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WO2019183368A1 - Batterie à électrolyte solide - Google Patents

Batterie à électrolyte solide Download PDF

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Publication number
WO2019183368A1
WO2019183368A1 PCT/US2019/023390 US2019023390W WO2019183368A1 WO 2019183368 A1 WO2019183368 A1 WO 2019183368A1 US 2019023390 W US2019023390 W US 2019023390W WO 2019183368 A1 WO2019183368 A1 WO 2019183368A1
Authority
WO
WIPO (PCT)
Prior art keywords
solid
state battery
lithium
group
anode
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/US2019/023390
Other languages
English (en)
Inventor
Marina Yakovleva
Kenneth Brian Fitch
Jian XIA
JR. William Arthur Greeter
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.)
Livent USA Corp
Original Assignee
FMC Lithium USA 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
Priority claimed from US16/359,707 external-priority patent/US11735764B2/en
Application filed by FMC Lithium USA Corp filed Critical FMC Lithium USA Corp
Priority to SG11202008910UA priority Critical patent/SG11202008910UA/en
Priority to EP19715691.2A priority patent/EP3769359A1/fr
Priority to CN201980030085.9A priority patent/CN112074976B/zh
Priority to JP2021500498A priority patent/JP7239672B2/ja
Priority to KR1020207027022A priority patent/KR102793242B1/ko
Priority to CN202411005068.9A priority patent/CN118970043A/zh
Publication of WO2019183368A1 publication Critical patent/WO2019183368A1/fr
Anticipated expiration legal-status Critical
Priority to JP2023031228A priority patent/JP7742855B2/ja
Ceased legal-status Critical Current

