WO2003063271A1 - Electrodes ameliorees pour piles de metal alcalin - Google Patents

Electrodes ameliorees pour piles de metal alcalin Download PDF

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Publication number
WO2003063271A1
WO2003063271A1 PCT/US2002/002349 US0202349W WO03063271A1 WO 2003063271 A1 WO2003063271 A1 WO 2003063271A1 US 0202349 W US0202349 W US 0202349W WO 03063271 A1 WO03063271 A1 WO 03063271A1
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WO
WIPO (PCT)
Prior art keywords
rechargeable battery
electrochemically
preliminary reactions
irreversible
preliminary
Prior art date
Application number
PCT/US2002/002349
Other languages
English (en)
Inventor
Robert A. Huggins
Andreas Netz
Original Assignee
Huggins Robert A
Andreas Netz
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Huggins Robert A, Andreas Netz filed Critical Huggins Robert A
Priority to PCT/US2002/002349 priority Critical patent/WO2003063271A1/fr
Publication of WO2003063271A1 publication Critical patent/WO2003063271A1/fr

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Classifications

    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/049—Manufacturing of an active layer by chemical means
    • H01M4/0492—Chemical attack of the support material
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • 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
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/044—Activating, forming or electrochemical attack of the supporting material
    • H01M4/0445—Forming after manufacture of the electrode, e.g. first charge, cycling
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

