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WO2016031082A1 - Matériau d'anode pour batterie au lithium-ion - Google Patents

Matériau d'anode pour batterie au lithium-ion Download PDF

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Publication number
WO2016031082A1
WO2016031082A1 PCT/JP2014/073420 JP2014073420W WO2016031082A1 WO 2016031082 A1 WO2016031082 A1 WO 2016031082A1 JP 2014073420 W JP2014073420 W JP 2014073420W WO 2016031082 A1 WO2016031082 A1 WO 2016031082A1
Authority
WO
WIPO (PCT)
Prior art keywords
anode material
lithium
carbon shell
carbon
sei
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.)
Ceased
Application number
PCT/JP2014/073420
Other languages
English (en)
Inventor
Qian CHENG
Noriyuki Tamura
Kentaro Nakahara
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
NEC Corp
Original Assignee
NEC Corp
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 NEC Corp filed Critical NEC Corp
Priority to JP2017511955A priority Critical patent/JP2017526144A/ja
Priority to PCT/JP2014/073420 priority patent/WO2016031082A1/fr
Publication of WO2016031082A1 publication Critical patent/WO2016031082A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/134—Electrodes based on metals, Si or alloys
    • 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
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

  • the present invention relates to a negative electrode (anode) material for a lithium ion battery.
  • the present invention relates to a composite anode material of carbon and silicon.
  • LIBs lithium-ion batteries
  • SEI solid-electrolyte interphase
  • Si silicon
  • Li 44 Si alloy a high theoretical specific capacity up to 4,200 mAh/g based on the formation of Li 44 Si alloy, which is 10 times higher than that of conventional carbon anodes (372 mAh/g corresponding to the formation of LiC 6 ).
  • Si expands volumetrically by up to 400% upon full lithium insertion (lithiation) to form the Li 44 Si alloy, and the alloy can contract significantly to return Si upon lithium extraction (delithiation), creating two critical challenges associated with
  • silicon-based anode materials degradation of the mechanical integrity of Si anode materials and SEI stability.
  • the SEI stability at the interface between Si and the liquid electrolyte is another critical factor in obtaining long cycle life; it is a very challenging issue and has not been effectively addressed for materials with large volume changes.
  • Electrolyte decomposition occurs due to the low potential of the anode and forms a passivation SEI layer on the surface of the anode material during battery charging.
  • the SEI layer is an electronic insulator but a lithium ion conductor; this results in the SEI eventually terminating growth at a certain thickness.
  • Si nanostructures have largely overcome mechanical fracture issues, their interface with the electrolyte is not static due to repetitive volume expansion and contraction. The issue of the SEI stability will be described with reference to Fig. 2.
  • Fig 2 is a schematic diagram of SEI formation on the surface of a conventional anode material composed of solid Si. Si particle 21 expands upon charging (lithiation) by changing into Si-Li alloy 23.
  • a thin layer of SEI 22 forms on the surface of Si-Li alloy 23 in the lithiated and expanded state.
  • Si-Li alloy 23 returns to Si particle 21, and SEI 22 can break down into separate pieces, exposing fresh Si surface to the liquid electrolyte.
  • new SEI continues to form on newly exposed Si surface, and this finally results in a very thick layer of SEI 22 on the outside of Si particle 21.
  • an anode material for a lithium-ion battery including: a carbon shell having an inner hollow space, and silicon particles included in the inner hollow space of the carbon shell.
  • liquid electrolyte only contacts the outer surface of the carbon shell and cannot substantially enter the inner hollow space.
  • lithium ions penetrate through the carbon shell and react with the inner Si particles.
  • the carbon shell is mechanically rigid, so the inner Si particles can expand in the inner hollow space. This inner expansion is possible because silicon is considerably softened upon significant lithium insertion.
  • the inner Si particles shrink back.
  • the interface with electrolyte is mechanically constrained and remains static during both lithiation and delithiation.
  • the Si particles expand and contract only in the inside of the carbon shell, and they are not in contact with SEI formation substances in the electrolyte.
  • Such a designed material provides two attractive points as an anode material: first, the static outer surface allows for the development of a stable SEI; and second, the inner hollow space allows for free volume expansion of Si particles without mechanical breaking.
  • Fig. 1 a schematic diagram of a production process for a composite anode material in one exemplary embodiment
  • Fig 2 a schematic diagram of SEI formation on the surface of a
  • Fig 3 a schematic diagram of SEI formation on the surface of the composite anode material of the exemplary embodiment
  • Fig. 4 Scanning Transmission Electron Microscopy (STEM) cross-section image of a negative electrode using the composite anode material of the exemplary embodiment as an active material;
  • Fig. 5 Scanning Electron Microscopy (SEM) image of the composite anode material of Example 1;
  • Fig. 6 STEM cross-section image of a negative electrode using the composite anode material of Example 1 as an active material
  • Fig. 7 STEM cross-section image of a negative electrode using the composite anode material of Example 2 as an active material. MODES FOR CARRYING OUT THE INVENTION
  • silicon sub-oxide (SiOx: 0 ⁇ x ⁇ 2) particle 1 having an appropriate particle size is provided as a starting material.