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Definitions

  • the present invention relates to a solid-state battery which includes a printable lithium composition.
  • Lithium and lithium-ion secondary or rechargeable batteries have found use in certain applications such as in cellular phones, camcorders, and laptop computers, and even more recently, in larger power application such as in electric vehicles and hybrid electric vehicles. It is preferred in these applications that the secondary batteries have the highest specific capacity possible but still provide safe operating conditions and good cyclability so that the high specific capacity is maintained in subsequent recharging and discharging cycles.
  • each construction includes a positive electrode (or cathode), a negative electrode (or anode), a separator that separates the cathode and anode, an electrolyte in electrochemical communication with the cathode and anode.
  • a positive electrode or cathode
  • a negative electrode or anode
  • a separator that separates the cathode and anode
  • an electrolyte in electrochemical communication with the cathode and anode.
  • lithium ions are transferred from the anode to the cathode through the electrolyte when the secondary battery is being discharged, i.e. , used for its specific application.
  • electrons are collected from the anode and pass to the cathode through an external circuit.
  • the lithium ions are transferred from the cathode to the anode through the electrolyte.
  • New lithium-ion cells or batteries are initially in a discharged state.
  • lithium moves from the cathode material to the anode active material.
  • the lithium moving from the cathode to the anode reacts with an electrolyte material at the surface of the graphite anode, causing the formation of a passivation film on the anode.
  • the passivation film formed on the graphite anode is a solid electrolyte interface (SEI).
  • SEI solid electrolyte interface
  • the lithium consumed by the formation of the SEI is not returned to the cathode. This results in a lithium-ion cell having a smaller capacity compared to the initial charge capacity because some of the lithium has been consumed by the formation of the SEI.
  • the present invention provides a solid-state battery with one or more components prelithiated, or lithiated with a printable lithium composition.
  • a solid-state battery comprising the printable lithium composition will have increased energy density and improved safety and manufacturability.
  • a solid-state battery 10 comprising an anode 12, a cathode 14 and a solid electrolyte 16 is provided in accordance with one embodiment of the present invention.
  • the solid-state battery may further include an anode current collector 20 and a cathode current collector 22.
  • a printable lithium composition is applied or deposited to a current collector, electrode and/or solid electrolyte of the solid-state battery.
  • the printable lithium composition may be used to form a monolithic lithium metal anode of various
  • the printable lithium composition may be used to prelithiate a solid electrolyte as described in US Patent No. 7,914,930 herein incorporated by reference in its entirety.
  • a solid-state secondary battery may include a positive electrode capable of electrochemically absorbing and desorbing lithium; a negative electrode capable of electrochemically absorbing and desorbing lithium, the negative electrode including an active material layer that comprises an active material, the active material layer being carried on a current collector; and a non-aqueous electrolyte.
  • a method includes the steps of: reacting lithium with the active material of the negative electrode by bringing the printable lithium composition into contact with a surface of the active material layer of the negative electrode; and thereafter combining the negative electrode with the positive electrode to form an electrode assembly.
  • the polymer binder is selected so as to be compatible with the lithium metal powder. “Compatible with” or“compatibility” is intended to convey that the polymer binder does not violently react with the lithium metal powder resulting in a safety hazard.
  • the lithium metal powder and the polymer binder may react to form a lithium-polymer complex, however, such complex should be stable at various temperatures. It is recognized that the amount
  • the polymer binder may have a molecular weight of about 1 ,000 to about 8,000,000, and often has a molecular weight of 2,000,000 to 5,000,000.
  • Suitable polymer binders may include one or more of poly(ethylene oxide), polystyrene, polyisobutylene, natural rubbers, butadiene rubbers, styrene-butadiene rubber, polyisoprene rubbers, butyl rubbers, hydrogenated nitrile butadiene rubbers, epichlorohydrin rubbers, acrylate rubbers, silicon rubbers, nitrile rubbers, polyacrylic acid, polyvinylidene chloride, polyvinyl acetate, ethylene propylene diene termonomer, ethylene vinyl acetate copolymer, ethylene-propylene copolymers, ethylene-propylene terpolymers, polybutenes,.
  • the binder may also be a wax
  • the rheology modifier is selected to be compatible with the lithium metal powder and the polymer binder.
  • the rheology modifier provides rheology properties such as viscosity.
  • the rheology modifier may also provide conductivity, improved capacity and/or improved
  • the rheology modifier may be the combination of two or more compounds so as to provide different properties or to provide additive properties.
  • Exemplary rheology modifiers may include one or more of carbon black, carbon nanotubes, graphene, silicon nanotubes, graphite, hard carbon and mixtures, fumed silica, titanium dioxide, zirconium dioxide and other Group IIA, IIIA, IVB, VB and VIA elements/compounds and mixtures or blends thereof.
  • Solvents compatible with lithium may include acyclic hydrocarbons, cyclic hydrocarbons, aromatic hydrocarbons, symmetrical ethers, unsymmetrical ethers, cyclic ethers, alkanes, sulfones, mineral oil, and mixtures, blends or cosolvents thereof.
  • suitable acyclic and cyclic hydrocarbons include n-hexane, n-heptane, cyclohexane, and the like.
  • suitable aromatic hydrocarbons include toluene, ethylbenzene, xylene, isopropylbenzene (cumene), and the like.