Definitions

  • This application relates to improvements in the properties of negative electrodes in alkali metal battery systems and the batteries that contain them.
  • the alkali metals are elements of the first group of the periodic table, lithium, sodium, potassium, rubidium, cesium and francium.
  • Alkali metal batteries consist of negative electrodes and positive electrodes that are separated by an electrolyte. Their charge and discharge processes involve the transport of the electroactive species (alkali metal ions) through the electrolyte back and forth between the positive and negative electrodes.
  • Alkali metal batteries are typically constructed in the discharged state. That is, the electroactive alkali metal is initially incorporated in the structure of the positive electrode, rather than the negative electrode. Under these conditions it is typical that both the positive and negative electrode materials are relatively insensitive to air and water vapor, and thus easy to handle. In contrast, the positive and, especially, the negative electrode materials are not stable in air after the battery is charged and some or all of the alkali metal has moved from the positive electrode to the negative electrode. This is why the final assembly of such batteries involves their enclosure in a hermetically sealed container after the introduction of the electrodes and the electrolyte.
  • the amount of charge, i.e. the number of alkali metal ions, entering or leaving the negative electrode is the same as the number of ions which enter or leave the positive electrode.
  • the amount of charge entering or leaving the two electrodes is the same, and the reversible charge capacity of the battery is limited by the amount of reversible capacity of the electrode with the lower value of reversible capacity.
  • the reversible capacity of an electrode is the amount of electrical charge, i.e. electroactive species, that can be repeatedly added to (supplied to), and deleted from (removed from), the electrode during the normal operation of the battery.
  • Electrodes can also have irreversible capacity. In the case of negative electrodes, for example, the amount of charge, i.e. the number of electroactive species, that can be removed, can be less than that which is supplied.
  • Battery systems for the storage of electrical energy may be constructed with alkali metals as the electroactive species. Lithium and sodium are the most common examples.
  • the alkali metal is lithium
  • current negative electrodes typically involve the insertion and extraction of the lithium from graphite and other carbons.
  • the maximum specific capacity of this negative electrode is determined by the amount of lithium that can be inserted into the graphite crystal structure. This is represented by the formula LiC 6 , and theoretically amounts to 372 mAh/g of carbon weight in the negative electrode. Practical values in commercial cells typically fall in the range 300-350 mAh/g.
  • Lithium-carbons are currently used as negative electrodes in lithium batteries,
  • lithium reacts with these oxides to produce multiple product materials.
  • One of them being a lithium-containing oxide that is electrochemically irreversible in the battery. This results in irreversible capacity.
  • one or more other product materials e.g. a metal or alloy, is formed that can subsequently react reversibly with additional lithium, producing reversible capacity.
  • the total amount of lithium that is initially absorbed in this electrode is composed of two parts. One part results in the formation of the lithium-containing oxide and is irreversible. The other part generates potentially reversible, and thus usable, capacity.
  • Non-oxide materials have been found that also have an initial capacity that contains both irreversible and reversible components. In those cases some of the lithium, or other alkali metal, that is put into the electrode when it is charged forms an electrochemically irreversible product and remains trapped, and is not accessible within the potential range of the operation of the electrode subsequently.
  • This invention provides for improved capacity of alkali metal batteries. This is due to a substantial improvement of the properties of the negative electrode. A number of otherwise attractive negative electrode materials suffer from a serious disadvantage due to their reaction with a large amount of extra alkali metal during the first charging cycle or cycles. This extra alkali metal cannot be recovered and employed during subsequent charge- discharge cycles. It therefore represents irreversible and unusable capacity in the negative electrode, which must be balanced by the presence of extra sacrificial capacity, with its concommitant mass and volume, in the positive electrode or elsewhere in the battery system, thus negatively affecting the properties of the battery as a whole.
  • the properties of such alkali metal battery negative electrodes can be substantially improved by performing one or more preliminary reactions , i.e. pre-trealment(s), or initial charging-discharging cycle or cycles, of the negative electrode prior to the final assembly of the battery.
  • the one or more preliminary reactions create product materials in the electrode, a subset of which are electrochemically irreversible in the battery prior to its final assembly.
  • These one or more preliminary reactions can be done either by the use of one or more chemical reactants, or by the employment of an electrochemical cell, to supply the required irreversible extra alkali metal, or a combination of chemical and electrochemical means. It can also be done at several different electrical or chemical potential levels, and involve the use of multiple cycles. It can be performed on individual electrode materials, on combinations of materials, on electrode components, or on assembled electrodes.
  • FIG 1 is a graph showing the relationship between the voltage and the capacity of Sn 2 BP0 6 glass upon cycling in a lithium cell.
  • a capacity of 980 mAh g Upon initial charging there is a capacity of 980 mAh g, but a capacity of only about 480 mAh/g is found during the first discharge. The difference, about 500 mAh/g, is irreversible capacity loss. Subsequent cycles evidence only the reversible 480 mAh/g.
  • FIG 2 is a graph showing the results of another lithium example, three discharge-charge cycles of SiO without a pre-lithiation charge-discharge cycle.
  • a t represents the magnitude of the capacity upon the first charging cycle
  • B t represents the magnitude of the capacity during the first discharge cycle.
  • a 2 and B 2 represent the magnitudes of the charging and discharging capacity in the second cycle
  • a 3 and B 3 the corresponding values for the
  • FIG 3 is a graph showing the results of three discharge-charge cycles of SiO after a preliminary electrochemical pre-lithiation charge-discharge cycle.
  • A represents the magnitude of the capacity upon the first charging cycle
  • B represents the magnitude of the capacity during the first discharge cycle.
  • a 2 and B 2 represent the magnitudes of the charging and discharging capacity in the second cycle
  • a 3 and B 3 the corresponding values for the third cycle.
  • This invention provides a method to limit the initial irreversible capacity in an alkali metal- based electrochemical cell, and thus the necessity for the presence of an additional alkali metal source material in the cell.
  • This external preliminary cycle, or cycles can be done either chemically or electrochemically, or a combination of the two.
  • One is to perform the initial charge-discharge cycle, or cycles, upon a prepared electrode, and the other is to perform the preliminary charge-discharge cycle, or cycles, upon one or more of the components of the final electrode structure.
  • the electrode may be preconditioned as fully charged, fully discharged, or an intermediate state prior to incorporation into the final battery system.
  • the electrode material in order for the charging part of the pre-lithiation cycle to be done chemically, the electrode material must react with a chemical lithium source that has a lithium activity greater than that of the material to be lithiated.
  • a chemical lithium source that has a lithium activity greater than that of the material to be lithiated.
  • a number of materials have been used as chemical lithium sources for reactants that operate at relatively high potentials, such as those used as positive electrode materials in lithium systems. This can also, in principle, be done with negative electrode materials.
  • the requirement is that the reaction potential of the lithium source must be lower than that of the material being Hthiated in order to supply lithium to it.
  • the reaction potential of the lithium source must be higher than that of the material being de- lithiated in order to remove lithium from it. Examples of well-known chemical lithium reactants and their reaction potentials are included in Table 2.
  • One is to perform the initial charge-discharge cycle or cycles upon a normal electrode structure by inserting said structure into a simple electrochemical cell external to the final battery and to use an alkali metal or some other alkali metal-containing material with the appropriate polarity as the alkali metal source and sink. After passing current through the cell in order to cause the charge-discharge reaction of the alkali metal, with the electrode structure, the pretreated electrode is removed, and subsequently inserted into the battery.
  • a variant would be to perform the initial alkali metal loading of the negative electrode structure in-situ within the cell, using an external alkali metal-providing electrode, prior to the final sealing of the cell. In any of these alternatives the electrode may be preconditioned as fully charged, fully discharged or an intermediate state, prior to final assembly.
  • the second possibility is to do the initial external electrochemical charge-discharge cycle or cycles on the primary electrode reactant, or on a combination of components, rather than upon the complete electrode.
  • This electrochemical pre-treatment can be done either galvanostatically or potentiostatically, or a combination of both.
  • the initial pre-treatment cycle is to be done galvanostatically and to be performed only once, other variations are possible.
  • the first charge-discharge cycle could include both galvanostatic and potentiostatic components.
  • Another variation would be to perform this initial pre-treatment using more than one cycle in order to increase the thoroughness of the reduction of the irreversible capacity.
  • This method can be utilized at elevated temperatures as well as at ambient temperatures. In some cases, this will increase the kinetics, or result in other advantages.
  • electrolyte employed for the alkali metal pre-treatment be the same as that utilized in the final electrochemical battery.
  • the alkali metal involved in the pre-treatment is different from the alkali metal that is involved in subsequent reversible reactions of the electrode in the battery.
  • lithium which is more reactive and also has a lower atomic weight, might be used to pre-treat a convertible negative electrode intended for use in a sodium battery.
  • An example of the use of this invention is the performance of an external electrochemical lithium charge-discharge cycle on SiO.
  • An electrode was constructed by placing of a 30 micrometer thick layer of SiO, plus a binder and electronically conducting carbon in the ratio (85/10/5), on a copper foil substrate by tape casting. This was followed by heating to about 110°C for 24 hours to drive off volatile parts of the binder. This electrode was then inserted into a simple air-tight coffee-bag type of cell with a fiberglass separator containing a liquid electrolyte (LiPF ⁇ in an EC-DEC solution) and also a lithium counter electrode. Current was passed through the cell at a rate of 0.1 mA/cm 2 for some 74 hours, until the potential reached 25 mV vs Li.
  • LiPF ⁇ liquid electrolyte

