US20130181160A1 - Stabilized, pure lithium metal powder and method for producing the same - Google Patents

Stabilized, pure lithium metal powder and method for producing the same Download PDF

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Publication number
US20130181160A1
US20130181160A1 US13/825,446 US201113825446A US2013181160A1 US 20130181160 A1 US20130181160 A1 US 20130181160A1 US 201113825446 A US201113825446 A US 201113825446A US 2013181160 A1 US2013181160 A1 US 2013181160A1
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acid
stabilized
lithium metal
metal powder
powder according
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US13/825,446
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Ulrich Wietelmann
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Albemarle Germany GmbH
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Chemetall GmbH
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Assigned to CHEMETALL GMBH reassignment CHEMETALL GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: WIETELMANN, ULRICH
Assigned to Rockwood Lithium GmbH reassignment Rockwood Lithium GmbH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHEMETALL GMBH
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/102—Metallic powder coated with organic material
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/14—Treatment of metallic powder
    • B22F1/145—Chemical treatment, e.g. passivation or decarburisation
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C24/00—Alloys based on an alkali or an alkaline earth metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/73—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals characterised by the process
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • H01M4/381—Alkaline or alkaline earth metals elements
    • H01M4/382—Lithium
    • 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
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • 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
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • 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
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
    • 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
    • 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
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]