  • Suitable symmetrical, unsymmetrical and cyclic ethers include di-n-butyl ether, methyl t-butyl ether, tetrahydrofuran, glymes and the like.
  • Commercially available isoparaffinic synthetic hydrocarbon solvents with tailored boiling point ranges such as Shell Sol® (Shell Chemicals) or Isopar® (Exxon) are also suitable.
  • a mixture of the polymer binder, rheology modifier, coating reagents, and other potential additives for the lithium metal powder may be formed and introduced to contact the lithium droplets during the dispersion at a temperature above the lithium melting point, or at a lower temperature after the lithium dispersion has cooled such as described in U.S. Patent No. 7,588,623 the disclosure of which is incorporated by reference in its entirety.
  • the thusly modified lithium metal may be introduced in a crystalline form or in a solution form in a solvent of choice. It is understood that combinations of different process parameters could be used to achieve specific coating and lithium powder characteristics for particular applications.
  • the printable lithium composition in accordance with the present invention can accommodate higher binder ratios, including up to 20 percent on dry basis.
  • Various properties of the printable lithium composition such as viscosity and flow, may be modified by increasing the binder and modifier content up to 50% dry basis without loss of electrochemical activity of lithium.
  • Increasing the binder content facilitates the loading of the printable lithium composition and the flow during printing.
  • the printable lithium composition comprises about 70% lithium metal powder and about 30% polymer binder and rheology modifiers.
  • the printable lithium composition may comprise about 85% lithium metal powder and about 15% polymer binder and rheology modifiers.
  • An important aspect of printable lithium compositions is the rheological stability of the suspension. Because lithium metal has a low density of 0.534 g/cc, it is difficult to prevent lithium powder from separating from solvent suspensions.
  • viscosity and rheology may be tailored to create the stable suspension of the invention.
  • a preferred embodiment shows no separation at greater than 90 days. This can be achieved by designing compositions with very high zero shear viscosity in the range of 1 x 10 4 cps to 1 x 10 7 cps. It is however very important to the application process that the compositions, when exposed to shear, exhibit viscosity characteristics in the ranges claimed.
  • the resulting printable lithium composition preferably may have a viscosity at 10s -1 about 20 to about 20,000 cps, and often a viscosity of about 100 to about 10,000 cps. At such viscosity, the printable lithium composition is a flowable suspension or gel.
  • the printable lithium composition preferably has an extended shelf life at room temperature and is stable against metallic lithium loss at temperatures up to 60°C, often up to 120°C, and sometimes up to 180°C.
  • the printable lithium composition may separate somewhat over time but can be placed back into suspension by mild agitation and/or application of heat.
  • the printable lithium composition comprises on a solution basis about 5 to 50 percent lithium metal powder, about 0.1 to 20 percent polymer binder, about 0.1 to 30 percent rheology modifier and about 50 to 95 percent solvent. In one embodiment, the printable lithium composition comprises on a solution basis about 15 to 25 percent lithium metal powder, about 0.3 to 0.6 percent polymer binder having a molecular weight of 4,700,000, about 0.5 to 0.9 percent rheology modifier, and about 75 to 85 percent solvent. Typically, the printable lithium composition is applied or deposited to a thickness of about 50 microns to 200 microns prior to pressing. After pressing, the thickness can be reduced to between about 1 to 50 microns. Examples of pressing techniques are described, for example, in US Patent Nos. 3,721 ,113 and 6,232,014 which are incorporated herein by reference in their entireties.
  • the printable lithium composition is deposited or applied to an active anode material on a current collector namely to form a prelithiated anode.
  • active anode materials include graphite and other carbon-based materials, alloys such as tin/cobalt, tin/cobalt/carbon, silicon-carbon, variety of silicone/tin based composite compounds, germanium-based composites, titanium based composites, elemental silicon, and germanium.
  • the anode materials may be a foil, mesh or foam. Application may be via spraying, extruding, coating, printing, painting, dipping, and spraying, and are described in co-pending US Patent
  • the active anode material and the printable lithium composition are provided together and extruded onto the current collector (e.g., copper, nickel, etc.).
  • the active anode material and printable lithium composition may be mixed and co extruded together.
  • active anode materials include graphite, graphite-SiO, graphite- SnO, SiO, hard carbon and other lithium ion battery and lithium ion capacitor anode materials.
  • the active anode material and the printable lithium composition are co extruded to form a layer of the printable lithium composition on the current collector.
  • the deposition of the printable lithium composition including the above extrusion technique may include depositing as wide variety patterns (e.g., dots, stripes), thicknesses, widths, etc.
  • the printable lithium composition and active anode material may be deposited as a series of stripes, such as described in US Publication No. 2014/0186519 incorporated herein by reference in its entirety.
  • the stripes would form a 3D structure that would account for expansion of the active anode material during lithiation.
  • silicon may expand by 300 to 400 percent during lithiation. Such swelling potentially adversely affects the anode and its performance.
  • the silicon anode material can expand in the X-plane alleviating electrochemical grinding and loss of particle electrical contact.
  • the printing method can provide a buffer for expansion.