Abstract

L'invention concerne un procédé pour réduire la capacité initialement irréversible d'une cellule électrochimique à base de métal alcalin et, par conséquent, la présence nécessaire de matériau source additionnel en métal alcalin dans ladite cellule, une ou plusieurs réactions préliminaires étant réalisées par des moyens électrochimiques ou chimiques et les réactions préliminaires se produisant avant l'assemblage final.
PCT/US2002/002349 2002-01-19 2002-01-19 Electrodes ameliorees pour piles de metal alcalin WO2003063271A1 (fr)

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PCT/US2002/002349 WO2003063271A1 (fr) 2002-01-19 2002-01-19 Electrodes ameliorees pour piles de metal alcalin

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7683359B2 (en) 2002-11-05 2010-03-23 Nexeon Ltd. Structured silicon anode
US8101298B2 (en) 2006-01-23 2012-01-24 Nexeon Ltd. Method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8585918B2 (en) 2006-01-23 2013-11-19 Nexeon Ltd. Method of etching a silicon-based material
US8642211B2 (en) 2007-07-17 2014-02-04 Nexeon Limited Electrode including silicon-comprising fibres and electrochemical cells including the same
US8772174B2 (en) 2010-04-09 2014-07-08 Nexeon Ltd. Method of fabricating structured particles composed of silicon or silicon-based material and their use in lithium rechargeable batteries
US8870975B2 (en) 2007-07-17 2014-10-28 Nexeon Ltd. Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8945774B2 (en) 2010-06-07 2015-02-03 Nexeon Ltd. Additive for lithium ion rechageable battery cells
US8962183B2 (en) 2009-05-07 2015-02-24 Nexeon Limited Method of making silicon anode material for rechargeable cells
US9012079B2 (en) 2007-07-17 2015-04-21 Nexeon Ltd Electrode comprising structured silicon-based material
US9184438B2 (en) 2008-10-10 2015-11-10 Nexeon Ltd. Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US9252426B2 (en) 2007-05-11 2016-02-02 Nexeon Limited Silicon anode for a rechargeable battery
US9608272B2 (en) 2009-05-11 2017-03-28 Nexeon Limited Composition for a secondary battery cell
US9647263B2 (en) 2010-09-03 2017-05-09 Nexeon Limited Electroactive material
US9853292B2 (en) 2009-05-11 2017-12-26 Nexeon Limited Electrode composition for a secondary battery cell
US9871248B2 (en) 2010-09-03 2018-01-16 Nexeon Limited Porous electroactive material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06267532A (ja) * 1993-03-11 1994-09-22 Fuji Elelctrochem Co Ltd リチウム二次電池の製造方法
JPH10294104A (ja) * 1997-04-17 1998-11-04 Hitachi Maxell Ltd リチウム二次電池の電極の製造方法
WO2002047185A2 (fr) * 2000-12-06 2002-06-13 Huggins Robert A Electrodes ameliorees destinees a des batteries au lithium