Definitions

  • Lithium is an alkali metal. As with the heavy element homologues of the first main group, it is characterized by strong reactivity relative to a plurality of materials. It reacts violently, often igniting, with water, alcohols and other materials containing protic hydrogen. Exposed to air, it is unstable reacting with oxygen, nitrogen and carbon dioxide. This is why it is usually handled under an inert gas (noble gases, such as argon) and stored under a protective layer of paraffin oil.
  • inert gas noble gases, such as argon
  • a further method for stabilizing lithium metal provides for heating the same in excess of the melting point thereof, stirring the melted lithium and bringing it into contact with a fluorinating agent, for example perfluoropentylamine (WO 2007/005983A2).
  • a fluorinating agent for example perfluoropentylamine (WO 2007/005983A2).
  • fluorinating agents are often toxic or caustic, which is why they are used with great caution in industrial practice.
  • a further method for a protective surface treatment of lithium metal envisions providing the same with a wax layer, for example a polyethylene wax layer (WO 2008/045557A1). It is disadvantageous, however, that this method requires the use of quite a large quantity of coating agent.
  • the examples that are listed in the mentioned patent application specify approximately 1%.
  • US 200810283155A1 discloses a method for stabilizing lithium metal that is characterized by the following steps: a) heating lithium metal powder in excess of the melting point thereof in order to produce melted lithium metal; b) dispersing the melted lithium metal; and c) bringing the melted lithium metal in contact with a phosphor-containing substance in order to generate a substantially continuous protective layer of lithium phosphate on the lithium metal powder.
  • Handling acidic, caustic materials phosphoric acid
  • phosphoric acid is generally disadvantageous, but particularly in the presence of lithium metal: upon being brought in contact with each other, both materials react violently releasing an enormous amount of heat.
  • explosive hydrogen gas is generated when reacting lithium metal with phosphoric acid.
  • US US2009/0061321 proposes the preparation of a stabilized lithium metal powder with a substantially continuous polymer coating.
  • the polymer can be selected from the group comprising polyurethanes, PTFE, PVC, polystyrol, etc.
  • this method provides the protected lithium metal with an undefined surface coating of organic substances that could interfere during any subsequent use thereof, for example the prelithiation of electrode materials.
  • the object of the invention seeks to provide a method for preparing lithium metal powder with a passivating cover layer
  • a lithium powder of this kind should be stable for days up to approximately 50° C. and in the presence of polar, reactive solvents, such as are used in the preparation of electrode coatings (for example, NMP).
  • the object is achieved by using saturated and/or unsaturated fatty acids and/or fatty acid esters according to the general formula I
  • R denotes C 10 -C 29 moieties
  • R′ stands for H or C 1 -C 8 moieties.
  • a pure lithium meaning particularly a lithium quality poor in sodium, is used as lithium source. Surprisingly, it was found that using a lithium metal that is poor in sodium, it is possible to obtain especially stable products that are safe to handle.
  • the lithium is heated under an inert gas (noble gas, for example dry argon) in an organic, inert solvent or solvent mixture (typically hydrocarbon-based) in excess of the temperature when melting occurs (180.5° C.).
  • an inert gas typically dry argon
  • organic, inert solvent or solvent mixture typically hydrocarbon-based
  • solvents typically hydrocarbon-based
  • the melting process occurs in an enclosed vessel and under pressurized conditions.
  • the passivation agent is added when melting is complete, and operation of the agitator system that is used for preparing the dispersion (typically a dispersion disc) is started.
  • the precise dispersion parameters (meaning mainly the rotation speed and the dispersion time) depend on the desired particle size. They further depend on the viscosity of the dispersion solvent as well as the individual geometric parameters of the agitation element (for example, diameter, precise position and toothing size). The person skilled in the art is easily able to conduct the corresponding experiments for delivering the desired particle size.
  • the agitator frequency is generally between 1,000 and 25,000 upm, preferably 2,000 to 20,000 upm.
  • the dispersion time meaning the time period during which the dispersion tool operates at full power, is between 1 and 30 minutes, preferably between 2 and 15 minutes.
  • the passivation agent therein can be added already together with the metal and solvent prior to the beginning of the heating phase. Preferably, however, it is only added after the metal has melted, meaning at temperatures >180° C. The addition can be in an uncontrolled fashion (meaning in one portion) during the dispersion process. Preferably, the passivation agent is added over a time period of approximately 5 s to 1000 s, especially preferred 30 s to 500 s.