  • the printable lithium formulation is used to form the anode, it could be co-extruded in a layered fashion along with the cathode and separator, resulting in a solid-state battery.
  • the printable lithium composition may be used to pre-lithiate an anode as described in US Patent No. 9,837,659 herein incorporated by reference in its entirety.
  • the method includes disposing a layer of printable lithium composition adjacent to a surface of a pre-fabricated/pre-formed anode.
  • the pre-fabricated electrode comprises an electroactive material.
  • the printable lithium composition may be applied to the carrier/substrate via a deposition process.
  • a carrier substrate on which the layer of printable lithium composition may be disposed may be selected from the group consisting of: polymer films (e.g., polystyrene, polyethylene, polyethyleneoxide, polyester, polypropylene,
  • thermodynamics by way of non limiting example.
  • Heat may then be applied to the printable lithium composition layer on the substrate or the pre-fabricated anode.
  • the printable lithium composition layer on the substrate or the pre-fabricated anode may be further compressed together, under applied pressure.
  • the heating, and optional applied pressure facilitates transfer of lithium onto the surface of the substrate or anode.
  • pressure and heat can result in mechanical lithiation, especially where the pre-fabricated anode comprises graphite. In this manner, lithium transfers to the electrode and due to favorable thermodynamics is incorporated into the active material.
  • the printable lithium composition can be supplied to the anode active material prior to assembly of the battery.
  • the anode can comprise partially lithium-loaded silicon-based active material, in which the partially loaded active material has a selected degree of loading of lithium through intercalation/alloying or the like.
  • the printable lithium composition may be incorporated into a three- dimensional electrode structure as described in US Publication No. 2018/0013126 herein incorporated by reference in its entirety.
  • the printable lithium composition may be incorporated into a three-dimensional porous anode, porous current collector or porous polymer or ceramic film, wherein the printable lithium composition may be deposited therein.
  • an electrode prelithiated with the printable lithium composition can be assembled into a cell with the electrode to be preloaded with lithium.
  • a separator can be placed between the respective electrodes.
  • Current can be allowed to flow between the electrodes.
  • an anode prelithiated with the printable lithium composition of the present invention may be formed into a second battery such as described in U.S. Patent No. 6,706,447 herein incorporated by reference in its entirety.
  • the cathode is formed of an active material, which is typically combined with a carbonaceous material and a binder polymer.
  • the active material used in the cathode is preferably a material that can be lithiated.
  • non-lithiated materials such as Mn0 2 , V 2 O 5, M0S 2 , metal fluorides or mixtures thereof, Sulphur and sulfur composites can be used as the active material.
  • lithiated materials such as uMh 2 0 4 and L1MO 2 wherein M is Ni,
  • Co or Mn that can be further lithiated can also be used.
  • the non-lithiated active materials are preferred because they generally have higher specific capacities, lower cost and broader choice of cathode materials in this construction that can provide increased energy and power over conventional secondary batteries that include lithiated active materials.
  • S-SBR Europrene Sol R 72613 10g of solution styrene butadiene rubber (S-SBR Europrene Sol R 72613) is dissolved in 90g toluene (99% anhydrous, Sigma Aldrich) by stirring at 21 °C for 12 hours. 6g of the 10wt% SBR (polymer binder) in toluene (solvent) is combined with 0.1g carbon black (Timcal Super P) (rheology modifier) and 16g of toluene and dispersed in a Thinky ARE 250 planetary mixer for 6 minutes at 2000 rpm.
  • S-SBR Europrene Sol R 72613 10g of solution styrene butadiene rubber (S-SBR Europrene Sol R 72613) is dissolved in 90g toluene (99% anhydrous, Sigma Aldrich) by stirring at 21 °C for 12 hours. 6g of the 10wt% SBR (polymer binder) in tolu
  • mAh loading of lithium can be controlled very consistently. For example, for a print of 0.275 lithium metal, the CV is about 5%.
  • the pre-lithiation effect of printable lithium composition can be evaluated by printing the required amount of printable lithium onto the surface of prefabricated electrodes.
  • the pre- lithiation lithium amount is determined by testing the anode material in half-cell format and calculating the lithium required to compensate for the first cycle losses due to formation of SEI, or other side reactions.
  • the capacity as lithium metal of the composition must be known and is approximately 3600mAh/g dry lithium basis for the compositions used as examples.
  • the pre-lithiation effect is tested using Graphite-SiO/NCA pouch cells.
  • the Graphite- SiO anode sheet has the following formulation: artificial graphite (90.06%) + SiO (4.74%) + carbon black (1.4%) + SBR/CMC (3.8%).
  • the capacity loading of the electrode is 3.59 mAh/cm 2 with 87% first cycle CE (columbic efficiency).
  • the printable lithium is applied onto a Graphite-SiO anode at 0.15 mg/cm 2 lithium metal.
  • the electrode is dried at 80°C for 100 min followed by lamination at a roller gap approximately 75% of the thickness of the electrode. A 7 cm x 7 cm electrode is punched from the printable lithium treated anode sheet.
  • the positive electrode has the following formulation: NCA (96%) + carbon black (2%) + PVdF (2%).
  • the positive electrode is 6.8 cm x 6.8 cm with capacity loading of 3.37 mAh/cm 2 .
  • the NCA cathode has 90% first cycle CE.
  • the anode to cathode capacity ratio is 1.06 and the baseline for full cell first cycle CE is 77%.
  • Single layer pouch cells are assembled and 1M LiPFe /EC+DEC (1 :1) is used as the electrolyte.
  • the cells are pre-conditioned for 12 hours at 21°C and then the formation cycle is conducted at 40°C.
  • the formation protocol is 0.1 C charge to 4.2V, constant voltage to 0.01 C and 0.1C discharge to 2.8V. In the described test 89% first cycle CE was demonstrated.