  • the range of x is preferably between 0.5 and 1.6, and more preferably about 1 , i.e., silicon monoxide.
  • the starting material can be prepared by oxidizing silicon or by coating pure silicon with silicon dioxide. Solid silicon monoxide particles are commercially available. Silicon dioxide particles including silicon particles can be used as a starting material.
  • the particle size of SiOx (starting material) defines the resultant size of the composite anode material.
  • SiOx particle 1 is coated with carbon layer to prepare carbon shell 2 (C coating).
  • the carbon shell can be formed by pyrolysis of hydrocarbons such as sugar or by using CVD method.
  • Temperatures in pyrolysis can be 500 to 1800°C.
  • the CVD method can be carried out by using carbon source with heating.
  • the carbon source is not restricted, examples of carbon source include hydrocarbons such as methane, ethane, ethylene, acetylene and benzene; organic solvents such as methanol, ethanol, toluene and xylene; and carbon monoxide.
  • Temperatures of CVD can be 400 to 1200°C.
  • the thickness of the carbon layer can be not greater than 100 nm, preferably not greater than 50 nm, most preferably not greater than 10 nm.
  • the carbon layer can be doped with boron (B), nitrogen (N), halogen such as fluorine (F), etc.
  • the outer size (diameter) of the carbon shell depends on the size of the starting material (SiOx particle 1) and thickness, and it can be 300 nm to 80 ⁇ , preferably 800 nm to 50 ⁇ , most preferably 1000 nm to 20 ⁇ .
  • a size of the anode material is in terms of the diameter of the carbon shell.
  • the carbon coated SiOx particle is subjected to heat treatment
  • the heat treatment can be carried out at a temperature range of 600 to 2000°C, preferably 800 to 1200°C under inert atmosphere such as N 2 , Ar or mixture thereof. Heating at the time of the carbon coating can be also as a part of this heat treatment.
  • Si particles 3 is developed by decomposing silicon monoxide to Si and Si0 2 or by crystalizing Si elements in SiOx particle 1 as well as silicon eliminated part is changed to Si0 2 4.
  • the growth of Si particles 3 can be controlled by heating conditions.
  • the size and number of Si particles are not limited if the total volume of Si particles in the state of expansion due to lithiation is less than that of the inner space of carbon shell 2. The size of Si particles decreases as the temperature increases.
  • the number of Si particles increases as the temperature increases.
  • the size of Si particles can be 1 nm to 20 ⁇ , preferably 5 nm to 10 ⁇ , most preferably 10 nm to 5 ⁇ .
  • the number of Si particles included in the inner hollow space of carbon shell can be not greater than 100, preferably not greater than 20, most preferably not greater than 5. This heat treatment can be omitted when using the silicon dioxide particle including silicon particles as the starting material.
  • Si0 2 4 is etched with etching solution such as aqueous hydrogen fluoride (HF) solution (Etching).
  • etching solution such as aqueous hydrogen fluoride (HF) solution (Etching).
  • the etching can be carried out at a temperature range of about 0 to 70°C for 0.5 to 48 hours.
  • concentration of HF solution can be about 5% to about 50% (cone. HF). It is preferable that all Si0 2 4 is removed, but a part of Si0 2 4 may be left in the carbon shell 2 if it does not affect the expansion and contract of Si particles 3.
  • (void) 5 is created in the inside of carbon shell 2 so that composite anode material 10 is completed.
  • Inner hollow space 5 is substantially a closed space from an outside of the carbon shell except that lithium ions allow passing the carbon shell.
  • Fig 3 is a schematic diagram of SEI formation on the surface of the composite anode material according to this exemplary embodiment.
  • Si particle 3 expands upon charging (lithiation) by converting to Si-Li alloy 31 in inner hollow space 5 of carbon shell 2.
  • a thin layer of SEI 32 which is lithium ion conductive forms on the surface of carbon shell 2.
  • Si-Li alloy 31 returns to Si particle 3, but SEI 32 can remain the shape as it is. In later cycles, SEI 32 can stably remain. In this way, the composite anode material of the exemplary embodiment does not consume lots of electrolyte for forming SEI.
  • Fig. 4 is Scanning Transmission Electron Microscopy (STEM) cross-section image of a negative electrode using the anode material of the exemplary embodiment as an active material. As shown in Fig. 4, the anode material of the exemplary embodiment does not break during preparing slurry and after pressing at the electrode formation. This is very surprised because it appeared that the carbon shell would be readily broken.