  • Fatty acids or fatty acid esters are used as passivation agents. These auxiliary agents have the advantage that they are commercially available and non-toxic, without remarkable steam pressure, and they do not generate a disturbing film made up of the elements oxygen, carbon and hydrogen on the metal surface.
  • auxiliary agents have the advantage that they are commercially available and non-toxic, without remarkable steam pressure, and they do not generate a disturbing film made up of the elements oxygen, carbon and hydrogen on the metal surface.
  • Examples of preferred passivation agents are: olein (oleic acid), stearic acid, palmitinic acid, lauric acid, myristinic acid, margaric acid, palmitoleinic acid, linolic acid, linolenic acid, either in pure form or as mixtures thereof.
  • the esters thereof can be used, for example fatty acid glycerides or the esters with monovalent alcohols, for example ethylates, propanolates or butylates.
  • Natural products such as rapeseed oil, olive oil, sunflower oil or linseed oil can especially preferably be used.
  • passivation agents generally 0.1 to 50 g are used per kg lithium metal.
  • the use of 1 to 10 g passivation agent per kg lithium metal is preferred.
  • the specific quantity depends on the concentration of the functional groups (these are, for example, carboxylic acid groups or carboxylate groups) inside the passivation agent, as well as on the degree of fineness of the metal powder that is to be generated: the higher the degree of fineness, the greater is the specific surface, and consequently the higher the need for passivation agent.
  • the lithium metal is used in the pure form thereof, meaning the metallic contaminations must be below 500 ppm in total.
  • the sodium content is limited to a maximum of 200 ppm.
  • the Na content is preferably ⁇ 100 ppm, especially preferred ⁇ 50 ppm.
  • the mean particle size of the metal powder according to the invention is max. 200 ⁇ m, preferably max. 100 ⁇ m, and especially preferred max. 50 ⁇ m.
  • Expedient coating agents are, for example, phosphor-containing compounds (such as phosphoric acid, lithium tris(oxalato)phosphate), fluorinating agents (for example perfluoropentylamine), waxes (for example, polyethylene wax) or polymer coatings (for example, with PU, PTFE, PVC or polystyrol).
  • Said additional passivation is done in a hydrocarbon solvent at temperatures below the melting point of lithium (meaning ⁇ 180.5° C.).
  • the lithium metal powder according to the invention demonstrates in the differential scanning calorimetry test (DSC test), when in suspension with N-methyl-2-pyrrolidone (water content ⁇ ca. 200 ppm) at a minimum of 15 hours storage at 50° C., and especially preferred at 100° C., no significant exothermal effect, particularly no “run-away phenomenon.” This behavior is explained in further detail in the following examples.
  • FIG. 1 the thermal behavior during storage of the metal powder according to Example 1 in NMP at 80° C. and 100° C. furnace temperature ( ⁇ ) and sample temperature (+, ⁇ );
  • FIG. 2 the thermal behavior during storage of the metal powder according to comparison example 1 in NMP at 50° C. furnace temperature ( ⁇ ) and sample temperature (+);
  • FIG. 3 the thermal behavior during storage of a metal powder (Na content 17 ppm) obtained according to Example 1 in NMP with a water content of 1%, furnace temperature ( ⁇ ) and sample temperature (+, ⁇ );
  • FIG. 4 the thermal behavior during storage of a metal powder having an Na content of 55 ppm obtain according to Example 1 at 50° C. and 100° C. furnace temperature ( ⁇ ) and sample temperature (+, x) in NMP (148 ppm water content);
  • FIG. 5 the thermal behavior during storage of a metal powder having an Na content of 55 ppm obtained according to Example 1 at 80° C. furnace temperature ( ⁇ ) and sample temperature (+) in NMP (200 ppm water content).
  • the suspension is drained onto a vacuum filter, the filter residue is washed multiple times with hexane until it is fee of oil, then vacuum-dried.
  • the suspension is drained onto a vacuum filter, the filter residue is washed multiple times with hexane until it is fee of oil, then vacuum-dried.
  • Example 2 and Comparison Example 2 demonstrate the substantially improved stability of the lithium metal powder according to the invention in contact with NMP: while the product according to the invention did not cause any significant exothermal effects at storage at 80° C., nor at 100° C. (the sample temperature remains visibly below the furnace temperature throughout the entire observation period), the metal powder that is not according to the invention shows already at storage at 50° C. a visible exothermal reaction. This can be recognized in that the sample temperature clearly exceeds the furnace temperature.
  • the especially preferred Li metal powder having an Na content of 17 ppm proves kinetically stable even in water-rich NMP.
  • the metal powder having a sodium content of 55 ppm is stable at storage temperatures of 50° C. and 80° C.; at 100° C., however, it shows an exothermal, but not a run-away effect. According to the DSC experiment at 100° C., 73% of the used lithium is still present in metallic form.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)
  • Powder Metallurgy (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
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US13/825,446 2010-09-28 2011-09-28 Stabilized, pure lithium metal powder and method for producing the same Abandoned US20130181160A1 (en)