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Abstract

La présente invention concerne une batterie à électrolyte solide comprenant une cathode, une anode et un électrolyte solide. Dans un mode de réalisation, la cathode, l'anode et/ou l'électrolyte solide sont formés à partir d'une composition de lithium imprimable comprenant une poudre de lithium métallique, un liant polymère compatible avec la poudre de lithium métallique, un modificateur de rhéologie compatible avec la poudre de lithium métallique, et un solvant compatible avec la poudre de lithium métallique et avec le liant polymère. Dans un autre mode de réalisation, du lithium est déposé sur l'électrolyte solide avec une composition de lithium imprimable comprenant une poudre de lithium métallique, un liant polymère compatible avec la poudre de lithium métallique, un modificateur de rhéologie compatible avec la poudre de lithium métallique, et un solvant compatible avec la poudre de lithium métallique et avec le liant polymère.
PCT/US2019/023390 2018-03-22 2019-03-21 Batterie à électrolyte solide Ceased WO2019183368A1 (fr)

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SG11202008910UA SG11202008910UA (en) 2018-03-22 2019-03-21 Solid-state battery
EP19715691.2A EP3769359A1 (fr) 2018-03-22 2019-03-21 Batterie à électrolyte solide
CN201980030085.9A CN112074976B (zh) 2018-03-22 2019-03-21 固态电池
JP2021500498A JP7239672B2 (ja) 2018-03-22 2019-03-21 固体電池
KR1020207027022A KR102793242B1 (ko) 2018-03-22 2019-03-21 전고체 배터리
CN202411005068.9A CN118970043A (zh) 2018-03-22 2019-03-21 固态电池
JP2023031228A JP7742855B2 (ja) 2018-03-22 2023-03-01 固体電池

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US201862646521P 2018-03-22 2018-03-22
US62/646,521 2018-03-22
US201862691819P 2018-06-29 2018-06-29
US62/691,819 2018-06-29
US16/359,707 US11735764B2 (en) 2018-03-22 2019-03-20 Printable lithium compositions
US16/359,707 2019-03-20
US16/359,725 US20190214631A1 (en) 2018-03-22 2019-03-20 Methods of applying printable lithium compositions for forming battery electrodes
US16/359,733 US20190221886A1 (en) 2018-03-22 2019-03-20 Solid-state battery
US16/359,725 2019-03-20
US16/359,733 2019-03-20

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PCT/US2019/023383 Ceased WO2019183363A1 (fr) 2018-03-22 2019-03-21 Procédés d'application de compositions de lithium imprimables pour former des électrodes de batterie

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US20220328799A1 (en) * 2021-04-08 2022-10-13 Livent USA Corp. Dry process for forming an electrode
WO2022216460A1 (fr) * 2021-04-08 2022-10-13 Fmc Lithium Usa Corp. Procédé par voie sèche pour former une électrode
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