  • STEM Transmission Electron Microscopy
  • a lithium-ion battery including a negative electrode comprising the anode material according to the above exemplary embodiment.
  • the anode material preferably has a capacity of at least 600 mAh/g, more preferably 800 mAh/g or more.
  • the battery also comprises a positive electrode comprising an active material, an electrolyte comprising a lithium salt dissolved in at least one non-aqueous solvent and a separator configured to allow electrolyte and lithium ions to flow between a first side of the separator and an opposite second side of the separator.
  • cathode materials can be used for practicing the present exemplary embodiment.
  • the cathode materials may be at least one material selected from the group consisting of lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, lithium vanadium oxide, lithium-mixed metal oxide, lithium iron phosphate, lithium manganese phosphate, lithium vanadium phosphate, lithium mixed metal phosphates, metal sulfides, and combinations thereof.
  • the cathode material may also be at least one compound selected from chalcogenide compounds, such as titanium disulfate or molybdenum disulfate.
  • lithium cobalt oxide e.g., Li x Co0 2 where 0.8 ⁇ x ⁇ l
  • lithium nickel oxide e.g., LiNi0 2
  • lithium manganese oxide e.g., LiMn 2 0 4 and LiMn0 2
  • All these cathode materials can be prepared in the form of a fine powder, nano-wire, nano-rod, nano-fiber, or nano-tube. They can be readily mixed with an additional conductor such as acetylene black, carbon black, and ultra-fine graphite particles.
  • a binder For the preparation of the positive and negative electrodes, a binder can be used.
  • the binder include polytetrafluoroethylene (PTFE),
  • the positive and negative electrodes can be formed on a current collector such as copper foil for the negative electrode and aluminum or nickel foil for the positive electrode. However, there is no particularly significant restriction on the type of the current collector, provided that the collector can smoothly path current and have relatively high corrosion resistance.
  • the positive and negative electrodes can be stacked with interposing a separator therebetween.
  • the separator can be selected from a synthetic resin nonwoven fabric, porous polyethylene film, porous polypropylene film, or porous PTFE film.
  • a wide range of electrolytes can be used for manufacturing the battery. Most preferred are non-aqueous and polymer gel electrolytes although other types of electrolytes can be used.
  • the non-aqueous electrolyte to be employed herein may be produced by dissolving an electrolyte salt (Li salt) in a non-aqueous solvent. Any known non-aqueous solvent which has been employed as a solvent for a lithium secondary battery can be employed.
  • a mixed solvent comprising ethylene carbonate (EC) and at least one kind of non-aqueous solvent whose melting point is lower than that of ethylene carbonate and whose donor number is 18 or less
  • a second solvent may be preferably employed as the non-aqueous solvent.
  • the second solvent to be used in the mixed solvent with EC functions to make the viscosity of the mixed solvent lowering than that of which EC is used alone, thereby improving an ion conductivity of the mixed solvent.
  • the second solvent having a donor number of 18 or less (the donor number of ethylene carbonate is 16.4)
  • the aforementioned ethylene carbonate can be easily and selectively solvated with lithium ion, so that the reduction reaction of the second solvent with the carbonaceous material well developed in graphitization is assumed to be suppressed.
  • the donor number of the second solvent is controlled to not more than 18, the oxidative decomposition potential to the lithium electrode can be easily increased to 4 V or more, so that it is possible to manufacture a lithium secondary battery of high voltage.
  • Preferable second solvents are dimethyl carbonate (DMC), methyl ethyl carbonate (MEC), diethyl carbonate (DEC), ethyl propionate, methyl propionate, propylene carbonate (PC), ⁇ - butyrolactone (y-BL), acetonitrile (AN), ethyl acetate (EA), propyl formate (PF), methyl formate (MF), toluene, xylene and methyl acetate (MA).
  • DMC dimethyl carbonate
  • MEC methyl ethyl carbonate
  • DEC diethyl carbonate
  • ethyl propionate methyl propionate
  • PC propylene carbonate
  • y-BL ⁇ - butyrolactone
  • AN acetonitrile
  • EA ethyl acetate
  • PF propyl formate
  • MF methyl formate
  • MA toluene
  • This second solvent may be employed singly or in a combination of two or more. More desirably, this second solvent should be selected from those having a donor number of 16.5 or less. The viscosity of this second solvent should preferably be 28 cps or less at 25°C.
  • the mixing ratio of the aforementioned ethylene carbonate in the mixed solvent should preferably be 10 to 80% by volume. If the mixing ratio of the ethylene carbonate falls outside this range, the conductivity of the solvent may be lowered or the solvent tends to be more easily decomposed, thereby deteriorating the charge/discharge efficiency. More preferable mixing ratio of the ethylene carbonate is 20 to 75% by volume. When the mixing ratio of ethylene carbonate in a non-aqueous solvent is increased to 20% by volume or more, the solvating effect of ethylene carbonate to lithium ions will be facilitated and the solvent
  • additives may be added.