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DE102010046699.9 2010-09-28
DE102010046699 2010-09-28
PCT/EP2011/066858 WO2012052265A2 (fr) 2010-09-28 2011-09-28 Poudre métallique de lithium stabilisée pure et son procédé de fabrication

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US15/595,152 Active 2031-11-27 US10655229B2 (en) 2010-09-28 2017-05-15 Stabilized, pure lithium metal powder and method for producing the same
US16/848,384 Active US11021797B2 (en) 2010-09-28 2020-04-14 Stabilized, pure lithium metal powder and method for producing the same

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US (3) US20130181160A1 (fr)
EP (1) EP2621650B1 (fr)
JP (1) JP5882335B2 (fr)
KR (1) KR101919329B1 (fr)
CN (1) CN103379972B (fr)
BR (1) BR112013007687A2 (fr)
CA (1) CA2811941C (fr)
DE (1) DE112011103269A5 (fr)
WO (1) WO2012052265A2 (fr)

Cited By (7)

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CN104157463A (zh) * 2014-08-15 2014-11-19 万星光电子(东莞)有限公司 负极片及其制备方法、锂离子超级电容器
US9649688B2 (en) 2012-12-19 2017-05-16 Rockwood Lithium GmbH Lithium powder anode
EP3171433A4 (fr) * 2014-07-14 2017-12-20 Sumitomo Metal Mining Co., Ltd. Particules d'oxyde composite de lithium-nickel enrobées et procédé de production de particules d'oxyde composite de lithium-nickel enrobées
US10160036B2 (en) * 2013-04-19 2018-12-25 Albemarle Germany Gmbh Stabilized lithium metal formations coasted with a shell containing nitrogen, and a method for the production of same
US10431818B2 (en) 2013-05-16 2019-10-01 Albemarle Germany Gmbh Active lithium reservoir for lithium-ion batteries
US10522819B2 (en) 2014-02-13 2019-12-31 Albemarle Germany Gmbh Stabilised (partially) lithiated graphite materials, methods for the production thereof and use for lithium batteries
US11848448B2 (en) 2018-03-09 2023-12-19 Lg Energy Solution, Ltd. Lithium secondary battery

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DE102015202611A1 (de) 2014-02-13 2015-08-13 Rockwood Lithium GmbH Galvanische Zellen und (teil)lithiierte Lithiumbatterieanoden mit erhöhter Kapazität und Verfahren zur Herstellung von Synthesegraphit-Interkalationsverbindungen
CN105762328B (zh) * 2014-12-15 2019-03-29 比亚迪股份有限公司 一种钝化锂粉及其制备方法、添加该钝化锂粉的正极材料及电池
DE102015202612A1 (de) 2015-02-13 2016-08-18 Rockwood Lithium GmbH Stabilisierte (teil)lithiierte Graphitmaterialien, Verfahren zu deren Herstellung und Verwendung für Lithiumbatterien
CN104835652A (zh) * 2015-03-24 2015-08-12 中航锂电（洛阳）有限公司 锂超级电容电池用嵌锂负极片及制备方法、锂超级电容电池
CN106001585A (zh) * 2015-03-31 2016-10-12 Tdk株式会社 稳定化锂粉和使用其的锂离子二次电池
CN107058761B (zh) * 2016-12-19 2019-06-11 天齐锂业股份有限公司 金属锂或锂合金中降除氮化物的方法
CN106756105B (zh) * 2016-12-19 2018-10-30 天齐锂业股份有限公司 金属锂或锂合金中氮化物的降除方法
CN108923046B (zh) * 2018-07-03 2021-08-31 江苏乐能电池股份有限公司 一种纳米多孔富锂磷酸铁锂材料的制备方法
CN115249787A (zh) 2021-04-28 2022-10-28 株式会社村田制作所 一种锂离子二次电池负极、其制备方法及锂离子二次电池

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9649688B2 (en) 2012-12-19 2017-05-16 Rockwood Lithium GmbH Lithium powder anode
US10160036B2 (en) * 2013-04-19 2018-12-25 Albemarle Germany Gmbh Stabilized lithium metal formations coasted with a shell containing nitrogen, and a method for the production of same
US10431818B2 (en) 2013-05-16 2019-10-01 Albemarle Germany Gmbh Active lithium reservoir for lithium-ion batteries
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US10655229B2 (en) 2020-05-19
US20170268110A1 (en) 2017-09-21
KR20130128389A (ko) 2013-11-26
EP2621650B1 (fr) 2020-12-09
BR112013007687A2 (pt) 2016-08-09
US20200240020A1 (en) 2020-07-30
KR101919329B1 (ko) 2018-11-19
US11021797B2 (en) 2021-06-01
DE112011103269A5 (de) 2013-09-12
JP2013545886A (ja) 2013-12-26
EP2621650A2 (fr) 2013-08-07
WO2012052265A3 (fr) 2013-05-30
CN103379972A (zh) 2013-10-30
CN103379972B (zh) 2016-03-09
WO2012052265A2 (fr) 2012-04-26
JP5882335B2 (ja) 2016-03-09
CA2811941C (fr) 2020-10-20
CA2811941A1 (fr) 2012-04-26

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