active metallic lithium powder and organic solvent or in air to generate, it strict control the preparation of lithium powder and test characterize during can avoid producing in the case of moisture in environment.Lithium powder without LiOH is very active, in faint yellow, basically identical with the color of lithium paper tinsel.
Above-mentioned metallic lithium powder is rolled on Cu paper tinsel as Electrode, make electrode, 1mol/LLiPF with metal lithium sheet6The solution of EC/DMC (volume ratio is 1:1) make electrolyte, Cellgard2400 micro-pore septum makees barrier film, makes 2032 type button cells.Use the charge-discharge performance of Wuhan indigo plant electricity battery test system (LANDCT2001A) test battery.Ibid, Electrode changing into pole piece and has rolled the silicon-carbon electrode of above-mentioned metallic lithium powder, remaining is constant, is prepared as 2032 type button cells and tests its charge-discharge performance.
Fig. 3 be metallic lithium powder prepared by the present embodiment put lithium capacity curve, be typical metallic lithium powder put lithium curve.The lithium capacity of putting of prepared metallic lithium powder is up to 3162mAh/g, is that lithium metal theory puts the 83% of lithium capacity (～3800mAh/g).It addition, Fig. 4 shows, first all charge and discharge capacity of the silicon-carbon cathode material of " benefit lithium " are not respectively 522mAh/g and 791mAh/g, and first all irreversible capacities are 269mAh/g, and head week coulombic efficiency only has 66.0%.The above-mentioned metallic lithium powder of weight about silicon-carbon cathode material 10% is rolled after electrode surface, first all charge and discharge capacity of surveyed silicon-carbon cathode material become 587mAh/g and 508mAh/g, first all irreversible capacities are reduced to 0mAh/g, and first all coulombic efficiencies have reached more than 100%.This result shows, prepared lithium powder can release substantial amounts of lithium, it is possible to improves the initial coulomb efficiency of silicon-carbon cathode material significantly, it is possible to effectively to lithium battery " benefit lithium ".
Embodiment 2
Adding 9.5g hexamethylene and battery grade lithium sheet that 0.5g thickness is 0.7mm in 50ml vial with cover, then seal, supersound process 30min in the ultrasonic instrument of 50W, temperature is not higher than 30 DEG C, then filters and be vacuum dried, obtains metallic lithium powder.
Embodiment 3
9.5g dimethyl carbonate and Li-Mg alloy (containing Li75%) that 0.5g particle diameter is 1～2mm is added in 50ml vial with cover; fill Ar protect and seal; supersound process 10min in the ultrasonic instrument of 100W; temperature is not higher than 40 DEG C; then filter and be vacuum dried, obtaining Li-Mg alloyed powder.
Embodiment 4
In 2ml centrifuge tube with cover, add 1gN-methyl pyrrolidone and the lithium silk of a diameter of 0.8mm of 0.05g, close the lid and seal, room temperature supersound process 2min in the ultrasonic instrument of 50W, then filters and is vacuum dried, obtaining metallic lithium powder.
Embodiment 5
The lithium grain that 2g particle diameter is 3mm is placed in stainless steel jar mill, adds 20g stainless steel ball, in 400 revs/min of lower ball-milling treatment 60min；After taking out stainless steel ball, addition 40g1,3-dioxy ring penta is as inert organic solvents, by ultrasonic cell disruption instrument supersound process 10min of 650W under Ar protective atmosphere, filters, vacuum drying, obtains metallic lithium powder.
Lithium metal has preferable ductility, bigger viscosity and relatively low fusing point, is simply being transformed into the thin lithium sheet being attached to stainless steel ball-milling top tank structure, needs follow-up supersound process just can be transformed into lithium powder after ball milling operation.
Embodiment 6
The aluminium lithium alloy (Li content 20%) of 10g particle diameter 20mm is placed in stainless steel jar mill; add 100g stainless steel ball; in 300 revs/min of lower ball-milling treatment 30min; 200g ethyl acetate is added as inert organic solvents after taking out stainless steel ball; by ultrasonic cell disruption instrument supersound process 30min of 400W under Ar protective atmosphere; filter, vacuum drying, obtain aluminium lithium alloy powder.
Application in terms of chemistry:
The lithium grain that 40ml normal hexane, 2.0g particle diameter are 1～2mm is added, by ultrasonic instrument supersound process 30min of 100W under Ar protective atmosphere, it is thus achieved that be dispersed with the hexane solution of metallic lithium powder in three neck round bottom.(chloro-butane reacts with lithium powder to be slowly added dropwise 13.2g chloro-butane under magnetic stirring, prepare butyl lithium, solvent is normal hexane), reflux after adding 2h, then standing sedimentation 8h, clear liquid is pressed in storage bottle with Ar, residue adds the stirring of 40ml normal hexane, settles 8h, merges twice supernatant, obtain butyl lithium solution, yield about 94%.But, if directly using lithium grain, prepare butyl lithium solution under identical condition, as long as its yield has about 72%.
Claims (9)
1. a lithium powder or the preparation method of lithium alloy powder, it is characterised in that comprise the steps:
1) lithium or lithium alloy are added in the container filling inert organic solvents；Described inert organic solvents is the organic solvent not reacted with lithium or lithium alloy；
2) sonicated, the described lithium powder must being saved in organic solvent or lithium alloy powder.
2. as claimed in claim 1 lithium powder or the preparation method of lithium alloy powder, it is characterised in that: step 2) sonicated after, also through filtering, be dried, obtain described lithium powder or lithium alloy powder.
3. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: described lithium alloy is alloy of Li and at least one composition in Be, Mg, Ti, Zr, V, Nb, Cr, Cu, Al, Sn and Sr.
4. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: described lithium or lithium alloy mass percent in described inert organic solvents are 0.01～40%.
5. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: it is x that described lithium accounts for the mass percent of lithium alloy, and meets 3%≤x ＜ 100%.
6. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: described inert organic solvents is varsol, esters solvent, amide solvent or ether solvent；Preferably, described varsol is hexamethylene, normal hexane or paraffin；Described esters solvent dimethyl carbonate or ethyl acetate；Described amide solvent is N-Methyl pyrrolidone；Described ether solvent is 1,3-dioxy ring penta.
7. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: the size on described lithium or at least one dimension of lithium alloy is not more than 10mm；When the size of described lithium or three dimensions of lithium alloy is all higher than 10mm, need to process through mechanical force so that it is size meets requirement.
8. as claimed in claim 1 or 2 lithium powder or the preparation method of lithium alloy powder, it is characterised in that: step 2) time of supersound process is 1～600min；The temperature processed is less than 180 DEG C, preferably 10～100 DEG C.
9. lithium powder as claimed in claim 1 or 2 or the preparation method of lithium alloy powder, it is characterised in that: seal after being full of dry air or noble gas in described container, then carry out ultrasound procedure；When the temperature of supersound process is higher than 100 DEG C, seals after filling with inert gas protection in described container and carry out ultrasound procedure again.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107261579A (en) * | 2017-06-22 | 2017-10-20 | 中科京投环境科技江苏有限公司 | A kind of method that pole plate is directly filled by slurry |
| CN107297507A (en) * | 2017-06-27 | 2017-10-27 | 浙江大学 | A kind of preparation method of sub-micron nano metal lithium particle |
| CN108832116A (en) * | 2018-06-20 | 2018-11-16 | 成都爱敏特新能源技术有限公司 | A kind of sheet metal lithium powder and preparation method thereof |
| CN109309201A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Porous carbon skeleton-nano particle composite material, its lithium metal compound, their preparation method and application |
| CN109713215A (en) * | 2018-12-25 | 2019-05-03 | 深圳市倍特力电池有限公司 | Mend lithium cathode sheet and preparation method thereof, lithium ion battery |
| CN109773199A (en) * | 2019-01-15 | 2019-05-21 | 中国科学院合肥物质科学研究院 | A kind of fast preparation method of multiple dimensioned lithium ball |
| CN111313013A (en) * | 2020-03-02 | 2020-06-19 | 同济大学 | Preparation method and application of lithium-tin alloy powder for lithium ion battery cathode |
| CN111584853A (en) * | 2020-05-29 | 2020-08-25 | 昆山宝创新能源科技有限公司 | Pre-lithiated negative electrode material and preparation method and application thereof |
| CN111889688A (en) * | 2020-08-05 | 2020-11-06 | 四川中科杰迈储能材料有限责任公司 | Safe and simple preparation method of metal lithium powder |
| CN114212766A (en) * | 2021-11-04 | 2022-03-22 | 湖南金硅科技有限公司 | Lithium-supplementing modified silicon material and preparation method and application thereof |
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| CN107261579A (en) * | 2017-06-22 | 2017-10-20 | 中科京投环境科技江苏有限公司 | A kind of method that pole plate is directly filled by slurry |
| CN107297507A (en) * | 2017-06-27 | 2017-10-27 | 浙江大学 | A kind of preparation method of sub-micron nano metal lithium particle |
| CN107297507B (en) * | 2017-06-27 | 2019-09-10 | 浙江大学 | A kind of preparation method of sub-micron-nano metal lithium particle |
| CN109309201A (en) * | 2017-07-26 | 2019-02-05 | 中能中科（天津）新能源科技有限公司 | Porous carbon skeleton-nano particle composite material, its lithium metal compound, their preparation method and application |
| CN108832116A (en) * | 2018-06-20 | 2018-11-16 | 成都爱敏特新能源技术有限公司 | A kind of sheet metal lithium powder and preparation method thereof |
| CN109713215A (en) * | 2018-12-25 | 2019-05-03 | 深圳市倍特力电池有限公司 | Mend lithium cathode sheet and preparation method thereof, lithium ion battery |
| CN109713215B (en) * | 2018-12-25 | 2022-03-11 | 深圳市倍特力电池有限公司 | Lithium-supplement negative plate, preparation method thereof and lithium ion battery |
| CN109773199A (en) * | 2019-01-15 | 2019-05-21 | 中国科学院合肥物质科学研究院 | A kind of fast preparation method of multiple dimensioned lithium ball |
| CN109773199B (en) * | 2019-01-15 | 2021-05-28 | 中国科学院合肥物质科学研究院 | Rapid preparation method of multi-scale lithium ball |
| CN111313013A (en) * | 2020-03-02 | 2020-06-19 | 同济大学 | Preparation method and application of lithium-tin alloy powder for lithium ion battery cathode |
| CN111584853A (en) * | 2020-05-29 | 2020-08-25 | 昆山宝创新能源科技有限公司 | Pre-lithiated negative electrode material and preparation method and application thereof |
| CN111889688A (en) * | 2020-08-05 | 2020-11-06 | 四川中科杰迈储能材料有限责任公司 | Safe and simple preparation method of metal lithium powder |
| CN111889688B (en) * | 2020-08-05 | 2022-12-23 | 四川物科金硅新材料科技有限责任公司 | Safe and simple preparation method of metal lithium powder |
| CN114212766A (en) * | 2021-11-04 | 2022-03-22 | 湖南金硅科技有限公司 | Lithium-supplementing modified silicon material and preparation method and application thereof |
| CN114212766B (en) * | 2021-11-04 | 2024-02-13 | 湖南金硅科技有限公司 | Lithium-supplementing modified silicon material and preparation method and application thereof |
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