  • the SEI layer has a role to suppress reactivity with the electrolyte solution (decomposition), and subjected to desolvation reactions due to delithiation of the lithium ion battery, and to suppress the structural physical degradation of the anode material.
  • the additives include vinylene carbonate (VC), propane sultone (PS), and cyclic disulfonic acid ester.
  • the Li salt is not limited to these. One of these Li salts may be used, or two or more of these Li salts may be used in combination.
  • a casing for the battery in the exemplary embodiment may be, for example, a laminate film in which a substrate, a metal foil and a sealant are sequentially laminated.
  • a substrate which can be used include a resin film with a thickness of 10 to 25 ⁇ made of polyester (PET) or Nylon.
  • a metal foil may be an aluminum film with a thickness of 20 to 40 ⁇ .
  • a sealant may be a rein film with a thickness of 30 to 70 ⁇ made of polyethylene (PE), polypropylene (PP), modified polypropylene (PP) or an ionomer.
  • SiO particles with diameter of 5 ⁇ were used as anode material C.
  • Si particles with diameter of 5 ⁇ were used as anode material D.
  • Slurry was prepared by mixing each of anode materials A to D, carbon black, and polyimide in a ratio of 90: 1 :9 in N-methylpyrrolidone (NMP).
  • NMP N-methylpyrrolidone
  • the slurry was coated on a Cu foil and dried at 120°C for 15 min to form a thin substrate. Then, the thin substrate was pressed to 45 ⁇ thick with the loading density of 50 g/m and then heat treated at 200°C for 2h in N 2 atmosphere to prepare a negative electrode.
  • SETM cross-section images of a negative electrode using the anode material A of Example 1 and the anode material B of Example 2 are shown in Figs. 6 and 7, respectively.
  • the negative electrode was used as a working electrode, while a metal lithium foil was used as a counter electrode.
  • a separator made of porous polypropylene film was interposed between the working electrode and counter electrode.
  • the electrolyte prepared by dissolving LiPF 6 in a mixed solvent of ethyl carbonate (DEC) and ethylene carbonate (EC) in a ratio of 7:3 in a concentration of 1 M, then a laminate half-cell was fabricated.
  • test cell was evaluated in initial charge capacity, coulombic efficiency, rate capabilities of 1C charge/0.1C discharge and 6C charge/0.1C discharge and capacity retention 1C after 100 cycles. Results are shown in Table 1.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Composite Materials (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

La présente invention concerne un matériau d'anode pour batterie au lithium-ion comprenant une coque carbone qui engendre un espace creux interne, et des particules de silicium comprises dans l'espace creux interne de la coque carbone.
PCT/JP2014/073420 2014-08-29 2014-08-29 Matériau d'anode pour batterie au lithium-ion Ceased WO2016031082A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2017511955A JP2017526144A (ja) 2014-08-29 2014-08-29 リチウムイオン電池用アノード材料
PCT/JP2014/073420 WO2016031082A1 (fr) 2014-08-29 2014-08-29 Matériau d'anode pour batterie au lithium-ion

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PCT/JP2014/073420 WO2016031082A1 (fr) 2014-08-29 2014-08-29 Matériau d'anode pour batterie au lithium-ion

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CN107623116A (zh) * 2017-09-22 2018-01-23 苏州海旭新材料科技有限公司 一种锂离子电池负极复合材料及其制备方法
EP3336937A1 (fr) * 2016-12-15 2018-06-20 StoreDot Ltd. Véhicules électriques à chargement rapide adaptatif au moyen de batteries émulant des supercondensateurs
CN108258230A (zh) * 2018-02-06 2018-07-06 深圳市普锐能源科技有限公司 一种锂离子电池用中空结构硅碳负极材料及其制备方法
JP2018113254A (ja) * 2016-12-15 2018-07-19 ストアドット リミテッド スーパーキャパシタエミュレーティングバッテリを利用した、適合可能な高速充電を備えた電動車両
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CN109411729A (zh) * 2018-10-30 2019-03-01 远东福斯特新能源有限公司 锂离子电池用多孔硅/碳中空复合材料及其制备方法
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US11128152B2 (en) 2014-04-08 2021-09-21 StoreDot Ltd. Systems and methods for adaptive fast-charging for mobile devices and devices having sporadic power-source connection
US10293704B2 (en) 2014-04-08 2019-05-21 StoreDot Ltd. Electric vehicles with adaptive fast-charging, utilizing supercapacitor-emulating batteries
US11560062B2 (en) 2014-04-08 2023-01-24 StoreDot Ltd. Software management of EV battery modules
US10199646B2 (en) 2014-07-30 2019-02-05 StoreDot Ltd. Anodes for lithium-ion devices
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