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06267532A (ja) * 1993-03-11 1994-09-22 Fuji Elelctrochem Co Ltd リチウム二次電池の製造方法
JPH10294104A (ja) * 1997-04-17 1998-11-04 Hitachi Maxell Ltd リチウム二次電池の電極の製造方法
WO2002047185A2 (fr) * 2000-12-06 2002-06-13 Huggins Robert A Electrodes ameliorees destinees a des batteries au lithium

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DATABASE INSPEC [online] THE INSTITUTION OF ELECTRICAL ENGINEERS, STEVENAGE, GB; 2001, NETZ A. ET AL.: "Investigations of a number of alternative negative electrode materials for use in lithium cells", XP002225806, Database accession no. 7186515 *
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Cited By (27)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8384058B2 (en) 2002-11-05 2013-02-26 Nexeon Ltd. Structured silicon anode
US7842535B2 (en) 2002-11-05 2010-11-30 Nexeon Ltd. Structured silicon anode
US8017430B2 (en) 2002-11-05 2011-09-13 Nexeon Ltd. Structured silicon anode
US7683359B2 (en) 2002-11-05 2010-03-23 Nexeon Ltd. Structured silicon anode
US9583762B2 (en) 2006-01-23 2017-02-28 Nexeon Limited Method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8585918B2 (en) 2006-01-23 2013-11-19 Nexeon Ltd. Method of etching a silicon-based material
US8597831B2 (en) 2006-01-23 2013-12-03 Nexeon Ltd. Method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8101298B2 (en) 2006-01-23 2012-01-24 Nexeon Ltd. Method of fabricating fibres composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US9871249B2 (en) 2007-05-11 2018-01-16 Nexeon Limited Silicon anode for a rechargeable battery
US9252426B2 (en) 2007-05-11 2016-02-02 Nexeon Limited Silicon anode for a rechargeable battery
US8940437B2 (en) 2007-07-17 2015-01-27 Nexeon Limited Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US9871244B2 (en) 2007-07-17 2018-01-16 Nexeon Limited Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US9012079B2 (en) 2007-07-17 2015-04-21 Nexeon Ltd Electrode comprising structured silicon-based material
US8870975B2 (en) 2007-07-17 2014-10-28 Nexeon Ltd. Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8642211B2 (en) 2007-07-17 2014-02-04 Nexeon Limited Electrode including silicon-comprising fibres and electrochemical cells including the same
US9184438B2 (en) 2008-10-10 2015-11-10 Nexeon Ltd. Method of fabricating structured particles composed of silicon or a silicon-based material and their use in lithium rechargeable batteries
US8962183B2 (en) 2009-05-07 2015-02-24 Nexeon Limited Method of making silicon anode material for rechargeable cells
US9553304B2 (en) 2009-05-07 2017-01-24 Nexeon Limited Method of making silicon anode material for rechargeable cells
US9608272B2 (en) 2009-05-11 2017-03-28 Nexeon Limited Composition for a secondary battery cell
US9853292B2 (en) 2009-05-11 2017-12-26 Nexeon Limited Electrode composition for a secondary battery cell
US10050275B2 (en) 2009-05-11 2018-08-14 Nexeon Limited Binder for lithium ion rechargeable battery cells
US8772174B2 (en) 2010-04-09 2014-07-08 Nexeon Ltd. Method of fabricating structured particles composed of silicon or silicon-based material and their use in lithium rechargeable batteries
US8945774B2 (en) 2010-06-07 2015-02-03 Nexeon Ltd. Additive for lithium ion rechageable battery cells
US9368836B2 (en) 2010-06-07 2016-06-14 Nexeon Ltd. Additive for lithium ion rechargeable battery cells
US9647263B2 (en) 2010-09-03 2017-05-09 Nexeon Limited Electroactive material
US9871248B2 (en) 2010-09-03 2018-01-16 Nexeon Limited Porous electroactive material
US9947920B2 (en) 2010-09-03 2018-04-17 Nexeon Limited Electroactive material

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